Small variations in powder composition lead to strong differences in part properties

Transcription

1 Small variations in powder composition lead to strong differences in part properties Insights from an Al-Sc alloy and a Ni-base superalloy Eric. A. Jägle, L. Wu, L. Lu, D. Raabe Department Microstructure Physics and Alloy Design Alloys for Additive Manufacturing Group

2 Outline 1. Strength variations in an Al-Sc alloy (Scalmalloy ): 2. Hot cracking in a Nickel-base superalloy: Inconel 738LC Eric Jägle Alloys for Laser Additive Manufacturing 1

3 Aluminium-Scandium Alloys strength / MPa breaking elongation / % Strengthening achieved by precipitation of Al 3 (Sc,Zr) nanoparticles upon ageing heat treatment Scalmalloy : AlMgScZr-alloys with hypereutectoid content of scandium developed by Airbus Rapid quenching necessary to retain supersaturation: melt spinning + hot compaction or LAM can be employed AlSi10Mg Scalmalloy Ultimate tensile strength Yield strength Elongation to fracture R. Hyland, Metall. Trans. A 23, 1947 (1992). produced by SLM C. Booth-Morrison et al., Acta Mater. 60, 4740 (2012) Sc Zr Eric Jägle Alloys for Laser Additive Manufacturing 2

4 The problem unexpected drop in strength? defects? precipitates? grain size? Same powder composition Similar process parameters Different powder atomization supplier Different SLM-machine vendor Eric Jägle Alloys for Laser Additive Manufacturing 3

5 Sample overview low ductility and strength? SAMPLE Powder atomization SLM machine Postheat treatment Yield strength / MPa Ductility / % VIGA EIGA EIGA Concept Laser Concept Laser SLM Solutions HT HT + HIP HT ^ EIGA: Electrode Inert Gas Atomization / VIGA: Vacuum Inert Gas Atomization HT: Heat treatment (4 h@ 325 C ) HIP: Hot Isostatic Pressing 325 C ) Eric Jägle Alloys for Laser Additive Manufacturing 4

6 Low ductility bonding defects on fracture surf. As-produced HIPed unmelted powder bonding defects Unmelted powder particles and bonding defects in samples produced by the SLM Solutions machine (samples 4 6) Bonding defects are not healed by HIPing! Eric Jägle Alloys for Laser Additive Manufacturing 5

7 Low ductility bonding defects on fracture surf um SAMPLE Powder EIGA EIGA EIGA machine Concept laser SLM Solutions SLM Solutions heat treatment HT + HIP HT HT + HIP ductility yield strength Defect area fraction Close to 0% 13.68% 14.62% 6 400um 400um Bonding defects are the reason for low ductility They cannot explain low yield strength (cf. sample 3) Eric Jägle Alloys for Laser Additive Manufacturing 6

8 Influences of unbonded zones on yield stress Unbonded zones lead to a reduction of load-bearing area in cross section Decrease of apparent yield stress But hardness measurement unaffected by bonding defects! bonding defects can t explain drop in hardness Eric Jägle Alloys for Laser Additive Manufacturing 7

9 The problem unexpected drop in strength? defects? precipitates? grain size? Same powder composition Similar process parameters Different powder atomization supplier Different SLM-machine vendor Eric Jägle Alloys for Laser Additive Manufacturing 8

10 Coarse precipitates in AP-material and powder courtesy of Airbus Defense and Space Large precipitates (20-50 µm diameter) in the SLMproduced parts are identified by EDX as Al 3 (Sc,Zr) They are only present in powder atomized by the EIGA process. Presumably the time in the liquid state is not long enough to dissolve them. R. Hyland, Metall. Trans. A 23, 1947 (1992). Eric Jägle Alloys for Laser Additive Manufacturing 9

11 Large precipitates: low strength, but high ductility SAMPLE Atomisation VIGA EIGA EIGA EIGA Y. strength / MPa Ductility/ % Large precipitates apparently don t deteriorate ductility! Cup-and-cone fracture around large precipitates Maybe they decrease strength by consuming solute, which then cannot lead to nm-size precipitates? Eric Jägle Alloys for Laser Additive Manufacturing 10

12 Influences of unexpected precipitates Concentrations in at.-% 3 Elements nominal composition composition sample 3 change Mg Al Si Sc Mn Zr Matrix Precipitates Area fraction 99.69% 0.31% Large precipitates only consume about 0.1% of Sc! Does this explain the remaining difference in yield strength? Sc Zr Eric Jägle Alloys for Laser Additive Manufacturing 11

13 Atom Probe Tomography of Al 3 Sc Sample No. 2 5 Number density ( /m 3 ) Average radius (nm) volume fraction ~2% ~2% Only small influence of coarse precipitates on secondary precipitates. Eric Jägle Alloys for Laser Additive Manufacturing 12

14 yield stress / MPa Estimation of strengthening by Al 3 Sc Bypassing mechanism: τ OR = Gb f r Cutting mechanism: τ c = γ 3 2 f r 6E v only ~15MPa difference! sample number Precipitate strengthening follows cutting mechanism due to the size. Sample 5 should be even a little stronger than sample 2! Eric Jägle Alloys for Laser Additive Manufacturing 13

15 build direction The problem unexpected drop in strength? reduced cross sectional area due to bonding defects? fewer nm-sized precipitates due to large precipitates? larger volume fraction of small, equiaxed grains Bonding defects and large ppts alone cannot explain drop in strength Strong difference in the fraction of small grains depends on the atomization process (!) Eric Jägle Alloys for Laser Additive Manufacturing 14

16 Grain refinement by intermediate precipitates? sample 1 sample 4 Sc 5%.at isosurface Mn 2%.at isosurface Mg 20%.at isosurface O 10%.at isosurface 100 nm Different number of medium-sized precipitates (20-50 nm) grain refinement during re-melting? Eric Jägle Alloys for Laser Additive Manufacturing 15

17 Different fractions of equiaxed grains IPF (001) VIGA EIGA Columnar grains Equi-axed grains Area fraction of equiaxed grains depends on atomization method! Eric Jägle Alloys for Laser Additive Manufacturing 16

18 Micro-hardness measurements No significant influence of grain size on hardness (and hence strength) Eric Jägle Alloys for Laser Additive Manufacturing 17

19 The problem unexpected drop in strength? reduced cross sectional area due to bonding defects? fewer nm-sized precipitates due to large precipitates? larger volume fraction of small, equiaxed grains Same powder composition Similar process parameters Different powder atomization supplier Different SLM-machine vendor Eric Jägle Alloys for Laser Additive Manufacturing 18

20 Observations of precipitates free zones Sc 5%.at isosurface Mn 2%.at isosurface Mg 20%.at isosurface O 10%.at isosurface 100 nm Width of PFZs is significant compared to radius of small, equiaxed grains Eric Jägle Alloys for Laser Additive Manufacturing 19

21 Precipitates free zone 40 nm 100 nm Sample No. 2 5 Total width / nm Width of ppt / nm Width of PFZ / nm Soft zone around PFZ may be 10 times wider than PFZ 1. Considering of the fine grain size (less than 1 µm), the PFZs may contribute significantly to low yield strength. Eric Jägle Alloys for Laser Additive Manufacturing 20 1 Fourmeau et al., Phil. Mag., 95 (2015) 3278

22 Small changes yield large differences? reduced cross sectional area due to bonding defects? wider PFZs may contribute to lower strength Bonding defects due to poor process parameters explain difference in ductility and partially explain difference in strength Different atomization process leads to coarse precipitates, that in turn bind Sc and Zr lead to a lower number of intermediate-size precipitates lead to a lower fraction of equiaxed grains lead to wider PFZs Eric Jägle Alloys for Laser Additive Manufacturing 21

23 Outline 1. Strength variation in an Al-Sc alloy (Scalmalloy ): 2. Hot cracking in a Nickel-base superalloy: Inconel 738LC Eric Jägle Alloys for Laser Additive Manufacturing 22

24 Problem: hot cracking in IN738LC Cracks are oriented parallel to build direction Intergranular microcracks worst case sample Z Eric Jägle Alloys for Laser Additive Manufacturing 23

25 What type of cracking? 1. Liquation cracks? 2. Strain age cracks? 3. Solidifcation cracks? no low-melting phases cracking without presence of g Upper melt pool Solidified liquid film on surface (a) Melt pool boundary Solidification cracking in laser welding of a Ni-base superalloy Lippold et al., Welding Metallurgy, 2012 Lower melt pool Z Hot cracks are probably solidification cracks Eric Jägle Alloys for Laser Additive Manufacturing 24

26 Solidification cracking Tensile stresses develop upon solidification and cooling shrinkage Liquid film persists to low temperatures Liquid film ruptures equilibrium No L S backdiffusion: Scheil-Gulliver model cracking Microsegregation during solidification exacerbates the problem by lowering solidus temperature Eric Jägle Alloys for Laser Additive Manufacturing 25

27 Crack chemistry part I Auger Electron Spectroscopy Atom Probe Tomography Intensity Cracked region Zr-ox. Ti-ox. Cr-ox. Ni Co Main Intensity Cracked region Al-ox. Si Ta Zr Nb Mo Main Ni B HAGB Intensity energy (ev) Non-cracked region Ni C Ti-ox.Cr-ox energy (ev) Co Ni Main Intensity Al-ox. energy (ev) Non-cracked region Mo Nb Ta W F Impact in analysis chamber energy (ev) Si and Zr enrichment on crack surface Main atomic percent% Distance (nm) B% Mo% C% Si% Zr% Eric Jägle Alloys for Laser Additive Manufacturing 26

28 attractive, i.e. LAGB repulsive, i.e. HAGB Solidification cracking theory: Rappaz/Boettinger at T=T m at T<T m g GB <2g SL liquid film thickness liquid film thickness => below melting point, liquid film is unstable at T=T m at T<T m g GB >2g SL liquid film thickness liquid film thickness there is a stable liquid film thickness even below T m Undercooling to make liquid film unstable: T b = γ gb 2γ sl 1 s f δ Eric Jägle Alloys for Laser Additive Manufacturing 27 Rappaz et al., Metall. Mater. Trans. A 34, 467 (2003).

29 Cracked GB misorientation 29 o 37 o 45 o GB number fraction GB on cracks (20 cracks) GB on whole cross section Y 26 o 30 o 25 o Misorientation Only HAGBs show cracking, as predicted by theory. X Eric Jägle Alloys for Laser Additive Manufacturing 28

30 Crack chemistry part II atomic percent% HAGB B% Mo% C% Si% Zr% HAGB LAGB Distance (nm) 2.5 There is a lot of Zr on HAGBs but none on LAGBs atomic percent% LAGB B% Mo% C% Si% Zr Ni B 10%C isosurface 5%B isosurface 5%Zr isosurface Eric Jägle Alloys for Laser Additive Manufacturing distance (nm)

31 Mystery: Why is Zr high on HAGBs? M. Rappaz, A. Jacot, and W.J. Boettinger, Metall. Mater. Trans. A 34, 467 (2003). attractive, i.e. LAGB repulsive, i.e. HAGB in our case: Zr conc. Model that correctly predicts misorientation-dependence of cracking predicts opposite behaviour of Zr µ-segregation Eric Jägle Alloys for Laser Additive Manufacturing 30

32 Samples with low Zr/Si content? Experiments Thermocalc Simulation (TTNi8) crack density / mm-10.3! high Zr,Si low Zr, Si Zr concentration 0.06 wt.-% 0.02 wt.-% Si concentration 0.07 wt.-% 0.01 wt.-% liquidus 1346 C +2K 1348 C +15K solidus equilibrium 1267 C 1282 C +25K solidus Scheil 1058 C 1083 C Cracking vanishes completely when Zr & Si are reduced (0.04% difference!) Cracking intensifies when C is reduced (probably due to less binding of Zr&Si in carbides) Solidus temperature increases by ~25K when excluding Zr, supporting µsegregation as reason for solidification cracking Eric Jägle Alloys for Laser Additive Manufacturing 31

33 Conclusions Small variations in powder composition, powder atomization, process parameters, post-processing can lead to large changes in defect density, precipitation, grain size, yield strength and ductility. Two examples: Unexpected drop of yield strength in an Al-Sc alloy Elimination of hot cracking in a Ni-base superalloy by Zr & Si reduction Eric Jägle Alloys for Laser Additive Manufacturing 32

34 Thank you for your attention. E. A. Jägle, Z. Sheng, L. Lu, L. Wu, J. Risse, A. Weisheit, D. Raabe, JOM, 68, 943 (2016) E. A. Jägle, L. Wu, F. Palm, D. Raabe, in preparation E. A. Jägle, L. Lu, J. Risse, D. Raabe, in preparation Acknowledgements: Lin Lu, Liang Wu, Philipp Kürnsteiner, Frank Palm (Airbus), Jeroen Risse (Fh-ILT) Funding by: Eric Jägle Alloys for Laser Additive Manufacturing 33