overview of cwru work on metallic glasses and advanced ... · overview of cwru work on metallic...
TRANSCRIPT
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Overview of CWRU Work on Metallic Glasses and Advanced/Additive Manufacturing
John J. Lewandowski
Department of Materials Science and Engineering Case Western Reserve University
Cleveland, OH 44106
August 5, 2015
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Outline • Overview of Glasses/Bulk Metallic Glasses
• Quasi-Static Flow Behavior – Stress State Effects on Flow Behavior at T << Tg – Stress State Effects on Flow Behavior at T ≈ Tg
• Quasi-Static Fracture Behavior
– Fracture Behavior/Damage Tolerance • Notch/Fracture Toughness • Effects of Chemistry Changes/Annealing-Induced Embrittlement
– Correlation with Elastic Constants – Alloy Design - Fe-based BMG, Ti-based BMG
• Toughening Approaches
• Creation of Micro/Nano Metallic Glass Wires – Review of Recent Techniques
– Initial Testing of Micro/Nano Wires
• Effects of Sample Size and Preparation on Plasticity • Advanced/Additive Manufacturing
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Acknowledgements Materials:
J. Poon – University of Virginia (Fe, Ti based, Ni-Ta-X) W.L. Johnson – Cal Tech (Zr based bulk & composite) J. Kajuch/A. Peker – Liquidmetal (Zr based) T. G. Nieh – LLNL/U Tenn (Cu based) G. Shiflet – University of Virginia (Al based, Ni-Ta-X) T. Hufnagel – Johns Hopkins Univ. (Hf and Zr based) L. Kecskes – ARL (Zr based composites) G. Wolter – Howmet (Zr based bulk & composites) W.H. Wang - Chinese Acad. Sciences (Mg and Ce based) A.L. Greer - Cambridge University (Zr based) M. Widom – CMU (Ni-Ta-X)
Students/Collaborators: P. Lowhaphandu L. Vatamanu J. Caris H. Hassan P. Wesseling F. Yuan A. Thurston B. Ko A. Shamimi Nouri A. Shabasy G. Sunny C. Tuma A Awadallah V. Prakash N. Stelmashenko A. Vormelker L. Deibler L. Kecskes M. Seifi J. Carter J. Booth N. Neilson
Interactions: ARL Univ. Cambridge Boeing Tohoku Univ. Pratt & Whitney CWRU Liquidmetal DARPA/DoE SRI ONR CAL TECH ARO Univ. Virginia Chinese Acad. Sci.
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Melt-Spinning Ribbon Thickness < 100 µm, Ribbon Width mm - 10’s mm
Can be Devitrified to Produce Nano-crystallline solid
Mechanical Testing Limited: Tension, Bend Testing, Hardness (Alignment Issues)
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Ref: Peker, A. and Johnson, W.L. Appl. Phys. Lett., vol. 63, 1993, p. 2342.
Increase in tg (Reduced Glass Transition Temperature) Lowers the Critical Cooling Rate to Produce Bulk Metallic Glasses
Guidelines: -Typically > 3 Elements - Difference Atom Sizes > 12% - Negative Heats of Mixing - Deep Eutectic - Dense Random Packing (small excess free volume 1%) (No Long Range Order) (MRO, SRO exist)
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Evolution of Metallic Glass Chemistry and Maximum Sizes
A. L. Greer et al., MRS Bull., 32 (8) (2007) p. 611
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R. Busch, JOM (2000)
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Greer/Ashby, Scripta Mater. (2006)
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Experimental Methods
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Superimposed Pressure Testing
Silicone Oil Rig Pressure = 2 GPa Can Heat Oil to 330oC
J.J. Lewandowski and P. Lowhaphandu, International Materials Reviews, Vol.43, No.4, 1998.
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Previous Work Summary
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J.J. Lewandowski and P. Lowhaphandu, International Materials Reviews, Vol.43, No.4, 1998.
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0
500
1000
1500
2000
2500
0 0.01 0.02 0.03 0.04 0.05 0.06True Strain
Tru
e St
ress
[MPa
]
Vitreloy450 MPa Hydrostatic Pressure
0.2 % Yield Strength = 2035 MPaFracture Strength = 2067 MPa
!f = 3.8%
0
500
1000
1500
2000
2500
0 0.01 0.02 0.03 0.04 0.05 0.06True Strain
Tru
e St
ress
[MPa
]
Vitreloy0.1 MPa Hydrostatic Pressure
Yield/Fracture Strength = 1986 MPa!
f = 0%
Specimen Fails in Shear
Lewandowski and Lowhaphandu, Philos. Mag. A, 2002, 82, 3427.
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> 40° > 50°
Lowhaphandu, Montgomery, and Lewandowski, Scripta Mat., 1999, 41(1), 19. Lewandowski and Lowhaphandu, Philos. Mag. A, 2002, 82, 3427.
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σf
σn
τc
τc= τ0 – α σn
τc= critical shear stress
τ0= shear stress in torsion
σn= normal stress
α = constant expressing the magnitude of normal stress dependence. �
Mohr-Coulomb Criterion
Lewandowski and Lowhaphandu, Philos. Mag. A, 2002, 82, 3427.
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0
200
400
600
800
1000
1200
-1500 -1000 -500 0 500 1000 1500!
n (MPa)
" c (M
Pa)
"c = "o
# $!n
"o = 963 MPa$ = 0.039
Lowhaphandu, Montgomery, Lewandowski, Scripta Mat., 1999, 41(1), 19. Lewandowski and Lowhaphandu, Philos. Mag. A, 2002, 82, 3427.
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Caris, J. and Lewandowski, J. Acta Materialia, Vol. 58, No. 3, Feb. 2010, pp. 126-136.
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Caris, J. and Lewandowski, J. Acta Materialia, Vol. 58, No. 3, Feb. 2010, pp. 126-136.
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Spitzig, WA, Richmond, O. Acta Mat’l, 32(3), 1984, 457. Wang, W.H. et al “EOS of BMGs Via Ultrasonic Method”, APL, 79(24), 3947, 2001. Wang, W.H. et al, Acta Materialia, 52,715, 2004.
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(17) Spitzig, WA, Richmond, O. Acta Mat’l, 32(3), 1984, 457. Haasen, P., Lawson, AW. Z. Metallk, 49, 1958, 280. Seeger, A., Haasen, P. Phil. Mag. 3, 1958, 470. (18-‐22)Wang, W.H. et al “EOS of BMGs Via Ultrasonic Method”, APL, 79(24), 3947, 2001. (18-‐22)Wang, W.H. et al, Acta Materialia, 52,2004, 715.
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Caris, J. and Lewandowski, J. Acta Materialia, Vol. 58, No. 3, Feb. 2010, pp. 126-136.
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Deformation Mechanism Map
• Inhomogeneous – Shear Localization w/o
macroscopic deformation – RT, near-Tg at high ė’s
• Homogeneous – Uniform Deformation – Superplastic – Near-Tg at low ė’s
• Effects of Pressure? – Implications
* Spaepen F. Acta Materialia 1979;25:407.
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J.J. Lewandowski, M. Shazly, A. Shamimi Nouri, Scripta Mater., 2006; 54(3), 337.
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Vormelker, et al, Matls Trans A, 39A(8), 1922-1934 (2008).
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Tensile Results (0.1 MPa)
20°C 260°C 330°C 380°C1x10-3 s-1 5x10-5 s-1 5x10-5 s-1 1x10-3 s-1 2x10-1 s-1 5x10-5 s-1
• Macroscopic Appearance: Displacement Control
Vormelker, et al, Matls Trans A, 39A(8), 1922-1934 (2008).
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T≈Tg Tension @ 0.1 MPa Stress Overshoot Regime Lower Strength/Viscosity High Plasticity Cavitation Zr-, La-BMG
Vatamanu et al, Mechanics of Materials, 67, pp. 86-93 (2013).
T≈Tg Tension @ Hi Pressure Stress Overshoot Regime High Strength/Viscosity Reduced Plasticity Catastrophic Shear Zr-, La-BMG
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Large Effects of Pressure as T≈Tg (Zr-BMG) - Effects Greatest at Stress Overshoot Conditions (603K) - Pressure-Induced Increases in Strength/Viscosity - Pressure-Induced Decreases in Ductility (Superplastic-Shear)
Vatamanu et al, Mechanics of Materials, 67, pp. 86-93 (2013).
*/** High Strain Rate
T(K) T/Tg P(MPa) σf P/UTS @ 0.1 MPa
RA% Fracture Mode
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Large Effects of Pressure as T≈Tg (La-BMG) - Effects Greatest at Stress Overshoot Conditions (373-383K) - Pressure-Induced Increases in Strength/Viscosity - Pressure-Induced Decreases in Ductility
(Superplastic Transition to Catastrophic Shear) Vatamanu et al, Mechanics of Materials, 67, pp. 86-93 (2013).
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Outline • Stress State Effects on Flow/Fracture of BMGs at RT (T << Tg)
– Minimal Effect of Superimposed Pressure on Strength/Plasticity
• Stress State and Temperature Effects on BMGs (T ≈ Tg) – BIG Effects of Superimposed Pressure on Strength/Plasticity
(Strength/Viscosity !!, Plasticity "")
• Quasi-Static Fracture Behavior
– Fracture Behavior/Damage Tolerance • Notch/Fracture Toughness • Effects of Chemistry Changes/Annealing-Induced Embrittlement
– Correlation with Elastic Constants – Alloy Design - Fe-based BMG, Ti-based BMG
• Toughening Approaches
• Creation of Micro/Nano Metallic Glass Wires – Review of Recent Techniques – Initial Testing of Micro/Nano Wires
• Effects of Sample Size and Preparation on Plasticity • Advanced/Additive Manufacturing
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0
20
40
60
80
100
120
140
0 50 100 150 200 250 300
4 mm plate7 mm plate
Effects of Notch Root Radius on Fracture Profile and Toughness of Zr-Ti-Ni-Cu-Be Bulk Metallic Glass
Notch Root Radius, µm
Frac
ture
Tou
ghne
ss, M
Pa√m
500 µm
Ref: P. Lowhaphandu and J.J. Lewandowski, Scripta Mater., vol. 38, no. 12, p. 1811, 1998.
500 µm
500 µm
500 µm
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JJ Lewandowski, M Shazly, A Shamimi Nouri, Scripta Mater., 2006; 54(3), 337.
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5 mm 5 mm
TOUGH BRITTLE
Lewandowski, Wang, Greer, Philos. Mag. Letters, 2005; 85(2), 77.
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PLASTICITY OR BRITTLENESS OF METALLIC GLASSES
• Amorphous Metals: (Competition Flow/Fracture) – Isotropic elastic constants
• Resistance to shear controlled by shear modulus, μ�• Resistance to dilatation controlled by bulk modulus, B
– Crack tip stresses produce dilatation • Low μ/B favors plasticity? • High μ/B favors brittleness? • How to measure plasticity/brittleness?
– Fracture Energy = G = 2ϒ– G = K2 (1-υ2) /E
– Elastic constants more easily measured in bulk metallic glasses • W.H. Wang - Chinese Academy Sciences • Joe Poon - Univ. Virginia • A. Kelly/A.H. Cottrell - University Cambridge • A.L. Greer - University of Cambridge • D. Schuele - CWRU
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Inset shows decrease in toughness with annealing time for Vitreloy 1. Figure shows a good correlation of embrittlement with changing μ/B.
Lewandowski, Wang, Greer, Philos. Mag. Letters, 2005; 85(2), 77.
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0.001
0.01
0.1
1
10
100
1000
0 0.2 0.4 0.6 0.8 1 μ/B
Pd77.5Cu6Si16.5 Fe50Mn10Mo14Cr4C16B6 Cu60Zr20Hf10Ti10 Zr57Ti5Cu20Ni8Al10 Zr41Ti14Cu12.5Ni10Be22.5 Zr57Nb5Cu15.4Ni12.6Al10 Ce70Al10Ni10Cu10 La55Al25Cu10Ni5Co5 Mg65Cu25Tb10 Pt57.5Cu14.7Ni5.3P22.5 Fe49Cr15Mo14C19B2Er1 (Fe0.9Co0.1)64.5Mo14C15B6Er0.5 (Cu50Zr50)94Al6 Er50Al24Y6Co20 Ce68Al10Cu20Co2 Cu47.5Zr47.5Al5 (Cu50Zr50)92Al8 (Cu50Zr50)92Al7Gd1 Fr
actu
re E
nerg
y,
G (k
J/m
2 )
Brittle
Tough
Lewandowski, Wang, Greer, Philos. Mag. Letters, 2005; 85(2), 77
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0.001
0.01
0.1
1
10
100
1000
0.1 0.2 0.3 0.4 0.5
ν
Pd77.5Cu6Si16.5 Cu60Zr20Hf10Ti10 Zr57Ti5Cu20Ni8Al10 Zr41Ti14Cu12.5Ni10Be22.5 Zr41Ti14Cu12.5Ni10Be22.5 (3/4hrs@623K) Zr41Ti14Cu12.5Ni10Be22.5 (1.5hrs@623K) Zr41Ti14Cu12.5Ni10Be22.5 (3hrs@623K) Zr41Ti14Cu12.5Ni10Be22.5 (6hrs@623K) Zr41Ti14Cu12.5Ni10Be22.5 (12hrs@623K) Zr41Ti14Cu12.5Ni10Be22.5 (24hrs@723K) Zr57Nb5Cu15.4Ni12.6Al10 Ce70Al10Ni10Cu10 Fe50Mn10Mo14Cr4C16B6 Mg65Cu25Tb10 Toughened (Partially Crystallized) Glass Window Glass Fused Silica Pt57.5Cu14.7Ni5.3P22.5 Fe49Cr15Mo14C19B2Er1 (Fe0.9Co0.1)64.5Mo14C15B6Er0.5 (Cu50Zr50)94Al6 Er50Al24Y6Co20 Ce68Al10Cu20Co2 Cu47.5Zr47.5Al5 (Cu50Zr50)92Al8 (Cu50Zr50)92Al7Gd1
Frac
ture
Ene
rgy,
G
(kJ
/m 2
)
Brittle
Tough
Lewandowski, Wang, Greer, Philos. Mag. Letters, 2005; 85(2), 77
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Gu, Lewandowski, et al, Acta Mater. 58, 1708 (2010)
Ti-Based BMG (5 mm thick)
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Gu, Poon, Shiflet, Lewandowski, Acta Mater (2010)
KIc > 110 MPa-m1/2 Thickest and toughest BMG to date
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Damage-tolerant BMGs
Nature Mater. 10, 123 (2010)
Pd79Ag3.5P6Si9.5Ge2 Zr61Ti2Cu25Al12 (ZT) Acta Mater. 58, 1708 (2010) Acta Mater. 60, 4940 (2012)
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Another toughening strategy
20 30 40 50 60 70 80
Zr61Ti2Cu25Al12
Inte
nsity
(a. u
.)
Diffraction angle 2 !
Zr56Co28Al16
Jun Yi, Wei Hua Wang and John J. Lewandowski Advanced Eng. Matl’s, 17(5), pp. 620-625.
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Crack deflection enhanced in pre-compressed BMGs
As-cast ZT ZT: 13.5 kN
As-cast ZC ZC: 9 kN
Jun Yi, Wei Hua Wang and John J. Lewandowski Advanced Eng. Matl’s, 17(5), pp. 620-625.
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Toughness Improvement of ZT & ZC
0 4 8 12
20
30
40
90
100
110
120
130 Toughness of ZTs
Toughness of ZCsTo
ughn
ess
(MP
a m
1/2 )
compressive load (kN)
c
0
1
2
3
Size of CSBZ
rp of as-cast ZT
Size (m
m)
Toughness of ZT and ZC were improved by 28.1% and 81.7% respectively. CSBZ: compressive shear band zone
Jun Yi, Wei Hua Wang and John J. Lewandowski Advanced Eng. Matl’s, 17(5), pp. 620-625.
ZC: Zr56Co28Al16 ZT: ZrTiCuAl
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Hoffman et al, Nature (2010) Composite Approaches
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Hoffman et al, Nature (2010)
Kc > 150 MPa-‐m1/2
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Jennifer Carter – CWRU (Effects of Orientation)
• All dendrites represented • IPF indicates random texture • Indexed: 40.5% • # Dendrites: 21
101
111
001
IPF Map Overlay
σa
*pole in tension direction
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Outline
• Stress State Effects on Flow/Fracture of BMGs at RT (T << Tg) – Minimal Effect of Superimposed Pressure on Strength/Plasticity
• Stress State and Temperature Effects on BMGs (T ≈ Tg) – BIG Effects of Superimposed Pressure on Strength/Plasticity
(Strength/Viscosity !!, Plasticity "")
• Quasi-Static Fracture Behavior
– Fracture Behavior/Damage Tolerance = f(µ/B, ν) • Alloy Design - Fe-based BMG, Ti-based BMG
• Creation of Micro/Nano Metallic Glass Wires – Review of Recent Techniques
– Initial Testing of Micro/Nano Wires
• Effects of Sample Size and Preparation on Plasticity • Advanced/Additive Manufacturing
– Metallic Glasses
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J.J. Lewandowski, M. Shazly, A.S. Nouri, Scripta Mater., 2006; 54(3), 337.
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Nanomoulding
Nature 2009, 457, 868
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Acta Mater. 2008 , 56, 5091 Nature Mater. 2010, 9, 215
FIB Milling Compression Tension
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Vormelker, et al., Metall. Mater. Trans. A 2008, 39, 1923
Zr41.25Ti13.75Cu12.5Ni10Be22.5
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Vormelker, et al., Metall. Mater. Trans. A 2008, 39, 1923
Macroscopic Appearance: Load Control
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Fabrication of Metallic Glassy Wires
Adv. Eng. Mater. 2010, 12, 1117
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Appearance and Structure of Metallic Glassy Wires
Adv. Eng. Mater. 2010, 12, 1117
20 40 60 80
Inte
nsity
2! (! )
Pd40
Cu30
Ni10
P20
Zr35
Ti30
Be27.5
Cu7.5
Zr65Cu15Ni10Al10
b
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Adv. Eng. Mater. 2010, 12, 1117
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Tensile fracture surface of 1.48 µm Pd40Cu30Ni10P20 wire
Yi, Wang and Lewandowski Acta Mater., 87, 1-7 (2015).
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!Plasticity of ‘Wires’ Increases at Nano-scale! No exposure to electron beam prior to tension test!
Yi,Wang,Lewandowski Acta Mater., 87,1-7 (2015).
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Shear Band Nucleus Size Estimate-Schuh et al, Acta Met,2004 Yi, Wang and Lewandowski Acta Mater., 87, 1-7 (2015)
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!Quantify Strain Along Axis of Wire After Fracture
Yi, Wang and Lewandowski Acta Mater., 87, 1-7 (2015)
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Yi, Wang and Lewandowski Acta Mater., 87, 1-7 (2015)
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Next: FIB large sample to smaller diameter (10 pA, 30 kV) Will sample neck again or fail in shear?
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FIB-machining large to small diameter damages material. Catastrophic shear instead of necking.
Yi, Wang and Lewandowski Acta Mater., 87, 1-7 (2015)
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Next Set of Tests: 1. Utilize Pt-deposition to adhere to manipulator (10 pA, 30kV) 2. Cut via FIB 3. Transport and adhere via Pt-deposition to Si substrate 4. Ion Mill: 15kV, 4nA, 1 µm x 1 µm 10 sec 5. Pull to failure in tension with beam off Yi, Wang and Lewandowski Acta Mater., 87, 1-7 (2015)
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418 nm
150 nm
Sample preparation via Pt-Deposition/Ion Mill changes plasticity. (Shear fracture now occurs instead of necking)
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Pristine sample exposed to electron beam: Bending in sample produced: Artifacts can be introduced during preparation
and/or testing! Yi, Wang and Lewandowski Acta Mater., 87, 1-7 (2015)
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Summary • Size Effects on Plasticity
– Fast Draw Method to Create Micro/Nano Wires – Initial Testing of Micro/Nano Wires
• Size ", Plasticity ! • Catastrophic Shear Transition to Ductile Rupture/Necking • Results Depend on Preparation/Test Technique
– Damage introduced during sample preparation and/or testing changes results • Need to Determine Stress vs Strain Behavior to Extend Results
• Stress State Effects on Flow/Fracture of BMGs at RT (T << Tg) – Quick Review of Pressure Effects on Crystalline Metals – Minimal Effect of Superimposed Pressure on Strength/Plasticity
• Stress State and Temperature Effects on BMGs (T ≈ Tg) – BIG Effects of Superimposed Pressure on Strength/Plasticity
(Strength/Viscosity !!, Plasticity "") – BIG Implications on Processing
• Very Different than Crystalline Metals, More Similar to Polymers
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Outline
CWRU Activities Connected to Additive/Advanced Manufacturing • ASTM F42 Definitions • Example of Desire for Corrosion Resistant and Damage Tolerant Coating
• Issues of Material Choice (Glass Forming, Damage Tolerant) • Thermal Stability, Microstructure Development, Properties
• America Makes/NAMII (National Additive Mfg Innovation Institute) • Powder Bed, Directed Energy Deposition (Laser Hot Wire)
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Additive Manufacturing Categories As defined by ASTM F42 Committee
Terminology Source: ASTM, Committee F42 on Additive Manufacturing Technologies
Category DescripLon
Binder Jetting (Polymer/Metal/Other) Liquid bonding agent selec^vely deposited to join powder
Material Jet^ng (Polymer) Droplets of build materials selec^vely deposited
Powder Bed Fusion (Polymer/Metal) Thermal energy selectively fuses regions of powder bed
Directed Energy DeposiLon (Metal) Focused thermal energy soVen/melts material as deposited
Sheet Lamina^on (Polymer/Metal) Sheet of material bonded together
Vat Photopolymeriza^on (Polymer) Liquid photopolymer selec^vely cured by light ac^va^on
Material Extrusion (Polymer) Material selec^vely dispensed through nozzle or orifice
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J Beuth, CMU
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! HVOF CoaLngs (Another High DeposiLon AM Process) ! Highly Dense, High Strength and Low Residual Tensile Stress or in Some Cases Compressive Stress
! Enables Much Thicker CoaLngs to be Applied than Previously Possible
! Amorphous Metal Powders
! High KineLc Energy, No Molten Metal Needed
▬ Need Proper9es of Metallic Glass as f (Temp., Time at Temp.)
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PotenLal ApplicaLons: Navy Corrosion Resistant CoaLngs; Storage Repository
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SchemaLc of DeformaLon Map for a Metallic Glass
Spaepen F. , Acta Metall. 25 (1977) 407-‐415.
Unique Flow Behavior as a f (Temperature)
Inhomogeneous Flow: ! Shear LocalizaLon ! RT ! Near Tg at very high strain rates
!!
Homogeneous Flow: ! Uniform deformaLon ! Near Tg at low and
Intermediate strain rates
!!
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Materials & Experimental Procedures: ! Materials used:
! Fe48Mo14Cr15Y2C15B6 (Drop-‐Cast Ingots, ORNL ; 5 mm dia. X 75 mm long)
▬ Tg: 560-‐575°C Tx: 623°C (Perepezko, et al., Intermetallics (2006) 14, 898)
! Hastelloy® Alloy C-‐22
! Stainless Steel 316L ! Instruments :
! High Temperature Micro-‐Hardness Tester ▬ Nikon QM
! XRD ▬ Scintag X1 apparatus using Cu-‐Kα radiaLon
! TEM ▬ JEOL 2010 FasTEM, operaLng at 200kV
A.S. Nouri, Y. Liu, JJ Lewandowski, Metall. Trans. A, 40A, 1314-‐ 1323 (2009).
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Strength vs. Temperature of Fe48Mo14Cr15Y2C15B6
0
500
1000
1500
2000
2500
3000
3500
4000
4500
0 100 200 300 400 500 600 700
Temperature (C)
Stre
ngth
(MP
a)Fe-Based #19283Stainless Steel 316LAlloy C-22
Strength = VHN/3
A.S. Nouri, Y. Liu, JJ Lewandowski, Metall. Trans. A, 40A, 1314-‐ 1323 (2009).
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! Hv EvoluLon vs. Time at Temperature
Hv
Temperature
Hv
at T
empe
ratu
re
Time
▬ Temperatures Chosen:
150°C, 275°C, 300°C, 400°C, 500°C, 575°C, 600°C, 620°C
Experimental Procedures: Thermal Exposure Effects
A.S. Nouri, Y. Liu, JJ Lewandowski, Metall. Trans. A, 40A, 1314-‐ 1323 (2009).
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Temperatures for Hardness Evolution Studies
Separate samples for each temperature
A.S. Nouri, Y. Liu, JJ Lewandowski, Metall. Trans. A, 40A, 1314-‐ 1323 (2009).
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Vickers Hardness vs. Time – T < Tg
A.S. Nouri, Y. Liu, JJ Lewandowski, Metall. Trans. A, 40A, 1314-‐ 1323 (2009).
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Vickers Hardness vs. Time – T ≈ Tg
A.S. Nouri, Y. Liu, JJ Lewandowski, Metall. Trans. A, 40A, 1314-‐ 1323 (2009).
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TEM Studies: ConvenLonal & In-‐situ
! TEM Sample PreparaLon:
! Samples were sliced to 0.5-‐0.8mm thickness
! Ground to 50µm thickness using dimpling grinder
! Gatan ion beam milling at 5kV (5 degrees angle) at room temperature
! TEM Experiments: (Yi Liu, Wayne State University)
! ConvenLonal TEM
! Performed on thermally-‐exposed samples from hardness test
! In-‐situ TEM
! crystallizaLon/structure evoluLon as a funcLon of temperature ! crystallizaLon/structure evoluLon as a funcLon of Lme at temperature
! Separate samples for temp./Lme combinaLons
A.S. Nouri, Y. Liu, JJ Lewandowski, Metall. Trans. A, 40A, 1314-‐ 1323 (2009).
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ConvenLonal TEM
As-‐Received 500°C for 300 min.
Gray domain White domain
55 +/-‐ 5 nm
A.S. Nouri, Y. Liu, JJ Lewandowski, Metall. Trans. A, 40A, 1314-‐ 1323 (2009).
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620°C for 150 min. 600°C for 60 min.
ConvenLonal TEM
A.S. Nouri, Y. Liu, JJ Lewandowski, Metall. Trans. A, 40A, 1314-‐ 1323 (2009).
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(b)
(c)
(a)
“Grey” Domain less Y, more Fe and Cr
“White” Domain more Y, less Fe and Cr
Crystallization starts in “Grey” Domain
Crystallization ends in “Grey” Domain
“White” Domain remains amorphous
Sequence of Structure EvoluLon A.S. Nouri, Y. Liu, JJ Lewandowski, Metall. Trans. A, 40A, 1314-‐ 1323 (2009).
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ConvenLonal TEM -‐ HREM
620°C for 150 min. 500°C for 300 min.
14 +/-‐ 2 nm
A.S. Nouri, Y. Liu, JJ Lewandowski, Metall. Trans. A, 40A, 1314-‐ 1323 (2009).
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In-‐situ TEM – EvoluLon as a FuncLon of Time at 500°C
RT 3 min. 6 min. 14 min.
33 min. 59 min. 94 min. 123min.
HeaLng rate: 10 K/min.
A.S. Nouri, Y. Liu, JJ Lewandowski, Metall. Trans. A, 40A, 1314-‐ 1323 (2009).
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In-‐situ TEM – EvoluLon as a FuncLon of Time at 620°C
RT 3 min. 6 min. 8 min.
12 min. 35 min. 64 min. 123 min.
HeaLng rate: 10 K/min.
A.S. Nouri, Y. Liu, JJ Lewandowski, Metall. Trans. A, 40A, 1314-‐ 1323 (2009).
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Fe23C6 Fe7C3
Analysis of the Crystalline Phase
Fe23C6:
FCC ; a=1.0578 nm
Fe7C3:
HCP ; a=0.6882 nm, c=0.454 nm
(111) spacing of (Fe,Cr)23C6 = 0.6107 nm
620°C/150 min. ( 100K/min.)
A.S. Nouri, Y. Liu, JJ Lewandowski, Metall. Trans. A, 40A, 1314-‐ 1323 (2009).
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! Hv EvoluLon vs. Time at Temperature
Hv
Temperature
Hv
at T
empe
ratu
re
Time
▬ Temperatures Chosen:
150°C, 275°C, 300°C, 400°C, 500°C, 575°C, 600°C, 620°C
Experimental Procedures: Thermal Exposure Effects
A.S. Nouri, Y. Liu, JJ Lewandowski, Metall. Trans. A, 40A, 1314-‐ 1323 (2009).
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(a) Perspective vi ew of hollow cylinder (shaft) with wear -resistant DAR -type HVOF coating having high -integrity interfacial bond on outer diameter.
(b) Plan view of hollow cylinder (shaft) with wear-resistant DAR -type HVOF coating with high integrity interfacial bond.
(c) Metallographic cross -section of wear -resistant DAR -type HVOF coating on hollow cylinder (shaft), at a magnification of 20 ×, showing bond of coating to the substrate.
(d) Metallographic cross -section of wear -resistant DAR -type HVOF coating on hollow cylinder (shaft), at a magnification of 100 ×, showing bond of coating to the substrate.
Examples of Cylinders w/Fe-‐Based Metallic Glass CoaLng
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Outline
CWRU Activities Connected to Additive/Advanced Manufacturing • ASTM F42 Definitions • Example of Desire for Corrosion Resistant and Damage Tolerant Coating
• Issues of Material Choice (Glass Forming, Damage Tolerant) • Thermal Stability, Microstructure Development, Properties
• America Makes/NAMII (National Additive Mfg Innovation Institute) • Powder Bed, Directed Energy Deposition (Laser Hot Wire)
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Summary
• Stress State Effects on Flow/Fracture of BMGs at RT (T << Tg) – Minimal Effect of Superimposed Pressure on Strength/Plasticity
• Stress State and Temperature Effects on BMGs (T ≈ Tg) – BIG Effects of Superimposed Pressure on Strength/Plasticity
(Strength/Viscosity !!, Plasticity "")
• Quasi-Static Fracture Behavior
– Fracture Behavior/Damage Tolerance = f(µ/B, ν) • Alloy Design - Fe-based BMG, Ti-based BMG
• Creation of Micro/Nano Metallic Glass Wires – Review of Recent Techniques
– Initial Testing of Micro/Nano Wires
• Effects of Sample Size and Preparation on Plasticity • Advanced/Additive Manufacturing
– Metallic Glass Coatings via HVOF