Structural Design Parameters for Germanium Jon Salem, Richard - - PowerPoint PPT Presentation

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Structural Design Parameters for Germanium

Jon Salem, Richard Rogers and Eric Baker NASA GRC 15th Department of Defense Electro-Magnetic Windows Symposium May 18th 2016

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https://ntrs.nasa.gov/search.jsp?R=20160012342 2018-05-07T09:25:52+00:00Z

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Germanium

• Good electromagnetic transmission in 2-15 μm range.

Used for specialty windows; solar cells; substrates.

• Space Act Agreement with an industrial partner to

determine the transient reliability of a proprietary, thermally and mechanically loaded, Ge window, along with the input design properties.

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Germanium

• Brittle transition metal.
• Relatively soft.
• Behaves like a soft, brittle ceramic.
• Stress corrosion cracking?
• What is the fracture toughness?

Objective

• Measure mechanical properties
• Perform transient reliability analysis.

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Material

• Single crystal beams
• Polycrystalline disks (2” & 5”Φ):
• Coarse, variable grain structure – not ideal for testing.

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25 mm 25 mm

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Anisotropy

• Anisotropy factor A* measures relative magnitude of

elastic anisotropy exhibited by a crystal. A* = 0 for isotropic materials, A* = 0 to 1 for many single crystals.

• Running mechanical test on off-axis planes can be

problematic if the anisotropy is large.

• Relatively low A* - proceed………….

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Total Anisotropy Factor (Ac

*+As *)

5 10 15 20 25

Approximate Stress/Series Stress (Plate Center)

0.98 1.00 1.02 1.04 1.06 1.08

Tetragonal and Trigonal Materials, {010}

BaTiO3 In Sn TiO2 Sapphire Quartz

Anisotropy Factor A*

2 4 6 8 10 12 14 16 18

Approximate Stress/Series Stress (Plate Center)

1.00 1.02 1.04 1.06 1.08 1.10

Cubic materials, {100} NiAl -SiC GaP Ge Si MgO Diamond

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• E<111> = 154.8 ± 0.9 GPa
• E<110> = 138.3 ± 0.2
• E<100> = 103.1 ± 0.6
• Epoly = 131, vpoly = 0.21

Young’s Modulus

• impulse excitation -

Ge McSkimin Bogardus McSkimin Mason Average NASA % Diff. Young’s Modulus (GPa) E<100> =

• 104. 4

102.0 102.2 103.7 103.1 103.1 0.0% E<110> = 138.7 136.7 137.0 138.0 137.6 138.3 0.5% E<111> = 155.8 154.2 154.5 155.1 154.9 154.8

• 0.1%

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}

Aggregate Constants Formula E

(GPa)

v Voigt 135 0.20 Hashin 133 0.21 Shtrikman 132 0.21 Reuss 129 0.21

• Well oriented germanium….

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Procedure

• Fracture Toughness -
• Three standard test methods (C1421):
• Different crack size and crack formation history.
• Different effort.
• Some methods don’t work well on some materials.

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W B ao a3 a2 a1 a1 a 2c

1= a1 /W o= ao /W =( a1+a2+a3) /3W

h Remove 4.5h to 5h

Precracked Beam (SEPB) Chevron Notch Beam (CNB) Surface Crack Flexure

(SCF)

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Fracture Toughness

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• Essentially similar on all planes.
• KIscf{jkl} = 0.74 ± 0.02 MPam.
• KIpb{100, 110} = 0.68 ± 0.04 MPam.
• ~10% difference between SCF and SEPB. Plasticity?
• Practical value of KI{jkl} = 0.68 ± 0.02 MPam.

Method {100} {110} {111} SEPB 0.67 ± 0.04 0.68 ± 0.01 0.72 ± 0.02 CNB 0.67 ± 0.03 0.69 ± 0.02 0.75 ± 0.03 SCF 0.74 ± 0.02 0.74 ± 0.02 0.74 ± 0.02

0.3 mm

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SCF Fracture Surfaces

• {100} is conchodial and exhibits cathedral

Wallner lines.

• The most planar surface occurs on the {110}.
• {111} is planar but tends to exhibit cleavage

steps.

• Secondary orientation was not fixed.

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{100}

<100>

{111}

<110> Precrack

0.5 mm

{110}

<100>

0.5 mm

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Cathedral Orientation

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<100> <110>

• Peak of cathedral corresponds to the <100> {100}.

{100}

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CNB Fracture Surfaces

• Ambient lighting:

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{110} Smooth, Flat - Cleavage {111} Stepped, Flat – Cleavage {100} Smooth, Rounded - Conchoidal

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CNB Fracture Surfaces

• Oblique lighting:

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{110} Fine Wallner lines Flat {111} Stepped Flat {100} Smooth, dimples, Rounded

Pores or inclusions?

0.3 mm

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0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1.0 1 2 3 4

Fracture Toughness, MPam L/t

Data of Jaccodine Cut off

KI{111} Data of Jaccodine

• Reported an energy equivalent value of 0.55 MPam.
• Used DCB w/ fracture mechanics solution that did not

include L/t effects.

• Reanalysis gives KI{111} = 0.69 ± 0.02 MPam (4):

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 Engineering value ~0.68 ± 0.02 MPam for low index planes

R.J. Jaccodine, “Surface Energy of Germanium and Silicon,” J. Electrochemical Soc., Vol. 110, No. 6, June, 1963, pp. 524-527.

Valid range

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Strength Testing

• Constant Stress Rate Tests

(5 MPa/s)

• Biaxial Flexure ring-on-ring (ROR)
• ~400 grit as-ground surfaces in

distilled, deionized water

• ~Polished surface in lab air

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ASTM C1499

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Fracture Strength & Weibull Statistics

• Polished m = 6; ground m = 9; spurious damage m = 4.
• Scale effect evident: 168 vs 215 MPa.
• Strength of 235 MPa is predicted vs 215 MPa (10%).

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θ m #/S

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Biaxial Fracture Patterns (polished)

• Repetitive pattern that makes fractography difficult:

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Fracture Path

• ground disk -

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Grinding Crack

#14-3, 36.1 MPa

Grain Boundary Grinding Lay Grinding Lay 8 mm Grain Boundary Grinding Crack

(#15-2)

• Crack initiated at a grinding scratch.
• Transited to a low index planes.
• Deflected at a grain boundary.

25 mm

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• Crack initiated from a semi-elliptical crack emanating

from a scratch.

• Turned onto the {111} plane:
• Opportunity to estimate the fracture toughness!
• KI{hkl} = 0.73 MPa√m.
• Why did the crack turn?

Fracture Path in a Polished ROR Disk

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9o from {110}

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Preferred Fracture Plane

• The fracture toughness on low index planes is similar, so why is

the {111} the preferred propagation plane?

• The {111} is the stiffest direction, and stiff directions exhibit high

stresses under displacement controlled situations (NiAl):

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• Stress concentration where the load ring intersects the

stiff direction! Anisotropy changes the stress distribution.

Ring loading Pressure loading

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Pressurized Plate

• Applying pressure avoids contacts:

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Stress, MPa

0 10 20 30 40 50 60 70 80 90 100 10 20 30 40 50 60 70 80 90 100

Stress, MPa

Tangential Stress, r/Rs = 0.2 Radial Stress, r/Rs = 0.2 Tangential Stress, r/Rs = 0.8 Radial Stress, r/Rs = 0.8 <100> <110> <111> Isotropic

• For a pressurized plate, the stress concentrations

at stiff directions are not exhibited. Better test! {110}

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Pressurized Plate (POR)

• Measured strength is ~20% greater than expected

from the ROR data because the stress concentration has been removed. ROR is conservative.

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Fracture Toughness

– semi-elliptical cracks on high index planes -

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• For polished specimens, KI = 0.77 ± 0.04 MPa√m (0.73-0.83).
• For grinding cracks, KI = 0.87 ± 0.04 MPa√m (0.80 – 0.90).
• Higher due to random orientation and transition to {111}.
• Caveat: local stress not precisely known…..

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Slow Crack Growth

• Experimental Approach -
• Constant Stress Rate Testing “dynamic fatigue”
• ASTM C1368
• Strength based approach with advantages &

disadvantages:

• rapid test; simple geometry
• samples the inherent, small flaws
• statistical scatter (many specimens needed)
• averaging of fatigue regions

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Experimental Procedure

• Constant Stress Rate Tests

(5 to 5 x 10-4 MPa/s)

• Biaxial Flexure (Ring-on-ring)
• Distilled, deionized water
• ~400 grit as-ground surfaces
• ~10 tests per stress rate
• ~40 tests

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Slow Crack Growth Analysis

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• Parameter extraction via regression:

 

 

 

1 1 2

1

 

 

n n i f

n B    

   

2 2 2 2

2 2 2 2

   



n Y A K n AY K B

* Ic n Ic

• Crack growth function:
• Constant stress rate testing:

] K K [ A AK = dt da = v

n IC I n I

* 

D log log 1 n 1 log

10 10 f 10

     

 

 

2 n i 10 10

1 n B log 1 n 1 D log



   

(Slope ) (Intercept )

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Constant Stress Rate Curve

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• Still some scatter.
• Medians clarify the trend.
• Slope is negative to zero  n > 100, no measurable SCG.

Ge

Russian Silica, Water Quartz-silica, water Corning 7980, water .

Stress Rate, , MPa/s 0.0001 0.001 0.01 0.1 1 10 100

Strength, Sf , MPa

20 30 40 50 60 80 100

Medians Water

Tosoh Fused Silica

Russian Silica, Water Quartz-silica, water Corning 7980, water .

Stress Rate, , MPa/s 0.001 0.01 0.1 1 10 100

Strength, Sf , MPa

20 30 40 50 60 70 80 10 100

Inert Strength Water

p = 0.15 p = 10-8

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Summary and Conclusions

• Ge exhibits similar fracture toughness of KI = 0.68 ±

0.02 MPa√m on low index planes. Lower than Si!

• Randomly oriented cracks exhibit higher apparent

toughness, but turn and propagate on the stiff {111} directions due to higher stresses (?)…..FEA.

• Natural cleavage plane appears to be the {110}.
• Weibull modulus varies from m = 4 (spurious) to m =

9 (ground).

• Strength varies from Sf = 40 MPa (ground) to 160

MPa (polished).

• Ge exhibits a Weibull scale effect, but does not

exhibit measurable SCG.

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Summary and Conclusions

• Aggregate, polycrystalline Young’s modulus and

Poisson’s ratio are Epoly = 131 GPa, vpoly = 0.21.

• ROR loading results in stress concentrations at the

stiff directions of single crystals.

• From a stress state point-of-view, a lower strength

measurement is expected………

• However, from an effective area perspective, a high

strength should be measured.

• Pressure loading (POR) is a better test method for

single crystals, because it avoids stress concentrations, but it is more effort……

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Potential Future Work

• Cyclic fatigue testing
• Finite element analysis of ROR specimens
• Testing of more pressure-on-ring specimens
• Further SCF testing
• SCG testing in other environments

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Acknowledgements

• Thanks to Terry McCue for SEM fractography.
• Thanks to the ISS Program and Penni Dalton for

funding & reviews.

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