Young - Barber - CSAT 2017 - Elevated Temperature Processing Effects On Cold Sprayed Materials - Final 05 - 23 - 17

Engineering, Test & Technology
Boeing Research & Technology | Elevated Temperature

Boeing Research Processing
& Technology
Effects on Cold Spray Materials
Elevated Temperature Process Effects

on Cold Sprayed Materials
Presented at Cold Spray Action Team (CSAT)
2017 Workshop
Northeastern University, Boston, MA
June 15, 2017
Ken Young
Brian Sparber
The Boeing Company
Boeing Research & Technology
Copyright © 2017 Boeing. All rights reserved.
Overview
Boeing Research & Technology | Elevated Temperature Processing
• Background and Applications

• Bulk Cold Spray Materials & Process
• Test Samples and Summary
• Annealed Mechanical Property Effects
– Tensile results
– Microstructure evaluations
– Fractography
• Summary / Path Forward
Copyright © 2017 Boeing. All rights reserved. 2

Background and Applications
• Previous Cold Spray Coatings Efforts on Rotor Blades

➢ Boeing-AATD Rotor Durability TIA
➢ Development work with Army Research Lab
➢ Demonstration of niobium on substrates (e.g. Inconel, Nickel, Titanium)
• Objectives for Cold Spray Annealing

➢ Reduction in residual stresses to minimize distortion
➢ Balance of strength and ductility
➢ Optimize adhesion and interlayer cohesion
➢ Reduction of defects that will reduce fatigue endurance limit
• End Goals
➢ Assess annealing benefits for coatings and repair applications
➢ Understand limitations (e.g. substrate temperature, mechanical properties)
➢ Identify potential candidates for structural/dynamic repairs (i.e. fatigue)

Cold Spray Materials & Process
• Coating Materials Evaluated

➢ Niobium, -30/+10 micron, mechanically fabricated
➢ Nickel-15Cobalt, -53/+15 micron, gas atomized
➢ Inconel 625, -45/+15 micron, gas atomized
• Cold Spray Process Conditions

➢ ARL collaboration
➢ CGT 4000 and VRC Gen III using helium
➢ Range of gas temperatures and pressures evaluated
▪ V/Vcr ≈ 1.5-1.6
▪ DPV evolution to track particle velocity and particle size
▪ ICP-8 for deflection and residual stress assessment

Cold Spray Materials & Process
• Anneal Process Conditions

➢ Boeing vacuum furnaces
▪ 9°F/min ramp up below 1560°F, and 18°F/min ramp up above 1560°F
▪ -18°F/min controlled vacuum cool to 1560°F, slow cool under vacuum (heaters off) to ambient
▪ Pressure maintained at less than 1x10^-4 torr
➢ Stress relief hold at 1560°F for 1 hour where applicable
➢ Anneal at set point ±10°F for 1 hour

Cold Spray Test Samples
• Tensile Sample Setup

➢ 90° deposition angle
➢ Deposit direction along tensile gauge (longitudinal)
➢ 0.003-0.004 inch each deposit layer thickness build up to 0.060 inch
➢ Machined to 0.040 inch net thickness
ASTM E8 sub-size tensile 1 in

▪ 1 inch gauge length
▪ 0.040 inch thickness
MTS load frame DL=0 Brittle

▪ Mechanical grips
▪ 0.005 in/in/min strain
control through YS Ductile
▪ 0.1 in/min extension to fail 44% EL

Test Summary
• Tensile Testing
➢ Annealing temperatures (detailed survey)
▪ As-deposited baseline
▪ 600°F to 2350°F (315°C to 1290°C)
➢ Deposit parameters for further optimization (limited to date, in progress)
▪ “Moderate” gas temperatures and pressures
▪ Other temperature and pressure combinations for future work
• Microstructure, Microhardness and Fractography
• Other Testing (in progress or planned)

➢ Digital Image Correlation (DIC)
➢ ICP deflection/residual stress
➢ Fatigue
➢ Erosion
Niobium

Niobium Properties vs. Anneal
Strength Maximized around 1000 F, and Ductility Increased with Temperature

Niobium Properties vs. Anneal
Hardness Tracked Closely with Ultimate Tensile Strength Results

Niobium Stress-Strain Curves
1000F
As-Dep.
1700F
2350F
Elastic modulus and yield strength are important design constraints

(i.e. ultimate tensile strength not always the driver)  closer look at Yield Strength
Niobium Stress-Strain Curves
1000F
Upper 0.2%
YS Peak As-Dep.
Offset YS
1700F
2350F
Elastic Modulus Increased when Annealed due to More Linear Stress Strain Curve, and
Yielding Changed from Offset Method (no upper yield peak) to Upper Peak at/above 1700F.
[Note, as-deposited curves required lower proportionality range for offset]
Niobium Microstructure
As-Deposited 1000 ºF (535 ºC) – 1 hour
0.001 inch 0.001 inch
Splat-type Morphology Similar Splat-type Morphology

Highlighted by Inter-Splat Boundaries Maximum Strength
Note Deformation Within Splats 12% Elongation
~2% Elongation Stress Relief + Strengthening
Etchant 1 Nitric Acid : 1 Hydrofluoric Acid : 1 Sulfuric Acid : 3 Water

Splat Boundaries
Discrete Splats
0.001 inch 0.001 inch
Splat-type Morphology Similar Splat-type Morphology

Highlighted by Inter-Splat Boundaries Maximum Strength
Note Deformation Within Splats 12% Elongation
~2% Elongation Stress Relief + Strengthening
No Discernible Change in Microstructure Compared to As-Deposited
Changes Are Evident In Fracture Surface (Ductility)
1700 ºF (825 ºC) – 1 hour 2350 ºF (1290 ºC) – 1 hour
0.001 inch 0.001 inch
Onset of Observed Recrystallization Further Recrystallization

Reduction in Inter-Splat Boundaries and Grain Growth
UTS Equivalent to As-Deposited UTS Below As-Deposited

33% Increase in Yield Strength Highest Ductility, 32% Elongation
20% Elongation
Recrystallization Occurs as Low as 1700 F (825 C), Reduces Strength and Increases Ductility
0.001 inch 0.001 inch
Onset of Observed Recrystallization Further Recrystallization

Reduction in Inter-Splat Boundaries and Grain Growth
UTS Equivalent to As-Deposited UTS Below As-Deposited

33% Increase in Yield Strength Highest Ductility, 32% Elongation
20% Elongation
Recrystallization Occurs as Low as 1700 F (825 C), Reduces Strength and Increases Ductility
Niobium Fractography
As-Deposited 1000 ºF (535 ºC) – 1 hour 2350 ºF (1290 ºC) – 1 hour

Reduction in Area
0.01 inch 0.01 inch 0.01 inch

Brittle Mixed Mode Fracture Ductile Fracture Ductile Fracture
~ 2% Elongation ~ 12% Elongation ~ 32% Elongation
Initial Strength Increased Strength Reduced Strength
Low Ductility Moderate Ductility Maximum Ductility
Post-Deposition Heat Treatment Offers Control of Strength and Ductility

As-Deposited Niobium Source Powder
0.001 inch 0.001 inch
Brittle Mixed Mode Fracture Mechanically Fabricated Angular Powder

Inter-splat and Cleavage Propagation -30 µm / +10 µm Size Distribution
2% Elongation Powder Size Correlates With Splat Size
Cold Sprayed Morphology Apparent in As-Deposited Brittle Fracture

As-Deposited Niobium Source Powder
Pit-etching
Areas “Jet”
Area
0.001 inch 0.001 inch
Brittle Mixed Mode Fracture Mechanically Fabricated Angular Powder

Inter-splat and Cleavage Propagation -30 µm / +10 µm Size Distribution
2% Elongation Powder Size Correlates With Splat Size
Cold Sprayed Morphology Apparent in As-Deposited Brittle Fracture

0.001 inch 0.001 inch
Ductile Fracture Ductile Fracture

Microvoid Coalescence (Larger) Microvoid Coalescence
No Recrystallization, 10% Elongation Partially Recrystallized, 32% Elongation
Cold Sprayed Morphology in Fractures Mostly Eliminated – Less Sensitive to Defects

Nickel-Cobalt

Nickel-Cobalt Properties vs. Anneal
Strength Decreased (No Local Maximum Observed), and Ductility Decreased (after 1000 F)

Nickel-15Co Stress-Strain Curves
0.2% Offset YS
As-Dep.
1000F
1450F
2350F
Elastic Modulus Decreased when Annealed, and Elongation also Decreased

(Evidence of Significant Grain Growth)
Nickel-15Co Stress-Strain Curves
1000F
Upper YS Peak
1450F
0.2%
Offset YS
2350F
Elastic Modulus Decreased when Annealed, and Elongation also Decreased

(Evidence of Significant Grain Growth)
Nickel-15Cobalt Microstructure
0.001 inch 0.001 inch
Splat-type Morphology Apparent Recrystallization

of Small Grains
Deformation Throughout Splat
40% Reduction in UTS vs As-Deposited
Consolidation Defect Around
72% Reduction in Yield Strength
Multiple Splats
Maximum Elongation, 42%
Onset of Recrystallization Results in Significantly Reduced Strength and Increased Ductility
Nickel-15Cobalt Microstructure
0.001 inch 0.001 inch
Splat-type Morphology Grain Growth Leads to Reduced

Strength and Ductility
Deformation Throughout Splat
Consolidation Defect Around
Multiple Splats
Heat Treatment Above 1000 F (535 C) Reduces Mechanical Properties Due to Grain Growth
Nickel-15Cobalt Fractography
0.001 inch 0.001 inch
Brittle Mixed Mode Fracture Ductile Fracture

Inter-splat and cleavage propagation Microvoid Coalescence
2% Elongation 46% Elongation

Nickel-15Cobalt Fractography
0.001 inch 0.001 inch
Brittle Mixed Mode Fracture Ductile Fracture

Inter-splat and cleavage propagation Microvoid Coalescence
2% Elongation 46% Elongation

Inconel 625

Inconel Properties vs. Anneal
Strength Maximum at (or before) 1200 F, and Ductility Increased with Temperature

Inconel 625 Stress-Strain Curves
1200F
Upper YS Peak
1700F
0.2% Offset YS
2350F
No Perceptible Yield Strength for As-Deposited or 1200 F.

1700 F Anneal has Upper Yield Peak, 2350 F used Offset Yield Strength.
Tensile Modulus (All 3 Materials)
Generally Trend (Niobium and Inconel) was Increase in Modulus with Stress
Relief, then Levels Off after Maximum Strength Anneal.
However, Nickel-Cobalt Modulus Decreased with Anneal Temperature.

Inconel 625 (As-Deposited)
As-Deposited Microstructure As-Deposited Fractography
0.001 inch 0.001 inch
Mixed High Deformation (Splat) and Brittle Mixed Mode Fracture

Low Deformation (Circular) Primarily Inter-Splat Propagation
Particle Morphology
~0% Elongation
Pre-existing Dendritic Structure
Indicative of Deformation Severity
As-Deposited Microstructure Offers Negligible Ductility

Inconel 625 (1700 °F, 927 °C – 1 hour)
1700 ºF (927 ºC) – 1 hour Microstructure 1700 ºF (927 ºC) – 1 hour Fractography
0.001 inch 0.001 inch
Onset of Recrystallization Primarily Ductile Microvoid Coalescence

No Evidence of Prior Dendritic Structure Some Inter-Splat Propagation Possible
10% Elongation
13% Strength Increase vs As-Deposited
Onset of Recrystallization Enhances Ductility and Strength up to 1700 F (927 C)

Summary
Examples of Materials/Conditions for Balanced Properties

Note: there may be substrate temperature limits
Cold Spray Anneal Elongation to
Strength (UTS) Tensile Modulus Potential Applications
Material Condition Failure
~1000°F/1hr 100 ksi 8-15% 15 Msi Repairing titanium, aluminum, etc

Niobium (stiffness matching)
As-deposited 85 ksi 2% 13 Msi Leading edge protective coating
Nickel or ~1000°F/1hr 70 ksi 45% 27 Msi Repairing nickel, steel, etc

Nickel-Co (more ductility or damage tolerance)
As-deposited 115 ksi 2% 28 Msi
~1700°F/1hr 175 ksi 10% 30 Msi Repairs requiring additional

Inconel 625
structural margin
As-deposited 155 ksi 0% 26 Msi
Elevated Temperature Conditioning Post-Cold Spray allows for Tuning Mechanical

Properties while Resulting in Stress Relieved Structure and Minimized Defects.
The Goal in this Study was to Find a Balanced Combination of Strength and Ductility,
while Identifying the Mechanisms for the Property Changes.

Summary
• Cold Spray Deposit Benefits of Elevated Temperature (Anneal)

➢ Protective coatings – low/no residual stress, reduced defects
➢ Component repair – reduced defects, improved mechanical properties
• Future Work / Path Forward

➢ Fatigue testing
➢ Adhesion assessment
➢ Deposit parameters and corresponding anneal
➢ Other materials for consideration and alignment with aircraft programs
➢ Component level evaluations
• Acknowledgements
➢ Army Research Laboratories
➢ Bruno Zamorano Senderos, Paul Wilson, John Delconte, Yutaka Oshikiri
(Boeing Research & Technology)
Questions?

Young - Barber - CSAT 2017 - Elevated Temperature Processing Effects On Cold Sprayed Materials - Final 05 - 23 - 17

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Engineering, Test & Technology

Boeing Research & Technology | Elevated Temperature

Elevated Temperature Process Effects

• Background and Applications

Copyright © 2017 Boeing. All rights reserved. 2

• Previous Cold Spray Coatings Efforts on Rotor Blades

• Objectives for Cold Spray Annealing

Copyright © 2017 Boeing. All rights reserved. 3

• Coating Materials Evaluated

• Cold Spray Process Conditions

Copyright © 2017 Boeing. All rights reserved. 4

• Anneal Process Conditions

Copyright © 2017 Boeing. All rights reserved. 5

• Tensile Sample Setup

ASTM E8 sub-size tensile 1 in

MTS load frame DL=0 Brittle

Copyright © 2017 Boeing. All rights reserved. 6

• Microstructure, Microhardness and Fractography

• Other Testing (in progress or planned)

Copyright © 2016 Boeing. All rights reserved. 8

Strength Maximized around 1000 F, and Ductility Increased with Temperature

Copyright © 2017 Boeing. All rights reserved. 9

Hardness Tracked Closely with Ultimate Tensile Strength Results

Copyright © 2017 Boeing. All rights reserved. 10

Elastic modulus and yield strength are important design constraints

As-Deposited 1000 ºF (535 ºC) – 1 hour

0.001 inch 0.001 inch

Splat-type Morphology Similar Splat-type Morphology

Etchant 1 Nitric Acid : 1 Hydrofluoric Acid : 1 Sulfuric Acid : 3 Water

Copyright © 2017 Boeing. All rights reserved. 13

As-Deposited 1000 ºF (535 ºC) – 1 hour

0.001 inch 0.001 inch

Splat-type Morphology Similar Splat-type Morphology

1700 ºF (825 ºC) – 1 hour 2350 ºF (1290 ºC) – 1 hour

0.001 inch 0.001 inch

Onset of Observed Recrystallization Further Recrystallization

UTS Equivalent to As-Deposited UTS Below As-Deposited

1700 ºF (825 ºC) – 1 hour 2350 ºF (1290 ºC) – 1 hour

0.001 inch 0.001 inch

Onset of Observed Recrystallization Further Recrystallization

UTS Equivalent to As-Deposited UTS Below As-Deposited

As-Deposited 1000 ºF (535 ºC) – 1 hour 2350 ºF (1290 ºC) – 1 hour

0.01 inch 0.01 inch 0.01 inch

Post-Deposition Heat Treatment Offers Control of Strength and Ductility

Copyright © 2017 Boeing. All rights reserved. 17

As-Deposited Niobium Source Powder

0.001 inch 0.001 inch

Brittle Mixed Mode Fracture Mechanically Fabricated Angular Powder

Cold Sprayed Morphology Apparent in As-Deposited Brittle Fracture

Copyright © 2017 Boeing. All rights reserved. 18

As-Deposited Niobium Source Powder

0.001 inch 0.001 inch

Brittle Mixed Mode Fracture Mechanically Fabricated Angular Powder

Cold Sprayed Morphology Apparent in As-Deposited Brittle Fracture

Copyright © 2017 Boeing. All rights reserved. 19

1000 ºF (535 ºC) – 1 hour 2350 ºF (1290 ºC) – 1 hour

0.001 inch 0.001 inch

Ductile Fracture Ductile Fracture

Cold Sprayed Morphology in Fractures Mostly Eliminated – Less Sensitive to Defects

Copyright © 2017 Boeing. All rights reserved. 20

Copyright © 2016 Boeing. All rights reserved. 21

Copyright © 2017 Boeing. All rights reserved. 22

Elastic Modulus Decreased when Annealed, and Elongation also Decreased