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NHSC Materials & Structures

David Marshall
Teledyne Scientific
Thousand Oaks, CA
dmarshall@teledyne.com
805-373-4170
Annual Review
Washington, August 6, 2013
NHSC-Materials & Structures Overview
www.nhsc-ms.net
NHSC Materials & Structures
UC Berkeley/ALS
R. Ritchie (mechanics,
imaging) Combine experiments and
multi-scale models into a
virtual test system
Computational tools
new experimental methods
new materials &
processing science
Teledyne Scientific
D. Marshall (materials & structures)
B. Cox (mechanics of materials)
UC Santa Barbara
F. Zok (structural materials)

U. of Texas
P. Kroll
(atomistics)
Missouri University
W. Fahrenholtz
G. Hilmas
(UHTCs)
U. of Colorado
R. Raj (high temp.
materials & properties)
U. of Miami
Q. Yang
(mechanics)
Collaborations, test and advisory support
AFRL/WPAFB (M. Cinibulk, T Parthasarathy)
ALS Berkeley, NASA, Boeing, ATK, Lockheed-Martin
AFOSR: A. Sayir
NASA: A. Calomino
National Hypersonic Science Center for
Materials and Structures
NHSC Materials & Structures
NHSC Materials & Structures
Highly integrated research program: graduate students & post docs
48 journal publications; 23 plenary/keynote presentations at
international conferences (including Mueller award lecture at
ICACC'12, 4 lectures at 2012 Ceramics Gordon Conference); 21
invited presentations at conferences; 16 conference proceedings;
30 other conference papers
Organized International Summer School on Materials for
Hypersonics, UCSB, Aug. 2011
Organized International workshop on high-temperature ceramic
composites, Boulder CO June 12-15 2012 www.engineceramics.org
Organized International conference on UHTCs, Austria, May 2013
Organized 7 Symposia at international meetings
Active collaborations with 10 universities
Sharing of data & modeling with AFRL, Army, NASA, Rolls Royce,
GE, DTU Denmark
NHSC-MS highlights
NHSC Materials & Structures
Univ. of Canterbury, NZ (S. Krumdieck, Raj, Marshall): PP-MOCVD
Univ. of Queensland, Australia (M. Smart, Marshall, Zok): Fabrication, laser
testing and modeling of non-eroding ablatively cooled materials
Univ. of Virginia (E. Opila, Hilmas, Fahrenholtz, Kroll, Raj, Marshall): O
18

diffusion studies in UHTCs and PDCs
von Karman Institute, SRI, U. Vermont (J. Marschall, Hilmas, Fahrenholtz):
plasmatron testing of UHTC materials
SRI (J. Marschall, Raj): atomic oxygen testing of Hf-O-Si-C systems
Leoben, Austria (G Dehm, Raj): high resolution and analytical TEM of UHTC
materials
Univ. Southampton (M. Spearing, Cox): Tomography of damage in composites
Kath. Univ. Leuven (S. Lomov, Cox): composite modeling
Loughborough Univ., UK (Cox): composite modeling
Univ. of Melbourne, Australia (Cox): composite modeling
RMIT, Australia (Chun, Yang): composite modeling
Tokyo Inst. Tech. (Y. Shinoda, Raj): PDC/HfO2 nanocomposite matrix
Active collaborations
NHSC Materials & Structures
Sustained hypersonic flight at high Mach No. limited by materials:
- High heat flux & heat loads
- High T, oxidation, shear, erosive conditions
- Active cooling -> very high thermal gradients
- Conditions vary with location
Materials and Structures for Propulsion Flowpath
Sharp leading edges
-Very high heat flux, small area
-Active cooling/heat pipes
possible, not preferred
UHTCs
- very high T, high conductivity
- limitation: oxidation resistance
Flowpath surfaces
Large area: weight critical
Active cooling in some regions
CMCs:
x3 weight reduction c.f. metals
Reduced heat flux absorbed

Selection of materials and conditions
NHSC Materials & Structures
Thin cooled textile-based
CMCs work in extreme heat
flux environments and have
potential to revolutionize
materials & structures for
hypersonics.
cool skin
hot skin
Attachment by compliant truss structure
cool skin
hot skin
Attachment by compliant truss structure
Gas flow
C-SiC composite
wall
Gas flow
Gas flow
C-SiC composite
wall
Gas flow
Morphing structures
What are the barriers to their
use?
- increase stability/life at high
temperatures: oxidation
- high fidelity modeling capability for
damage & lifetime
- improved ability to test materials
CMC s and UHTCs: limitations
UHTCs (diborides) have
temperature capability and
thermal conductivity needed
for sharp leading edges &
struts
Active cooling
ZrB
2
: T> 2000
o
C
NHSC Materials & Structures
Image microstructure
Build hierarchical
geometry generator
Port to computational
mesh for each scale
Constitutive laws
Monte Carlo predictions
- strength, temp, diffusion,
damage
New materials & processing New experimental methods Virtual test
Atomistic modeling
Thermal transport
Structure
Oxygen diffusion
Processing modeling
PP MOCVD
CVD
Liquid precursors
Material synthesis
- Processing (HP, PP-
MOCVD, PIP)
- Properties
- Oxidation resistance
Synchrotron CT
- Imaging microstructure
- In situ testing/imaging
at 1500 C
Laser-based testing
- High thermal gradients
-In situ strain mapping
at high T
Doped diborides
(2000 C)
Hf-PDC based CMCs
(1600 C)
Numerical methods
for discrete damage
(AFEM)
UCB
UCSB/TSC/UCB/UTA
TSC/UCSB
UCSB/Miami
Miami
UTA
UCSB
MS&T
U.Col, TSC
UCB/TSC
UCol
MS&T
TSC
TSC, U.Col, Miami
Miami
Present
Planned
Supply of material and/or data
Present
Planned
Supply of material and/or data
Overview of Research Activities and
Collaborations
NHSC Materials & Structures
Doping ZrB
2
to increase oxidation resistance
Discovery (Hilmas & Fahrenholtz):
-doping with W and other transition metals can reduce
oxidation rate x5

What is the mechanism?
- Promote sintering and densification of ZrO
2
scale?
- Dissolve in glass phase and increase stability?

ZrB
2
Based Ceramics for Hypersonic Flight
Experiments & thermodynamic modeling (Hilmas & Fahrenholtz)
Select dopants (phase diagrams +)
Measure oxidation kinetics/microstructure
Controlled expts.: sintering ZrO2 + B
2
O
3
and B
2
O
3
+TM ;
measure effect of TM on evaporation rate of borate glasses

Atomistics (Kroll)
Effect of dopants on structure & stability of B
2
O
3
glasses
20 m
glass
ZrO
2

+
glass
ZrB
2
- SiC
SiC-depleted
ZrB
2
NHSC Materials & Structures
stable composition:
B
2
Si
2
O
7
(with cryst.
struct.!)
enthalpy of formation from melts
structure change towards sp
3
-B


Atomistic modeling: B
2
O
3
-WO
3
-SiO
2

Adding W increases enthalpy. Solubility limit ~6-10 mol%
Adding W promotes tetrahedral bonding at edge of WO
3

clusters
MS&T synthesizing model glasses for NMR studies
(quantify tetrahedral B)
P. Kroll
(1) Amorphous structures of B
2
O
3
+ WO
3

Adding Si increases enthalpy except for
composition B
2
O
3
+ 2(SiO
2
)
=> New stable structure, B
2
Si
2
O
7
?
(2) Amorphous structures of B
2
O
3
+ SiO
2

metal clustering in SiO
2
and B
2
O
3
(-Ta-O)
5
-

WO
6
-chain

Hf, Nb, Ta, Mo, W additives in borosilicate melts
trend of metal oxide clustering
MS&T: metal segregations might cause layers &
provide oxidation barriers!?
(3) TM-oxides in B
2
O
3
and SiO
2

NHSC Materials & Structures
Key Findings Missouri S&T

1. Studying how TM additions stabilize B
2
O
3
to higher temperatures:
Thermogravimetric analysis showed that TM additions reduce the
evaporation rate of B
2
O
3
, using W, Nb, or Zr additions

Onset of B
2
O
3
evaporation shifts to higher temperatures
Lowest weight losses for Nb
2
O
5
-B
2
O
3
glasses

Molecular dynamics (MD) simulations at UTA (Kroll) predict increased
BO
4
units (increased glass stability) with TM additions
TM-oxide-B
2
O
3
glasses with 2, 4, and 8 mol% W, Nb, or Zr were
prepared
Glasses phase separate to produce nearly pure B
2
O
3
and crystalline TM
oxides during cooling. No BO
4
units were identified at room temperature
using Raman or NMR.
MD models may still be correct, and the glasses need to be characterized
at elevated temperatures (NMR) to compare BO
4
fraction to model
predictions.
10
Doping ZrB
2
to increase oxidation resistance
NHSC Materials & Structures
Key Findings Missouri S&T
2. Studying how TM additions change the oxidation scale morphology:
Pressureless sintering of ZrO
2
and ZrO
2
-B
2
O
3
with 4 or 16 mol% WO
3

Increased ZrO
2
grain size and density - 16 mol% WO
3
most effective
Sub-stoichiometric oxide (TM stabilized?) was detected in the oxidation scale at
the interface between the ZrB
2
matrix and surface oxide layer.
Double oxidation of ZrB
2
-SiC planned (
16
O
2
followed by
18
O
2
), with Univ. of
Virginia (Opila), using TOF-SIMS analysis of
18
O
2
diffusion profile in
16
O
2
oxide
to characterize oxidation kinetics. If initial experiments are successful, additional
ZrB
2
-TM samples will be sent for testing.

3. Testing in relevant environments:
Samples delivered to Univ. of Vermont (Fletcher) for 2
nd
round of ICP testing,
with improved diagnostics of evolved species, to be followed by scale thickness
and microstructural analysis.
Samples delivered to AFRL (Parthasarathy/Cinibulk) for testing in the scramjet
test rig.
11
Doping ZrB
2
to increase oxidation resistance
NHSC Materials & Structures
Ceramic composites (CMCs)
- C-SiC & SiC-SiC based materials
Virtual test
Micro tomography
(Ritchie)
DIC (Zok)
Geometry generator
(Cox)
Mesh generator
(Cox)
micro tomography
(Ritchie)
DIC (Zok)
AFM (Yang)
Matrix & coating
materials
Comparisons expt.
DIC (Zok)
AFM (Yang)
material compositions
oxidn. behavior
oxidn. mechanisms
(Raj)
Atomistics (Kroll)
- Effect of Hf on
structure & stability of
PDCs
Hf-Si-C-O-N material
system

angle interlock weaves
10 m
HfO2
reinfiltrated
Hf-PDC in
shrinkage
crack
Hf-PDC
GB phase
rigid scaffold
rigid network of
large particles
Multilayer
HfO2/PDC
CVD
SiC
fiber
tow
HfO2
Hf-PDC
HfO2
1 mm
0.1 m
1 m
10 m
HfO2
reinfiltrated
Hf-PDC in
shrinkage
crack
Hf-PDC
GB phase
rigid scaffold
rigid network of
large particles
Multilayer
HfO2/PDC
CVD
SiC
fiber
tow
Multilayer
HfO2/PDC
CVD
SiC
fiber
tow
HfO2
Hf-PDC
HfO2
1 mm
0.1 m
1 m
NHSC Materials & Structures
New high temperature oxidation-resistant
materials for matrices & coatings
PDCs contain excess carbon
relative to stoichiometric
compositions of Si-C-N-O.
Evidence for segregated carbon network
inhibiting diffusion
Extreme reactivity during pyrolysis (800
1000
o
C) produces good bonding with oxides
and nonoxides
Form unusual phases with transition metal
oxides, e.g. zircon, hafnon. How effective are
they in protecting against UHT oxidation?
Ionescu, Papendorf, Kleebe, Poli, Mu ller, Riedel
J. Am. Ceram. Soc., 93 [6] 17741782 (2010)
Raj, Kroll, Marshall
Hf segregation in
Hf-SiCNO powder 50 h / 1500
o
C
Polymer-derived ceramics (SiCNO, SiCO)
NHSC Materials & Structures
New high Temp oxidation-resistant
materials for matrices & coatings
Hf-SiCNO polymer-derived ceramics
Experiments & thermodynamic modeling (Raj)
Selection of dopants (bond energy considerations)
Measurements of oxidation kinetics and relation to
microstructure
Processing development and modeling to form
matrices and coatings
- 100% PDC: Molecularly mixed HfSiCNO
- nanoHfO
2
+ 10-20vol%PDC
- dual Phase HfO
2
/SiC NanoComposites
Atomistics (Kroll)
Atomic structure
What are the rate-limiting diffusion paths?
What is the role of carbon sheets: barrier to diffusion or
easy path for diffusion?
What is the role of dopant atoms?
2.0m
1.5m 1.5m
Defect Site
1 m
SiC
1500C, 10hrs
2.0m
1.5m 1.5m
Defect Site
1 m
SiC
1500C, 10hrs
HfSiCNO Matrix (infiltration)
NHSC Materials & Structures
Hf-SiCNO polymer-derived ceramics
Experiments & thermodynamic modeling (Raj)
Increases thermal conductivity
Strength retention at 1600C
HfO
2
/SiC nano composites
1600
o
C 100h, ambient air
Oxidation and phase transformation in HfSiCNO / HfO
2
materials
HfO
2
(light)

HfSiO
4
(dark)

Unoxidized

Oxide layer

Hf-Si-C-N
1500
o
C 1000 hours
Solubility limit of Hf and phase evolution in oxidizing & inert
environments measured
Oxidation rate in dry O
2
not reduced relative to SiC
Ready formation of hafnon in relatively dense surface layer of
hafnon/HfO
2
-> potential for better performance in water vapor
environments
Evidence for improved resistance to erosion in flowing water vapor
Bubble formation at SiO
2
/SiC interface found to be a limiting
mechanism - bubble formation inhibited in Hf-Si-C-N-O system
Modeling provides new insights:
- oxidation map defines ranges of pO
2
/Temp conditions for bubble
formation
- bubble nucleation critical
- role of interface/surface energies & dopants -> atomistic
calculations
NHSC Materials & Structures
Atomistic modeling
ideal Si-O-Si bridges may cover SiC(100)
some bonds to SiO
2
-matrix favorable
large voids formed
interface energy computed: 1.4 J/m
2

UTA & CU Boulder: how will HfO
2
impact interface
and, ultimately, CO bubble formation
P. Kroll
(i) SiC-SiO
2
-interfaces
Atomistic modeling
Interfaces in SiCO ceramics: at the oxidation front
SiC-SiO
2
-interface: balancing bonds and bridges
Interface energy 1.4 J/m
2
attaching graphene layers to 2H-SiC
how graphene bonds to SiC
various bonding modes encountered
NMR signals identifying interface features
(ii) SiC-C interfaces
Current work & outlook
metal oxides in SiBO; thermodynamics
favorable interfaces, , (theor.) yield strength
coarsed-grained kinetic MC modeling
NHSC Materials & Structures
enthalpy of formation for melts
local environments &Raman-spectroscopy
Atomistic modeling
bond population paralleling Raman data
solubility limit of HfO
2
in SiCNO <1 mol%
HfO
n
-polyhedra tend to cluster
CU Boulder: Raman spectroscopy &
detecting limiting solubility of HfO
2
in HfSiCNO
P. Kroll
Modeling HfSiCNO compounds
in SiO
2
AH
mix
1.2 eV/HfO
2
, => early coarsening

in B
2
O
3
AH
mix
0.54 eV/HfO
2
, => higher solubility
CU Boulder: coarsening of HfO
2
-SiO
2
films
Solubility of HfO
2
in B
2
O
3
and SiO
2

A
H
i
n
s
e
r
t

[
e
V
]

# HfO
2
units added
NHSC Materials & Structures
Virtual test studies: controlled
variations/defects in weave structure
C-SiC composite
- 2-layer angle interlock weave
- CVI fiber coatings
- polymer-derived matrix
- controlled weave defects
Local
shear
bands
Uniform
shear
hole
Larger weft
spacing
NHSC Materials & Structures
Current experiments for Virtual test
C-SiC composite test specimens with
controlled defects in woven preform
- Through-thickness holes, local weave distortion,
global shear (10%), localized shear band
- Imaging by CT to provide tow geometry as input for
A-FEM
- DIC for long range geometry characterization
- Load in tension with DIC and CT to observe
damage development
- Calibrate cohesive law with tests on composites with
undisturbed weave structure
- directly compare AFEM predictions and DIC
observations of damage development in the
defective composite specimens
- Assess sensitivity of composite properties to weave
defects
NHSC Materials & Structures
3-D microstructural characterization
& geometry generator: unit cell level
Compound visualization of statistical parameters
5
m
m
Compound visualization of statistical parameters
5
m
m
Tow cross
sectional
area
M. Blacklock, B. Cox
3-D image of C-SiC
composite
computational mesh
from geometric model
analogue of Markov
chain method for tow
axis coordinates
stochastic irregular
elliptical cylinder for
each tow
problem: interpenetration
solution: enforce known
topology of textile
Statistical description of geometry
Tow paths
Cross-sectional areas
Orientation of cross section
Deviations from mean
Correlation lengths
create replicas of textile
reinforcement with same
statistics as those measured
NHSC Materials & Structures
Individual fiber path within a fiber
bundle mapped
Matrix porosity measure
3D Spatial information of voids
3D spatial information of fibers
for modeling fibers in tows
Colors indicate individual
segmented fiber within the entire
bundle

3-D X-ray CT microstructural
characterization: fiber level
HiNicalon-S mini composite
H Bale
NHSC Materials & Structures
3-D microstructural characterization
& geometry generator
length scales > unit cell
DIC measurements to map warp
crown positions
Fourier analysis
Autocorrelation analysis for long
range variations
Spatial derivatives of deviations
from ideal weave structure

Input for geametry generator

M. N. Rossol, T. Fast, D.B. Marshall, B.N. Cox, F.W. Zok, Characterizing in-
plane geometrical variability in textile ceramic composites, 2013
M. Rossol
NHSC Materials & Structures
Synchrotron imaging of structure and damage
Compound visualization of statistical parameters
5
m
m
Compound visualization of statistical parameters
5
m
m
Tow cross
sectional
area
3-D microstructural
characterization &
geometry generator
8 8 octopole octopole 1000W 1000W
IR lamps IR lamps
X X- -rays
rays
dog dog- -bone bone
sample sample
water water
cooling cooling
and sample and sample
mount access mount access
360 deg 360 deg
thin window thin window
0.25 mm Al 0.25 mm Al
Lamp
Lamp
Lamp
Lamp
Lamp
to load cell and water cooling to load cell and water cooling
guideway guideway
motor and motor and
gearbox gearbox
X-rays
load cell load cell
furnace furnace
section section
with with
active active
cooling cooling
Octopole Octopole IR lamp IR lamp
arrangement arrangement
water water
cooling cooling
LBNL design : LBNL design : J.Nasiatka J.Nasiatka, , A.MacDowell A.MacDowell
8 8 octopole octopole 1000W 1000W
IR lamps IR lamps
X X- -rays
rays
dog dog- -bone bone
sample sample
water water
cooling cooling
and sample and sample
mount access mount access
360 deg 360 deg
thin window thin window
0.25 mm Al 0.25 mm Al
Lamp
Lamp
Lamp
Lamp
Lamp
to load cell and water cooling to load cell and water cooling
guideway guideway
motor and motor and
gearbox gearbox
X-rays
load cell load cell
furnace furnace
section section
with with
active active
cooling cooling
Octopole Octopole IR lamp IR lamp
arrangement arrangement
water water
cooling cooling
LBNL design : LBNL design : J.Nasiatka J.Nasiatka, , A.MacDowell A.MacDowell
crack
2D 2D tomographic tomographic slices with no load slices with no load
SiC-SiC composite: RT in situ loading
High temperature in situ stage (1700
o
C)
Resolution < 1m
Input to constitutive
law calibration in
virtual test
R. Ritchie, H. Bale,
Cox, Marshall
NHSC Materials & Structures
In-situ testing on single tow SiC
f
/ SiC
m
in tension at 1750C
Load Extension Curve
(Single tow 1750C)
0
20
40
60
80
100
120
140
160
0.00 0.05 0.10 0.15 0.20 0.25 0.30 0.35
Extension (mm)
L
o
a
d

(
N
)
H. Bale
Bale, Haboub, MacDowell, Nasiatka, Parkinson, Cox, Marshall , Ritchie, Nature Materials, 2013
NHSC Materials & Structures
In-situ testing on a three layer angle
interlock ceramic textile specimen under
tension at 1750C

False colors indicate tests carried at
ultra high temperatures.
Click on the plot to run animation
Load Extension Curve
(Textile 1750C)
0
20
40
60
80
100
120
140
160
180
0 0.1 0.2 0.3 0.4 0.5 0.6
Extension (mm)
L
o
a
d

(
N
)
H. Bale
Bale, Haboub, MacDowell, Nasiatka, Parkinson, Cox, Marshall , Ritchie, Nature Materials, 2013
NHSC Materials & Structures
At room temp. At 1850C at 100N
Fiber
matrix
matrix
BN
BN
SiO
2
High temperature in situ tomography
- Increased Image resolution
SEM Image
detection of fiber coating damage
H. Bale
NHSC Materials & Structures
SiCSiC woven composites (25
o
1750
o
C)

SiCSiC single-tow mini-composites
- Influence of notches at 25
o
1750
o
C
- degradation of BN coatings at 1850
o
C
- controlled oxidation at 1500
o
C
- creep
High temperature in situ tomography
- New in situ tests
SiO
2
NHSC Materials & Structures
Damage evolution
length scales > unit cell
John Shaw
Hole in
fabric
Pristine
Drilled
hole
0.1% global strain
Surface profile Surface profile 0.4% strain
After failure
In situ measurement of surface
strains by DIC
Direct correlation of crack locations
with underlying weave structure
Post-mortem cross sections for
depth information
warp & weft loading directions;
pristine and defect weave
structures; drilled holes
NHSC Materials & Structures
Numerical methods for discrete
damage evolution: A-FEM
Account for multiple, arbitrary, interacting intra-element discontinuities (cracks,
material boundaries) without additional external nodes or degrees of freedom
Used with standard FEM solvers (ABAQUS)
Explicit element equilibrium equation => numerical accuracy, efficiency, &
robustness
Improvement in numerical efficiency >100 c.f. X-FEM
Enables unified treatment of evolution from a weak discontinuity to a strong
discontinuity within single element
Extended to 3-D
- no need for additional DoFs (as in X-FEM) or pre-assigned phantom nodes
- no need for algorithm to track and project evolution of crack as in X-FEM & PNM
- constitutive law calibration & comparison of simulations with DIC & -CT
Q. Yang
(a) (b)
x
y
+
O
5'
6'

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5
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( )
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o o
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(c)
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(a) (b)
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2
u
4
6'
4 4
,
x
F u
4 4
,
y
F v
l
+
O
8'
1
u

O
(c)
(b) Mode -II traction-separation law
1 s
o
sc
o
2 s
o
s
o
1 s
o
sc
o
2 s
o
2
t
1
t
t
1
t
2
t
* s
o
*
t
1
4
3
2
5
GII
1
o
2
o
1 n
o
o
2 n
o
nc
o
n
o
(a) Mode I traction-separation law
*
o
* n
o
1
4
3
2
5
GI
*
t
Augmented finite element method (A-FEM)
NHSC Materials & Structures
Comparison of 2-D simulation
and in situ tomography
In situ tomography 1750
o
C
NHSC Materials & Structures
Surface profile 0.05% global strain
0.1% global strain
0.2% global strain 0.4% global strain 0.61% (failure)
Comparison: 3-D AFEM with DIC
measurements of multiple crack evolution
0.1%
0.05%
0.2%
0.4%
NHSC Materials & Structures
Some next steps for Virtual test
Expand the virtual test tools and capabilities
- Virtual test pipeline for other test cases & loading
configurations
- Explore sensitivity of properties to statistical
variability in microstructure
- Sensitivity matrix for constitutive properties
- Controlled variability in fiber tow architectures
- Non-sequential correlations in geometry generation
(e.g., for long-range preform distortions)
- Fiber-scale geometry characterization and nonlinear
fracture