MEMS/Microsystems:

MEMS/Microsystems:
Design,FabricationandTest
SiddharthaP.Duttagupta
DepartmentofElectricalEngineering
Department
of Electrical Engineering
IndianInstituteofTechnologyBombay
sdgupta@ee.iitb.ac.in; sid duttagupta@yahoo.com
sdgupta@ee.iitb.ac.in;sid_duttagupta@yahoo.com

IITBEEMEMSOverview
Research, Education, Training, Collaboration:
Crossinstitution research: 2 microfluidics for electronics
cooling lowstress MEMS switch,
cooling,
switch Microfuel cells,
cells RF MEMS
transceiver, Multiferroic RF inductor, Polymer accelerometer,
also activities in Suman Mashruwala Lab and Biosciences Dept
MEMS institute elective (EE701), also dept electives in
Mechanical (P Gandhi) and Biosciences (R Srivastava)
Training: Annual MEMS TCAD Workshops sponsored by NPMASS
(May 2012)
Partners: IITB (Centre Res Nano Tech Science, Earth Sciences,
Mechanical, Physics, Systems & Control*), Mumbai Univ., VJTI,
Univ. Pune, CMET, Nanded Univ., SAMEER, IIT Hyderabad, NPCIL,
DRDO (NMRL,
(NMRL RCI),
RCI) VNIT (+INUP),
(+INUP) ISM Dhanbad (+NPMASS),
(+NPMASS)
BITS(Dubai)*, Cal Univ*, Joint Science Academies SRF Programme*

GreenEnergyManagementSystems
IntegrationandOptimization
Components

Source
SolarPV SPV
FuelCell FC

Converters
DCtoDC
DCtoAC

SolarPV
Array

DC

Fuel
Cell

DC

DC
DC

AC

DC

DC

DC

ACGrid

DCLoad

DCsource

Storage
Battery
UltraCapacitor

Load
VariableDC
VariableAC

Tidal
Power
Generation

AC
C

DC
C
DC

DC
Conversion

Storage
Battery,
UltraCap

Onchip
power

Distribution

Partners:VAgarwal,AGuha,MNGandhi,DRamakrishnan,AAgrawal,SGSingh(IITB),
KPRay(SAMEER),SAGangal (UPune),GJPhatak (CMET),TCS,CGL,Datar ,Sasken

Motivation and Scope

p
M lti
MultipurposeDCsupplyfromNonConventionalSources
DC
l f
N C
ti
lS

MicroscaleEnergySourceforonchippower

DegradationMonitoring forlowsystemlifetimecost

ReliablePowerGenerationunderNonOptimalConditions

Background- Fuel Cell

Electrochemical conversion
Device (Hydrogen Cell)
+
Reactants

Fuel (H2)
at Anode

Oxidant (O2)
at Cathode

Electrolyte

Load
_
Layered
Bi Cubic
Fuel Cell
Stack

Other Fuels Hydrocarbons, Alcohols [1]

Other Oxidants Chlorine
High Energy conversion efficiency (80%)
Operational temp. < 1000C

Applications

Direct Methanol Fuel Cell

Fuel Cell vehicle create electricity using H2 fuel and O2 from air [1]
Uninterrupted power supply instant protection from momentary power failure
Emergency
g
yp
power systems
y
and Cogeneration
g
for small scale networks

[1] Fuel Cell Handbook , Fundamentals and Survey of Systems,

John Wiley Publication, ISBN 0-471-49926-9 , 2003, Vol. 1, pp. ix 23

05 / 30

Ideal (thermodynamic)
Fuel Cell EMF at No Load

I
VA A ln
I0
Oh i Region
Ohmic
R i

VR R.I
Concentration
Polarization
Region

VC mI m e

nI m

Cell Voltage V

Activation Loss
Tafel Equation

1.0

1. Activation
Region
Power Density Curve

0.5

2. Ohmic Region
I V Curve
Current Density A/cm2

A system constant
I0 current density where voltage starts to drop initially
R Ohmic resistance by polymer electrolyte membrane
m, n - mass transfer parameters
Im start of non-linear region start of mass transfer

Cell Power Density W//cm2

Fuel Cell Operation

3. Mass Transport or
Concentration Region

E
Thermodynamically
e ody a ca y
predicted Fuel cell
Voltage o/p theoretically

Overall dependence between the

the voltage and the current density

V0 E VA VR VC

Methodology I
Fuel Cell Development
Size, Power Density
Requirements

Field Test
Design
YES
NO
CompactModel

NO

Design
OK?

Cellmeets
Application
S
Specs?
?

YES
Fabrication

LabTest

Fuel Cell Design Objectives

Uniform distributionoffuelandoxidantinsidecell
Uniformtemperaturedistributioninsidecell
Minimize reactant/product cross over
Minimizereactant/productcrossover
Electricalcontactsvs.porosity(GDLinterfacewithelectrode)
Properselectionofmaterials (electrode,membrane)

Ion Flux Map Micro-PEM Fuel Cell

D i Characteristics
Design
Ch
t i ti
Cell length (L) 200 micron
Channel height 10 micron
Channel width 70 micron
Rib width 90 micron
GDL width 30 micron
Porous
P
electrode
l t d thi
thickness
k
50 micron
i
Membrane thickness 50 micron
GDL electric conductivity 1000 S/m
Inlet H2 mass fraction (anode) 0.743
Inlet H2O mass fraction (cathode) 0.023
Inlet oxygen mass fraction (cathode) 0.228
Anode inlet flow velocity 0
0.2m/s
2m/s
Cathode inlet flow velocity 0.5m/s

Permeability (porous electrode) 2.36 E -12 m2

Membrane conductivity 10 S/m

Assumptions
Membrane is 100% humidified
No hydrogen cross over
Uniform temperature distribution
Reacting gases are ideal
Water produced is in gaseous state

[3] Ramesh P.,S.S Dimble,V Agarwal, S.P Duttagupta ,Performance of miniature fuel cells with segmented contacts attached to the
9
GDL,International conference on Electric Power and Energy Systems, Sharjah, 2011

Conventional PEM Fuel Cell Components

Proton Exchange Membrane Fuel Cell PEMFC [1]
Fuel Cell Chemistry

Anode

Anode Side
2H2 => 4H+ + 4e-

Conducts electrons freed from

hydrogen molecules so that the free
e- can be used in external circuitry

Cathode Side
O2 + 4H+ + 4e- => 2H2O
Net Reaction
2H2 + O2 = 2H2o
Electrolyte (PEM)

Anode,
Fuel
H2

Cat ode,
Cathode,
Oxidant
O2
Proton
Exchange
Membrane,
Electrolyte

Catalyst,
Platinum
Nano
Particles

Conducts only +ve ions and blocks electrons. Hydration Reqd.

NAFION is most widely used proton conductor in fuel cells [2]
Not easily patterned using photolithography, not easy to integrate
Bonding with Si is challenging under working Fuel Cell conditions

Channels etched on anode

disperses the hydrogen gas equally
over the surface of the catalyst

Cathode
Conducts electrons back from
external
t
l circuitry
i it to
t catalyst
t l t where
h
+
they recombine with O2 and H
Channels etched on cathode
distribute the oxygen
yg
to the surface
of the catalyst

[1] Fuel Cell Handbook , Fundamentals and Survey of Systems,

John Wiley Publication, ISBN 0-471-49926-9 , 2003, Vol. 1, pp. ix 23

10 / 30

Nano-Porous Si Membrane [2]

B)

A)

Prime grade boron doped p type

double side polished <100> Silicon
wafer with 100 mm diameter
and 0.02 ohm - cm resistivity

Post-lithography
i d
f Si3N4 Etching
for
Et hi
windows
Si Membrane Thickness 100 -meter

D)

C)
Each well area - 0.0625 cm2
Reactive Ion Etching with SF6 Plasma
selective removal of Si3N4
Silicon Substrate

Stripping for photoresist removal

Deep Reactive Ion Etching of Silicon
through wells to create Silicon Membrane
Photoresist

Silicon Nitride Insulator

[2] Kaun-Lun Chu et al. , A Nanoporous Silicon Membrane Electrode Assembly for OnChip Micro Fuel Cell Applications, IEEE, Journ. MEMS Syst., Vol .15, (2006) 671

NP Si Membrane Formation [2]

AB)

AB) I

800 nm thick Silicon Nitride film

Deposition on both sides of wafer
ICPCVD or LPCVD

Removal of native oxide by immersion of

Silicon Wafer in Buffered Oxide Etch Soln.

AB) III

AB) II

Application of photoresist coating

On Silicon Nitride surface

Silicon Substrate

Photoresist

Photolithography
Silicon Nitride Insulator

Photo Mask

[2] Kaun-Lun Chu et al. , A Nanoporous Silicon Membrane Electrode Assembly for OnChip Micro Fuel Cell Applications, IEEE, Journ. MEMS Syst., Vol .15, (2006) 671

SEM TOP View of Silicon Well

Formed after DRIE of Substrate [2]

Low Magnification - 500 Micro Meters

Side View of Well Walls in Silicon

High Magnification - 100 Nano Meters

[2] Kaun-Lun Chu et al. , A Nanoporous Silicon Membrane Electrode Assembly for OnChip Micro Fuel Cell Applications, IEEE, Journ. MEMS Syst., Vol .15, (2006) 671

NP Si Membrane Formation [2]

Nanoporous Si membrane

F)

E)
50 nm Chrome and Gold layer sputtered
at wafer back for electrical contact generation.
AZ 4903 photoresist spin coated on Cr-Au
layer to protect from acid etching

Nanoporous membrane after electro - chemical etching.

Cr - Au and Photoresist still existing

G)
Cr - Au
C
A llayer and
d Photoresist
Ph t
i t removed
d by
b
Piranha solution and Chrome etchant
Piranha solution - 1:3 volume ratio of 30 wt. % H2O2 (aq.) : 98 wt.% H2SO4
AZ 4903 Photoresist

Cr-Au Layer

Porous Silicon Membrane

[2] Kaun-Lun Chu et al. , A Nanoporous Silicon Membrane Electrode Assembly for OnChip Micro Fuel Cell Applications, IEEE, Journ. MEMS Syst., Vol .15, (2006) 671

Setup for Nano Porous

Membrane Formation in Silicon [2]
Electrolyte is constantly stirred by magnetic rotor, constant current of 40 mA/cm2
passed through 4 circular membranes
Silicon
Anode

Platinum
at u
Cathode

ElectrolyteEthanol and
49wt.% HF 1:1

Nanopores are
formed by
electrochemical
etching of Silicon
Membrane

In volume

15 / 30

[2] Kaun-Lun Chu et al. , A Nanoporous Silicon Membrane Electrode Assembly for OnChip Micro Fuel Cell Applications, IEEE, Journ. MEMS Syst., Vol .15, (2006) 671

SEM Image of
Porous Silicon Membrane

[2] Kaun-Lun Chu et al. , A Nanoporous Silicon Membrane Electrode Assembly for OnChip Micro Fuel Cell Applications, IEEE, Journ. MEMS Syst., Vol .15, (2006) 671

Nano Porous (DFAFC)

Silicon Membrane Fuel Cell [2]
5 M Formic Acid and
0.5 M H2SO4 is Fuel

Fuel

This TiO2 layer makes anode

catalyst layer surface hydrophilic.
Hence, fuel gets attracted to
catalyst to ease anode reaction

Reactions
Voltage

Load

Current

Silicon Bulk
Silicon Nitride Insulator
Platinum Cathode

Porous Silicon Membrane

Insulation (TiO2 or SiO2)
Prevents short circuit
between anode and cathode

Gold Contact Layer

Palladium Anode

[2] Kaun-Lun Chu et al. , A Nanoporous Silicon Membrane Electrode Assembly for OnChip Micro Fuel Cell Applications, IEEE, Journ. MEMS Syst., Vol .15, (2006) 671

Micro Fuel Cell Test Parameters

DynamicImpedanceSpectroscopy
Ionfluxmapping
fl
i
Transientimpact,fuel/oxidantcontaminants
Transientimpact,downstreampowerconverternoise
Degradation(fueldepletion,hotspotformation,catalystpoison)

Fuel Cell Test Setup

References PEMFC Design & Fabrication

[1] Fuel Cell Handbook , Fundamentals and Survey of Systems, John Wiley
Publication ISBN 0-471-49926-9
Publication,
0 471 49926 9 , 2003,
2003 Vol.
Vol 1,
1 pp.
pp 1 23
[2] Kaun-Lun Chu et al. , A Nanoporous Silicon Membrane Electrode
Assemblyy for On-Chip Micro Fuel Cell Applications, IEEE, Journal of
Michroelectro-mechanical Systems, Vol.15, No.- 3, June 2006, pp. 671 -677
[3] Ramesh P., S.S Dimble, V. Agarwal, S.P Duttagupta, Performance
of miniature fuel cells with segmented contacts attached to the GDL
GDL,
International conference on Electric Power and Energy Systems,
Sharjah, 2011

20 / 30

Methodology-II
MEMSSensorNetworkforReliableOperation
of Field Deployed AirBreathingPEMFuelCell
ofFieldDeployed
Air Breathing PEM Fuel Cell

MarkettrendinFCresearchistoreducecomponentcost
Researchcanreducesystemcostinthelongrunbyreverting
degradationinFC
g
increaseshybridsourcelifetime
y
f
WSNbasedpredictivecontrolhelpstostabilizeFCpoweroutput

FuelCellPerformanceParameters
Studyofoutputpowerdropbecauseof
Degradationofelectrodeandionmasstransportthroughmembrane
CoreleaseofCOwithH
Corelease of CO with H2 fuel(anode)andCOfromair(cathode)
fuel (anode) and CO from air (cathode)
poisonsthenanoPtcrystalsofelectrode irreversibledamage
CO2 co
contaminant(anode)reducespO
ta
a t (a ode) educes pO2 o
offuel
ue reversibledamage
e e s b e da age
Impactofpowerconvertersonelectrodeelectrochemicalsurfacearea
LowfrequencyreverseripplefromDCACconverters
HighswitchingfrequencyandloadfluctuationofDCDCconverters
Localizedvariationinhumidityandtemperature(hotspots)
Impactsnearelectrodemembranemorphology(ionflow)

Field Deployed Air PEMFC-Reliable Operation

range sensing through
backscattering
air in

CO sensor grid
- proximity plume
tracking and
f
forecasting
ti

air fuel cell

protecting chamber

laser
diode

H2 fuel

nozzle
l flap
fl
control

humid air

air out
air
fuel
cell
CO sensor

electric
heater
coil

vapor

compressed
O2 storage
t

water

25 / 34

CO Estimation in Dynamic Smoke Plume

Assumption: No air velocity network of 8 CO sensors placed elliptically

vertical
profile

horizontal
profile

mean

CO Gaussian dispersion profile

- to be estimated

Localization of CO dispersion profile

- estimated using ML estimation

CO propagation constant determined experimentally 2.65

CO2 propagation constant 2.3

25 / 30

Optimization of Proton Transport in Membrane

PerFluoroSulfonic polymer (NAFION) membrane in
hydrophobic domain shows morphological stability
NAFION

in

hydrophilic

domain

responsible

for

proton transport
Membrane fully hydrated to maintain continuous
ionconductivity through hopping mechanism
Very high membrane humidity floods the membrane
reducing ion conductivity, lower fuel cell power output
Optimizationofmembranehumidityformaximum
ionconductivityistobestudied

Multi-parameter FC Degradation

Fuel Cell
Power Density
water vapor mass
fraction at cathode

CO2 mass fraction

at cathode

dynamic change in
electrode impedance
for change in CO
y at cathode air
density

dynamic
membrane
impedance

time (minutes)

Conclusion: FC Testing & Optimization

System initiation and stabilization
Specific disruption is effected and dynamic output power
measured over long period of operation.
operation System switched off.
off
System restart, adjustments to restore power levels
Power differential measure of deterioration of PEMFC
Degradation
g
changes
g effected in PEMFC p
physical
y
model
PEMFC electrical parameters updated (coupled models)
Degradation minimization: FC technology + WSN feedback

References Fuel Cell Optimization

1)

2)

3)

4)

5)
6)
7)
8)

9)

S.Mitra,K.Tuckley,andS.P.Duttagupta,2DLocalizationandthreatestimationofnoxiousgassource
originatingfromburiedlandfills,ProceedingsofInternationalConference,USCUDAR2011,Prague,Czech
Republic,Sep.2011,pp.148 154.
S.Mitra,S.P.Duttagupta,K.Tuckley,andS.Ekram,Wirelesssensornetworkbasedlocalizationandthreat
estimationofhazardouslandfillgassource,InPress ProceedingsofIEEEInternationalConference,ICIT
2012,Athens,Greece,March2012.
S.Mitra,S.P.Duttagupta,K.Tuckley,andS.Ekram,3Dadhocsensornetworksbasedlocalizationandrisk
assessmentofburiedlandfillgassource,NAUN/WSEASInternationalJournalofCircuits,Systemsand
Signal Processing Vol 6 Issue 1 February 2012 pp 75 86.
SignalProcessing,Vol.6,Issue1,February2012,pp.75
86
S.Mitra,Ramesh P.,M.Bhattacharyya,andS.P.Duttagupta,Multimodesensingtechniqueforcarbon
monoxideplumetrackingandforecastingforreliablefielddeployedairbreathingPEMfuelcelloperation,
InPress ProceedingsofISPTS1,Pune,India,March2012.
M.W.Elis,M.R.VSpakovsky,D.J.Nelson,Fuelcellsystems:efficient,flexibleenergyconversionforthe21st
century,ProceedingsofIEEE,InvitedPaper,Vol.89,No.12,December2001,pp.18081818.
W.P.Teagan,J.Bentley,andB.Barnett,Costreductionsoffuelcellsfortransportapplications:fuelprocessing
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Y. Gao, M. Ehsani Systematic
Y.Gao,M.Ehsani
Systematicdesignoffuelcellpoweredhybridvehicledrivetrain,
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Electric Machines and
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C.Changsong,D.Shanxu,Y.Jinjun,Researchofenergymanagementsystemofdistributedgenerationbased
onpowerforecasting,inProceedingofInternationalconferenceonElectricalMachinesandSystems,ICEMS
2008,October2008,pp.27342737.
T G M R T J K l B k tt
T.G.McRae,T.J.Kulp,Backscatterabsorptiongasimaging:anewtechniqueforgasvisualization,Journalof
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11) T.Zhou,H.Liu,A3DmodelforPEMfuelcellsoperatedonreformate,JournalofPowerSources,Vol.138,
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Acknowledgement
Dr. M. Bhattacharyya, Dr. A.V. Kshirsagar,
Dr. S. Mehta (Post-doctoral Research Scholar)
B Patnaik, SS Dimble, Ramesh P, A Das,
U Chatterjee, R Rashmi, S Mitra, K Ghosh,
Aswini U,
U SG Kulkarni,
Kulkarni P Tamboli,
Tamboli M Mandal,
Mandal
B Somaiah, S Roy (Ph.D. Research Scholar)
S Shyamsundar, J Mohod, H Manaswala, N Patel,
P Chafekar, D Soni (M.Tech. Research Scholar)