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le centre collectif de l’industrie technologique belge
High Value Manufacturing

Density/porosity control of sintered 316L stainless steel
        parts shaped by additive manufacturing

                      15-11-2012



                                 le centre collectif de l’industrie technologique belge
Table of contents

       •   Porous metallic parts

       •   3D-printing Prometal process

       •   Sintering cycle

       •   Characterization

       •   Property ranges of 316L powders

       •   Examples




                                    © sirris 2007 | www.sirris.be | info@sirris.be   3
Porous metallic parts

•   Shaping by powder metallurgy  lots of parameters
     •   Porosity range from a few % to 90%
•   Application list:
     •   Filtration
     •   Distributing/dispersing/damping
     •   Airing/cooling
     •   Lightening
     •   Catalysts supports
     •   Prosthesis
•   But simple geometries (Pressing, MIM)




                                                        4
Porous metallic parts

•   Additive manufacturing  no limit in shape + integrated
    functionalities
    •   SLM            1 step
                       no control of porosity
    •   3D-printing    indirect route: shaping + sintering
                       possibility to control porous characteristics




              R10:
1000x500x280mm                                             RXD:
                                                           60x40x15mm




                                                                        5
3D- Printing Prometal Process




                                             3. Sintering
                                                    Complete

                                                        Partial
 1. Curing     2. Debinding - presintering
(green part)          (brown part)           (3’. Infiltration)




                                                                  6
Sintering cycle

•   From a powder tap to full dense material
     •   Passing by porous state
           •   Opened to 92% density, then closed


•   Evolution functions of:
     •   Initial state
           • Packing density
           • Particle size distribution
           • Particle shape
     •   Sintering conditions
           • Temperature
           • Time
           • (Atmosphere)


•    Stop at different stage to keep or eliminate porosity following
    target application


                                                                        7
Characterization

•   Density – porosity (opened and closed)  Archimedes (3 weightings)

•   Permeability k  Darcy (flux Q through thickness L and surface A under DP)

                      Q.L.µ
                 k=
                      A.∆P


•   Pore size (bubble point and Hg porosimetry)  Washburn


                    − 4.γ . cos θ
               d=
                         P



                                             © sirris 2007 | www.sirris.be | info@sirris.be   8
Property ranges for 316L powders
                                                100                                                                                                                        40
                                                                                      22µm

•   Effect of sintering T°                             95                             31µm
                                                                                      20-53µm
                                                                                                                                                                           35


    (90min at T°) for 4
                                                                                      45-90µm
                                                       90                                                                                                                  30




                                                                                                                                                                                Opened porosity (%)
                                Relative density (%)
    spherical powders                                  85                                                                                                                  25


                                                       80                                                                                                                  20


                                                       75                                                                                                                  15


                                                       70                                                                                                                  10


                                                       65                                                                                                                  5


                                                       60                                                                                                                   0
                                                         1180             1200       1220   1240     1260   1280   1300    1320    1340   1360    1380    1400   1420   1440
                                                                                                               Temperature (°C)



                                                                           0,9
Porous part        Dense part                                             0,89
                                                                          0,88                                                                           1315°
•   Effect of sintering time                                              0,87                                                                           C
                                                            Density (-)




                                                                          0,86                                                                           1335°
    at 3 T° for 31µm                                                      0,85
                                                                                                                                                         C
                                                                                                                                                         1345°
    powder                                                                0,84
                                                                          0,83
                                                                                                                                                         C

                                                                          0,82
                                                                          0,81
                                                                                 0          50       100     150     200     250        300      350
                                                                                                 Time at sintering temperature (min.)                                                                 9
Property ranges for 316L powders

                      35                                                                   1,00E-12                       •   Pore size and permeability
                               22µm
                                                                                                                              functions of opened
                                                                                                                              porosity for 4 spherical
                               31µm
                      30
                               20-53µm

                                                                                                                              powders
Mean pore size (µm)




                               45-90µm                                                     1,00E-13
                      25




                                                                                                      Permeability (m²)
                      20

                                                                                           1,00E-14

                      15                                                                                                  •   Link between parameters:
                                                                                                                               •   Powder size sets pore size
                      10
                                                                                           1,00E-15                            •   Thermal cycle sets final
                                                                                                                                   density/porosity
                       5
                                                                                                                               •    all defines permeability

                       0                                                                   1,00E-16

                                                                                                                              Main challenge: shrinkage
                           0   5         10    15       20          25   30      35   40
                                                                                                                          •
                                                                                                                              control!
                                              Opened porosity (%)




                                                                              Pore mean size
                                                                              Permeability                                                                      10
Property ranges for 316L powders

                                45-90µm powder
        Gas atomised particles                Water atomised particles

                            Sintered 90min at 1395°C




65% density – 35% opened porosity               47% density – 53% opened porosity
Mean pore size    35µm                          Mean pore size    30µm
Permeability      10-12m²                       Permeability      10-12m²


                                           © sirris 2007 | www.sirris.be | info@sirris.be   11
Examples
                                            Ø 70mm
                                            Pores 30µm
                                            Perméa. 10-12 m²




                           L 270mm
       Ø 50mm              Pores 17µm

      Pores 30µm     Perméa. 5.10-13 m²
                                                                   L 30mm
  Perméa. 10-12 m²




                                  Ø 300mm
                                                                    L 90mm
                                  Pores 35µm
                                                                   Pores 35µm
                              Perméa.   10-12   m²
                                                               Perméa. 10-12 m²   12
Thank you for your attention !




                    Bruno.Verlee@sirris.be

                                         13

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2012 11-15-high-value-manufacturing-sirris-verlee

  • 1. le centre collectif de l’industrie technologique belge
  • 2. High Value Manufacturing Density/porosity control of sintered 316L stainless steel parts shaped by additive manufacturing 15-11-2012 le centre collectif de l’industrie technologique belge
  • 3. Table of contents • Porous metallic parts • 3D-printing Prometal process • Sintering cycle • Characterization • Property ranges of 316L powders • Examples © sirris 2007 | www.sirris.be | info@sirris.be 3
  • 4. Porous metallic parts • Shaping by powder metallurgy  lots of parameters • Porosity range from a few % to 90% • Application list: • Filtration • Distributing/dispersing/damping • Airing/cooling • Lightening • Catalysts supports • Prosthesis • But simple geometries (Pressing, MIM) 4
  • 5. Porous metallic parts • Additive manufacturing  no limit in shape + integrated functionalities • SLM  1 step  no control of porosity • 3D-printing  indirect route: shaping + sintering  possibility to control porous characteristics R10: 1000x500x280mm RXD: 60x40x15mm 5
  • 6. 3D- Printing Prometal Process 3. Sintering Complete Partial 1. Curing 2. Debinding - presintering (green part) (brown part) (3’. Infiltration) 6
  • 7. Sintering cycle • From a powder tap to full dense material • Passing by porous state • Opened to 92% density, then closed • Evolution functions of: • Initial state • Packing density • Particle size distribution • Particle shape • Sintering conditions • Temperature • Time • (Atmosphere) •  Stop at different stage to keep or eliminate porosity following target application 7
  • 8. Characterization • Density – porosity (opened and closed)  Archimedes (3 weightings) • Permeability k  Darcy (flux Q through thickness L and surface A under DP) Q.L.µ k= A.∆P • Pore size (bubble point and Hg porosimetry)  Washburn − 4.γ . cos θ d= P © sirris 2007 | www.sirris.be | info@sirris.be 8
  • 9. Property ranges for 316L powders 100 40 22µm • Effect of sintering T° 95 31µm 20-53µm 35 (90min at T°) for 4 45-90µm 90 30 Opened porosity (%) Relative density (%) spherical powders 85 25 80 20 75 15 70 10 65 5 60 0 1180 1200 1220 1240 1260 1280 1300 1320 1340 1360 1380 1400 1420 1440 Temperature (°C) 0,9 Porous part Dense part 0,89 0,88 1315° • Effect of sintering time 0,87 C Density (-) 0,86 1335° at 3 T° for 31µm 0,85 C 1345° powder 0,84 0,83 C 0,82 0,81 0 50 100 150 200 250 300 350 Time at sintering temperature (min.) 9
  • 10. Property ranges for 316L powders 35 1,00E-12 • Pore size and permeability 22µm functions of opened porosity for 4 spherical 31µm 30 20-53µm powders Mean pore size (µm) 45-90µm 1,00E-13 25 Permeability (m²) 20 1,00E-14 15 • Link between parameters: • Powder size sets pore size 10 1,00E-15 • Thermal cycle sets final density/porosity 5 •  all defines permeability 0 1,00E-16 Main challenge: shrinkage 0 5 10 15 20 25 30 35 40 • control! Opened porosity (%) Pore mean size Permeability 10
  • 11. Property ranges for 316L powders 45-90µm powder Gas atomised particles Water atomised particles Sintered 90min at 1395°C 65% density – 35% opened porosity 47% density – 53% opened porosity Mean pore size 35µm Mean pore size 30µm Permeability 10-12m² Permeability 10-12m² © sirris 2007 | www.sirris.be | info@sirris.be 11
  • 12. Examples Ø 70mm Pores 30µm Perméa. 10-12 m² L 270mm Ø 50mm Pores 17µm Pores 30µm Perméa. 5.10-13 m² L 30mm Perméa. 10-12 m² Ø 300mm L 90mm Pores 35µm Pores 35µm Perméa. 10-12 m² Perméa. 10-12 m² 12
  • 13. Thank you for your attention ! Bruno.Verlee@sirris.be 13