Alabama Center for Nanostructured
Materials (ACNM)
Mahesh V. Hosur, PI/Director
Center for Advanced Materials
Tuskegee University
Tuskegee, AL 36088
Annual EPSCoR Meeting, Feb. 13, 2007, Huntsville, AL
ACNM Mission/Goals
•
Synthesize
and
produce
bulk
nanocrystalline
materials
and
develop
new
materials
with
enhanced
thermal,
physical
and
mechanical
properties
•
Integrate
research
and
education
in
the
area
of
Nanotechnology
•
Initiate
new,
as
well
as
enhance
existing
partnerships
with
industry
and
academia
to
attract
new
funding
through
development
of
joint
proposals
•
Educate
and
graduate
underrepresented
students
with
expertise
in
the
area
of
Nanotechnology
•
Conduct
National
and
regional
workshops,
summer
high
school
and
undergraduate
student
internship
programs
Research, Education, Training and Outreach
Personnel
University
Faculty
Grad.
Students
Undergrad.
Students
High School
Students
Tuskegee
5
18
8
8
Alabama A& M
8
4
5
-
Auburn
1
1
-
-
UAH
3
5
1
-
USA
1
1
1
-
18
29
15
8
Out of 29 graduate students, 15 are PhD students with 8 of them being
African
-
Americans, 5PhD students are being supported by the alabama
State Graduate Student Research Program
It is anticipated that at least 5 PhD students will graduate by May 2008
GSRP Awardees
Ivy K. Jones Wanda D. Jones Merlin Theodore
Jean Michael Taguenang
Bopah Chhay
ACNM Outcomes
•
Journal/conference Publications: 64
•
Presentations at the national and international conferences
•
Organizing and chairing sessions at international conferences
•
M.S. Thesis (5), Undergraduate technical reports
•
Summer high school program
•
Graduate courses in Nanotechnology at TU and USA
•
Participation of students in oral and poster presentation
competitions
•
Increased number of proposals submitted and funded
•
Publicity
–
Visit to the center by President Bush, April 19, 2006
–
First article of TU EPSCoR program appeared in Montgomery
advertiser on July 25, 2005:
http://www.montgomeryadvertiser.com/NEWSV5/storyV5tuske
gee25w.htm
President Bush Visits Tuskegee University
Center for Advanced Materials (T
-
CAM)
-
April 19, 2006
“I met some students who knew lot about nanotechnology
-
PhD candidates who knew
lot about nanotechnology”
-
President Bush, April 19, 2006
Summer High School Program
Eric Rousell, Jr.
Selma Early College High School (10th grade)
Future Career: Aerospace or Marine
Engineering
While in this program, I learned about
Material Science and Engineering. We also
learned about nanotechnology and how it is
being applied in numerous applications in our
everyday lives. I learned a lot and would like
to come back next year.
-----
Eric Rousell, Jr.
Summer 2006 High School Students
with their mentors
Collaborations
National/Federal Labs: Oak Ridge National Laboratory,
National High Magnetic Filed Laboratory, ARL, AFRL,
Navy, NRL, ORNL, NASA
-
MSFC
Academia: Cornell, Purdue, Univ. of Delaware, Mississippi
State University, Carnegie Mellon Univ., University of
Alabama, Tuscaloosa, Florida State University
Industry: Raytheon, Boeing, IBM, USP
International: Japanese National Institute for Metals,
University of Liverpool
Course Development
Nanocomposite Materials (Dr. Rangari, TU with Dr.
Anter from FSU, 10 students)
•
Nanoscale material synthesis, properties and applications
•
Theory, modeling and simulation studies
•
Synthesis mechanisms and morphological changes in nanoscale
materials systems, as well as the properties of materials at the
nanoscale
Nanocomposites (Dr. Parker, USA, 16 students)
•
Dielectric, electric, magnetic, optical and mechanical properties of
nanocomposites
•
Research and analyze published work dealing with
applications
Research Themes
•
Synthesis,
Processing,
Modeling,
Characterization
of
nanophased
fibers,
matrices,
composites,
and
sandwich
constructions
(Tuskegee)
•
Nano
-
layered
nanoparticles,
Glassy
Polymeric
Composites
(Alabama
A
&
M,
Tuskegee)
•
Molecular
Dynamic
simulations
(Auburn)
•
Modeling
and
processing
of
nanoparticles
under
the
influence
of
magnetic
field
(Univ
.
of
South
Alabama,
Tuskegee)
•
LC
Based
Chemical
and
Biological
Sensor
Using
Capacitive
Transduction,
Integrated
Nanophotonics,
LC
Polar
Anchoring
Measurements
(Univ
.
of
Alabama,
Huntsville)
Thermal and Mechanical Properties of CNF/
Epoxy Nanocomposite
Matrix: SC
-
15 Epoxy
Reinforcement: Carbon Nano Fiber
0 wt. %, 1 wt. %, 2 wt. % and 3 wt. %
Storage
Modulus
70
%
improvement
Glass Transition Temp.
7
o
C
increase
Tensile Modulus
17.4%
improvement
Tensile Strength
19.4%
improvement
0
4
0
8
0
1
2
0
1
6
0
2
0
0
T
e
m
p
e
r
a
t
u
r
e
(
C
)
0
4
0
0
8
0
0
1
2
0
0
1
6
0
0
2
0
0
0
S
t
o
r
a
g
e
M
o
d
u
l
u
s
(
M
P
a
)
o
N
e
a
t
E
p
o
x
y
1
w
t
.
%
C
N
F
2
w
t
.
%
C
N
F
3
w
t
.
%
C
N
F
0
.
0
0
0
.
0
1
0
.
0
2
0
.
0
3
0
.
0
4
S
t
r
a
i
n
0
2
0
4
0
6
0
8
0
S
t
r
e
s
s
(
M
P
a
)
N
e
a
t
E
p
o
x
y
1
w
t
.
%
C
N
F
/
E
p
o
x
y
2
w
t
%
C
N
F
/
E
p
o
x
y
3
w
t
.
%
C
N
F
/
E
p
o
x
y
1
0
0
1
0
0
0
1
0
0
0
0
1
0
0
0
0
0
1
0
0
0
0
0
0
N
u
m
b
e
r
o
f
C
y
c
l
e
s
3
5
4
0
4
5
S
t
r
e
s
s
(
M
P
a
)
N
e
a
t
E
p
o
x
y
1
w
t
.
%
C
N
F
/
E
p
o
x
y
2
w
t
.
%
C
N
F
/
E
p
o
x
y
3
w
t
.
%
C
N
F
/
E
p
o
x
y
0
.
0
0
0
.
2
0
0
.
4
0
0
.
6
0
D
i
s
p
l
a
c
e
m
e
n
t
(
m
m
)
0
2
0
0
4
0
0
6
0
0
8
0
0
1
0
0
0
L
o
a
d
(
N
)
3
%
C
N
F
/
E
p
o
x
y
2
%
C
N
F
/
E
p
o
x
y
1
%
C
N
F
/
E
p
o
x
y
N
e
a
t
E
p
o
x
y
Fracture toughness
23% increase in fracture toughness
was observed in 2 wt% system
Fatigue
Performance
At the same fatigue stress level,
140% improvement
in fatigue life
was observed in 2 wt% system by
the bridging effect of CNF
Mechanical Properties of
Nanophased Nylon Fibers
0
5
10
15
20
25
0
200
400
600
800
Strai n in %
stress in MPa
With the use of 1% silica spherical
nanoparticles by weight,
an increase of
100 to 150%
in the tensile properties
was observed in nylon
-
6.
It was also observed that the fibers
infused with 1% by weight whisker form of
Si
3
N
4
exhibited
more than 300%
improvement in tensile strength
.
TEM picture of Nylon
-
Si
3
N
4
Aligned
Nano whisker
Experimental
-
Flexural Results
VARTM results
Hand
-
Layup results
Flexural stress
-
strain plot
Flexural
Strength,
MPa
% Gain/
Loss in
strength
Flexural
Modulus, GPa
% Gain/
Loss in
modulus
Neat
380
±
3. 3
-
37.57
±
0.77
-
1% Nanoclay
426
±
10.81
12.10
43.8
±
2. 13
16.58
2% Nanoclay
498
±
12. 81
31.05
46.2
±
0. 81
22.97
3% Nanoclay
446
±
8. 95
17.36
46.9
±
1. 22
24.8
0
1
0
0
2
0
0
3
0
0
4
0
0
5
0
0
0
0
.
0
0
3
0
.
0
0
6
0
.
0
0
9
0
.
0
1
2
1
%
n
a
n
o
c
l
a
y
2
%
n
a
n
o
c
l
a
y
3
%
n
a
n
o
c
l
a
y
N
e
a
t
c
o
m
p
o
s
i
t
e
S
t
r
a
i
n
,
m
/
m
F
l
e
x
u
r
a
l
s
t
r
e
s
s
,
M
P
a
Fabric: 8
-
layered plain weave
3k, Resin: SC
-
15 Epoxy,
Nanoclay: Nanocor
®
I
-
28E
Impact Response
VARTM results
Fabric: 8
-
layered plain weave 3k, Resin: SC
-
15 Epoxy, Nanoclay: Nanocor
®
I
-
28E
Neat 1%
2% 3%
Impact Energy: 30J
Sample Damage Area (mm
2
)
Neat 1144
1% 860
2% 660
3%
920
Different Methods of Functionalization
Oxidation
Fluorination
Amino
-
functionalization
HNO
3
/H
2
SO
4
F F F
F F F
C
O
OH
OH
C
O
NH
2
Flexural 3
-
point bend test
Material
Max. Strength
(MPa)
Modulus
(GPa)
Epon 862 neat
139.7
±
7.1
3.5
±
0.08
Nanocomposite/ MWCNT
-
UNMOD
152.1
±
20.2
4.1
±
0.2
Nanocomposite/ MWCNT
-
COOH
151.1
±
14.9
4.8
±
0.6
Nanocomposite/ MWCNT
-
F
136.1
±
12.2
3.6
±
0.0
Nanocomposite/MWCNT
-
NH
2
162.8
±
4.6
4.2
±
0.1
Conventional polymer foams
are produced, for example, by introducing gas
bubbles into liquid monomer
Syntactic Foams
are produced by embedding pre
-
formed hollow/solid
microspheres within a polymer matrix
PVC Foam (open cell)
PUR Foam (closed cell)
PVC Foam (closed cell)
Syntactic Foam
Microballoons act as cells of the conventional foam
They are very similar to the cellular, gas expanded solidified liquid
A tertiary system whereas conventional foams are binary system
Syntactic Foam (TU)
Matrix
SC
-
15 Epoxy
Part A: diglycidylether of bisphenol
-
A,
Part B: Diethelene tri amine (DETA)
Viscosity: 300 cps, Density: 1.09 g/cc
Microballons
K
-
15 (3M)
Size: 30
-
105
µ
m
Avg. Density: 0.15 g/cc
Avg. wall thickness: 0.7
µ
m
Nanoparticles
Nanoclay
-
K10 (Sigma Aldrich Inc.)
Shape: Plate type
Avg. surface area: 220
-
270 m
2
/g
Manufacturing of Nanophased Syntactic
Foam (TU)
0
1
0
2
0
3
0
0
0
.
5
1
.
0
1
.
5
2
.
0
N
e
a
t
s
a
m
p
l
e
1
w
t
%
N
a
n
o
c
l
a
y
2
w
t
%
N
a
n
o
c
l
a
y
3
w
t
%
N
a
n
o
c
l
a
y
S
t
r
a
i
n
,
%
S
t
r
e
s
s
,
M
P
a
Flexural
strength
(MPa)
Improvement
in strength
(%)
Flexural
modulus
(GPa)
Improvement
in modulus (%)
Neat
sample
17.7
±
0.21
-
1.33
±
0.039
-
1 wt%
Nanoclay
20.3
±
0.13
14.7
1.50
±
0.036
12.8
2 wt%
Nanoclay
25.1
±
0.15
41.8
1.57
±
0.043
18.0
3 wt%
Nanoclay
22.8
±
0.11
28.8
1.57
±
0.035
18.0
Mechanical Properties of Syntactic
Foam (TU)
Flexural test results of the samples indicate a maximum
improvement in strength and modulus of about 42%
and 18% respectively for 2 wt % nanoclay system
0
500
1000
1500
2000
Storage Modulus (MPa)
20
40
60
80
100
120
140
160
Temperature (°C)
–––––– Neat sample
– – – 1 wt% nanoclay
–––– · 2 wt% nanoclay
–– – – 3 wt% nanoclay
Universal V3.8B TA Instruments
0.0
0.1
0.2
0.3
0.4
Tan Delta
20
40
60
80
100
120
140
160
Temperature (°C)
–––––– Neat sample
– – – 1 wt% nanoclay
–––– · 2 wt% nanoclay
–– – – 3 wt% nanoclay
Universal V3.8B TA Instruments
Thermal Properties of Syntactic Foam (TU)
Storage modulus
(MPa)
% Change
Loss modulus
(MPa)
% Change
T
g
(
0
C)
Change
(
0
C)
Neat sample
1220
±
12
-
123.2
±
0.23
-
105
±
0.32
-
1 wt% Nanoclay
1497
±
26
22.7
145.6
±
0.41
18.2
109
±
0.43
4
2 wt% Nanoclay
1590
±
21
30.3
157.4
±
0.82
27.8
112
±
0.19
7
3 wt% Nanoclay
1292
±
18
5.9
128.8
±
0.11
4.5
109
±
0.22
4
Storage modulus increased by 30% and also 7
0
C increase in glass transition
temperature is observed for 2 wt % nanoclay system
Thermal Properties of Syntactic Foam (TU)
-20
0
20
40
60
80
Dimension Change (µm)
20
40
60
80
100
120
140
160
180
Temperature (°C)
–––––– Neat sample
– – – 1 wt% nanoclay
–––– · 2 wt% nanoclay
–– – – 3 wt% nanoclay
Universal V3.8B TA Instruments
Coefficient of thermal expansion was found
using the formula as follows:
The slope of the initial portion of the curves
give the value for dL/dT and L is the
thicknesses of the samples
CTE (
µ
m/m
0
C)
Change
(
0
C)
Neat sample
41.9
±
0.62
-
1 wt% Nanoclay
40.5
±
0.33
-
1.4
2 wt% Nanoclay
39.7
±
0.93
-
2.2
3 wt% Nanoclay
35.1
±
0.39
-
6.8
dT
dL
L
*
1
TMA results exhibited 70C decrease in
CTE value for 3 wt % nanoclay system
Objectives
Traditional Technology
—
BiTe/SbTe Semiconductors
21st Century Technology
---
Metal/Insulator
nano superlattice
Results
Higher Thermoelectric figure of merit
Approach
Zn
4
Sb
3
/ CeFe
(4
-
x)
Co
x
Sb
12
nano
-
layered superlattices
Si
1
-
x
Ge
x
/Si after
Bombardment by 5 MeV Si Ions
Au/SiO
2
Metal nano particle superlattice
Future Plans
Produce a prototype high temperature
metal/insulator thermoelectric generator
for direct energy conversion of waste heat
Thermoelectric Generator
(with superlattice nano particles): AAMU
Summary
•
50 to 1000 nanolayers were
produced in house.
•
Post Irradiation reduced thermal
conductivity, increased electrical
conductivity as well as increase
Seebeck Coefficient.
•
Thus Figure of Merit increased.
ZT=(S
2
σ
T)/
Figure of Merit (ZT)
+V
2
-
V
xB
+V
1
Neutral Return
Mass Selector
Pump
Acceleration
and focusing
Electric arc nano
Particle Source
Nano particle production and electro
magnetic mass separation:
AAMU
Approach
1 Produce 10
-
100 nm metal particles
2 Use ion beam techniques
for mass separation
3 Use optical techniques
to characterize size distribution
Future Plans
•
Continue student involvement in nano
scale technology research
?µ
(Nano particles for innovative solar
cells)
?µ
Work with Tuskegee University for tests
of carbon composites with nano
particle additives
Objective
Involve
undergraduate students
in significant nano technology
Results
Optical evidence of 2
-
5 nm
silver nano particle production
300
400
500
600
700
0.0
0.2
0.4
0.6
43.5 nm
03 November 2006
Test009 and 010 Cary 5000
Optical absorption spectrum of silver nanoparticles on glass
(Obtained by electric arc in normal atmosphere)
Sample 2
Sample 2 immersed in H
2
O
-Log ( 1/T )
Wavelength (nm)
Approach
1 CNT: Electrical and Mechanical
2 Al
2
O
3
and SiC, Electrical
3 Ion Beam Surface Modification
Controlled cell adhesion
Controlled porosity
Collaborate closely with carbon
composite pioneers at Tuskegee University
Objectives
To Enhance
1 Mechanical properties: Hardness, Stiffness, Strain to
fracture
2 Transport properties: Electrical, Thermal, Fluid diffusion
3 Biocompatibility
Future
Plans
Technology
Transfer
Aerospace
Medical
Consumer
Carbon Nano Tube
50
m
m
10
-
30 nm
Glassy Polymeric Carbon Composites
AAMU
0.00
0.05
0.10
0.15
0.20
0.25
0
5
10
15
20
25
30
35
40
45
50
55
Pure GPC
GPC/CNT 1 wt%
GPC/CNT 2 wt%
GPC/CNT 3 wt%
GPC/CNT 5 wt%
GPC/CNT 10 wt%
Stress (MPa)
Strain (%)
10%
5%
3%
2%
1%
Virgin
GPC CNT
Composite
Results
50%
Increased
strain to failure
300%
Increased
stiffness
High Temperature (3000
°
C), Low Density (1.45 /cm
3
)
Thermal expansion (zero), Inert (except oxygen)
Magnetic Field
-
Induced Nanoparticle
Dispersion (USA)
•
Good
dispersion
of
heavy
metallic
nanoparticles
(iron
oxide)
under
magnetic
field
•
Development
of
lab
scale
magnetic
field
device
•
Modeling
magnetic
field
dependence
of
nanoparticle
dispersion
•
Good
agreement
between
experimental
results
10
1
10
2
10
-1
10
0
10
1
10
2
Flocculation Rate vs. Magnetic Field Density
Vma
1/2
Flocculation Rate
Capture
efficiency
versus
(root)
magnetic
velocity
for
various
thicknesses
of
the
surfactant
layer
indicating
the
extent
to
which
the
surfactant
layer
thickness
frustrates
the
process
of
agglomeration
Capture Efficiency Vs Magnetic Velocity
for different surfactant layer thicknesses
Summary of Research Activities of
Auburn ACNM Team
(a)
(b)
Ab initio calculated (a) lattice thermal expansion and (b) elastic constants of Al
2
O
3
.
•
Study thermal and mechanical properties through molecular modeling and simulation
•
Model structure and properties of hard ceramic fillers and soft polymer matrix
•
Modeling of Si
3
N
4
, Al
2
O
3
, SiC, and TiO
2
•
Initiated simulation studies using LAMMPS code developed by Sandia National Lab.
Perfluorocyclobutyl (PFCB) optical waveguides with air trenches
(partial support for 2 PhD students)
Ring Resonator Design with
Air Trench Splitters
Measurement of AWG in
PFCB
ACNM
-
UAH Effort
•
Nanofabrication of air trenches in PFCB waveguides enables high efficient,
extremely compact planar optical components
•
Fabricated smallest arrayed waveguide (AWG) utilizing nano
-
patterned air
trench reflector
•
Fabricated a compact ring resonator utilizing nano
-
patterned air trench
splitters
Integrated Nanophotonics
Nanophotonic wave structure significantly reduces waveguide loss
New waveguide allows meter propagation distance propagation rather than mm
Proposal Submission
Funded Grants: ($3.985 M)
•
A Research and Educational Partnership in Nanomaterials between Tuskegee University and
Cornell University, 8/1/06
-
7/31/11,
($2.55 M with $2.1 M TU share)
•
Enhancement of Research Infrastructure in the Materials Science and Engineering Program
at Tuskegee University,
9/1/06
-
8/31/08,
($1.0 M)
•
Characterizations of Nanocomposites and Composite Laminates, Air Force/HBCU/MI
program
8/1/05
-
7/31/07 ($225 K, subcontract from Clarkson Aerospace, Inc.)
•
Modeling High
-
rate Material Responses for Impact Applications,
11/1/05
-
10/31/06
(subcontract from Mississippi State Univ. $100K)
•
SBIR Phase I: Advanced Composites Research to Reduce Costs, 6/15/2006,
Ondax Inc.
($105K)
•
STTR Phase I: Nanocluster characterization in Volume Holographic Glass
gratings,6/25/2006,
Ondax Inc. ($105K)
Other non funded proposals
•
$ 881 K (TU being prime)
•
$ 18.35 M (with Mississippi State and Florida Atlantic with TU share of $2.05 M)
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