From Prototyping to Serial Production - 3D-Printing in Ceramic Manufacturing

 
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From Prototyping to Serial Production - 3D-Printing in Ceramic Manufacturing
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From Prototyping to Serial Production –
3D-Printing in Ceramic Manufacturing

F. Raether, J. Vogt

For two decades, Additive Manufacturing (AM) was used mainly for the rapid prototyping of visual or
functional models. However, with growing awareness of its potential and increasing performance of
3D-printers, it becomes more and more relevant for small- and medium-scale production. Quality Man­
agement (QM) was no major issue in the period of prototyping but – besides production cost, process
­integration and automation – it becomes a key enabling factor for the implementation of AM methods
 in industrial production. It turns out that several challenges are to be met especially by ceramic AM to
 comply with customary manufacturing methods.

1 Introduction                                     in the small scale production of ceramic       thermal stress and damage in ceramic parts.
There are five main reasons for the strong         parts.                                         For that reason, powder bed fusion and dir­
growth of AM in component production:           The growing variety of AM methods has             ected energy deposition have only minor
• It enables extremely lightweight construc­   been classified in seven main categories:         importance in the AM-based production of
  tions, saving energy in transportation and    Powder bed fusion, directed energy depos­         ceramics. The remaining five categories still
  heating technology (Fig. 1 a).                ition, material jetting, material extrusion,      include a multitude of methods and vari­
• It can substitute complex constructions      sheet lamination, binder jetting and vat          ations, reflecting the ingenuity of engineers
  customarily fabricated from many individ­     photopolymerisation (ISO 17296-1). The            all over the world. However, this diversity
  ual components by integration in a single     first two of these categories comprise            can drive quality managers to despair.
  piece, saving assembly costs (Fig. 1 b).      ­single stage processes, where forming and
• It can be used for the manufacturing of       densification is done simultaneously. The        2 Quality management with
  individual components and is of particu­       other five categories require two stages in      AM of ceramics
  lar interest for the replacement of bones,     ceramic 3D-printing. In the first stage, green   When ceramic parts are fabricated by AM,
  teeth or organ parts in medical engineer­      parts are formed, and in a second stage, the     several challenges are to be met to achieve
  ing.                                           green parts are processed in a subsequent        high strength and reliability as well as net
• It allows for the production on demand,       heat treatment to obtain the final products.     shape performance. As usual, strength and
  enabling new routes in logistics and spare     Recent reviews on AM of ceramics can be          reliability are controlled by microstructure
  parts supply.                                  found in [1, 2].                                 homogeneity and surface roughness. Both
• It eliminates the manufacture of expen­       In one stage AM processes, high tempera­         are harder to achieve with AM than with
  sive moulds, which is extremely important      ture gradients are applied, creating high        standard production. Deformation during

  Friedrich Raether, Joachim Vogt
  Fraunhofer Center for High Temperature
  Materials and Design (HTL)
  95448 Bayreuth
  Germany

  Corresponding author: F. Raether
  E-mail: friedrich.raether@isc.fraunhofer.de

  Keywords: additive manufacturing,
  3D-printing, industrial production,           Fig. 1 a–b Ceramic parts produced by 3D-printing: a) lightweight container for heat
  quality management                            treatment of ceramic fibres; b) high temperature sensor for simultaneous measurement
                                                of gas flow and temperature

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                                                                                                   plementation of AM in production started
                                                                                                   with polymers, followed by metals and is
                                                                                                   in an early stage in the case of ceramics.
                                                                                                   This chronology is reflected by the number
                                                                                                   of AM standards available for AM with dif­
                                                                                                   ferent materials.
                                                                                                   So far, no specific standard for ceramic 3D-
                                                                                                   printing exists. However, a number of gener­
                                                                                                   al standards can be used, e.g.: ISO 52910-
                                                                                                   17 for DFAM, ISO 52915-16 for file formats,
                                                                                                   ISO 52921-13 for coordinate systems and
                                                                                                   test methodologies. Furthermore, a new
                                                                                                   VDI guideline on the DFAM of ceramics (VDI
                                                                                                   3405 Sheet 3.6) is currently in preparation
                                                                                                   [4].
                                                                                                   In the following sections, we address some
                                                                                                   general aspects of quality control in 3D-
Fig. 2 Survey on quality issues related to 3D-printing of ceramics
                                                                                                   printing of ceramics which are relevant
                                                                                                   beyond individual AM methods. First of all,
sintering impairs net shape performance. In        overhanging parts requiring support struc­      the control of green compact quality is out­
addition, with direct printing techniques, i.e.    tures during printing and sintering. Design     lined, followed by the heat treatment and
material jetting and material extrusion, net       for Additive Manufacture (DFAM) becomes         final component inspection.
shape performance often is deteriorated by         a separate discipline among the traditional
deviations during the printing process itself.     Design for Manufacturing and Assembly           3 Control of green compact
An in-line dimensional control of printed          (DFMA).                                         quality
parts, which is used in a closed loop, is          Specific software is available to support       Since nearly all ceramic AM techniques
rarely used but would be strongly recom­           construction engineers [3]. However, spe­       are two-stage processes, first of all green
mended. Since the feedstock has to ful­            cialists in the field of DFAM are rare, and     compacts are formed, which are available
fil additional requirements compared to            the majority of engineers need professional     for quality inspection. Yet, AM forming pro­
standard production, feedstock inspection          development to utilise the full potential of    cesses are more complex than customary
is a critical issue in quality management          AM. Other specific issues affect the process­   forming processes.
of AM processes (Fig. 2). Happily, numer­          ing, plant monitoring and final inspection      Considering this, it is very helpful to opti­
ous well suited methods, e.g. rheological          (compare Fig. 2).                               mise 3D-printing parameters and feedstock
measurements, are available for feedstock          Depending on its field of application, AM       properties on the basis of key figures de­
control.                                           has to fulfil the same standards as custom­     rived from the green compacts. In doing so,
AM in particular offers completely new de­         arily production processes, e.g. EN/AS 9100     the subsequent heat treatment can be de­
sign possibilities, e.g. freeform surfaces, grid   in aerospace, IATF 16949 in the automotive      veloped separately (compare next section)
structures, undercuts and cavities. On the         industry and ISO 13485 in medical technol­      – reducing the complexity of the entire pro­
other hand, special restrictions exist, e.g.       ogy. Due to its technical complexity, the im­   cess development considerably. The criteria
                                                                                                   for green compact quality are the same as
                                                                                                   for customary forming: close match to set
                                                                                                   shape, homogenous and dense packing of
                                                                                                   ceramic particles, homogenous distribution
                                                                                                   of the binder, smooth surfaces and absence
                                                                                                   of flaws like voids or delaminations.
                                                                                                   Therefore, in principle the same methods can
                                                                                                   be used for characterisation of AM green
                                                                                                   compacts as those with standard processes
                                                                                                   [5]. However, due to the complex geom­etry
                                                                                                   of AM green parts, measuring shape usually
                                                                                                   is more complicated than with green parts
                                                                                                   from standard forming processes.
Fig. 3 a–b Measurement of homogeneity and layer structure of 3D-printed alumina                    This suggests using Computed Tomography
green compacts: a) cross section of a part produced by binder jetting measured by com-             (CT) as a non-contact method, which can
puted tomography; b) cross section of a part produced by vat photopolymerisation and               measure any shape, e.g. very fine struts
measured by scanning electron microscopy after cross section polishing                             or cavities. In addition, micro- or nano-CT

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Fig. 4 Heat and mass flow during debinding                                  Fig. 5 Work flow during systematic optimisation of debinding
                                                                            cycles

detects flaws and rough structures at the          to resolve details of microstructure. By         Yet, these structures are one of the most
parts’ surfaces.                                   means of cross section polishing, a clean        powerful characteristics of AM components.
Moreover, CT can be used to analyse special        cut through the green compact can be ob­         In order to overcome difficulties with heat
structural features occurring with AM. There       tained. Scanning Electron Microscopy (SEM)       treatment, a systematic approach is re­
are three two-stage AM techniques using            is used to investigate the structure with        quired which is outlined in the following
a layerwise building of the 3D-structure:          high resolution (Fig. 3 b). It can be observed   paragraphs separately for debinding and
sheet lamination, binder jetting and vat           that the particle density between the layers     sintering.
photo­ poly­merisation. Structuring is done        is lower. The overall homogeneity is much        The thermal decomposition and combustion
within the layers, after the entire com­pon­       higher than in case of binder jetting, being     of binder and other organic constituents
ent has been divided into slices. In any case,     typical for slurry based AM processes. The       during debinding is accompanied by endo­
the interface between the layers deserves          same key figures as discussed with CT in         thermic and exothermic processes, com­
special attention.                                 the previous paragraph are extracted from        bined with enhanced gas pressure within
Fig. 3 a shows a vertical cross section            the SEM images. These can be used for an         the pore channels of the green compact
through an alumina green part from a CT            optimisation of rheology of the feedstock        during outward flow of gaseous pyrolysis
measurement. The part was fabricated via           and the printing parameters. Basically, the      products (Fig. 4). Temperature gradients and
binder jetting, using a dry alumina powder         mentioned principles for green compact in­       overpressure lead to local stress concentra­
which was spread in a building chamber             spection can also be applied to the other        tion and failure if the corresponding stresses
layer by layer and selectively impregnated         two-stage AM processes for ceramics.             exceed the strength of the compacts.
with a binder [6]. In this process, only flow­                                                      Debinding can be simulated in a Finite
able powders can be used, limiting the par­        4 Quality issues during                          Elem­ent (FE) model, in which pyrolysis and
ticle size to coarse powders with a diameter       heat treatment                                   combustion reactions, gas flow within the
above 10 µm.                                       In principle, the issues occurring during        pore channels and at the surfaces, and heat
It can be seen that the interface between          debinding and sintering of 3D-printed parts      flow and heat production/consumption due
the layers has a lower density, which is at­       are similar to customary green compacts.         to these reactions are combined (Fig. 5).
tributed to insufficient filling of pores in the   Nevertheless, the optimisation of heat treat­    Based on the temperature and pressure dis­
top layer when the next layer is set up on         ment is often more difficult.                    tribution, mechanical stresses are calculat­
top. The variation in X-ray density in the         Depending on the AM process, debinding           ed during the entire debinding cycle. Based
vertical direction is a measure for the inter­     requires special care due to high binder         thereon, debinding cycles are adapted to
layer homogeneity, while the variation of          concentration and/or low adhesion be­            ensure that stresses are always well below
X-ray density in the horizontal direction is       tween layers, which frequently causes de­        the strength limit.
a key figure for the overall microstructure        lamination or cracking.                          In order to achieve a sufficient accuracy of
homogeneity. Equations and interpretation          Sintering is often complicated in AM pro­        the simulation, a certain amount of experi­
for this quantity are given in [7].                cesses with a lower green density such as        mental data is required (compare Fig. 5).
Fine ceramic particles with diameters below        binder jetting when compared to customary        Standard thermal analysis, simultaneously
1 µm can be used in slurry based processes         forming processes. This leads to enhanced        using thermogravimetry, differential scan­
like vat photopolymerisation [6]. In this          shrinkage and warping, mostly superim­           ning calorimetry and mass spectrometry
case, slurry layers are applied in the vat and     posed by an anisotropic shrinkage. Dis­tort­     (TG-DSC-MS) delivers input for very small
select­ively cured by light. The resolution of     ions of shape are especially serious in case     samples, which correspond to individual
most CT devices however is not sufficient          of complex and filigree structures.              elem­ents in the later FE simulations.

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                                                                                                 binder jetting with a silicon melt, e.g., has
                                                                                                 been used for some years to produce high
                                                                                                 temperature components [13]. The contain­
                                                                                                 ers shown in Fig. 1 a are fabricated in the
                                                                                                 same way. The advantage of melt infiltration
                                                                                                 is the avoidance of shrinkage and sintering
                                                                                                 distortions. It is especially useful for green
                                                                                                 parts with low sintering activity, as they are
                                                                                                 typical for binder jetting. Melt infiltration
                                                                                                 processes can be optimised by in situ meas­
                                                                                                 urement and FE simulations as well [14].

                                                                                                 5 Final inspection of
Fig. 6 a–b Non-standard equipment required for data acquisition of debinding
                                                                                                 AM components
­optimisation: a) thermooptical measuring furnace equipped with weight sensor, bells for         Dimensional inspection is one of the most
 sound emission measurement and an optical beam path for dimension measurement;                  important tasks in quality control of AM
 b) multi-sample-holder for 4-point bending strength tests on six partially debinded             parts. However, compared to customary
 specimens                                                                                       measuring, it becomes more difficult when
                                                                                                 dealing with complex structures with cav­
Specific thermooptical measuring (TOM)           A validation of the methodology as stated       ities etc. CT can be used as a universal tool
furnaces are used to measure larger              above was already published previously          for dimensional control, independently of
samples and to obtain other quantities           [8], and examples for 3D-printing will be       structural constraints. In using special algo­
(Fig. 6 a). TOM methods are also relevant        published soon. The methodology is con­         rithms, the deviation between actual geom­
for the validation of simulations by sound       sidered powerful, since it can be applied       etry and target geometry can be quantita­
emission measurements, sensitively detect­       to any shape, once the model with the           tively measured.
ing cracks in the samples during the thermal     parametrized material data has been set up.     Fig. 7 shows as an example a sintered
cycle. Additional material properties have to    If the shape is simple and component di­        acoustic bell out of alumina for sound
be measured to obtain a sufficient data          mensions are small, simplified methods are      emission meas­urements produced by vat
base for a realistic simulation of debinding     available. They are based on a formal kinetic   photopolymerisation (compare section 4).
(compare Fig. 5).                                approach for debinding and need much less       Sintering deformations were calculated ac­
A delicate task is the mechanical testing of     experimental and numerical effort [9, 10].      cording to section 4. Deviations are indicat­
partially debinded samples, since they are       However, for more complicated parts these       ed by a colour code. From this, key figures
very fragile. A multi-sample-holder (Fig. 6 b)   simple methods cannot identify optimum          for quality control and process optimisation
and highly sensitive load cell are used to       debinding conditions. The effort in obtain­     can be derived. Likewise, internal defects
measure these samples at different tem­          ing additional data for the accurate model      can be detected. The measured structures –
peratures.                                       rapidly pays off, if different components are   including large defects – are transferred to
                                                 manufactured from the same feedstock.           FE models where loads are applied to check
                                                 A similar approach, i.e. an experiment-         for significant impairments of application
                                                 based continuum FE model, has also been         properties.
                                                 developed for the simulation of sintering.      Frequently, attractive sculptures are printed
                                                 Input data for sintering are shrinkage, ther­   as demonstrators for the capability of AM
                                                 mal diffusivity and viscous material prop­      (Fig. 8 a). However, they are rarely suited
                                                 erties. Again, special TOM furnaces were        for a quantitative comparison of dimen­
                                                 developed to obtain these data [11]. The        sional tolerances. Instead, test geometries
                                                 FE model combines temperature field, sin­       are proposed, for which CAD files can be
                                                 tering kinetics and mechanical stresses. It     downloaded on the internet [15]. These
                                                 also considers gravity and friction, which is   test structures are designed for the evalu­
                                                 important for sintering of 3D-printed parts.    ation of thin walls, stairs, angles, needles,
                                                 A detailed description of the model and its     holes etc. within 3D-printed structures. As
                                                 validation was published recently [12].         an example, Fig. 8 b shows an alumina test
                                                 Sometimes, in order to obtain dense parts,      structure printed by vat photopolymerisa­
                                                 the infiltration of the porous compacts         tion simultaneously checking several struc­
Fig. 7 Difference between set geometry           with a melt is an interesting alternative to    tural features.
and final shape of an alumina bell               sintering. Thereby, the melt is soaked into     The surface roughness of AM parts can be
(height 54 mm) produced by vat                   the pore channels by capillary forces. The      critical due to stress concentration and also
­photopolymerisation                             infiltration of SiC parts manufactured by       for aesthetic reasons. It can be measured

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by laser scanning microscopy nearly inde­
pendently of the surface shape. At the HTL,
in-house software is used to extract several
key figures to estimate local stress concen­
tration. As with CT data, the surface scans
can be transferred to FE models, in which
they are evaluated in terms of allowed
stresses. If surfaces are not smooth enough
or dimensional tolerances are very strict,
machining is unavoidable. For that purpose,
                                                Fig. 8 a–b Alumina components made by vat photopolymerization: a) sculpture of Rich-
automated machining centres with five axes      ard Wagner, a famous composer from the city of Bayreuth; b) standard test geometry
are available which can adjust freeform sur­
faces to set shapes.

6 Future trends
In addition to product quality, costs are a
key performance indicator for use of AM in
ceramic production. They are affected by
throughput and production time. The bottle
neck for throughput usually are the prep­ar­
ation of the printing process, the 3D-print­
ing process itself and the post-processing of
the parts. Since the subsequent heat treat­
ment can be performed in large furnaces
handling many parts in parallel, it usually
doesn’t affect throughput.
On the other hand, the limiting factor for
                                                Fig. 9 Setup of a FFS printer at the HTL and schema illustrating the FFS printing process
production time often is the heat treatment,
especially when long debinding steps are
required. Production time is an important       nificantly reduced by process automation          ited by sintering, where a careful adaption
issue for production on demand, allowing        and the integration of the respective equip-      of shrinkage properties is required. Other­
new business models with higher added           ment.                                             wise problems occur, which are well known
value.                                          New AM methods arise with an increasing           from the co-firing of multilayer structures. It
Optimisation of debinding as outlined in        frequency. Among them, two step methods           is estimated that the initial enthusiasm and
chapter 4 is essential for utilising this po­   based on ceramic slurries are most relevant       the current disillusion with respect to intro­
tential. Avoiding costly finishing processes    for ceramic production. Slurries enable           duction of AM in ceramic production will be
by net shape printing and sintering pro­        small particles and particle mixtures and         replaced by selective use of AM in custom­
cesses is a cost-relevant topic as well. The    lead to relatively high green densities. Up       ized production of small series. AM meth­
sintering optimisation methods indicated in     to now, the highest resolution is obtained        ods and printers can be carefully selected
chapter 4 can be used to minimise shape         using two-photon polymerization [16] and          according to the specific production task.
deviations. Other important cost factors are    highest homogeneity was measured with             The growth rate of AM in ceramic produc­
raw materials.                                  local electrophoretic deposition [17].            tion will be controlled by quality and cost of
Today, feedstocks for 3D-printing are much      The latter requires a lot of work for practical   AM processes.
more expensive than standard raw mater­         use, yet. Layerwise Slurry Deposition (LSD)
ials. Recycling of unused feedstock is an       [2] and Free Flow Structuring (FFS) [18] are      Acknowledgement
important cost factor in all powder bed         promising slurry based processes, which can       The authors gratefully acknowledge the
based AM methods. Depreciation is another       be used for larger components. Fig. 9 shows       help of T. Martini, M. Stepanyan, M. Römer
important cost factor in ceramic AM.            an FFS-printer for free-flow-deposition of a      and T. Kreutzer for help with the measure­
Typically, 3D-printers cost several hundreds    ceramic slurry on a dried powder bed. LSD         ments.
of thousand euros. Nevertheless, there is a     and FFS can be used for multi-material
strong trend to smaller and cheaper devices     printing, e.g. by adding other materials via      References
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