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Selective Laser Melting of Net-Shaped Oxide Ceramics


                   State of the Art in Selective Laser Melting of
                   Alumina Zirconia Ceramics
                   June 2012



                   Yves Hagedorn
Outline




          Introduction
          Process Development
          Properties of Manufactured Parts
          Cost Drivers
          Conclusion
Introduction                                 SLM of Net-shaped Ceramics

Competences Rapid Manufacturing Department
 Process Development
 Qualifying Selective Laser Melting (SLM)
  for enlarging the scope of applicable
  materials
 Improving component’s quality
 Increasing productivity
 Developing systems and components


Application Development
 Qualifying Selective Laser Melting (SLM)
  for series Production
       Tooling
       Dental applications
       Medical implants
       Turbo machinery
       Mechanical engineering
                                                                          3
Introduction                             SLM of Net-shaped Ceramics

Selective Laser Melting (SLM) for Ceramics
 Principle




  3D-CAD Model
     in slices



                                                      Complex, net-
                                                      shaped part in
                                                      series material




  Powder material


                                                                        4
Introduction                                            SLM of Net-shaped Ceramics

SLM Readily Applied in Industry
 Some Industrial Applications
 for Metals

 Tooling                 Spacecrafts             Medical




                         © GFE Inno-Shape


 Undercuts               Complexity              Individuality
  Internal structures    Filigree structures    Tool-less production
   as cooling channels     without joining         of customized parts



                                                                                     6
Introduction                                    SLM of Net-shaped Ceramics

SLM for Ceramics
 Advancements in SLM Allow for
 Fabrication of 3D Ceramics

Positive Material       SLM                     Industrial
Properties              Manufact. Process       Application
+ Mechanical Strength   + Tool - Free           Medical Applications
+ Wear Resistance       + Complex Geometries     Dental Restorations
+ Thermal Resistance    + Fast                   Implants
+ Bio-Compatible        + High Material Yield
+ Esthetics             + Cost Efficient        High-Tech Applications
                                                 Aerospace
                                                 Automotive




                                                                             7
Introduction                                                  SLM of Net-shaped Ceramics

Selective Laser Melting (SLM) for Ceramics
 Main Objective
 Development of SLM process for ceramics


Current Application
 Framework for dental restorations from
  alumina / zirconia compounds



    Exploitation of high material strength


    Improved esthetics compared to Cr/Co

                                             ® BEGO Medical 2002                           8
Outline




          Introduction
          Process Development
          Properties of Manufactured Parts
          Cost Drivers
          Conclusion
Process Development                                              SLM of Net-shaped Ceramics

The System Al2O3 / ZrO2
 Eutectic System
 Utilization of eutectic powder ratio



    Simultaneous crystallization of
    alumina / zirconia crystals




    Fine-grained microstructure



                                         S. M. Lakiza and L. M. Lopato. J.Am.Ceram.Soc.80 (1997), 893- 902

                                                                                                        10
Process Development                      SLM of Net-shaped Ceramics

SLM for Ceramics
 Approach
 Complete melting of ceramic material



    High densities




    High strength




                                                                  11
Process Development                  SLM of Net-shaped Ceramics

SLM for Ceramics
 First results
 High density
 Micro-cracks throughout material


    High thermal gradients during
    selective melting




    Low strength of manufactured
    objects (10 MPa)




                                                              12
Process Development                                          SLM of Net-shaped Ceramics

SLM for Ceramics
 Experimental Setup I/II              Homogenisation   Scanner
                                      optics

 CO2 laser-preheating
                                                                        Nd:YAG-laser

                                                             Focussing optics

                                                                                Pyrometer
    Decrease of thermal gradients
    during selective laser melting   CO2 -laser beam                                Powder distribution
                                     (preheating)

                                     Heat                                             Powder reservoir
                                     isolation


                                                                  Substrate
    Crack-free specimens                 SLM part                Building
                                                                 plattform




                                                                                                     13
Process Development         SLM of Net-shaped Ceramics

SLM for Ceramics
 Experimental Setup II/II




                                                     14
Process Development             SLM of Net-shaped Ceramics

Experimental Conduction
 Thermal Image
 High-Temperature preheating



    Preheating temperature
    ~ 1800°C




    Homogenous temperature
    distribution




                                                         15
Process Development                                            SLM of Net-shaped Ceramics

Experimental Challenges




                    High Density
               1      > 99 %

                    Crack free specimens
               2      High-temperature pre-heating

                    High Mechanical Strength
               3      > 500 MPa (DIN Norm for dental restorations)

                    High Surface Quality
               4      Rz < 100 µm (own specification)




                                                                                        16
Outline




          Introduction
          Process Development
          Properties of Manufactured Parts
          Cost drivers
          Conclusion
Properties of Manufactured Parts   SLM of Net-shaped Ceramics

Density & Powder
 Spherical Powder
 Excellent flowing ability



    Full density


    No crack formation




                                               1 mm
                                                            18
Properties of Manufactured Parts           SLM of Net-shaped Ceramics

Microstructure
SEM Image
 Al2O3 matrix (dark)

 Dendritic structure of ZrO2
  crystals (bright)

 Tunable fine-grained
  microstructure




    Complete melting of ceramic material
                                                                    19
Properties of Manufactured Parts                                            SLM of Net-shaped Ceramics

High-temperature Creep                                        Creep of Alumina / Zirconia Material
 Sintered vs. SLM                               30,00%



 Loading with 200 g                            25,00%
                                                                                                             SLM
                                                20,00%
 Eutectic material ratio




                                   Elongation
                                                15,00%


 Max. elongation ~ 24%                         10,00%
                                                                                                             Sintered
                                                5,00%


                                                0,00%
                                                         1600°C/2h 1650°C/2h 1650°C/4h 1700°C/2h 1700°C/4h
                                                                      Temperature/time

                                       This Analysis has been performed by Innalox bv, Netherlands




    SLM material shows decreased creep compared to sintered material
                                                                                                              20
Properties of Manufactured Parts                            SLM of Net-shaped Ceramics

XRD Analysis
 Crystallographic distribution
 Tetragonal ZrO2 crystals

 Phase shift ZrO2:
  tetragonal  monoclinic




                                            This Analysis has been performed by TNO Science and
                                            Industry, Netherlands




    Self healing abilities of ZrO2 persist despite complete melting
                                                                                           21
Properties of Manufactured Parts                    SLM of Net-shaped Ceramics

Mechanical Strength
Test Samples
 Eutectic material ratio

 Dimensions: ø 18 mm x 2.5 mm

 Flexural strength > 500 MPa

 Flexural strength of sintered
  material > 1000 MPa
                                                      Load
                                         Specimen




                                                                    Support
    Mechanical strength sufficient for                r = 5 mm
    dental restorations (DIN Norm)                                            22
Properties of Manufactured Parts                       SLM of Net-shaped Ceramics

Mechanical Strength




     Conventionally     10 mm               SLM                    10 mm

    Max. load 2299 N                       Max. load 1435 N
    Material:        ZrO2                  Material:         Al2O3/ZrO2
    Rz value:        ~ 10 µm               Rz value:         ~ 100 µm


    Minimum load for application  1000 N


    Sufficient strength for application despite weaker material and poor
    surface quality                                                             23
Properties of Manufactured Parts          SLM of Net-shaped Ceramics

Surface Quality
 Dimensional Accuracy
 Milled part ~ 50 µm

 SLM part ~ 150 µm




                                                          5 mm




    Accuracy not sufficient for fitting
                                                                   24
Properties of Manufactured Parts                       SLM of Net-shaped Ceramics

Surface Quality
 Scanning Strategy
                                                                      Hatch
 Large melt pool due to high
  temp. preheating

 Contour / hatch                                                      Contour

 Impact on surface quality                                            Contour
     Contour parameters                                                spacing
     Contour spacing




    Improved surface quality due to small melt pool size at contour
                                                                                25
Properties of Manufactured Parts          SLM of Net-shaped Ceramics

 Surface Quality
  Contour Parameters I/II




                             Rz ~ 112 µm                       2 mm
                             Sa ~ 54 µm
Laser output:     150 W
Scanning speed:   250 mm/s



                                                                      26
Properties of Manufactured Parts                     SLM of Net-shaped Ceramics

 Surface Quality
  Contour Parameters II/II




                             Rz ~ 60 µm                                   2 mm
                             Sa ~ 14 µm
Laser output:     40 W
Scanning speed:   120 mm/s


       Surface quality strongly depends on geometry
                                                                                 27
Properties of Manufactured Parts                    SLM of Net-shaped Ceramics

Demonstration Object
 Improved Surface Quality
 Surface roughness Rz < 100 µm

 Further improvements foreseen
  (Rz < 50 µm)



                                                                        10 mm




    Employment of SLM for ceramic dental restorations
    possible

    New challenging applications needed
                                                                             28
Outline




          Introduction
          Process Development
          Properties of Manufactured Parts
          Cost Drivers
          Conclusion
SLM of Net-shaped Ceramics

   Cost drivers SLM Ceramics
                                                                                   Assumptions
                                  50

                                          Milled part ~ 30 €                         Powder (200 €/kg)
Cost of dental restoration in €




                                  40

                                                                                     Electricity (20 kWh)
                                  30

                                                                                     Depreciation (5 years)
                                  20

                                                                                     Manufacturing time (20 h/50 parts)
                                  10
                                                     SLM part 22 €                   Personnel costs (25 Euro/h)
                                  0
                                   -100   -50    0      50     100     150   200     Total investment (450 000 Euro)
                                                Relative change in %


                                  SLM is competitive compared to milled dental restorations
                                                                                                                       30
Outline




          Introduction
          Process Development
          Properties of Manufactured Parts
          Cost Drivers
          Conclusion
SLM of Net-shaped Ceramics

Conclusion




                  First Bridges Produced
             1    Sufficient strength, fitting subject to improvements

                  Great Environmental Gain
             2    20 crowns  50 g material

                  Great Economical Gain
             3    Forming & densification  1 process step

                  Possible new Applications
             4     Increased thermal stability




                                                                                      32
SLM of Net-shaped Ceramics




Thank you for your attention!
                       The research was partly funded by the
                       European 6th framework project „Custom
                       IMD“




Thanks to our project partners!


Dipl.-Ing. Dipl.-Wirt.-Ing. Yves Hagedorn M.Sc.
Tel.: +49-(0)241-8906-674
Fax: +49-(0)241-8906-121
Hagedorn@ilt.fraunhofer.de
www.ilt.fraunhofer.de
                                                                                         33

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Yves Hagedorn - Fraunhofer Institute for Laser Technology

  • 1. Selective Laser Melting of Net-Shaped Oxide Ceramics State of the Art in Selective Laser Melting of Alumina Zirconia Ceramics June 2012 Yves Hagedorn
  • 2. Outline Introduction Process Development Properties of Manufactured Parts Cost Drivers Conclusion
  • 3. Introduction SLM of Net-shaped Ceramics Competences Rapid Manufacturing Department Process Development  Qualifying Selective Laser Melting (SLM) for enlarging the scope of applicable materials  Improving component’s quality  Increasing productivity  Developing systems and components Application Development  Qualifying Selective Laser Melting (SLM) for series Production Tooling Dental applications Medical implants Turbo machinery Mechanical engineering 3
  • 4. Introduction SLM of Net-shaped Ceramics Selective Laser Melting (SLM) for Ceramics Principle 3D-CAD Model in slices Complex, net- shaped part in series material Powder material 4
  • 5. Introduction SLM of Net-shaped Ceramics SLM Readily Applied in Industry Some Industrial Applications for Metals Tooling Spacecrafts Medical © GFE Inno-Shape Undercuts Complexity Individuality  Internal structures  Filigree structures  Tool-less production as cooling channels without joining of customized parts 6
  • 6. Introduction SLM of Net-shaped Ceramics SLM for Ceramics Advancements in SLM Allow for Fabrication of 3D Ceramics Positive Material SLM Industrial Properties Manufact. Process Application + Mechanical Strength + Tool - Free Medical Applications + Wear Resistance + Complex Geometries  Dental Restorations + Thermal Resistance + Fast  Implants + Bio-Compatible + High Material Yield + Esthetics + Cost Efficient High-Tech Applications  Aerospace  Automotive 7
  • 7. Introduction SLM of Net-shaped Ceramics Selective Laser Melting (SLM) for Ceramics Main Objective  Development of SLM process for ceramics Current Application  Framework for dental restorations from alumina / zirconia compounds Exploitation of high material strength Improved esthetics compared to Cr/Co ® BEGO Medical 2002 8
  • 8. Outline Introduction Process Development Properties of Manufactured Parts Cost Drivers Conclusion
  • 9. Process Development SLM of Net-shaped Ceramics The System Al2O3 / ZrO2 Eutectic System  Utilization of eutectic powder ratio Simultaneous crystallization of alumina / zirconia crystals Fine-grained microstructure S. M. Lakiza and L. M. Lopato. J.Am.Ceram.Soc.80 (1997), 893- 902 10
  • 10. Process Development SLM of Net-shaped Ceramics SLM for Ceramics Approach  Complete melting of ceramic material High densities High strength 11
  • 11. Process Development SLM of Net-shaped Ceramics SLM for Ceramics First results  High density  Micro-cracks throughout material High thermal gradients during selective melting Low strength of manufactured objects (10 MPa) 12
  • 12. Process Development SLM of Net-shaped Ceramics SLM for Ceramics Experimental Setup I/II Homogenisation Scanner optics  CO2 laser-preheating Nd:YAG-laser Focussing optics Pyrometer Decrease of thermal gradients during selective laser melting CO2 -laser beam Powder distribution (preheating) Heat Powder reservoir isolation Substrate Crack-free specimens SLM part Building plattform 13
  • 13. Process Development SLM of Net-shaped Ceramics SLM for Ceramics Experimental Setup II/II 14
  • 14. Process Development SLM of Net-shaped Ceramics Experimental Conduction Thermal Image  High-Temperature preheating Preheating temperature ~ 1800°C Homogenous temperature distribution 15
  • 15. Process Development SLM of Net-shaped Ceramics Experimental Challenges  High Density 1 > 99 %  Crack free specimens 2 High-temperature pre-heating  High Mechanical Strength 3 > 500 MPa (DIN Norm for dental restorations)  High Surface Quality 4 Rz < 100 µm (own specification) 16
  • 16. Outline Introduction Process Development Properties of Manufactured Parts Cost drivers Conclusion
  • 17. Properties of Manufactured Parts SLM of Net-shaped Ceramics Density & Powder Spherical Powder  Excellent flowing ability Full density No crack formation 1 mm 18
  • 18. Properties of Manufactured Parts SLM of Net-shaped Ceramics Microstructure SEM Image  Al2O3 matrix (dark)  Dendritic structure of ZrO2 crystals (bright)  Tunable fine-grained microstructure Complete melting of ceramic material 19
  • 19. Properties of Manufactured Parts SLM of Net-shaped Ceramics High-temperature Creep Creep of Alumina / Zirconia Material Sintered vs. SLM 30,00%  Loading with 200 g 25,00% SLM 20,00%  Eutectic material ratio Elongation 15,00%  Max. elongation ~ 24% 10,00% Sintered 5,00% 0,00% 1600°C/2h 1650°C/2h 1650°C/4h 1700°C/2h 1700°C/4h Temperature/time This Analysis has been performed by Innalox bv, Netherlands SLM material shows decreased creep compared to sintered material 20
  • 20. Properties of Manufactured Parts SLM of Net-shaped Ceramics XRD Analysis Crystallographic distribution  Tetragonal ZrO2 crystals  Phase shift ZrO2: tetragonal  monoclinic This Analysis has been performed by TNO Science and Industry, Netherlands Self healing abilities of ZrO2 persist despite complete melting 21
  • 21. Properties of Manufactured Parts SLM of Net-shaped Ceramics Mechanical Strength Test Samples  Eutectic material ratio  Dimensions: ø 18 mm x 2.5 mm  Flexural strength > 500 MPa  Flexural strength of sintered material > 1000 MPa Load Specimen Support Mechanical strength sufficient for r = 5 mm dental restorations (DIN Norm) 22
  • 22. Properties of Manufactured Parts SLM of Net-shaped Ceramics Mechanical Strength Conventionally 10 mm SLM 10 mm Max. load 2299 N Max. load 1435 N Material: ZrO2 Material: Al2O3/ZrO2 Rz value: ~ 10 µm Rz value: ~ 100 µm Minimum load for application  1000 N Sufficient strength for application despite weaker material and poor surface quality 23
  • 23. Properties of Manufactured Parts SLM of Net-shaped Ceramics Surface Quality Dimensional Accuracy  Milled part ~ 50 µm  SLM part ~ 150 µm 5 mm Accuracy not sufficient for fitting 24
  • 24. Properties of Manufactured Parts SLM of Net-shaped Ceramics Surface Quality Scanning Strategy Hatch  Large melt pool due to high temp. preheating  Contour / hatch Contour  Impact on surface quality Contour Contour parameters spacing Contour spacing Improved surface quality due to small melt pool size at contour 25
  • 25. Properties of Manufactured Parts SLM of Net-shaped Ceramics Surface Quality Contour Parameters I/II Rz ~ 112 µm 2 mm Sa ~ 54 µm Laser output: 150 W Scanning speed: 250 mm/s 26
  • 26. Properties of Manufactured Parts SLM of Net-shaped Ceramics Surface Quality Contour Parameters II/II Rz ~ 60 µm 2 mm Sa ~ 14 µm Laser output: 40 W Scanning speed: 120 mm/s Surface quality strongly depends on geometry 27
  • 27. Properties of Manufactured Parts SLM of Net-shaped Ceramics Demonstration Object Improved Surface Quality  Surface roughness Rz < 100 µm  Further improvements foreseen (Rz < 50 µm) 10 mm Employment of SLM for ceramic dental restorations possible New challenging applications needed 28
  • 28. Outline Introduction Process Development Properties of Manufactured Parts Cost Drivers Conclusion
  • 29. SLM of Net-shaped Ceramics Cost drivers SLM Ceramics Assumptions 50 Milled part ~ 30 € Powder (200 €/kg) Cost of dental restoration in € 40 Electricity (20 kWh) 30 Depreciation (5 years) 20 Manufacturing time (20 h/50 parts) 10 SLM part 22 € Personnel costs (25 Euro/h) 0 -100 -50 0 50 100 150 200 Total investment (450 000 Euro) Relative change in % SLM is competitive compared to milled dental restorations 30
  • 30. Outline Introduction Process Development Properties of Manufactured Parts Cost Drivers Conclusion
  • 31. SLM of Net-shaped Ceramics Conclusion  First Bridges Produced 1 Sufficient strength, fitting subject to improvements  Great Environmental Gain 2 20 crowns  50 g material  Great Economical Gain 3 Forming & densification  1 process step  Possible new Applications 4 Increased thermal stability 32
  • 32. SLM of Net-shaped Ceramics Thank you for your attention! The research was partly funded by the European 6th framework project „Custom IMD“ Thanks to our project partners! Dipl.-Ing. Dipl.-Wirt.-Ing. Yves Hagedorn M.Sc. Tel.: +49-(0)241-8906-674 Fax: +49-(0)241-8906-121 Hagedorn@ilt.fraunhofer.de www.ilt.fraunhofer.de 33