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Al2O3 Particle Erosion Induced Phase Transformation: Structure, Mechanical Property, and Impact Toughness of an SLM Al-10Si-Mg Alloy - MDPI
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Article
Al2O3 Particle Erosion Induced Phase Transformation:
Structure, Mechanical Property, and Impact Toughness of an
SLM Al-10Si-Mg Alloy
Bo-Chin Huang and Fei-Yi Hung *

                                          Department of Materials Science and Engineering, National Cheng Kung University, Tainan 701, Taiwan;
                                          frt4y6asd@gmail.com
                                          * Correspondence: fyhung@mail.ncku.edu.tw

                                          Abstract: This study investigated the microstructure, mechanical properties, impact toughness,
                                          and erosion characteristics of Al-10Si-Mg alloy specimens manufactured using the selective laser
                                          melting (SLM) method with or without subsequent T6 heat treatment. Furthermore, the erosion
                                          phase transformation behavior of the test specimens was analyzed, and the effect of the degradation
                                          mechanism on the tensile mechanical properties and impact toughness of the SLM Al-10Si-Mg alloy
                                          specimens before and after particle erosion was compared. The experimental results indicated that
                                          the Al-10Si-Mg alloy subjected to T6 heat treatment has better erosion resistance than the as-fabricated
                                          material. The tensile strength and fracture toughness of both specimen groups decreased due to the
                                          formation of microcracks on the surface caused by particle erosion. Nevertheless, the erosion-induced
                                          silicon nanoparticle solid solution softens the Al matrix and improves the elongation of the SLM
         
                                   Al-10Si-Mg alloy.
Citation: Huang, B.-C.; Hung, F.-Y.
Al2 O3 Particle Erosion Induced Phase
                                          Keywords: Al-Si-Mg alloy; selective laser melting (SLM); mechanical properties; impact toughness;
Transformation: Structure,                erosion wear
Mechanical Property, and Impact
Toughness of an SLM Al-10Si-Mg
Alloy. Nanomaterials 2021, 11, 2131.
https://doi.org/10.3390/                  1. Introduction
nano11082131                                    Selective laser melting (SLM) is a type of powder bed fusion technology in which
                                          three-dimensional (3D) objects are gradually built layer by layer. This makes the technology
Academic Editor: Jordi Sort               suitable for manufacturing parts with complex geometric shapes. This emerging manufac-
                                          turing technology has been applied to different metallic materials such as cobalt-chromium
Received: 2 July 2021                     alloys [1], stainless steel [2,3], aluminum-based alloys [4,5], magnesium alloys [6,7], and
Accepted: 19 August 2021
                                          titanium alloys [8,9].
Published: 21 August 2021
                                                Among Al alloys, Al-10Si-Mg alloy is one of the first to be subjected to SLM. The
                                          silicon content of Al-10Si-Mg alloy is close to the eutectic point of aluminum–silicon binary
Publisher’s Note: MDPI stays neutral
                                          alloys, and the material has a small solidification range during melting, which makes it
with regard to jurisdictional claims in
                                          suitable to be manufactured using SLM [10,11]. Moreover, Al-10Si-Mg alloy has good
published maps and institutional affil-
                                          fluidity because its aluminum and silicon composition is close to the eutectic composition,
iations.
                                          which makes it one of the most suitable candidates for the SLM process. Research on Al-
                                          10Si-Mg alloy has focused on the specific microstructure and mechanical strength caused by
                                          the rapid cooling in the SLM process [10–15]. One study pointed out that specimens with
                                          different construction directions used in fatigue tests were fabricated using SLM [16] and
Copyright: © 2021 by the authors.         investigated the high cycle fatigue life of specimens with different construction directions
Licensee MDPI, Basel, Switzerland.
                                          and subjected to different heat treatment conditions [14]. The results indicated that the
This article is an open access article
                                          microstructure evolution characteristics and mechanical properties of SLM Al-10Si-Mg
distributed under the terms and
                                          alloy were highly valuable. Notably, particle erosion is an important mechanism that causes
conditions of the Creative Commons
                                          material damage in many engineering applications. However, few comprehensive reports
Attribution (CC BY) license (https://
                                          have discussed the wear resistance of Al-10Si-Mg alloy specimens [17–19]. Previously, we
creativecommons.org/licenses/by/
4.0/).
                                          used SiO2 particles to conduct erosion experiments for evaluating the wear resistance of

Nanomaterials 2021, 11, 2131. https://doi.org/10.3390/nano11082131                                   https://www.mdpi.com/journal/nanomaterials
Al2O3 Particle Erosion Induced Phase Transformation: Structure, Mechanical Property, and Impact Toughness of an SLM Al-10Si-Mg Alloy - MDPI
Nanomaterials 2021, 11, 2131                                                                                                                    2 of 17

                                      Al-10Si-Mg
                       Nanomaterials 2021,             alloy
                                           11, x FOR PEER    and
                                                            commercial 4384 Al alloy and confirmed that Al-10Si-Mg alloy has 2 of 17
                                                          REVIEW
                                    excellent wear resistance [17].
                                         In this study, Al2 O3 ceramic particles were used instead of SiO2 particles in erosion
                                    experiments to create
                                                    reportsahave
                                                             considerably
                                                                  discussed harsher
                                                                             the wearwear     environment
                                                                                        resistance           for examining
                                                                                                   of Al-10Si-Mg             the erosion-
                                                                                                                  alloy specimens  [17–19]. Previ-
                                    induced phase ously,   we used SiO
                                                     transformation     2 particles
                                                                       and          to conduct
                                                                             material   failure erosion  experiments
                                                                                                 mechanism            for evaluating
                                                                                                               of Al-10Si-Mg   alloy.the
                                                                                                                                       Bywear re-
                                                    sistance of
                                    using the SLM process       Al-10Si-Mgfrom
                                                             parameters     alloy and
                                                                                  [17],commercial   4384 Aland
                                                                                         tensile, erosion,  alloyimpact
                                                                                                                  and confirmed  that Al-10Si-Mg
                                                                                                                         test specimens
                                    were fabricatedalloy
                                                      fromhas excellent wear
                                                            Al-10Si-Mg        resistance
                                                                          alloy  powder[17].by means of SLM to compare the effects
                                                         In this study, Al 2O3 ceramic particles were used instead of SiO2 particles in erosion
                                    of heat treatment and erosion phase transformation behavior on the mechanical strength
                                                    experiments to create a considerably harsher wear environment for examining the ero-
                                    and impact toughness of the material. The establishment of related wear degradation
                                                    sion-induced phase transformation and material failure mechanism of Al-10Si-Mg alloy.
                                    mechanisms is important for academic research and to provide references for SLM Al-Si-
                                                    By using the SLM process parameters from [17], tensile, erosion, and impact test speci-
                                    Mg alloy applications.
                                                    mens were fabricated from Al-10Si-Mg alloy powder by means of SLM to compare the
                                                           effects of heat treatment and erosion phase transformation behavior on the mechanical
                                     2. Materials and Methods
                                                    strength and impact toughness of the material. The establishment of related wear degra-
                                          In this study, wemechanisms
                                                     dation   used Al-10Si-Mg        alloyfor
                                                                              is important   specimens
                                                                                               academic manufactured        by the references
                                                                                                          research and to provide   Industrialfor SLM
                                    Technology Research
                                                     Al-Si-MgInstitute   (ITRI; ITRI self-developed AM250, Hsinchu, Taiwan). More-
                                                                 alloy applications.
                                    over, the Al-10Si-Mg alloy powder (according to ASTM F3318, Taiwan Circle Metal Powder
                                                     2. Materials
                                    Co., Ltd., Tainan,   Taiwan) and used Methods
                                                                             to fabricate these specimens was produced by ITRI. Its
                                    chemical composition  In this   study, we used
                                                               is summarized          Al-10Si-Mg
                                                                                   in Table   1. Thealloy specimens
                                                                                                      powder    has amanufactured     by the Industrial
                                                                                                                       spherical appearance
                                    and an average Technology
                                                     particle sizeResearch
                                                                      of 35 µm.Institute    (ITRI; ITRI self-developed
                                                                                   A continuous-wave                      AM250, Hsinchu,
                                                                                                           laser with a wavelength     of 1064 Taiwan).
                                    nm and a spot size of 100 µm was employed as the energy source. The laser power was Metal
                                                     Moreover,     the  Al-10Si-Mg   alloy  powder  (according   to ASTM   F3318, Taiwan   Circle
                                    300 W, scanningPowder
                                                       speed 700Co., mm/s,
                                                                      Ltd., Tainan,
                                                                                hatchTaiwan)
                                                                                      space 35used
                                                                                                 µm,toand
                                                                                                        fabricate
                                                                                                            powder these specimens
                                                                                                                      layer          was30produced
                                                                                                                             thickness      µm.       by
                                                     ITRI. Its chemical composition is summarized in Table 1. The powder has a spherical ap-
                                    The process parameters are summarized in Table 2. The relationship between the printed
                                                     pearance and an average particle size of 35 μm. A continuous-wave laser with a wave-
                                    arrangement and construction direction of the SLM Al-10Si-Mg specimens on the substrate
                                                     length of 1064 nm and a spot size of 100 μm was employed as the energy source. The laser
                                    and the specifications
                                                     power wasof the300specimens
                                                                        W, scanning are  illustrated
                                                                                       speed          in Figures
                                                                                              700 mm/s,            1 and
                                                                                                          hatch space     2, respectively,
                                                                                                                      35 μm,   and powder and
                                                                                                                                            layer thick-
                                    the finished product    is  depicted    in  Figure  3.
                                                     ness 30 μm. The process parameters are summarized in Table 2. The relationship between
                                                    the printed arrangement and construction direction of the SLM Al-10Si-Mg specimens on
                                    Table 1. Chemicalthe
                                                       composition of Al-10Si-Mg
                                                         substrate and            alloy. (wt.%).
                                                                       the specifications  of the specimens are illustrated in Figures 1 and 2,
                                                    respectively, and the finished product is depicted in Figure 3.
                                                      Si        Fe     Cu     Mn      Mg      Ni      Zn       Pb          Sn            Ti      Al
                                      Composition 10.00 Table
                                                          0.551. Chemical
                                                                  0.05    0.45    0.65of Al-10Si-Mg
                                                                          composition     0.05    0.10      0.05
                                                                                                    alloy. (wt.%).         0.05      0.15       Bal.

                                           Si       Fe     Cu      Mn          Mg        Ni             Zn           Pb            Sn          Ti         Al
                                  Table 2.
                         Composition       Process 0.55
                                        10.00      parameters employed
                                                           0.05    0.45 in this0.65
                                                                                 study. 0.05            0.10        0.05          0.05        0.15        Bal.
                                                                                                                             Layer
                                         Laser Power Table 2. ProcessSpeed
                                                         Scanning     parameters employed in this study.
                                                                                  Beam Size           Hatch Space
                                                                                                                           Thickness
                                            300 W            Laser700
                                                                   Power
                                                                      mm/s Scanning Speed
                                                                                    35 µm          Beam Size
                                                                                                           100 µm Hatch Space30 µm
                                                                                                                                Layer Thickness
                                                                300 W         700 mm/s               35 μm          100 μm           30 μm

                                    Figure 1. The relationship between the printed arrangement and construction direction of the
                                    Al-10Si-Mg specimens on the substrate.
Al2O3 Particle Erosion Induced Phase Transformation: Structure, Mechanical Property, and Impact Toughness of an SLM Al-10Si-Mg Alloy - MDPI
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   Nanomaterials 2021, 11, x FOR PEER REVIEW                                                                                          3 of 17

      Figure 1. The relationship between the printed arrangement and construction direction of the Al-10Si-Mg specimens on
Nanomaterials 2021, 11, 2131                                                                                              3 of 17
      the substrate.
         Figure 1. The relationship between the printed arrangement and construction direction of the Al-10Si-Mg specimens on
         the substrate.

                                                Thedetailed
                                    Figure2.2.The
                                    Figure           detailedspecifications
                                                              specifications of of
                                                                                 thethe specimens
                                                                                     specimens     used
                                                                                                used     in this
                                                                                                     in this     study:
                                                                                                             study:      (a)tensile
                                                                                                                    (a) the  the tensile  test specimens;
                                                                                                                                    test speci-
                                    Figure 2. The detailed specifications of the specimens used in this study: (a) the tensile test speci-
                                    (b) the(b)
                                    mens;   erosion   test specimens;
                                               the erosion               (c) (c)
                                                           test specimens;   thetheimpact  toughness
                                                                                      impact toughnessspecimens.
                                                                                                       specimens.
                                    mens; (b) the erosion test specimens; (c) the impact toughness specimens.

                                        Figure 3. The finished as-fabricated Al-10Si-Mg specimens.

                                         In this study, the specimens were subjected to T6 heat treatment, which involves two
                                    stages  of solution
                                        Figure            treatment
                                                 3. The finished     at 510 °C forAl-10Si-Mg
                                                                   as-fabricated     2 h, followed   by artificial aging treatment at 170
                                                                                                 specimens.
                                        Figure 3. The finished as-fabricated Al-10Si-Mg specimens.
                                    °C for 6 h. The as-fabricated Al-10Si-Mg specimens were categorized as group F, and the
                                    specimens
                                          In
                                          In thissubjected
                                              this  study,   to T6
                                                             the
                                                    study, the     heat treatment
                                                                 specimens
                                                                 specimens      werewere
                                                                                were       categorized
                                                                                       subjected
                                                                                       subjected       T6asheat
                                                                                                    to T6
                                                                                                   to       group
                                                                                                           heat     FH. The naming
                                                                                                                 treatment,
                                                                                                                 treatment,    whichprin-
                                                                                                                               which   involves two
                                                                                                                                       involves  two
                                    ciples
                                    stages are  summarized      in Tableat3. 510
                                                                             To examine     the microstructure    of the as-fabricated  Al-
                                    stages of solution treatment at 510 C for 2 h, followed by artificial aging treatment170
                                             of solution    treatment            °C◦  for  2 h, followed    by  artificial  aging  treatment  at   at
                                    10Si-Mg    specimens
                                         ◦ C 6for           with different   construction    directions,were
                                                                                                         the plane   perpendicular   to the
                                    170for
                                    °C         h. 6The   as-fabricated
                                                     h. The               Al-10Si-Mg
                                                              as-fabricated    Al-10Si-Mg specimens
                                                                                               specimens were   categorized
                                                                                                                    categorizedas group   F, and
                                                                                                                                    as group      the
                                                                                                                                              F, and
                                    construction direction was defined as the z surface, and the planes parallel to the construc-
                                    specimens
                                    the specimens  subjected    to T6 heat
                                                        subjected            treatment    werewere
                                                                                                 categorized     as group FH. The      naming prin-
                                    tion direction were     defined to
                                                                     as T6
                                                                        the heat  treatment
                                                                             x surface  and y surface, categorized
                                                                                                         as illustratedasingroup
                                                                                                                            FigureFH.
                                                                                                                                   4. The naming
                                    ciples are summarized
                                    principles are summarizedin Table  3. To3.examine
                                                                 in Table               the the
                                                                                To examine   microstructure
                                                                                                microstructureof the  as-fabricated
                                                                                                                   of the             Al-
                                                                                                                          as-fabricated
                                    10Si-Mg specimens
                                    Al-10Si-Mg   specimenswith different
                                                             with         construction
                                                                   different             directions,
                                                                              construction           the the
                                                                                             directions,  plane  perpendicular
                                                                                                              plane   perpendicularto the
                                                                                                                                       to
                                    construction  direction
                                    the construction        was defined
                                                       direction           as the as
                                                                 was defined      z surface, and theand
                                                                                     the z surface,  planestheparallel
                                                                                                               planes to  the construc-
                                                                                                                        parallel  to the
                                    tion directiondirection
                                    construction   were defined   as the xas
                                                            were defined    surface  and y surface,
                                                                               the x surface         as illustrated
                                                                                             and y surface,          in Figure
                                                                                                             as illustrated     4.
                                                                                                                            in Figure   4.
Al2O3 Particle Erosion Induced Phase Transformation: Structure, Mechanical Property, and Impact Toughness of an SLM Al-10Si-Mg Alloy - MDPI
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                       Table 3. The naming principles and post-processing conditions.
                                            Table 3. The naming principles and post-processing conditions.
                           Group                                Post-Processing Conditions
                                                              Group                          Post-Processing Conditions
                              F                                        Raw material
                             FE                              F material after T6 heat treatment
                                                            Raw                                      Raw material
                                                            FE                           Raw material after T6 heat treatment
                             FH                             FH
                                                                Raw material + Erosion wear Raw material + Erosion wear
                            FHE                       Raw material
                                                           FHE after T6 heat treatment   + Erosion
                                                                                  Raw material after wear
                                                                                                     T6 heat treatment + Erosion wear

                                               Figure 4. The naming principles of the relationship between different observation planes and the
                       Figure 4. The naming principles of the relationship between different observation planes and the
                                               construction direction.
                       construction direction.
                                                  The F and FH specimens were cold embedded and ground in order using #80~#4000
                            The F and FH specimens       were cold embedded and ground in order using #80~#4000
                                            SiC sandpaper, followed by polishing using a 0.04 µm SiO2 polishing solution. The
                       SiC sandpaper, followed
                                            specimens of each using
                                                  by  polishing       groupawere0.04 immersed
                                                                                      μm SiO2 polishing
                                                                                                    in Keller’s  solution.
                                                                                                                    etchingThe      speci-(19 mL HNO + 9 mL
                                                                                                                              solution                    3
                       mens of each group were    immersed       in   Keller’s   etching    solution     (19  mL   HNO    3 + 9 mL HCl
                                            HCl + 6 mL HF + 19 mL H2 O) for approximately 20 s, and the microstructures of the
                       + 6 mL HF + 19 mL H     O) for approximately
                                            z 2surface   and x surface20         s, and
                                                                              were        the microstructures
                                                                                      observed      using an optical  of the   z surface (OM; BX41M-LED,
                                                                                                                             microscope
                       and x surface were observed       using    an   optical   microscope       (OM;     BX41M-LED,         Olympus,
                                            Olympus, Tokyo, Japan). Notably, only the z surface and x surface were analyzed herein.
                       Tokyo, Japan). Notably,   only the zthe
                                            Furthermore,        surface      and x were
                                                                     specimens       surface    were analyzed
                                                                                            analyzed                 herein. Further-
                                                                                                           using a scanning       electron microscope (SEM;
                       more, the specimensSU-5000,
                                             were analyzed       using     a scanning     electron    microscope
                                                        Hitachi, Japan) and an X-ray diffractometer (XRD;             (SEM;D8  SU-5000,
                                                                                                                                  Discover, Bruker, Karlsruhe,
                       Hitachi, Japan) and an   X-ray diffractometer
                                            Germany)      to observe the (XRD;         D8 Discover,
                                                                               morphology                  Bruker,pool
                                                                                                of the melting        Karlsruhe,     Ger- the phase structure,
                                                                                                                           and examine
                       many) to observe therespectively.
                                               morphology of the melting pool and examine the phase structure,
                       respectively.              A tensile test was performed in which the F and FH groups of specimens were
                            A tensile test was   performed
                                            stretched            in which
                                                         at a speed             the F and and
                                                                          of 1 mm/min,          FH the
                                                                                                     groups      of specimens
                                                                                                           results   of each group   were  were obtained as the
                       stretched at a speedaverage
                                             of 1 mm/min,        and theobtained
                                                        of the values         results ofineachfive group
                                                                                                    test runs.wereThe obtained
                                                                                                                          hardness as theof the specimens was
                       average of the valuesanalyzed
                                               obtainedininHRFfive test
                                                                      units runs.  The hardness
                                                                              by using      a Rockwell of the   specimens
                                                                                                              hardness         was(AR-10
                                                                                                                           tester    ana- Hardness Testing
                       lyzed in HRF units Machine,
                                            by using Mitutoyo,
                                                         a Rockwell     Taipei, Taiwan). An erosion test was conductedMa-
                                                                           hardness     tester   (AR-10     Hardness      Testing       in which the specimens
                       chine, Mitutoyo, Taipei,
                                            wereTaiwan).
                                                  placed on   An theerosion
                                                                       carriertest   waserosion
                                                                                 of the    conducted       in which
                                                                                                    equipment          the specimens
                                                                                                                    (Figure    5). The erodent solid particles
                       were placed on the carrier  of theinerosion
                                            employed         this testequipment
                                                                          were irregular(Figure
                                                                                              Al25).
                                                                                                   O3 The    erodent
                                                                                                        ceramic         solid (hardness:
                                                                                                                   particles    particles 2000 HV, Rich Sou
                       employed in this testTechnology
                                             were irregular Co.,Al    2O3 ceramic
                                                                   Ltd.,   Kaohsiung, particles
                                                                                            Taiwan)(hardness:     2000ofHV,
                                                                                                         with sizes            Rich Sou
                                                                                                                           125–150     µm. The erosion rate in
                       Technology Co., Ltd.,   Kaohsiung,
                                            units  of g/g was  Taiwan)
                                                                     defined with
                                                                                as sizes   of 125–150
                                                                                    the total    mass ofμm.  the The   erosion
                                                                                                                  removed          rate individed by the total
                                                                                                                               material
                                            mass as
                       units of g/g was defined    of the
                                                       the total
                                                            erodent mass  particles   hitting the
                                                                             of the removed           specimen
                                                                                                   material         surface.
                                                                                                               divided          Following
                                                                                                                            by the   total the experimental
                       mass of the erodentmethods
                                             particles used
                                                         hittingin [20],    the test was
                                                                     the specimen           performed
                                                                                         surface.   Followingwith 200    g of Al2 O3 ceramic particles each
                                                                                                                    the experimental
                                            time,                                                                 2 (the flying speed of Al O particle is
                       methods used in [20],   the and   the inlet
                                                   test was            pressure
                                                                performed          was200
                                                                                 with     fixed
                                                                                             g ofatAl 3 2kg/cm
                                                                                                         O3 ceramic     particles each             2 3
                                            about 66was
                       time, and the inlet pressure     m/s).fixedTheatimpingement
                                                                           3 kg/cm2 (theangle flying(the    angle
                                                                                                         speed   of between      the erosion
                                                                                                                     Al2O3 particle       is     direction of the
                                            erodent particles
                       about 66 m/s). The impingement         angle  and    theangle
                                                                         (the    material    surface)
                                                                                        between     the was      gradually
                                                                                                           erosion    direction     of the from 15◦ to 90◦ in
                                                                                                                               increased
                                                                  ◦
                       erodent particles andincrements
                                              the material of 15    . The was
                                                               surface)      maximum
                                                                                  graduallyand increased
                                                                                                 minimumfrom   erosion15°rates   ofin
                                                                                                                            to 90°   thein-test pieces in both the
                                            F  and  the   FH   groups      were   30  ◦ and 90◦ , respectively. The failure was dominated by the
                       crements of 15°. The maximum and minimum erosion rates of the test pieces in both the
                       F and the FH groupsductile    cutting
                                               were 30°    andmechanism.           T6 heat
                                                                  90°, respectively.       Thetreatment
                                                                                                  failure wasimproved      the ductility
                                                                                                                   dominated       by the of the material and
Al2O3 Particle Erosion Induced Phase Transformation: Structure, Mechanical Property, and Impact Toughness of an SLM Al-10Si-Mg Alloy - MDPI
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                                ductile cutting mechanism. T6 heat treatment improved the ductility of the material and
                                precipitatedthe
                                precipitated  thenano-strengthening
                                                  nano-strengtheningMg
                                                                    Mg2Si
                                                                        Si phase, which can improve the wear resistance
                                                                      2 phase, which can improve the wear resistance
                                of  the material.
                                of the material.

                                Figure5.5.(a)
                                Figure     (a)The
                                               Theerosion
                                                   erosion  test
                                                          test   equipment
                                                               equipment   developed
                                                                         developed     by group;
                                                                                   by our our group;   (b)definition
                                                                                                 (b) the   the definition  of impingement
                                                                                                                     of impingement angle.
                                angle.
                                       To explore the differences in the wear mechanisms of the as-fabricated Al-10Si-Mg
                                alloy To    explore before
                                        specimens    the differences
                                                              and after inT6the
                                                                             heatwear    mechanisms
                                                                                    treatment,           of themicroscope
                                                                                                 an electron    as-fabricated
                                                                                                                            andAl-10Si-Mg
                                                                                                                                 an optical
                                 alloy   specimens   before    and  after T6  heat   treatment,   an  electron microscope
                                microscope were used to observe the erosion surface morphology and erosion subsurface        and  an optical
                                 microscope     were  used    to observe   the  erosion   surface    morphology    and
                                characteristics of the specimens, respectively. Moreover, in the erosion process, high- erosion  subsurface
                                 characteristics
                                speed    impingementof the
                                                         of specimens,
                                                             the erodent Al respectively.    Moreover, in the erosion process, high-
                                                                               2 O3 particles on the specimen surface can generate a
                                 speed
                                high      impingement
                                       temperature     of 400–500     ◦
                                                          of the erodent     Al2O3 Under
                                                                        C [21–24].    particles
                                                                                              theoninfluence
                                                                                                     the specimen   surface
                                                                                                              of local       can generate
                                                                                                                       pressure   and higha
                                 high temperature
                                temperature,           of 400–500
                                                  the matrix    of the°CAl[21–24].
                                                                            alloy isUnder      the influence
                                                                                       softened,               of local are
                                                                                                    and microcracks     pressure   and high
                                                                                                                            generated.     In
                                 temperature,
                                this              the matrixthe
                                      light, to investigate     of the  Al alloyofiserosion
                                                                    influence         softened,
                                                                                             on and    microcracksstrength
                                                                                                  the mechanical     are generated.    In this
                                                                                                                              and fracture
                                 light, to investigate
                                toughness     of the SLMthe      influencealloy,
                                                             Al-10Si-Mg       of erosion    on FH
                                                                                    the F and    the groups
                                                                                                      mechanical    strength after
                                                                                                              of specimens     and erosion
                                                                                                                                     fracture
                                 toughness     of the SLM     Al-10Si-Mg     alloy,  the  F and   FH   groups  of specimens
                                were denoted FE and FHE, respectively. The naming principles are summarized in Table           after  erosion
                                                                                                                                            3.
                                 were
                                In  orderdenoted   FE and
                                           to explore   the FHE,
                                                             phaserespectively.
                                                                     transformation  Theand
                                                                                          naming     principles
                                                                                              degradation       are summarized
                                                                                                             behaviors   caused byinsevere
                                                                                                                                        Table
                                 3. In order
                                particle       to explore
                                           erosion          the phase transformation
                                                    [20], approximately       1000 g of Aland2 O3 degradation     behaviors
                                                                                                    ceramic particles         caused
                                                                                                                       was used        by se-
                                                                                                                                   to erode
                                 vere sides
                                both    particle  erosion
                                              of the tensile[20],
                                                               andapproximately        1000 g specimens,
                                                                    the impact toughness        of Al2O3 ceramic
                                                                                                             and theparticles
                                                                                                                      erosion was    usedof
                                                                                                                                direction   to
                                the erodent particles was parallel to the construction direction of the specimens (Figure 6).
Al2O3 Particle Erosion Induced Phase Transformation: Structure, Mechanical Property, and Impact Toughness of an SLM Al-10Si-Mg Alloy - MDPI
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 Nanomaterials 2021, 11, 2131                                                                                                                        6 of 17

                                 erode both sides of the tensile and the impact toughness specimens, and the erosion di-
                                 rection of the erodent particles was parallel to the construction direction of the specimens
                                   To our6).
                                 (Figure   knowledge,    no reports
                                             To our knowledge,      noon  the effect
                                                                       reports        of effect
                                                                                 on the  particle  erosion erosion
                                                                                                of particle on the mechanical    strength
                                                                                                                      on the mechanical
                                   and impact
                                 strength  and toughness     of SLM Al-10Si-Mg
                                                impact toughness                   alloy arealloy
                                                                      of SLM Al-10Si-Mg       available.  In this study,
                                                                                                    are available.       X-ray
                                                                                                                    In this    diffraction
                                                                                                                            study, X-ray
                                   spectroscopy    (Bruker  AXS  GmbH,     Karlsruhe,  Germany)     was  also  used
                                 diffraction spectroscopy (Bruker AXS GmbH, Karlsruhe, Germany) was also used to ana-to analyze the  phase
                                   structure  of the  erosion  surfaces   of the FE  and   FHE   groups   of specimens
                                 lyze the phase structure of the erosion surfaces of the FE and FHE groups of specimens toto demonstrate
                                   the generation
                                 demonstrate    the mechanism     of particle erosion
                                                     generation mechanism              induced
                                                                                of particle       phase
                                                                                             erosion     transformation.
                                                                                                      induced               XRD test uses
                                                                                                                 phase transformation.
                                   copper
                                 XRD   testas the copper
                                            uses   target, Cu-Kα   radiation
                                                           as the target,      with radiation
                                                                            Cu-Kα   a wavelength withofa1.5418  Å, the scanning
                                                                                                         wavelength     of 1.5418 range
                                                                                                                                   Å , theof
                                   2θ is from  20 ◦ to 100◦ , and the scanning speed is 3◦ /min.
                                 scanning range of 2θ is from 20° to 100°, and the scanning speed is 3°/min.

                                Figure 6.6.
                                  Figure Tensile
                                            Tensileand
                                                    andimpact
                                                        impacttoughness
                                                                toughnesstest
                                                                           testspecimens
                                                                                specimensafter
                                                                                          aftererosion.
                                                                                                erosion.

                                 3.3.Results
                                      Resultsand
                                               andDiscussion
                                                   Discussion
                                 3.1.
                                   3.1.Microstructural
                                        MicrostructuralCharacteristics
                                                        Characteristicsand
                                                                        andMaterial
                                                                            MaterialProperties
                                                                                     Properties
                                       Figure
                                          Figure7 7presents
                                                     presentsthe   themicrostructures
                                                                        microstructures of the  the as-fabricated
                                                                                                     as-fabricatedAl-10Si-Mg
                                                                                                                         Al-10Si-Mgspecimens
                                                                                                                                        specimensbefore be-
                                   andand
                                 fore     after  T6T6
                                             after    heat
                                                         heat treatment
                                                                 treatment(groups
                                                                              (groupsFFand  andFH)
                                                                                                 FH) on on the surfaces
                                                                                                                  surfaces parallel
                                                                                                                              parallel(x (xsurface)
                                                                                                                                             surface)and and
                                   perpendicular       (z  surface)    to the  construction
                                 perpendicular (z surface) to the construction direction.       direction.     The   microstructure
                                                                                                                     microstructure of the F groupof
                                                                                                                                       of  the   F group
                                 ofspecimens
                                    specimenson     onthethex xsurface
                                                                  surfacepresents
                                                                            presents melting
                                                                                        meltingpools
                                                                                                   poolswith    fish-scale-like
                                                                                                             with                 shapes,
                                                                                                                    fish-scale-like   shapes,as illustrated
                                                                                                                                                  as illus-
                                   in Figure
                                 trated         7a, with
                                          in Figure          a width
                                                        7a, with         of approximately
                                                                     a width    of approximately 100 µm,100 which
                                                                                                              μm, whichis close  to thetospot
                                                                                                                             is close            size of
                                                                                                                                           the spot       the
                                                                                                                                                       size
                                 oflaser  sourcesource
                                    the laser       [25]. The[25].depth
                                                                     The of  theseofmelting
                                                                           depth               pools is approximately
                                                                                       these melting                           30 µm, and
                                                                                                            pools is approximately          30there
                                                                                                                                                 μm, are
                                                                                                                                                       andno
                                   microholes
                                 there             between layers,
                                         are no microholes                indicating
                                                                    between    layers,that   the SLMthat
                                                                                         indicating        process
                                                                                                               the SLMparameters
                                                                                                                           process were     appropriately
                                                                                                                                     parameters       were
                                   controlled     [26].   On    the  z surface,    the laser  source     left a  strip-shaped
                                 appropriately controlled [26]. On the z surface, the laser source left a strip-shaped laser      laser  scanning      track,
                                   as  illustrated     in  Figure     7b.   The   extremely     fast  cooling      rate  in the
                                 scanning track, as illustrated in Figure 7b. The extremely fast cooling rate in the SLM pro-     SLM   process      caused
                                   segregation
                                 cess               in the Al-10Si-Mg
                                       caused segregation                     alloy duringalloy
                                                                    in the Al-10Si-Mg          solidification,      leading to the
                                                                                                     during solidification,           formation
                                                                                                                                   leading     to theoffor-
                                                                                                                                                        long
                                   dendritic    crystals    [27]. After    T6 heat                        ◦ C, 2 h → (510   ◦
                                 mation    of long    dendritic      crystals  [27].treatment     (510 treatment
                                                                                      After T6 heat                     170 °C,
                                                                                                                              C, 22h),
                                                                                                                                    h →the 170
                                                                                                                                            outline
                                                                                                                                                  °C, 2ofh),
                                                                                                                                                          the
                                   melting
                                 the  outlinepools
                                                of the  and    the scanning
                                                          melting      pools and trajectory   disappeared,
                                                                                     the scanning     trajectory  and   coarse silicon
                                                                                                                      disappeared,     and particles    were
                                                                                                                                              coarse sili-
                                   formed.
                                 con  particlesThe    supersaturated
                                                   were    formed. The silicon         was redissolved
                                                                             supersaturated       silicon was intoredissolved
                                                                                                                     the aluminum  into matrix,
                                                                                                                                        the aluminumand the
                                   resulting   microstructure         is depicted    in Figure   7c,d.    Notably,    the fine
                                 matrix, and the resulting microstructure is depicted in Figure 7c,d. Notably, the fine grains  grains  distribute     at the
                                   boundaries      of   melting     pool,  and    on  the above    of  fine   grains   present
                                 distribute at the boundaries of melting pool, and on the above of fine grains present radi-     radiation-distributed
                                   columnar grains.columnar
                                 ation-distributed          After T6 heat      treatment,
                                                                         grains.    After T6silicon
                                                                                                heat precipitation
                                                                                                        treatment, silicontransformed      into spherical
                                                                                                                                 precipitation      trans-
                                 formed into spherical form, with grain distribution converted into equiaxed grains due and
                                   form,   with   grain    distribution      converted     into  equiaxed       grains   due  to  homogenization          to
                                   recrystallization.
                                 homogenization and recrystallization.
                                          Considering that the silicon content in the aluminum matrix and the morphology of
                                   the precipitated silicon significantly influence the wear resistance of the Al-Si alloy [28,29],
                                   the detailed structure of the melting pools was observed using SEM, and the silicon content
                                   in different regions of the structure was analyzed using EDS. As illustrated in Figure 8,
                                   the silicon content of the aluminum matrix was approximately 10.65 wt.%, which is close
                                   to the silicon content of the Al alloy powder used in this study. The silicon content at the
                                   boundary of the melting pools was approximately 18.40 wt.%. Therefore, the boundary
                                   zone was termed the Si-rich phase [10,13,17]. These organizational differences have an
                                   important effect on the subsequent erosion characteristics obtained in this study.
Al2O3 Particle Erosion Induced Phase Transformation: Structure, Mechanical Property, and Impact Toughness of an SLM Al-10Si-Mg Alloy - MDPI
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                                       Figure 7. Microstructure of the specimens in different observation planes: group F specimens on the
                                       planes (a) parallel and (b) perpendicular to the construction direction, and group FH specimens on
                                       the planes (c) parallel and (d) perpendicular to the construction direction.

                                              Considering that the silicon content in the aluminum matrix and the morphology of
                                       the precipitated silicon significantly influence the wear resistance of the Al-Si alloy [28,29],
                                       the detailed structure of the melting pools was observed using SEM, and the silicon con-
                                       tent in different regions of the structure was analyzed using EDS. As illustrated in Figure
                                       8, the silicon content of the aluminum matrix was approximately 10.65 wt.%, which is
                                       close  to7.the
                                         Figure          silicon content
                                                    Microstructure            of the Alinalloy
                                                                      of the specimens           powder
                                                                                          different        usedplanes:
                                                                                                    observation    in this study.
                                                                                                                         group      The silicon
                                                                                                                               F specimens on thecontent
                                       Figure   7. Microstructure       of the specimens  in different  observation    planes: group  F specimens  on the
                                       at the boundary of the melting pools was approximately 18.40 wt.%. Therefore, the
                                         planes  (a) parallel and   (b) perpendicular to the  construction direction, and group  FH specimens  on bound-
                                       planes  (a)
                                         the zone    parallel
                                             planeswas         and
                                                      (c) parallel   (b)
                                                                   andtheperpendicular
                                                                        (d) perpendicularto  the
                                                                                          to the construction
                                                                                                 construction   direction,
                                                                                                               direction.   and group   FH specimens   on
                                       ary                  termed           Si-rich phase    [10,13,17].  These    organizational differences have
                                       the planes (c) parallel and (d) perpendicular to the construction direction.
                                       an important effect on the subsequent erosion characteristics obtained in this study.
                                              Considering that the silicon content in the aluminum matrix and the morphology of
                                        the precipitated silicon significantly influence the wear resistance of the Al-Si alloy [28,29],
                                        the detailed structure of the melting pools was observed using SEM, and the silicon con-
                                        tent in different regions of the structure was analyzed using EDS. As illustrated in Figure
                                        8, the silicon content of the aluminum matrix was approximately 10.65 wt.%, which is
                                        close to the silicon content of the Al alloy powder used in this study. The silicon content
                                        at the boundary of the melting pools was approximately 18.40 wt.%. Therefore, the bound-
                                        ary zone was termed the Si-rich phase [10,13,17]. These organizational differences have
                                        an important effect on the subsequent erosion characteristics obtained in this study.

        Figure 8. (a) Detailed morphology of the melting pool and (b) silicon content in different regions of the melting pool.
        Figure 8. (a) Detailed morphology of the melting pool and (b) silicon content in different regions of the melting pool.

                                            The
                                            The SLM
                                                  SLM process       creates aa microstructure
                                                          process creates       microstructure with    with aa nonuniform
                                                                                                                nonuniform distribution
                                                                                                                                   distribution of    of silicon
                                                                                                                                                         silicon
                                     particles
                                     particles inside
                                                   insidethethematerial.
                                                                material.The The evolution
                                                                                     evolution  of the   phase
                                                                                                    of the       structure
                                                                                                             phase    structure afterafter
                                                                                                                                       heatheat
                                                                                                                                              treatment      was
                                                                                                                                                     treatment
                                     analyzed
                                     was analyzed  usingusing
                                                            XRD,XRD,
                                                                   and the
                                                                        andresults      are presented
                                                                              the results     are presented in Figure    9. The
                                                                                                                 in Figure      9. diffraction
                                                                                                                                    The diffraction peaks    cor-
                                                                                                                                                          peaks
                                     responding       to  the α-Al   phase  clearly    appeared      in the  XRD    patterns
                                     corresponding to the α-Al phase clearly appeared in the XRD patterns of the F and FH         of  the  F and    FH   groups
                                     of  specimens.
                                     groups               A comparison
                                                of specimens.                betweenbetween
                                                                    A comparison          FiguresFigures
                                                                                                      8 and 98 revealed
                                                                                                                  and 9 revealedthat the     supersaturated
                                                                                                                                          that  the supersat-
             Figure 8. (a) Detailed morphology
                                     silicon      of thesolution
                                                solid    melting pool and
                                                                    was    (b) silicon content
                                                                         redissolved       into  inthe
                                                                                                    different regions of
                                                                                                        aluminum           the melting
                                                                                                                        matrix     and   pool.
                                                                                                                                           precipitated      into
                                     urated silicon solid solution was redissolved into the aluminum matrix and precipitated
                                     coarse    silicon
                                     into coarse         particles,
                                                      silicon        thus causing
                                                               particles,               the diffraction      peakpeak
                                                                                                                    corresponding          to silicon    to rise.
                                              The SLM     process  creates thus   causing
                                                                           a microstructure   thewith
                                                                                                    diffraction
                                                                                                         a nonuniform       corresponding
                                                                                                                            distribution          to silicon
                                                                                                                                            of silicon         to
                                     In  addition,
                                     rise.  In         the
                                                addition,   magnesium
                                                             the magnesium content     in
                                                                                  content theinAl-10Si-Mg
                                                                                                the   Al-10Si-Mgalloy    was
                                                                                                                       alloy    1
                                                                                                                               waswt.%,
                                       particles inside the material. The evolution of the phase structure after heat treatment was   1     and
                                                                                                                                        wt.%,     because
                                                                                                                                                 and   becausethe
                                     the   diffraction
                                       analyzed     usingpeak
                                                           XRD,corresponding
                                                                 and the results are to the  Mg2 Si in
                                                                                         presented     nanoparticles
                                                                                                          Figure 9. The was       close to
                                                                                                                            diffraction      the α-Al
                                                                                                                                           peaks   cor- phase
                                     (Al   (1 1  1)), the  Mg
                                       responding to the α-Al   Si phase   diffraction     peak     was  not  clear   in  case   of
                                                               2 phase clearly appeared in the XRD patterns of the F and FH groups   the   F and    FH groups
                                       of  specimens.     A  comparison   between      Figures    8 and   9 revealed    that
                                     of specimens. Furthermore, the hardness data of the specimens are shown in Figure 10.     the  supersaturated
                                       silicon to
                                     Owing       solid
                                                    the solution
                                                         extremelywasfine
                                                                       redissolved      into the aluminum
                                                                           grains produced          by the rapid matrix
                                                                                                                     coolingand inprecipitated     into
                                                                                                                                     the SLM process,         the
                                       coarse   silicon  particles, thus causing    the  diffraction   peak   corresponding
                                     HRF hardness of the F group of specimens reached 98. The heat treatment process changed      to  silicon  to  rise.
                                       In addition,
                                     the               the magnesium
                                           silicon structure             content in
                                                                 and released          the Al-10Si-Mg
                                                                                    residual               alloy was
                                                                                                stress, which           1 wt.%,the
                                                                                                                   reduced         andhardness
                                                                                                                                         because the of the FH
                                     group of specimens to 75.
Al2O3 Particle Erosion Induced Phase Transformation: Structure, Mechanical Property, and Impact Toughness of an SLM Al-10Si-Mg Alloy - MDPI
(1 1specimens.
                                     1)), the MgFurthermore,
                                                 2Si phase diffraction    peak data
                                                                the hardness   was not   clear
                                                                                    of the     in case of
                                                                                            specimens   arethe  F andinFH
                                                                                                             shown         groups
                                                                                                                         Figure 10. of
                                                                                                                                    Ow-
                               specimens.
                                   ing to theFurthermore,
                                               extremely finethe grains
                                                                 hardness   data of by
                                                                         produced   the the
                                                                                         specimens   are shown
                                                                                             rapid cooling         in Figure
                                                                                                              in the         10. Ow-the
                                                                                                                      SLM process,
                               ingHRFto the extremely
                                          hardness   of fine
                                                         the Fgrains
                                                                group produced   by the reached
                                                                         of specimens     rapid cooling
                                                                                                   98. Thein the
                                                                                                               heatSLM   process,process
                                                                                                                     treatment    the
                               HRF     hardness   of the   F group    of  specimens  reached    98. The    heat  treatment
                                   changed the silicon structure and released residual stress, which reduced the hardness of process
                               changed
                                   the FHthe  silicon
                                            group      structure and
                                                   of specimens        released residual stress, which reduced the hardness of
                                                                   to 75.
Nanomaterials 2021, 11, 2131                                                                                                          8 of 17
                               the FH group of specimens to 75.

                                  Figure 9. XRD patterns of the as-fabricated Al-10Si-Mg alloy before and after T6 heat treatment.
                               FigureFigure
                                      9. XRD9. patterns of the of
                                               XRD patterns    as-fabricated  Al-10Si-Mg
                                                                  the as-fabricated       alloy before
                                                                                    Al-10Si-Mg         and after
                                                                                                alloy before and T6 heat
                                                                                                                 after T6treatment.
                                                                                                                          heat treatment.

                   Figure 10. HRF hardness of the as-fabricated Al-10Si-Mg alloy before and after T6 heat treatment.
                Figure 10. HRF hardness of the as-fabricated Al-10Si-Mg alloy before and after T6 heat treatment.
                                 3.2. of
             Figure 10. HRF hardness  Particle  Erosion Wear
                                         the as-fabricated    Mechanism
                                                           Al-10Si-Mg alloy before and after T6 heat treatment.
                                           According
                                  3.2. Particle Erosionto    studies
                                                          Wear          in the literature [30–32], when a ductile metal material is hit
                                                                  Mechanism
                               3.2. Particle
                                     with    Erosion
                                           erodent      Wear  Mechanism
                                                      particles,  the  peak   erosion rate  appears   at the                                   ◦ –30◦ .
                                        According to studies in the literature           [30–32],   when    a impingement
                                                                                                               ductile metal angles      of 15
                                                                                                                                  material   is hit
                                     Theerodent
                                  with    erosionto
                                     According       rates  of the
                                                       studies
                                                    particles,   in Fthe
                                                                the    and
                                                                     peak    FH groups
                                                                          literature
                                                                             erosion      ofappears
                                                                                      [30–32],
                                                                                      rate    specimens
                                                                                                 whenatathe as impingement
                                                                                                                functions
                                                                                                           ductile   metalof    the  impingement
                                                                                                                              material
                                                                                                                                  angles isofhit
                                                                                                                                              15°–
                               with  angle
                                     erodentare  illustrated
                                                particles,    in
                                                            the   Figure
                                                                  peak     11.
                                                                         erosionThe erosion
                                                                                   rate       rates
                                                                                        appears     of
                                                                                                   at  the
                                                                                                      the   specimens
                                                                                                           impingement   in
                                  30°. The erosion rates of the F and◦ FH groups of specimens as functions of the impinge-   both
                                                                                                                              anglesgroups
                                                                                                                                       of     peaked
                                                                                                                                           15°–
                                     at an
                               30°.ment
                                    The     impingement
                                         erosion
                                         angle  arerates      angle
                                                           of the
                                                      illustrated  F   of 30
                                                                   inand    FH, 11.
                                                                       Figure    while
                                                                                    Thethe
                                                                                 groups   of minimum
                                                                                             specimens
                                                                                         erosion          erosion
                                                                                                   rates ofasthe     rate occurred
                                                                                                               functions
                                                                                                                  specimens of the         90◦ . The
                                                                                                                                       at groups
                                                                                                                                    impinge-
                                                                                                                                 in both
                                     erosion  rate   decreasedinasFigure
                                                                      the impingement      angle   increased            ◦
                                                                                                                after 30 rate
                                                                                                                          , which
                               ment   angleatare
                                  peaked      anillustrated
                                                   impingement        angle  11. Thewhile
                                                                              of 30°, erosiontherates of the specimens
                                                                                                 minimum       erosion          bothindicated
                                                                                                                             inoccurred
                                                                                                                                      groups      that
                                                                                                                                            at 90°.
                                     the  ductile   cutting  mechanism         dominated    the  wear   fracture   of
                               peaked at an impingement angle of 30°, while the minimum erosion rate occurred at 90°. both    groups.   In   general,
                                     the metallic materials with higher hardness have better wear resistance, but the results
                                     presented in Figure 11 indicated that the wear resistance of the FH group of specimens was
                                     superior to that of the group F specimens under all impingement angles. To clarify the wear
                                     mechanism, we inspected the morphology of the erosion surface by using SEM (Figure 12),
                                     and the results indicated that under impingement by irregularly shaped erodent particles,
                                     many sharp grooves were formed in the F group of specimens because the Al2 O3 particles
                                     cut through the material surface. By contrast, the FH group of specimens had a softer
                                     matrix due to the heat treatment; the scratches on the erosion surface were gentler, and
                                     many lip structures were formed adjacent to the erosion grooves. The main reason is
Al2O3 Particle Erosion Induced Phase Transformation: Structure, Mechanical Property, and Impact Toughness of an SLM Al-10Si-Mg Alloy - MDPI
sults presented in Figure 11 indicated that the wear resistance of the FH group of speci-
                             mens was superior to that of the group F specimens under all impingement angles. To
                             clarify the wear mechanism, we inspected the morphology of the erosion surface by using
                             SEM (Figure 12), and the results indicated that under impingement by irregularly shaped
Nanomaterials 2021, 11, 2131 erodent particles, many sharp grooves were formed in the F group of specimens because                                   9 of 17
                             the Al2O3 particles cut through the material surface. By contrast, the FH group of speci-
                             mens had a softer matrix due to the heat treatment; the scratches on the erosion surface
                             were gentler, and many lip structures were formed adjacent to the erosion grooves. The
                             main reason     is that
                                      that heat       heat treatment
                                                    treatment           can generate
                                                                  can generate          strengthening
                                                                                   strengthening       MgMg    2Si nanoprecipitates in
                                                                                                            2 Si nanoprecipitates in the aluminum
                             the aluminum
                                      matrix [33,34], which increases the resistance of the material
                                                matrix   [33,34],  which   increases  the  resistance   of the   materialtoto  wear
                                                                                                                                  wearandand microcrack
                             microcrack formation. Therefore, the lip structures were not completely separated from
                                      formation. Therefore, the lip structures were not completely separated from the surface,
                             the surface, which led to the superior wear resistance of the Al-10Si-Mg alloy [21,24].
                                      which led to the superior wear resistance of the Al-10Si-Mg alloy [21,24]. Moreover, based
                             Moreover, based on the erosion subsurface morphologies corresponding to different im-
                             pingementon the    erosion
                                           angles,          subsurface
                                                     as depicted          morphologies
                                                                   in Figure                  corresponding
                                                                               13, the FH group     of specimens   tohad
                                                                                                                       different
                                                                                                                           a higherimpingement
                                                                                                                                     sur-          angles,
                                      as depicted
                             face roughness            in Figure
                                                 than the   F group13,
                                                                     of the  FH group
                                                                        specimens          of specimens
                                                                                      because                 had a of
                                                                                                the softer matrix     higher    surface
                                                                                                                         the former    led roughness than
                                      the F group
                             to the formation      of lipofstructures.
                                                             specimens      because
                                                                       However,        the softer
                                                                                    because          matrix
                                                                                               changes   in the ofmomentum
                                                                                                                    the formercompo-
                                                                                                                                   led to the formation
                                      of liptostructures.
                             nent normal                        However,
                                                the erosion surface    of the because     changes
                                                                              Al2O3 particles        in theincrease
                                                                                                gradually       momentum         component normal to
                                                                                                                        as the impinge-
                                      the erosion
                             ment angle     increases,surface     of the
                                                          many pits        Al2 O3inparticles
                                                                      appeared                  gradually
                                                                                      both groups    at highincrease
                                                                                                                impingementas the   impingement angle
                                                                                                                                  angles.
                             Therefore,   in the follow-up
                                      increases,     many pits  experiments,
                                                                    appeared1000      g of Al
                                                                                  in both      2O3 particles
                                                                                            groups     at high wasimpingement
                                                                                                                     used to study angles.
                                                                                                                                       the      Therefore,
                             erosion-induced       phase transformation
                                      in the follow-up         experiments,   of 1000
                                                                                 both groups
                                                                                        g of Alof O
                                                                                                 2 3specimens
                                                                                                       particles   at an
                                                                                                                     was  impingement
                                                                                                                            used   to  study  the erosion-
                             angle ofinduced
                                        90°. Furthermore,       the effects ofof
                                                   phase transformation         the  phase
                                                                                   both      transformation
                                                                                         groups    of specimens  induced
                                                                                                                      at anby   the heat
                                                                                                                             impingement      angle of 90◦ .
                             generated   due to particle
                                      Furthermore,        theimpingement
                                                               effects of theand   erosion-induced
                                                                                phase   transformation microcracks
                                                                                                             inducedonbythe     mechan-
                                                                                                                              the heat generated due to
                             ical properties and impact toughness of the SLM Al-10Si-Mg alloy were evaluated.
                                      particle impingement and erosion-induced microcracks on the mechanical properties and
                                      impact toughness of the SLM Al-10Si-Mg alloy were evaluated.

                                       Figure 11. Erosion rate of the as-fabricated Al-10Si-Mg alloy before and after T6 heat treatment as a
  Nanomaterials 2021, 11, x FOR PEER
                             Figure 11.REVIEW
                                        Erosion rate of the as-fabricated Al-10Si-Mg alloy before and after T6 heat treatment as a                  10 of 17
                             functionfunction  of the impingement
                                      of the impingement   angle.       angle.

                                         Figure
                                       Figure  12.12. Erosion
                                                   Erosion    surface
                                                            surface   morphology
                                                                    morphology     of as-fabricated
                                                                               of the the as-fabricated Al-10Si-Mg
                                                                                                    Al-10Si-Mg alloy alloy
                                                                                                                     beforebefore andT6
                                                                                                                            and after after
                                                                                                                                        heatT6
                                         heat treatment.
                                       treatment.
Al2O3 Particle Erosion Induced Phase Transformation: Structure, Mechanical Property, and Impact Toughness of an SLM Al-10Si-Mg Alloy - MDPI
Nanomaterials 2021, 11, 2131                                                                                                                    10 of 17

                                 Figure 12. Erosion surface morphology of the as-fabricated Al-10Si-Mg alloy before and after T6
                                 heat treatment.

         Figure
         Figure 13.
                13. Erosion
                    Erosion subsurface
                            subsurface morphology
                                       morphology of
                                                  of the
                                                     the as-fabricated
                                                         as-fabricated Al-10Si-Mg alloy before
                                                                       Al-10Si-Mg alloy before and
                                                                                               and after
                                                                                                   after T6
                                                                                                         T6 heat
                                                                                                            heat treatment.
                                                                                                                 treatment.

                                 3.3.
                                 3.3. Erosion
                                       Erosion Induced
                                                 Induced Phase
                                                            Phase Transformation
                                                                    Transformation
                                       In
                                        In particle erosion, theceramic
                                           particle   erosion,    the    ceramic  particles
                                                                                     particleshithit
                                                                                                  thethesurface
                                                                                                            surfaceof the
                                                                                                                        of metal   specimens
                                                                                                                           the metal             at high
                                                                                                                                         specimens     at
                                 speed,   and   their  kinetic    energy   is  converted     into  heat   energy,     which
                                 high speed, and their kinetic energy is converted into heat energy, which can generate        can  generate    temper-
                                 atures   of 400–500
                                 temperatures            °C instantaneously
                                                   of 400–500                       [22,23,31]
                                                                   ◦ C instantaneously           and cause
                                                                                             [22,23,31]    andsurface      oxidation
                                                                                                                  cause surface         to formtoAlform
                                                                                                                                    oxidation        2O3.

                                 As   depicted    in  Figure     14a,b,  the   F group   of   specimens      transformed
                                 Al2 O3 . As depicted in Figure 14a,b, the F group of specimens transformed into the FE         into the  FE  group    of
                                 specimens     after   erosion.     The  diffraction    peaks    corresponding
                                 group of specimens after erosion. The diffraction peaks corresponding to Al2 O3 were  to  Al 2O3 were generated at

                                 six  specificatdiffraction
                                 generated        six specificangles      2θ, and
                                                                   diffraction        the 2θ,
                                                                                 angles   same  andresults
                                                                                                     the samewere     obtained
                                                                                                                   results  werefor    the F group
                                                                                                                                   obtained    for theofF
                                 specimens     transformed
                                 group of specimens               into the FE
                                                            transformed      intogroup
                                                                                   the FEof group
                                                                                             specimens.      A comparison
                                                                                                     of specimens.               of the XRD
                                                                                                                          A comparison         patterns
                                                                                                                                            of the  XRD
                                 of  the F, of
                                 patterns    FE,the
                                                  FH, F, and
                                                         FE, FH,FHEand groups
                                                                           FHEof     specimens
                                                                                  groups            with thatwith
                                                                                             of specimens          of the
                                                                                                                        thatAlof
                                                                                                                               2Othe
                                                                                                                                  3 ceramic
                                                                                                                                       Al2 O3 particles
                                                                                                                                                ceramic
                                 used    in the
                                 particles   used erosion
                                                     in the experiment         revealedrevealed
                                                              erosion experiment           that only     sixonly
                                                                                                       that    specific    diffraction
                                                                                                                     six specific         peaks peaks
                                                                                                                                    diffraction    corre-
                                 sponding     to  the  Al    O   phase    of  the  erodent     particles   appeared       in
                                 corresponding to the Al2 O3 phase of the erodent particles appeared in the patterns of the
                                                           2   3                                                             the  patterns    of  the FE
                                 and   FHE   groups     of specimens.      Notably,     no  ceramic     particles    remained
                                 FE and FHE groups of specimens. Notably, no ceramic particles remained on the erosion            on  the  erosion   sur-
                                 face  of the
                                 surface       specimens
                                           of the  specimens   observed
                                                                   observed  using
                                                                                usingSEM
                                                                                       SEM  (Figure
                                                                                               (Figure12).
                                                                                                         12).ItItcan
                                                                                                                   canbebeinferred
                                                                                                                           inferredthat
                                                                                                                                      that the
                                                                                                                                            the particle
                                 erosion caused (1) the formation
                                                               formation of  of a surface
                                                                                  surface Al Al22O33 film;
                                                                                                      film; (2)
                                                                                                             (2) high
                                                                                                                  high temperature
                                                                                                                         temperature of the surface
                                 to lead to redissolution of the supersaturated silicon into the α-Al matrix, resulting in a
                                 slight dip in the silicon phase diffraction peak of the specimens        specimens after after the
                                                                                                                                 the particle
                                                                                                                                     particle erosion;
                                                                                                                                                erosion;
                                 (3) deformation of the grains after erosion and microcrack formation [34]. In this light, it
                                 is interesting to investigate the effect of particle erosion on the mechanical strength and
                                 fracture toughness of the SLM Al-10Si-Mg alloy.           alloy.

                                 3.4. Changes in Tensile Mechanical Properties Caused by Erosion
                                      The F and FH groups of specimens were compared, as illustrated in Figure 15a,b. The
                                 yield strength (YS) and ultimate tensile strength (UTS) of the F group of specimens reached
                                 181.63 and 297.75 MPa, respectively, but their uniform elongation (UE) and total elongation
                                 (TE) were both 1.87% (low ductility). After T6 heat treatment, the UTS decreased from
                                 297.75 to 286.02 MPa; YS increased from 181.63 to 221.09 MPa; UE and TE increased to
                                 2.33% and 2.70% (ductility improvement), respectively. The morphologies of the tensile
                                 fracture surface and the tensile fracture subsurface of the F and FH groups of specimens
                                 are depicted in Figure 16a,b. The F group of specimens had insufficient ductility and broke
                                 before necking. By contrast, the FH group of specimens, on which small dimples were
                                 observed upon tensile fracture, had higher ductility. Based on a comparison of the tensile
                                 fracture subsurface presented in Figure 16c,d, the F group of specimens fractured within
                                 an extremely short time, resulting in a sharper fracture subsurface profile than that of the
                                 FH group of specimens. The difference between the two groups can be compared more
                                 clearly by using the enlarged views presented in Figure 16e,f. The failure of the FH group
Nanomaterials 2021, 11, 2131                                                                                                     11 of 17

                                  of specimens was attributed to the maximum shear stress induced by the tensile force, and
           Nanomaterials 2021, 11, x FOR PEER REVIEW                                                                                        11 of 1
                                  the fracture subsurface profile was undulating and oriented at approximately 45◦ with
                                  respect to the tensile direction.

                 Figure 14. XRD pattern:  (a) XRD
                                  Figure 14.  the F pattern:
                                                    group of(a)specimens  converted
                                                                the F group         to FEconverted
                                                                            of specimens  after erosion;
                                                                                                    to FE(b) theerosion;
                                                                                                          after  FH group    of specimens
                                                                                                                         (b) the FH group con-
                 verted to FHE after
                                  of erosion.
                                     specimens converted to FHE after erosion.

                                       According     to thein
                                             3.4. Changes   literature [23], the local
                                                               Tensile Mechanical       high temperature
                                                                                   Properties               and high pressure gener-
                                                                                              Caused by Erosion
                                  ated by the impact    of high-speed   particles during   erosion  softened
                                                   The F and FH groups of specimens were compared, as          theillustrated
                                                                                                                    matrix in in
                                                                                                                               theFigure
                                                                                                                                   region15a,b. Th
                                  close to 200
                                             yield strength (YS) and ultimate tensile strength (UTS) of the F group ofthespecimen
                                                µm  below   the Al-alloy surface.  In addition, ceramic   particles   accompanying
                                  fluid hit the  surface
                                             reached      of the
                                                       181.63    metal
                                                               and      specimen
                                                                    297.75          at high speeds,
                                                                           MPa, respectively,    but which   distorted
                                                                                                      their uniform       and deformed
                                                                                                                        elongation   (UE) and tota
                                  the crystal  grains  near  the surface and   generated   microcracks   [35].  Thus,
                                             elongation (TE) were both 1.87% (low ductility). After T6 heat treatment, in this study, the
                                                                                                                                       the UTS de
                                  F and FHcreased
                                               groupsfrom
                                                       of specimens    were   subjected   to particle erosion   with   an  impingement
                                                              297.75 to 286.02 MPa; YS increased from 181.63 to 221.09 MPa; UE and TE
                                  angle of 90  ◦ on both sides to analyze the changes in their mechanical properties and impact
                                             increased   to 2.33% and 2.70% (ductility improvement), respectively. The morphologies o
                                  toughness (Figure 6).
                                             the tensile fracture surface and the tensile fracture subsurface of the F and FH groups o
                                             specimens are depicted in Figure 16a,b. The F group of specimens had insufficient ductil
                                             ity and broke before necking. By contrast, the FH group of specimens, on which smal
                                             dimples were observed upon tensile fracture, had higher ductility. Based on a comparison
                                             of the tensile fracture subsurface presented in Figure 16c,d, the F group of specimens frac
                                             tured within an extremely short time, resulting in a sharper fracture subsurface profil
Nanomaterials 2021, 11, 2131                                                                                                     12 of 17

                                         After erosion, the YS and UTS of the FE group of specimens decreased from 182.63
                                   and 297.75 MPa to 145.77 and 261.86 MPa, respectively, compared with the F group of
                                   specimens. The YS and UTS of the FHE group of specimens decreased from 221.09 and
                                   286.02 MPa to 147.74 and 197.03 MPa, respectively, compared with the FH group of
                                   specimens. By contrast, the UE and TE of the FE group of specimens increased from 1.87%
                                   to 4.93%, compared with the F group of specimens. The UE and TE of the FE group
Nanomaterials 2021, 11, x FOR PEER REVIEW                                                                                       12 of of
                                                                                                                                       17
                                   specimens increased from 2.33%. The experimental results indicate that under severe
                                   erosion conditions, the tensile strength of the as-fabricated Al-10Si-Mg alloy decreases, but
                                   the softening of the Al matrix due to the high surface temperature increases the elongation
                                    than that of the
                                   significantly.     FH group ofafter
                                                    Furthermore,    specimens.
                                                                         erosion,The     difference
                                                                                   Young’s          between
                                                                                               moduli  of the the two groups
                                                                                                              specimens          can
                                                                                                                            of the twobe
                                    compared     more clearly by using  the enlarged    views  presented  in Figure  16e,f. The
                                   groups tend to decrease (Figure 16), indicating that erosion not only affects the changes in  failure
                                    of the FH
                                   tensile      groupand
                                            strength  of specimens
                                                         elongation was   attributed
                                                                     but also  directlytodegrades
                                                                                          the maximum    shear
                                                                                                   material     stress induced
                                                                                                            elasticity.           by the
                                                                                                                        The coefficient
                                    tensile force, and the fracture subsurface    profile  was  undulating  and  oriented   at approxi-
                                   of elasticity (Figure 17). These results directly affect the impact toughness of SLM Al-10Si-
                                    mately
                                   Mg        45° with respect to the tensile direction.
                                        alloy.

                                 Figure 15. (a) Mechanical strength and (b) elongation of the F, FH, FE, and FHE groups of specimens.
                                  Figure 15. (a) Mechanical strength and (b) elongation of the F, FH, FE, and FHE groups of speci-
                                  mens.
Nanomaterials 2021, 11, 2131                                                                                                           13 of 17
             Nanomaterials 2021, 11, x FOR PEER REVIEW                                                                                             13 of

  Nanomaterials 2021, 11, x FOR PEER REVIEW                                                                                             14 of 17

                                     tensile
                  Figure 16. (a,b) Tensile     strength
                                            fracture       andmorphology;
                                                       surface   elongation (c,d)
                                                                              but also directly
                                                                                  fracture       degrades
                                                                                           subsurface;        materialviews
                                                                                                        (e,f) enlarged elasticity.
                                                                                                                               of the The  coeffi-
                                                                                                                                      fracture subsur-
                                   Figure  16.
                                     cient of   (a,b) Tensile  fracture surface morphology;  (c,d) fracture  subsurface; (e,f) enlarged   views
                  face of F and FH groups     of elasticity
                                                 specimens.(Figure 17). These results directly affect the impact toughness of SLM
                                   ofAl-10Si-Mg
                                      the fracture subsurface
                                                      alloy.      of F and FH groups of specimens.

                                                    According to the literature [23], the local high temperature and high pressure gene
                                              ated by the impact of high-speed particles during erosion softened the matrix in the regi
                                              close to 200 μm below the Al-alloy surface. In addition, ceramic particles accompanyi
                                              the fluid hit the surface of the metal specimen at high speeds, which distorted and d
                                              formed the crystal grains near the surface and generated microcracks [35]. Thus, in th
                                              study, the F and FH groups of specimens were subjected to particle erosion with an im
                                              pingement angle of 90° on both sides to analyze the changes in their mechanical propert
                                              and impact toughness (Figure 6).
                                                    After erosion, the YS and UTS of the FE group of specimens decreased from 182.
                                              and 297.75 MPa to 145.77 and 261.86 MPa, respectively, compared with the F group
                                              specimens. The YS and UTS of the FHE group of specimens decreased from 221.09 a
                                              286.02 MPa to 147.74 and 197.03 MPa, respectively, compared with the FH group of spe
                                              imens. By contrast, the UE and TE of the FE group of specimens increased from 1.87%
                                              4.93%, compared with the F group of specimens. The UE and TE of the FE group of spe
                Changes in the stress–strain  imens
                                             curve of increased
                                                      SLM       from alloy
                                                           Al-10Si-Mg 2.33%.  Theand
                                                                            before experimental
                                                                                       afterafter   results
                                                                                             erosion:        indicate
                                                                                                      (a) groups      that
                                                                                                                 F andFFE  under
                                                                                                                          and     severe erosi
     Figure 17.17.
       Figure      Changes in the stress–strain curve  of SLM Al-10Si-Mg  alloy before and        erosion: (a) groups   and FE(b)
                                                                                                                               and
     groups  FH and
       (b) groups  FHFHE.
                      and FHE.                conditions, the tensile strength of the as-fabricated Al-10Si-Mg alloy decreases, but t
                                              softening of the Al matrix due to the high surface temperature increases the elongati
                                              significantly.
                                   3.5. Changes              Furthermore,
                                                  in Impact Toughness  Causedafter erosion, Young’s moduli of the specimens of the tw
                                                                                by Erosion
                                              groups tend to decrease (Figure 16), indicating that erosion not only affects the changes
                                         In this study, an impact fracture test was performed to evaluate the impact toughness
                                   of the specimens from the four groups. The energy absorbed per unit area was calculated
                                   at the point of specimen fracture. The morphology of the impact fracture surface was ob-
                                   served with SEM to clarify the fracture mechanism. Figure 18 shows that the impact frac-
                                   ture toughness of the specimens increased by approximately 20% after the T6 heat treat-
                                   ment. However, due to the composite effect of microcracks and the matrix softening
Nanomaterials 2021, 11, 2131                                                                                                    14 of 17

                               3.5. Changes in Impact Toughness Caused by Erosion
                                        In this study, an impact fracture test was performed to evaluate the impact toughness
                                   of the specimens from the four groups. The energy absorbed per unit area was calculated
                                   at the point of specimen fracture. The morphology of the impact fracture surface was
                                   observed with SEM to clarify the fracture mechanism. Figure 18 shows that the impact
                                   fracture toughness of the specimens increased by approximately 20% after the T6 heat
                                   treatment. However, due to the composite effect of microcracks and the matrix softening
                                   caused by the erosion, the impact toughness of the specimens decreased. Comparing group
                                   F and FE, as well as group FH and FHE, respectively, the impact toughness decreased by
                                   about 11%. The surface morphology of the region near the starting point of the fracture was
                                   inspected using SEM (Figure 19). The F group of specimens exhibited superior ductility,
                                   and their fracture-induced dimples were smaller and denser than those of the FH group of
                                   specimens. Compared with the characteristics of tensile failure, the specimens are subjected
                                   to the shear force, which is rapid and parallel to the fracture surface during the impact,
                                   so that the specimens of groups FE and FHE have the same cracking wave pattern as the
                                   impact direction. After erosion, the surface layer of the SLM Al-10Si-Mg alloy was softened
                                   at high temperatures, and the microcracks induced by erosion directly decreased Young’s
Nanomaterials 2021, 11, x FOR PEER REVIEW
                                   modulus of the material, thus leading to a decrease in the impact toughness of the15SLM  of 17
                                   Al-10Si-Mg alloy.

                               Figure   18.Impact
                                Figure18.   Impacttoughness
                                                     toughnessofofspecimens
                                                                   specimensfrom
                                                                              fromeach group
                                                                                    each     before
                                                                                         group      (F, (F,
                                                                                               before   FH)FH)
                                                                                                            andand
                                                                                                                afterafter
                                                                                                                       (FE,(FE,
                                                                                                                            FHE) erosion
                                                                                                                                FHE) ero-
                               in terms
                                sion     of theofenergy
                                     in terms           absorbed
                                                  the energy       per unit
                                                             absorbed   perarea.
                                                                            unit area.
Nanomaterials 2021, 11, 2131                                                                                                     15 of 17
                                                Figure 18. Impact toughness of specimens from each group before (F, FH) and after (FE, FHE) ero-
                                                sion in terms of the energy absorbed per unit area.

                                  Figure 19. Impact fracture surfaces of the (a) F, (b) FE, (c) FH, and (d) FHE groups of specimens.
                               Figure 19. Impact fracture surfaces of the (a) F, (b) FE, (c) FH, and (d) FHE groups of specimens.

                               4. Conclusions
                               (1)   After the T6 heat treatment of SLM Al-10Si-Mg alloy, the supersaturated silicon solid
                                     redissolved into the aluminum matrix and formed strengthening Mg2 Si nanopre-
                                     cipitates in the aluminum matrix. The SLM process produced extremely fine grains
                                     with high hardness. After the T6 heat treatment, the microstructure of the material
                                     changed, and stress was released, which reduced the hardness of the material.
                               (2)   The maximum and minimum erosion rates of the F and FH groups of specimens
                                     occurred at 30◦ and 90◦ , respectively. The erosion fracture was dominated by the
                                     ductile cutting mechanism. The T6 heat treatment improved the ductility of the
                                     material and generated strengthening Mg2 Si nanoprecipitates, which can improve
                                     the wear resistance of the material.
                               (3)   The tensile strength of the SLM Al-10Si-Mg alloy decreased after erosion. The high
                                     surface temperature induced by particle impingement softened the aluminum matrix
                                     and increased the elongation significantly. Moreover, erosion of the die reduced
                                     Young’s modulus and impact toughness of the SLM Al-10Si-Mg alloy.

                               Author Contributions: Methodology, B.-C.H.; investigation, B.-C.H.; data curation, B.-C.H.; writing—
                               original draft preparation, B.-C.H.; writing—review and editing, F.-Y.H.; supervision, F.-Y.H. All
                               authors have read and agreed to the published version of the manuscript.
                               Funding: This research received no external funding.
                               Institutional Review Board Statement: Not applicable.
                               Informed Consent Statement: Not applicable.
                               Data Availability Statement: The data presented in this study are available on request from the
                               corresponding author.
                               Acknowledgments: The authors are grateful to the Instrument Center of National Cheng Kung
                               University and the Ministry of Science and Technology of Taiwan (Grant No. MOST 108-2221-E-006-
                               140-MY3) for their financial support.
                               Conflicts of Interest: The authors declare no conflict of interest.
Nanomaterials 2021, 11, 2131                                                                                                          16 of 17

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