Mechanics of Cold Spray:

From Splats to Coatings

Pranjal Nautiyal
Cheng Zhang, Victor Champagne, Benjamin Boesl, Arvind Agarwal
Florida International University, Miami
 Challenges with Mechanical Properties of Cold
Sprayed Deposits

Brittle failure due to Crack propagation

Very low ductility incomplete bonding along weak interfaces
[Rokni et al. Surf. Coat. Technol. 2017] [Hall et al. J. Thermal Spray [Loganathan et al. J. Thermal
Technol. 2017] Spray Technol. 2017]

Common Factor: Inter-splat boundaries critically influence the mechanical properties

What is the fundamental mechanism governing deformation/ failure of splat interfaces?
 Splat Sliding

Fmax - 2 µFadh N
s=
AM

Chen et al. ACS Appl. Mater. Interf. 2009

Very low inter-splat friction (~10-4 N)

Leads to easy activation of splat sliding

Splat Sliding is anticipated to depend on microstructure characteristics:

Splat Sliding = f (Splat geometry, Porosity, Inter-particle bonding)
 Challenge: How do we engineer new materials/ parts or perform
structural repair with ‘predictable’ mechanical response?

Patriot Missile Launcher B1 Bombers Forward General Electric T700

Equipment Bay Panels Engine Front Housing

One possible way: Trial and error – spray and test in iteration!
Ø Expensive - material costs can be very high
Ø Time-consuming – large number of experiments
Ø Labor intensive – highly skilled manpower
V K Champagne, Cold Spray Action Team 2018; MOOG Cold Spray Repair
 Our Approach

Material System Investigated: 6061 Aluminum Alloy – an aerospace alloy with wide applications

Filling the knowledge gap:

What deformation mechanisms are activated at “multiple hierarchical
levels” and their net effect on properties of cold sprayed deposits?
 Seeing is believing!
In-situ Mechanics Approach

Real-time Imaging
Ø Can identify and test ‘specific’ features of interest
Ø Observe the deformation mechanisms in real-time
Ø Correlate the observed mechanisms with stress-strain characteristics
 Coatings and Splat Structures
6061 Al coatings sprayed using: (i) Air, and (ii) Helium gas
Air processed Al6061 He processed Al6061
(Top Surface) (Top Surface)

(Cross-section) (Cross-section)

Particles retain their spherical morphology Flattening of particles takes place

Porous microstructure Denser microstructure
 Failure and Delamination of Coating Observed Optically

Air-Processed Coating He-Processed Coating

• Brittle in nature • Relatively superior ductility

• Extensive coating delamination after • Limited coating delamination after failure
failure
Mechanical Deformation of the Coatings
Flexural Characterization

• He-processed coating exhibits 4 times

higher failure stress compared to Air-
processed coating

• Ductility of He-processed coating is much

higher (~1.8 mm deflection at failure)

Nautiyal et al. Mater. Sci. Eng. A 737 (2018) 297

How can we understand this drastic difference in mechanical response?

Digital Image Correlation Analysis (DIC)
of Real-Time SEM Video
Micromechanical Tester inside
electron microscope chamber
Real-time SEM Video Superimposed Strain Contours

Nautiyal et al. Mater. Sci. Eng. A 737 (2018) 297-309

Spatial and Temporal Resolution of Strains

Residual strain at zero load amplitude:

§ About 70% for air-sprayed coating
§ Only 20% for He-sprayed coating

Nautiyal et al. Mater. Sci. Eng. A 737 (2018) 297-309

 Splat Sliding Factor
Based on comparison of cold-sprayed microstructure and a bulk microstructure
(same material)
𝛆𝐢
𝐒𝐒𝐟 = 𝛆
𝐬

εs: strain in bulk microstructure; εi : strain in cold sprayed microstructure

The bulk benchmark was chosen as the 6061 Al substrate

• SSf computed to be ~1.4 for He-sprayed coating and ~2 for Air-sprayed coating

The factor is an indicator of splat sliding in coatings and can be used to develop
process maps for cold spray process conditions, post-process treatment etc.

Nautiyal et al. Mater. Sci. Eng. A 737 (2018) 297-309

 High Temperature Mechanics
@ Microstructural Length Scales

Aluminum – low melting metal – mechanical properties sensitive

to temperature

Temperature rise during in-service conditions can induce ‘creep’

Complex interplay of material softening and work hardening

during high temperature deformation

Vital for cold spray application in airplanes, jets, helicopters, missile launchers etc. –
Prone to high-temperature exposure due to vibrations, engine proximity, fire etc.
Creep Response of CS 6061 Al Coating
As a function of temperature
In-situ Nanoindentation

There is pronounced creep at elevated temperatures

Nautiyal et al. Surf Coat Technol 372 (2019) 353-360
 High Temperature Creep
Strain Rate-Stress Relationship

Indentation Stress Governing Creep

Temperature Exponent (n) Mechanism

Room Temperature 6.8 Power Law Dislocation

176°C 2.7 Solute Drag

300°C 6.6 Power Law Dislocation

400°C 4.2 Power Law Dislocation

0
Indentation Stress Indentation Strain Rate Power Law Creep Equation: ε̇ = Cσ+ exp −
4 8 :9 12
𝜎= 𝜀̇ = n is stress exponent, an indicator of creep mechanism
56 9 :;

Oikawa and Karashima, Metall Trans 5 (1974) 1179; Nautiyal et al. Mater Sci Eng A 630 (2015) 131; Mayo and Nix, Acta Metall 36 (1988) 2183;
Shi and Northwood, J Mater Sci 1993; Hsiao and Huang, Metall Mater Trans A 2002
Comparison of Deformation Mechanisms
Material pile-up Material pile-up

5 µm RT 5 µm 176°C

NO pile-up Prominent plastic flow and

splat delamination

10 µm 300°C 10 µm 400°C
Nautiyal et al. Surf Coat Technol 372 (2019) 353-360
Nautiyal et al. Surf Coat Technol 372 (2019) 353-360
 Real Time Snapshots from In-situ Video
① t=0 ② t=50 s ③ t=200 s
INDENTER PROBE

Splat
Delamination

Signs of stress concentration Crack

10 µm 10 µm 10 µm
Propagation

• Splat boundaries: stress-concentration

• Indentation induces inter-splat sliding
• Plastic deformation + Crack propagation
• Delamination/ pull-out phenomena
Nautiyal et al. Surf Coat Technol 372 (2019) 353-360
 Splat-Substrate Adhesion: Interface Mechanics

Mechanism(s) of De-bonding

Nature of Adhesion Strength

Interface Bonding

Critical for Surface Engineering/

Structural Repair
Experimental set-up (In-situ indenter + scratch stage)
Lateral force transducer
Conospherical tip

Sample stage with

lateral motion

Single splats (6061 Al)

on 6061 Al substrate
Initial contact
Splat detachment observation

Plasticity is a prerequisite for debonding?

Lateral force up to detachment = 3114.4 µN
Milling of Splats to expose Splat-Substrate Interface

Before After
 Nature of Bonding observed from Sectioned Splats

Intimate splat-substrate bonding Intermediate bonding Inferior bonding

Indistinguishable interface Minor interface cracks Interfacial gaps
In-situ loading of milled splats
Debonding and Splat Sliding

Lateral force up to detachment = 1517.1 µN

 Interface Debonding and Splat Sliding Mechanisms in Real Time:
Crack propagation + Plastic deformation

t=1.4s t=2.13s

Crack Initiation
Splat Sliding

t=1.9s
t=1.6s
Complete
De-bonding

Crack Propagation along

splat-substrate interface
Purely Plastic Deformation and No Splat Sliding
 Interface Matters!
Debonding
and sliding

Prominent ‘pre-existing’
interface crack 200.4 kPa

Intimate interface adhesion

1984.95 kPa
An order of magnitude difference in strength!
Comparison with reported
bond strengths for CS 6061 Al:
- 75 MPa (Glue based): on
6061 Al substrate
[Source: MOOG]
- 103 MPa (Glueless): on
C355 Al substrate
[Honeywell, CSAT 2016]
 Mechanics of Cold-Sprayed Materials:
Connecting the Dots for New Material Development

Microstructure Response to Resultant Bulk

Single Splat
Mechanical Loading Mechanical Response
OurMechanics
Goal:

Application of this multi-scale mechanics correlation for new material development by

cold spray

Efforts underway to study a much harder refractory metals (eg. Ta), where deformation
mechanisms would be significantly different from relatively softer Aluminum alloys

In-situ observation will enable understanding of fundamental deformation mechanisms

Splat Strains Failure Stress
Adhesion Strength Inter-splat Cracks Failure Strain
 Acknowledgements

Grant W911NF15-2-0026 Sample Processing - South Dakota School of Mines & Technology

Microscopy facilities
Presidential Fellowship
Award
Thank you

Pranjal Nautiyal
pnaut001@fiu.edu
pranjaln.23@gmail.com
Back up Slides
Processing:
He as the carrier gas with pressure and temperature at the gun as 3.45
MPa and 384.3°C, respectively
 Recovery resistance (Rs)
BDC
R= = 2.263
E

Y. Chen et al. ACS Appl. Mater. Interf. 1 (2009)

235; Bao et al. Acta Mater. 52 (2004) 5397