AFOSR

EOARD Materials & Nanotech

AFOSR Spring Review
18 March 2011

Lt Col Randall ‘Ty’ Pollak

Program Manager
AFOSR/EOARD
Air Force Office of Scientific Research
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 Discussion

• My background
• Broad portfolio overview
• Challenges & opportunities of interest
• Selected projects

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 Materials Background
My Road to London
• PhD, MS&E, AFIT 2005
Gigacycle fatigue test methods
• AFRL/RX, Oct 05–Jul 06
Metallic thermal protection system roadmap
Electronic and optical materials (line mgmt)
• Naval Postgraduate School, Jul 07–Sep 10
Modeling Lamb waves for crack detection (SHM)
Carbon nanotubes (CNTs) for crack detection,
strengthened joints, and heat xfer nanofluids Clustered network of CNTs
Bily/Kwon/Pollak, Appl Compos Mater 17 (2010)

CNT nanofluid
CNTs functionalized with carboxyl side groups
Maximum likelihood analysis of Ti-6Al-4V data Burkholder/Kwon/Pollak, J Mater Sci (2011) 3
Pollak/Palazotto, Probabilist Eng Mech 24 (2009)
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 EOARD Portfolio Overview

NAME: Lt Col Pollak

BRIEF DESCRIPTION OF PORTFOLIO:

Find, fund, and/or facilitate Materials S&T in Europe, Middle East, former
Soviet Union, and Africa for future air, space, cyberspace applications

LIST SUB-AREAS IN PORTFOLIO:

Structural & extreme Materials for energy

environment materials applications

Electronic, optical, & Materials development

magnetic materials & modeling tools

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Belgium
2-D conjugated polymers
UK
Morphing skin materials
High strain rate analysis
Switzerland
High-thruput tribology
France
Multiscale modeling
Organic EO polymers
Portugal
Liquid crystals
2010 Active Efforts
The Netherlands Germany
Hybrid superconductors High-throughput experimentation
Atomic clusters
Russia
High-temp superconductors
Ukraine
Tribology & coatings
Super/magneto-elastic alloys
Ceramic composites
Ultrasonic sensing
Romania
Functionalized DNA
Israel
Silicon-air batteries

Morocco & Egypt

CSP only
Italy
Spain Austria & Czech Republic
Catalytic nanostructures
Nano shape memory alloys High-temp nanocoatings 5
Ultra high-temp ceramics
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 Which Way to Go?

Electronic, optical, Materials for

magnetic materials energy

Structural /
Materials extreme
tools environment
materials

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 Evolution of Materials Science
Shaping Challenges & Opportunities Ahead
YESTERDAY / TODAY TODAY / TOMORROW
Processing Properties Integrated and
Structure
as output inverse design
Properties

Performance

Design / analysis at
micro-level Design / analysis at
0.1
0.0
1.0

0.9
nano & atomic-level
0.2
0.8
0.3

]
.%
0.7

Pt
[at
High-throughput methods

[at
0.4
0.6

Pd

.%
]
0.5
0.5
0.6
0.4

1 test  1 data point 0.7

0.8
0.3

0.2
0.9
0.1
1.0
0.0
0.0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1.0

Fe [at.%]

Descriptive modeling Predictive modeling

Destructive / post- Non-invasive / near

mortem imaging real-time imaging
7
 Broad Scientific Challenges
…and Transformational Opportunities
• Predicting compositions and micro/nanostructures of interest for
structural, high temperature, and other materials
 Ab initio methods, multi-scale methods, improving computational efficiency
• Rapid screening for mechanical and environmental properties
 Bulk properties vs. micro/nano-scale properties, methods of accelerating
degradation, novel rapid fabrication techniques
• Utilizing more available data from conventional tests
 Volumetric imaging, quantification of features, novel test techniques
• Consideration to actual state & its evolution in predictive models
 Get ―enough but no more‖ data to characterize state, correlate / validate
SHM/NDE techniques, appropriate inputs to damage models
• Other emerging capabilities of AFRL interest?
Enabling future capabilities…
-- Tailor the material systems and structures for the application
-- Efficiently screen and test to validate models and optimize parameters
-- Predict residual properties based on actual state of component 8
 Selected Projects

• High-throughput experimentation
• Nanopillar shape memory alloys
• Morphing skin materials
• High strain rate simulation
• X-ray tomography for composites fatigue

9
 High-Throughput Experimentation
Optical Screening for Amorphous Materials
Prof Alfred Ludwig, Ruhr Univ Bochum (Germany), Sep 2010 – Aug 2011
EOARD funded (Materials & Space Tech)
Tech POC: Dr Dan Miracle, RXB
Unique combinatorial sputtering system

Challenge: Metallic glasses are of interest due to remarkable

properties (strength, ductility, corrosion resistance)… but time
consuming and expensive to wade through solution space
Objective: Rapidly develop materials libraries of metallic
glasses which exhibit high crystallization temps and superior
corrosion resistance in O2 environment Alloy gradient compositions using 10
up to 5 targets on 4-inch wafers
Images: Ludwig and RUB Dept of Micro & Nano Materials website
 High-Throughput Experimentation
(continued)
Approach: Automated x-ray diffraction of wafers
(capability -100ºC to 900ºC)
1. Deposit amorphous thin films
2. Determine compositions through automated EDX
3. Characterize structure through automated XRD
and high-throughput resistivity tests as f(T)
4. Develop optical screening method based on
change in reflectivity upon phase change
5. Use reflectivity changes to characterize corrosion
resistance for alloys with high crystallization temp
-1.000
0.0
1.0 0.3667
0.0035 Resistivity changes indicate crystallization First results of parallel optical screening 1.733
3.100
0.1
of oxidation in air for Fe-Pt-Pd system 0.9 Color code: 4.467
5.833
0.00.2 Intensity change 7.200
1.0 0.8 8.567
proportional to 9.933
0.0030 689 K 0.10.3 oxidation 11.30

]
0.9

.%
0.0 0.7 12.67

Pt
1.0 14.03

[at
0.20.4

[at
15.40
0.1 0.8 0.6

Pd
16.77

.%
0.9
 [Ohm*m]

18.13
0.30.5

]
Ramp rate: 1.7 K/s

]
0.0025 19.50

.%
0.2 0.7 0.5

Pt
20.87
0.8

[at
22.23

[at
0.40.6 23.60
0.6

Pd
0.3 0.4

.%
]
24.97

.%
0.7

Pt
(Amorphous Ni-Ti- 26.33

]
0.50.7

[at
27.70
0.5

[at
0.4 0.3
0.0020 based alloy) Pd 0.6
29.07

.%
30.43
0.60.8 31.80
717 K 0.4

]
0.5 0.2 33.17
0.5 34.53
0.70.9 35.90
0.6 0.3 0.1 37.27

0.0015
0.7
0.81.0
0.4

0.3
0.2 0.0
40°C
38.63
40.00

0.9 0.0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1.0
0.8 0.1

0.0010 0.9
1.0
0.2
Fe [at.%]
0.0
190°C
300 400 500 600 700 800 900 0.0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.1 0.8 0.9 1.0
1.0
Fe [at.%] 0.0
T [K] 0.0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1.0 210°C 11
Images: Ludwig and RUB Dept of Micro & Nano Materials website Fe [at.%]
 Nanopillar Shape Memory Alloys
Nanostructures for Ultra High Damping
Prof Jose San Juan, Univ of Basque Country (Spain), Jul 2010 – Jul 2011
EOARD funded 1st year  AFOSR planning 2nd year (Dr Les Lee)
FIB milling
Challenge: Materials with significant energy absorption / damping
capability needed for blast mitigation and vibration suppression
Objective: Develop large area micro/nano pillars of Cu-Al-Ni shape
memory alloy (SMA) exhibiting high damping (Phase 2—multilayers)

Damping comparison

Damping proportional
to area enclosed

12
Images: San Juan and San Juan/Nó/Shuh, Nat Nanotechnol 4 (2009)
 Nanopillar Shape Memory Alloys
(continued)
SMA transformation

II to III Martensite variants compatible

with the applied stress are induced

II. At a critical stress c III. All the Austenite could be

Martensite is induced transformed to Martensite

Recovery when the stress is withdrawn

I. Elastic deformation IV. The transformation is

of the Austenite Pillar reversible during unloading

Micro/nanopillar testing has shown

Approach (Phase 1):
100s of cycles w/o residual strain
1. Produce single crystal Cu-Al-Ni slides
2. Produce micro-pillar arrays by optical microlithography (design/optimize process)
3. Characterize microstructure and martensitic transformation (SEM/SPM)
4. Nano-indentation & nano-compression of individual pillars – compare to FIB samples
5. Design new micro-compression test for multi-pillar array 13
Images: San Juan and San Juan/Nó/Shuh, Adv Mater 20 (2008)
 Development of Morphing Skins
Example of a Transition Success
Dr Prasad Potluri, Univ of Manchester (UK), Sep 2008 – Nov 2010
EOARD seed funds  AFRL/RX funding
Tech POC: Dr Jeff Baur, RXBC
Challenge: Morphing skin materials must
allow large area change yet remain strong
Woven/cross-ply reduces area in shear,
but not extensional deformation; while
knitted fabrics have limited elongation
range, less strength, harder to manufacture

Objective: Develop hyper-elastic yarns for use in woven/cross-ply fabrics

Tunable by altering
Low modulus
parameters
High modulus

Knee point
14
Images: Potluri, AFRL-AFOSR-UK-TR-2010-0003
 Development of Morphing Skins
(continued)

Biaxial braid set-up

Triaxial braided yarn

Relaxed vs. stretched

Creating a biaxial braided sample
(larger extensions in triaxial)

15
Images: Potluri, AFRL-AFOSR-UK-TR-2010-0003
 Development of Morphing Skins
(continued)

Results: Experimental testing & analytical

modeling of yarns in tension  skin material
then manufactured, tested, and modeled

Triaxial yarns with

silicone matrix

Influence of matrix
modulus (E)
Added: Development and shipment
of 3-D weaving machine for AFRL/RX
(next slide)

16
Images: Potluri, AFRL-AFOSR-UK-TR-2010-0003
 Development of Morphing Skins
(continued)

To be shipped to AFRL/RX after training at

Univ of Manchester (Spring 2011)

Possibilities for use and further collaboration:

• Design/manufacture 3D woven preforms with
various fibers (carbon, glass, ceramic, hybrids)
• Geometrical and meso-mechanical modeling of
textile composites
• Modeling of 3D woven preforms subjected to
forming forces (compaction, in-plane shear,
biaxial tension and bending)
• Addition of smart sensors/actuators in 3D weaves
• Development of novel morphing skins

17
Image: Potluri, development as of Jan 2010
 High Strain Rate Analysis
Using Low Strain Rate Analogue
Dr Clive Siviour, Univ of Oxford (UK), Sep 2009 – Sep 2013
AFRL/RW funding, Tech POC: Dr Jennifer Jordan, RWME
Challenge: Mechanical response and damage at high strain rates is of key importance to
design more tolerant and functional materials, but timescales of real-time diagnostics and
imaging techniques are generally inadequate at high strain rates
Objective: Develop analogue techniques using low strain rate tests at different temperatures
to mimic high strain rate behavior

Polymers (e.g., rubbers in

plastic bonded explosives)
are particularly difficult to
characterize at high rates
• Project will study PVC w/ plasticizer

Funding 3-year PhD student

(extension to 4 years due to
delay in matriculation)
• WOS to Eglin planned for Jun 11

18
Images: Moser/Nau (Fraunhofer EMI), from High Resolution Damage Diagnostics & Predictive Modeling Workshop (2010)
 Growing Interest in 3-D
Characterization Methods
160
DARPA/ONR Dynamic 3-D Digital
140 Structure Program (FY05-10)

120

100
Publications*

Snapshots of growing grain using x-ray topotomography

Ludwig et al, Mat Sci Eng A-Strut 524 (2009)
80

Jun 2010 – ONRG Workshop I

60 Mar 2011 – ONRG/EOARD Workshop II

40

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* ISI Web of Science search: ―x-ray‖ + ―tomography‖ (for subject areas which include ―materials science‖)
 3-D Characterization Example
Fatigue of Low-Cost Composites using XCT

First of its kind void analysis and

comparison with fatigue performance
 Only possible thru non-invasive CT

Micro XCT imaging

  

Reconstructed microstructure of glass/epoxy specimen

20
Images: Lambert/Chambers/Sinclair/Spearing , Univ of Southampton (publication in preparation, used with permission)
 3-D Characterization Example
(continued)
Data for compressive failures under fully-reversed loading:
Specimen Cycles to Number of Void Average Volume of Total
failure voids in content void the largest volume of
() analysis (%) volume single void largest 1%
volume (mm3) (mm3) of voids
(mm3)
C9 21,649 9,831 3.22 0.0119 2.48 42.29
C14 32,003 10,598 2.95 0.0115 2.10 40.18
C10 59,697 14,255 2.75 0.007 1.62 40.33
C13 60,710 10,583 3.27 0.0115 1.79 40.11
C20 107,725 10,827 2.52 0.0087 0.89 31.70

120,000

100,000
Life (cycles) 

80,000

60,000

40,000

20,000
Largest Void Volume (mm3)  Inner ply delamination reduced
0
0 0.5 1 1.5 2 2.5 3
global buckling load by 87%
21
Data and Micrographs: Lambert/Chambers/Sinclair/Spearing , Univ of Southampton (publication in preparation, used with permission)
 Understanding Fatigue Damage in
Composites through Microtomography
Prof Ian Sinclair and Prof Mark Spearing, IN DEVELOPMENT FOR 2011
EOARD (w/ ONRG contribution) to fund 3-yr PhD student
Challenge: Accurate modeling / prediction of damage processes in composites requires
identification, quantification, and understanding of key internal microscale features
Objective: Use high-res XCT to investigate fatigue of fiber-reinforced aerospace composite
– identify critical features, develop detection techniques, statistically quantify, link to models
Expected Payoffs: Insights, inputs, and validation for AFRL composite materials damage
modeling, jumping point for future investigations exploiting tomography data

Transverse (90º) cracking

Longitudinal (0º) cracking

Delamination

0º fiber breaks
22
In situ XCT of carbon/epoxy composite damage
Images: Sinclair/Spearing
 Theme for Way Ahead

Needs
• Better / more predictive modeling
• Optimizing parameters at nanoscale
• Reduce materials development cycle
Background
• Failure of structural materials
• Nanotech for structural,
thermal, & health monitoring
• Probabilistics / T&E / Sys Eng

Reduce development cycle by

developing novel data-rich
methods to predict, develop, test,
& monitor aerospace materials
Opportunities
• European excellence in hybrids and composites
• High-throughput experimental and predictive technologies
• High-resolution imaging capabilities
• DoD interest and activity in non-invasive characterization 23
 Wrap Up

• Portfolio spans materials

spectrum supporting AFRL
• Looking for technologies with
relatively broad impact to reduce
materials development cycle
• Emphasis on structural and
environmental, but not exclusive

Lt Col Randall ‗Ty‘ Pollak DSN 314-235-6115

EOARD Comm +44 1895-616115
Unit 4515 randall.pollak@london.af.mil
APO, AE 09421-0014 (randall.pollak@us.af.mil)

24
 AFRL Technical Links
Materials & Manufacturing
Air Vehicles
RXL – Metals, Ceramics, NDE
Dr Mike Cinibulk (ceramics) Dr Ed Forster (hybrid materials)
Dr Dennis Dimiduk (computational MS&E)
Dr Jim Larsen (behavior & life prediction)
Dr Eric Lindgren (non-destructive evaluation)
Dr Pat Martin (metals)
Dr Lee Semiatin (processing) AFOSR
Dr Mike Uchic (microscale testing)
Dr Michael Berman
RXB – Nonmetallic Materials Dr Hugh DeLong
Mr Max Alexander (EM hardening materials) Dr Fariba Fahroo
Propulsion Dr Charles Lee
Dr Jeff Baur (hybrids, composites)
Dr Rick Hall (computational methods) Dr Nelson Forster (engine materials) Dr Les Lee
Dr Benji Maruyama (carbon nanotubes) Dr Lewis Rosado (engine materials) Dr Mark Maurice
Dr Dan Miracle (nanotech, amorphous) Dr Larry Scanlon (solid state ionics) Dr Ali Sayir
Dr David Mollenhauer (composites) Dr David Stargel
Dr Rajesh Naik (nanomaterials)
Dr Ajit Roy (thermal transport materials)
Dr Andrey Voevodin (high temp materials)
Munitions
RXP – Survivability & Sensor Materials Dr Bill Cooper (blast effects & energetics)
Dr Jim Grote (organic polymer photonics) Dr Jennifer Jordan (energetic materials)
Dr Ruth Pachter (materials modeling)
Dr Augustine Urbas (metamaterials) Continue to develop based on needs and opportunities… 25

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