Alabama Center for Nanostructured Materials (ACNM)

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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
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ACNM Mission/Goals
Research, Education, Training and Outreach

• 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

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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
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GSRP Awardees
Ivy K. Jones
Wanda D. Jones Merlin
Theodore
Jean Michael
Taguenang Bopah Chhay
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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/storyV5
  tuskegee25w.htm

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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
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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
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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

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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

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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)

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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.
70 improvement
Storage Modulus
Glass Transition Temp.
7oC increase
Tensile Modulus
17.4 improvement
Tensile Strength
19.4 improvement
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
Fracture toughness
23 increase in fracture toughness was observed
in 2 wt system
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Mechanical Properties of Nanophased Nylon Fibers
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 Si3N4 exhibited more
than 300 improvement in tensile strength.
Aligned Nano whisker
TEM picture of Nylon-Si3N4
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Experimental-Flexural Results
VARTM results
Fabric 8-layered plain weave 3k, Resin SC-15
Epoxy, Nanoclay Nanocor I-28E
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
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Impact Response
VARTM results
Fabric 8-layered plain weave 3k, Resin SC-15
Epoxy, Nanoclay Nanocor I-28E
Impact Energy 30J Sample Damage
Area (mm2) Neat
1144 1
860 2
660 3 920
Neat 1
2 3
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Different Methods of Functionalization

• Oxidation
• Fluorination
• Amino-functionalization

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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-NH2 162.8 4.6 4.2 0.1
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Syntactic Foam (TU)

• 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

• 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

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Manufacturing of Nanophased 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 µm Avg. Density 0.15 g/cc Avg. wall thickness 0.7 µm
Nanoparticles Nanoclay- K10 (Sigma Aldrich Inc.) Shape Plate type Avg. surface area 220-270 m2/g
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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
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
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Thermal Properties of Syntactic Foam (TU)
Storage modulus (MPa) Change Loss modulus (MPa) Change Tg (0C) Change (0C)
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 70C
increase in glass transition temperature is
observed for 2 wt nanoclay system
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Thermal Properties of Syntactic Foam (TU)
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 (µm/m0C) Change (0C)
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
TMA results exhibited 70C decrease in CTE value
for 3 wt nanoclay system
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Thermoelectric Generator (with superlattice nano
particles) AAMU
Results Higher Thermoelectric figure of merit
Objectives Traditional TechnologyBiTe/SbTe
Semiconductors 21st Century Technology---Metal/Ins
ulator nano superlattice
Approach Zn4Sb3 / CeFe(4-x)CoxSb12
nano-layered superlattices Si1-xGe x/Si after
Bombardment by 5 MeV Si Ions Au/SiO2 Metal nano
particle superlattice
ZT(S2sT)/?
Figure of Merit (ZT)

• 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.

Future Plans Produce a prototype high
temperature metal/insulator thermoelectric
generator for direct energy conversion of waste
heat


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Nano particle production and electro magnetic
mass separation AAMU
Objective Involve undergraduate students in
significant nano technology

• 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
• (Nano particles for innovative solar cells)
• Work with Tuskegee University for tests of
  carbon composites with nano particle additives

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Glassy Polymeric Carbon Composites AAMU
High Temperature (3000 C), Low Density (1.45
/cm3) Thermal expansion (zero), Inert (except
oxygen)
Objectives To Enhance 1 Mechanical properties
Hardness, Stiffness, Strain to fracture 2
Transport properties Electrical, Thermal, Fluid
diffusion 3 Biocompatibility
Approach 1 CNT Electrical and Mechanical 2 Al2O3
and SiC, Electrical 3 Ion Beam Surface
Modification Controlled cell adhesion Controlled
porosity Collaborate closely with
carbon composite pioneers at Tuskegee University
Future Plans Technology Transfer Aerospace Medical
Consumer
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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

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Capture Efficiency Vs Magnetic Velocity for
different surfactant layer thicknesses

• 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

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Summary of Research Activities of Auburn ACNM Team

• Study thermal and mechanical properties through
  molecular modeling and simulation
• Model structure and properties of hard ceramic
  fillers and soft polymer matrix
• Modeling of Si3N4, Al2O3, SiC, and TiO2
• Initiated simulation studies using LAMMPS code
  developed by Sandia National Lab.

(b)
(a)
Ab initio calculated (a) lattice thermal
expansion and (b) elastic constants of Al2O3.
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Perfluorocyclobutyl (PFCB) optical waveguides
with air trenches (partial support for 2 PhD
students)
ACNM-UAH Effort
Measurement of AWG in PFCB
Ring Resonator Design with Air Trench Splitters

• 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

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Integrated Nanophotonics
Nanophotonic wave structure significantly reduces
waveguide loss New waveguide allows meter
propagation distance propagation rather than mm

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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)