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Nanostructured Materials forNanostructured Materials for
Energy conversion devices (Solar &Energy conversion devices (Solar &Fuel cells)Fuel cells)
ByDr. Velumani Subramaniam
Coordinador de Relaciones Internationales yProfesor InvestigadorDepartment of Electrical EngineeringCinvestav-Zacatenco Campus, Mexico cityhttp://cori.cinvestav.mx/velumani
[email protected] or [email protected]
http://cori.cinvestav.mx/velumanimailto:[email protected]:[email protected]:[email protected]:[email protected]://cori.cinvestav.mx/velumani -
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ResearchInterests
Fuel cells&
Hydrogen storage
Solar cells- usingnanostructures
Corrosion protection-Theft sensors
Coatings(nanoparticles)Nanoelectronics
Trimetallic nanoComposites
Pd-Co-Mo, Pd-Co.AuPd-Co-Ni
Identification oflow cost bipolar Platesand various protective
nano Coating(Ni-Cr & Polymers)
Dep and charof nanostructure
Materials- CISCIGS CdTe, CdSe,
PMeT, CdS
On the way toEstablish the
Technology
Main and the mostExpensive part
in any Oil Industry
Identification ofvarious coatingMaterials incl
polymer-metalNano composites
Photovoltaic cellson Micro-chips andnanointerconnects
Lab-on-Chip withoutexternal
Power connections
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Ongoing ProjectsOngoing Projects
1) Titanium dioxide (TiO-2) Nano tube Solar cells using CdX (S or Se) nanocrystals with P3HT
sensitizers, (Participant) CONACyT-INDIA project, (2006
2009)
2) Theoretical and experimental Analysis of Pd-Co-Mo, Pd-Co-Au and Pd-Co-Ni composites for its
catalytic activity in PEM fuel cells, (Principal Investigator) CONACyT, 2007-2008, Mexico
3) Fabrication of high efficiency solar cells using nanostructured materials, (Principal Investigator)
GOOGLE-TEC innovation cell, Tecnologico de Monterrey-
campus Monterrey, Mexico (April 2007
March
2009)
4) Nano-engineered 3-Dimensional impregnation of nano-catalysts [Pt, Pd(70)-Co(20)-Au(10) and
Pd(70)-Co(20)-Mo(10)) on CNT for PEM Fuel Cells BY S. Velumani (PI) -
ITESM & A. M. Kannan(PI),
ASU -
A joint project with Arizona state university & ITESM
Oct 2007 to Sept 2009.
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NEW Interdisciplinary
program
1.
Electrical Engr
2.
Physics
3.
Chemistry
4.
Biotechnology
5.
Cellular biology
6.
Materials Science
40 Professors3 unidades
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Fuel cells are electrochemical devices that can efficientlyFuel cells are electrochemical devices that can efficiently convertconvert
thethe
chemical energy (oxidation potential) of the fuel directly intochemical energy (oxidation potential) of the fuel directly into electricalelectrical
energy.energy.
They operate like batteries and are similar in components and chThey operate like batteries and are similar in components and ch
aracteristics,aracteristics,
but unlike batteries, they do not get exhausted and arebut unlike batteries, they do not get exhausted and are environmentallyenvironmentally
friendlyfriendly..
As long as fuelAs long as fuel
is supplied to the cell along with an oxidant (typically air),is supplied to the cell along with an oxidant (typically air), thethe
fuel cell continues to produce electrical energy and heat.fuel cell continues to produce electrical energy and heat.
Additional benefits includeAdditional benefits include low maintenance, excellent load performancelow maintenance, excellent load performance, etc., etc.
Consequently, this conversion is not limited by the CarnotConsequently, this conversion is not limited by the Carnots cycle ands cycle and
efficiencies as high as 90%efficiencies as high as 90%
can be obtained.can be obtained.
What is a Fuel cellWhat is a Fuel cell
Fuel CellHydrogen
Oxygen
Electricity
Heat
Water
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- +
ANODE CATHODE
AIRGAS
ELECTRONS
HYDROGEN
IONS
DC VOLTAGE
Functional DiagramFunctional DiagramFunctional Diagram
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On going work at fuel cell lab
Simulation of Pd-Co-Au, Pd-Co-Mo nanocatalysts for the
PEM fuel cells
Nano-engineered 3-Dimensional impregnation of nano-
catalysts [Pt, Pd(70)-Co(20)-Au(10) and Pd(70)-Co(20)-Mo(10))on CNT for PEM Fuel Cells
Fabrication of stainless steel, alum inium, Teflon bipolar
plates at TEC
Exploring the possibilities of nanocoatings for thesebipolar plates to increase the conductivity (reduce ohmic losses)
Fabrication of fuel cell motor cycle
Design of fuel cell stack using the PLM (product life cyclemanagement)
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Different types of fuel cellsDifferent types of fuel cells
Fuel cells types Electrolyte
electrode
Working
temperatures
Fuel Oxidant Electrical
efficiency
PEMFC
Polymer electrolyte
membrane FC
Nafion
Electrodes with Pt
30 - 80C pure H2
Air or pure O2
~ 35%
DMFC
Direct Metanol FC
Nafion 30 - 80C Metanol
Airo r pure O2
~ 25%
AFCAlkaline FC
KOH concentratecarbon Electrodes with Pt, Ag
catalyst
60 - 100C pure H2Air or pure O2 ~ 35%
PAFC
Phosphoric acid FC
H3PO4 concentrate
Electrodes with Pt
~ 200C H2, CH4, CH3OH
Air
~ 40%
MCFC
Molten carbonate FC
Molten carbonate, Li2CO3/
Na2CO3
nickel Electrodes
~ 650C H2, CH4
Air
~ 50%
SOFC
Solid oxide FC
Ceramic solid oxide and
nickel Electrodes
~ 1000C H2, CH4, CH3OH,
Air
~ 55%
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FUEL CELL - Where to make an entry for nano?
Forces Driving Fuel cells
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TEM micrograph of a Pt-Ru/herringbone graphitic carbon nanofiber nanocompositeprepared by the Lukehart group
When tested as an anode catalyst in a working DMFC, this nanocomposite
exhibits a DMFC performance 50% greater than that recorded for a
commercial
Pt-Ru catalyst.
PtRu/carbon fiber attachment
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Assembly of PEM
Teflon sealing
Screws with
non-conductivesealing
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Stainless Steel Bipolar Plate
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Characterization Efficiency
(4)
In the case of the aluminum bipolar plates, the OCV was:
Efficiency calculations:
(3)
(5)
(6)
In the case of the stainless steel bipolar plates, the OCVwas:
,
,
.
.
VVBPALc
90846.0=
%04.69%10025.1==
FCAL
BPAL
c
f
V
VVBPSSc
903365.0=
%66.68%10025.1==
BPSS
BPSS
c
f
V
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A SEM image of theNitrided NiCr coating
on the stainless steel
coupon
CHARACTERISTICS OF NiCr COATINGS for BP
NiCr
Mapping of the Ni and Cr particles on the surface of thecoupons showing a uniform distribution of distribution of both
elements
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Nanosys500 sputter deposition system
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Molecular Simulation of Pd-Co-Au, Pd-Co-
Mo and Pd-Co-Ni (nanocomposites) for fuelcell catalytic applications Theory Behind the Software
CASTEP is based on Density FunctionalTheory (DFT).
CASTEP is based on a supercell approach.
All studies must be performed on a [email protected]
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The Chosen Structure: A5
B1
C1
A5
B3
C1An other version of
A5
B3
C1
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Collaborative project with ASU
Nano-engineered 3-Dimensional impregnation of nano-catalysts [Pt,
Pd(70)-Co(20)-Au(10) and Pd(70)-Co(20)-Mo(10)) on CNT for PEM FuelCells
Goals
Reduction of Pt loading in Proton Exchange Membrane fuel
cells (PEMFCs) with 3 dimensional distribution of catalysts over multi-walled carbon nanotubes (MWCNTs)
Introduction of novel loading technique in 3 dimensional
forms for the 100 % utilization of catalysts
Replacement of Pt catalysts with novel Pd-Co-Mo and Pd-Co-
Au nanocatalysts.
Fabrication and performance analysis of single cell using
novel catalysts and three dimensional impregnation of catalysts and
To promote Student and Faculty exchange programs between
ASU and ITESM in the masters and doctoral programs
To establish a platform for establishing an Energy Center
(Nanotechnology and Fuel cells) through NSF- CONACYT forproducing work ready graduates in [email protected]
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Supercell for the adsorbed CO specie on the Pd-Co-Mo (1 1 0) plane, Simulation of Pd-Co-Au
species and 3-dimensional distribution of nanocatalysts over CNT
electrolyte
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Led
indicador
Fuel Cell
FuelCell
Stack
Vlvula
reguladora
Tanque de
hidrgeno
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Nanostructured Semiconductors
Nano structured semiconductors have attracted researchers interest for
their potential applications in optoelectronic devices like solar cells and
sensors.
Size Tailoring Band Gap Tuning
Wide Band gap Semiconductor Good Window material
A wide band gap semiconductor allows transmission of shorterwavelengths
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Low Material use and less energy intensive processing leads to lower
cost
Easier to fabricate large area devices required for PV applications
Performance comparable to single crystal materials
Manufacturing Technology is well established
Less stringent requirement on material properties
Easier Integration of device structure
THIN FILM SOLAR CELLSTHIN FILM SOLAR CELLS
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CdTe, CIS (CuInSe2), CIGS & TiO2
Thin film CdTe, CIGS and CIS - based solar cells have shown high
efficiencies in both small area devices and large area modules.
The direct band gap of these materials results in a large optical
absorption coefficient, which in turn require only 1-2 m of activelayer. Thickness of silicon wafer is generally 150 to 300 m.
Dye-sensitized TiO2 solar cells are environmentally friendly, low
cost and of large area
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Various Solar Cells structures
Window materials: ZnO:Al, TCO, SWCNT
CdZnTe or CIGS- Photon absorbing layer under the window, usuallydoped p-type, energy gap suited to solar spectrum
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Probable physical preparationtechniques
Physical Evaporation
Nanolithography
Laser Ablation
Mechanical grinding
Using templates
Sputtering
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Probable chemical preparationtechniques
Bio-reduction
Sol-gel
Electrochemical deposition
Phase transition
Passivating agents
Studies on synthesis of CuInGaSe nano
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Studies on synthesis of CuInGaSe2 nano-particles, ZnO:Al, CuIn(x)Ga(1-x)Se2, MW-
CBD CdZnS
Ingeniera Elctrica (SEES), CINVESTAV, Mxico.
PhD students working on the theme
B.Vidhya Bhojan
Ing. Rodrigo Cue Sampedro
Ing. Jagadeesh Babu
Masters Students
Ing. Rajesh Roshan Biswal
Ing. Ivn No Prez Ramrez
Ing. Pablo Itzam Reyes Figueroa
Ing. Arturo Lopez VillalpandoVillalpando
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Experimental details
In the preparation of CIGS nano powders, coppergranules (>99.9% pure), selenium and indium powders(>99.9% pure) and fine chips/granules of gallium wereweighed to correspond to the stoichiometry ofCuIn0.5Ga0.5Se2.
Five different mixtures dry, semi-dry and wet wereused.
This blended elemental mixture and Stainless balls wereloaded in a stainless container inside an argon-filledglove box.
The ball-to-powder weight ratio (BPR) was maintainedat 5 : 1. Milling was conducted using a SPEX-8000mixer/mill at 1200 rpm. [email protected]
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Experimental
Constituents Millingtime(hrs) Totalgrams(milled)
A Elemental
and
metal
powders(Cu,In,Ga
and
Se)powder11.5 12
B Powder1(dry) 1.5 2C Powder1+5mlethanol(wet) 1.5 2D Powder1+5mltetraethyleneglycol (wet) 1.5 2E Powder1+5dropsof ethylenediamine(semi
dry)1.5 2
All the chemicals are from Sigma Aldrich , tetraethylene glycol is from Merck [email protected]
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Reaction
The reactants (Cu,In,Ga and Se) is initiated by mechanical energysuch as collision and friction with the SS balls.
The explosive reaction ends in a short time. The reaction may be atype of chain reaction.
After the reaction is completed, the synthesized CIS powder ispulverized by the planetary ball milling.
T. Wada, H. Kinoshita / Journal of Physics and Chemistry of Solids 66 (2005) 19871989
Reaction mechanism for the preparation of CuInSe2
by MCP
Results and discussions
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10 20 30 40 50 60 70 80
Intensit
y(arbunits)
2 Theta
(112)
InSe
(220)/
(204) (312)/
(116)
(400) (332)
A
B
C
D
E
SeSe
The broadening of the peaks ,due to the small size particles. Ethyl alcohol doesnt affect the already formed CIGS structure . Trace of second phase InSe and Se is observed with Ethylene diamine andTetra ethylene glycol respectively.
Structural
(211)
(dry)
(wet)
(semi dry)
XRD pattern of chalcopyriteCIGS.
Grainsize
D=(0.94)/(Cos)
Where =1.54 ,
FWHM
The
average
grain
sizeA
8.93nm
B
8.143nm
C
7.918nmD7.922nmE
7.55nm
Results and discussions
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SEM-Morphology (dry)
A) 1.5 hrs milled B) 3 hrs milled
The surface area of particles will increase and nanoparticles will be in intimate contact witheach other. The nano particles have a strong cohesive force and they tend to
join very easily
forming clusters [1]
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Morphology Wet milled
C) 1.5 hrs dry followed by addition
of 5ml ethyl alcohol and milled for1.5 hrs more
D) 1.5 hrs dry followed by addition
of 5ml tetra ethylene glycol and milledfor 1.5 hrs more
Some flake like structuresXRD results show the presence of Se apartfrom CIGS, may be this prevents theformation of clusters and so more uniform
distribution is observed.
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Morphology semi dry
Different granular shapes
E) 1.5 hrs dry followed by additionOf 5 drops of ethylenediamine and milled
for 1.5 hrs more
CIGS milled for 1.5 hrs
Supports the SEM image-Individual nano
particles have tendency to form nanoparticle
agglomerates during milling process.Some separate nano particles of 11 to 30nm
is observed.
FESEM
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Semi dry
(112)
(220)/(204)
(312)/(116)(400)
(332)
TEM micrograph of an
Agglomerate of nano-Particles in which darkparticles are Surroundedby non-dense materials.
* fine bright spots in the
pattern are related to the
Nanocrystalline phase of
CIGS .[Powder Technology
191 (2009) 235239]
E-with ethylene diamine [email protected]
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OPTICAL STUDIES
The band gap was determinedBy drawing the straight lineThrough the absorption edge
At 1068nm
h(eV)=1240/
Eg
=1.16eV400 600 800 1000 1200
0.5
1.0
1.5
2.0
2.5
3.0
Absorbance
Wavelength(nm)
3 hrs
with ehthanol(3 hrs)
45 mins
This value of Eg
is in good agreement with the reported band gap values CuIn0.56
Ga0.44
Se2
(1.14 eV)[Synthesis of CuInS2, CuInSe2, and Cu(InxGa1-x)Se2 (CIGS) Nano crystal Inks
for Printable Photovoltaics,
J. Am. Chem. Soc., 2008, 130 (49), 16770-16777].
The bandgap value of nanocrystal dispersions were also consistent with energy of thecorresponding bulk compound( 1.23eV).
The prepared powder is dispersed in methanol and the absorbance spectra ismeasured by UV-Vis spectrophotometer Schimadzu Japan. The band gap energiesof the Cu(In0.5
Ga0.5
)Se2
nano crystals is determined from room temperature
absorbance spectra.
Absorbance spectra of CIGS nano particle dispersions
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MW-CB Deposition of CdZnS
CdSO4 , ZnSO4 , NH3SO4, Ammonium hydroxide.
Well cleaned glass substrates.-(Ultrasonic cleaning with soapsolution,acetone,ethanol and degreasing with isopropyl alcohol).
100 ml solution , kept in microwave for radiation time of 60s ,90s
and 150s seconds. Cleaned glass substrates kept vertically in thesolution.
Deposited for different values of Y=[ZnSO4]/{[CdSO4]+[ZnSO4]}(0.1,0.3,0.5,0.7 and 0.9)
Cleaned with deionised water , after deposition.
Deposition turned whitish yellow with the increase in Zn content.
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Microwave heating
Schematic of microwave heatingThe transfer of microwave energy is rapid
and direct with any absorbing material.
This rapid energy transfer creates non
equilibrium conditions resulting In high
instaneous temperatures(Ti)
These high Ti activate a higher percentage
of molecules above the Required activation
energy.
With energy transmitted directly to thereactants, the more energizedMolecules will form products more
rapidly.
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Microwave set-up
To find the hot spot
Electrical connections
STRUCTURAL
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20 30 40 50 60 70
arbunits
2 Theta
Zn=0.5
Zn=0.3
Zn=0.1
Radiation time 60s
(002)
(110)
20 30 40 50
Intensity(arbunits)
2 Theta
Y=0.9
Y=0.7
Y=0.3
Y=0.1
Y=0
Radiation time 90s
(002)
2
shiftto
SlightlyhigherValue,withZnIncorporation.
diffraction peaks associated with the Hexagonal Wurtzite structure of CdZnS
Increase in
crystallinity
0.1 & 0.3
20 30 40 50 60 70
arbunits
2 theta
Zn=0.9
Zn=0.7Zn=0.5
Zn=0.3
Zn=0.1
(002)
Radiation time 150s
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Morphology
Scanning electron micrographs for a)Y=0.1,b)Y=0.3,c)Y=0.5,d)Y=0.7 and e)Y=0.9 for CdZnS thin films
deposited at 90s radiation time
There are more voids on the
film surface with the increase
in Zn concentration. This is inagreement with the structural
inferiority observed in the Xrd
result for Zn concentrations
above 0.5
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Morphology
Localized heating of thin films with Y=0.7 and 0.9 deposited for 150s radiation time
The clusters observed in the SEM images are actually composed
of numerous self assembled nano particles of 10 to 20 .
growing crystallites contacted each other at their bases, the
sidewalls zipped together until a balance was reached between
the energy associated with eliminating surface area, creating a
grain boundary
FESEM image of CdZnS of Y=0.3, 60s radiation
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EDX-composition
Y Cd At% Zn at% S at% Zn/Cd Cd/S
0.1 57.32 6.34 36.34 0.11 1.57
0.3 55.03 7.95 37.01 0.144 1.48
0.5 51.90 10.20 37.90 0.196 1.370.7 50.65 14.37 34.98 0.284 1.44
Y Cd At% Zn at% S at% Cd/Zn Cd/S
0.1 59.16 5.14 35.71 0.086 1.66
0.3 54.26 7.67 38.06 0.141 1.43
0.5 50.23 19.23 30.54 0.383 1.64
0.7 44.98 25.56 29.46 0.571 1.53
0.9 33.89 41.12 25.00 1.219 1.36
60s
90s
Cd surplus in CdS results in a considerable concentration of traps
and recombination states below the gap .
There is a steady increase in the Zn/Cd composition, with very
little change in the Cd/S composition , which ensures the
replacement of Cd by Zn ions.
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General schematic ofa residential PV
system with batterystorage
What to do here?
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AFM images of the ZnSe nanorods synthesized by electrodeposition
Electrochemical synthesis and characterization of zinc selenide thin filmsJ MATER SCI 41 (2006) 35533559 by T. MAHALINGAM, A. KATHALINGAM, S. VELUMANI et al
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Guest Editor, Special issue from the journal Vacuum, an Elsevier publication forthe IMRC 2008, To be published in 2009
Guest Editor, Special issue from the journal Advanced Materials Research (ATransTech Publication, Switzerland) for IMRC-2007, To be published in 2009.
Guest Editor, Special issue from the journal NanoResearch (A TransTechPublication) for 3rd Mexican Workshop on Nanostructured Materials, Vol 5, 2008
Editorial board member, NanoTrends, A journal of Nanotechnology and itsApplications, An International Online BiMonthly Publication, ISSN 0971-418X
Guest Editor, Special issue from the journal Materials Characterization (An ElsevierPublication) for IMRC-2005, Vol 58, Issue 8-9, 2007
Guest Editor, Special issue from the journal NanoTrends, A journal ofNanotechnology and its Applications (An International Journal from Nano Science andTechnology Consortium, C-56, A/ 28, Sector-62, Noida, U.P., India) for anInternational conference - Nanotech-2006 held at Coimbatore Institute of Technology,
Coimbatore India from 25
th
to 28
th
June 2006.
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Chairman for Symposium 13 on, Advances in Semiconducting materialsIMRC2008, Aug 16 to 20, 2009, Cancun, Mexico.
Chairman Workshop on Nanostructured Materials, June 11 to 13, 2008, atCinvestav, Mexico.
Chairman for Symposium 19 on, Advances in Semiconducting materialsIMRC2008, Aug 17 to 21, 2008, Cancun, Mexico.
Chairman for Symposium 19 on, Advances in Semiconducting materialsIMRC2007, Oct 26 to 1st Nov 2007, Cancun, Mexico.
Co-Chair, Symposium 6 Materials Characterization, IMRC-2007, at Cancun,Mexico
Academic coordinator for a course (CADI) on Nanostructured materials and
fuel cellsfrom 5th to 8th June 2007, at ITESM- Campus Monterrey
Co-Chair, Symposium 6Materials Characterization, IMRC-2006, at Cancun,Mexico.
Joint Organizing Secretary (International), Nanotec 2006, Coimbatore Instituteof Technology, Coimbatore, India, June 23 & 24, 2006.
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