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Nano/Micro-Electro-Mechanical-Sensor Systems

V. Ramgopal Rao
Centre of Excellence in Nanoelectronics,
Department of Electrical Engineering
Indian Institute of Technology (IIT) Bombay, Powai,
Mumbai, India
http://www.ee.iitb.ac.in/~rrao
Email: rrao@ee.iitb.ac.in

IIT Bombay

MICRO/NANO TECHNOLOGIES - AAA


Micro/Nano-fabrication technologies ideally suited for India:
Diverse Applications, high-tech, batch processing and low
cost per die
Nanotechnology sustained high levels of funding in focused
high technlogy areas with product/technology as a focus
Build Multi-disciplinary Research Teams
Available, Accessible and Affordable technologies

more than half of Indias population is under the age of 25, and one million

people a month are expected to join the labour force over the next decade.
Technologies that help youth excel & acquire skills

Indias massive agricultural sector employs about 60% of the population, yet

accounts for only about 17% of total GDP


Use innovation/technology as a vehicle to improve productivity

healthcare a major concern, rural health infrastructure hardly existent


14 million persons are infected with TB in India and more than 300,000 deaths occur every

year; about 2 million cases of malaria are recorded every year, by 2015 close to 5 million
infected with AIDS; 17.1 million lives are claimed by cardiovascular diseases, with 82% of
deaths occurring in low- and middle-income countries like India. India is home to about 40
Million diabetic patients .
Add to this: 42% Indians live on $2 per day & 22 Million population pushed below poverty

line annually due to healthcare expenditure

Security- a major concern area for India


Energy Besides all other energy related areas, we need to also focus on

Energy Scavenging Technologies (Vibrations, microwave energy..)


>> Available, Accessible and Affordable technologies

B. K. Chakravarthy
Industrial Design Centre, IIT Bombay

Students/Post-docs:

Seena, Nitin Kale, Manoj Joshi, Sheetal Patil, Prashanthi, Abhinav

Prasad, Deepika Reddy, Dilip Agarwal, Sudip Nag, Naveen Kadayinti,


Neena, Avil Fernandez, Sahir Gandhi, Gaurav Chatterjee, Rashi

Nathawat , Yashwant, Sandeep Surya Goud, Mihir,

Faculty Collaborators:

S.Mukherji (Immobilization), Dept. of Bio-Sciences & Engg.


D.K.Sharma (Instrumentation): Dept. of Electrical Engineering

Anilkumar (Surface coatings), Dept. of Chemistry


M.Shojaei (ASIC Design); Dept. of Electrical Engineering
P.R.Apte (Fabrication): Dept. of Electrical Engineering
C.P.Rao (Calixerines): Dept of Chemistry
M. Ravikanth (Porphyrins): Dept of Chemistry
Prita Pant (Nano-indentation): Dept. of Metallurgy & Mat.Sci.
V.R.Palkar (Multi-ferroics), Dept. of Electrical Engg.
B. K. Chakravarthy (Prototype-development) Industrial Design Centre
Amit Agarwal (Micro-fluidics), Dept. of Mechanical Engineering
T.Kundu (photo-thermal), Dept of Physics
IIT Bombay
Funding from NPSM, DIT,V.R.
NPMASS,
DST
Rao: rrao@ee.iitb.ac.in

IIT Bombay

A Rs. 300 Crore National Nano-fabrication Facility @ IIT Bombay


created from funding by DeitY, other agencies and industries. A
similar centre (CENSE) in operation at IISc Bangalore. Two new
centres being created at IIT Delhi & IIT Madras.

IIT Bombay

CEN IIT Bombay

CEN IIT Bombay

IIT Bombay

CEN IIT Bombay

IIT Bombay

Multi Disciplinary nature of Activities in the CEN

Total number of IITB Faculty members using the CEN@IITB: 56

IIT Bombay

Total number of IITB Ph.D. Students using the CEN Facility @ IITB: 101

IIT Bombay

IIT Bombay

What is Nanotechnology ?
Engineering of materials at the
Nanoscale in order to achieve useful
functions
A place for every atom and every atom in its place
How small is a Nano-meter really?
the length finger nails grow roughly in one second

IIT Bombay

Nanoscale = High Ratio of Surface Area to Vol.


Repeat 24 times

For example, 5 cubic centimeters about 1.7 cm per side of


material divided 24 times will produce 1 nanometer cubes and
spread in a single layer could cover a football field
Source: Clayton Teague, NNI

M. Meyyappan, NASA Ames Res. Center

IIT Bombay

What really is Nanotechnology ?


size dependence
At the nanometer scale, properties become size-dependent

4R
1
Higher surface to volume ratio (sphere):

3
Spherical iron nanocrystals
4 R
R
2

3
Surface to volume ratio
J. Phys. Chem. 1996,
A 3 nm iron particle hasVol.
50%
atoms
on the surface
100,
p. 12142
A 10 nm particle
20% on the surface
A 30 nm particle
only 5% on the surface
For example,
(1) Thermal properties melting temperature
(2) Mechanical properties adhesion, capillary forces
(3) Optical properties absorption and scattering of light
(4) Electrical properties tunneling current
(5) Magnetic properties superparamagnetic effect
New properties enable new applications

IIT Bombay

More than Moore Era of CMOS Scaling


Spintronics,
Molecular
Electronics
Etc. s

Adapted from Evolution scenario for III-V/Ge devices on Si platform through (Takagi et al., ICSICT, 2010
pp.50-53, 2010)
IIT Bombay

V.Ramgopal Rao

More than Moore Era in CMOS

M. B. Wolfgang et al., 2010, "More than Moore" White paper (Intel)


IIT Bombay

IIT Bombay

An Ultra-sensitive Piezo-resistive
Polymer Cantilever Technology
iSens: A point of care system for Cardiac Diagnostics

Explosive Detection/Other Environmental sensors


Technology Enablers for Web enabled Cardiac
monitoring
System-in-Package solutions
IIT Bombay

An Ultra-sensitive Piezo-resistive
Polymer Cantilever Technology
iSens: A point of care system for Cardiac Diagnostics

Explosive Detection

Technology Enablers for Web enabled Cardiac


monitoring
System-in-Package solutions
IIT Bombay

10

iSens: A point of care system for Cardiac


Diagnostics
Ischaemic heart disease is the leading cause of death globally. About
one-third of all the deaths in the world are attributed to cardiac
problems. (Lancet 2006; 367: 1747-1757).
57 million (80%) deaths were in low-income countries. (Circulation
2001; 104: 2746-2753) , & (N Engl J Med 2004; 350 (24): 24382440).
Between 1990 and 2020, these diseases are expected to increase by
120% for women and 137% for men in developing countries,
compared with 30-60% in developed countries. (Circulation 2001; 104:
2855-2864).
By 2010, 60% of the world's heart disease is expected to occur in
India. (BMJ 2004; 328: 807-810).
South Asians have a high prevalence of risk factors, have Ischaemic
heart disease at an earlier age than people in developed countries. (J
Am Coll Cardiol 2001; 38: 682-687, JAMA 2007; 297: 286-294).
IIT Bombay

iSens : Considerations

Inexpensive, smart, rugged sensors that can be used


outside laboratories.
Should be relevant to present ground realities in India.
Changing lifestyles have made South Asians susceptible
to cardiac dysfunctions such as Acute Myocardial
Infarction.

Damage to an area of heart muscle occurs due to


inadequate supply of oxygen to that area.
Diagnosis of AMI done through various clinical and
pathological tests (e.g. ECG, CPK-MB levels, Troponin I
& T levels, myoglobin, etc.).
40% lawsuits in USA for wrong AMI diagnosis
V.R. Rao: rrao@ee.iitb.ac.in

IIT Bombay

11

Molecular Markers
Enzymatic markers
Creatine kinase-Total (CK)
Creatine kinase MB (CK-MB)
Lactate dehydrogenase (LDH)
Aspartate aminotransferase (AST)
Glycogen phosphorylase isoenzyme BB (GPBB)
Protein molecules
Troponin
Myoglobin
FABP
Cell-free laddered DNA fragments
V.R. Rao: rrao@ee.iitb.ac.in

IIT Bombay

Molecular Markers: Issues


Concentration & change of concentration
across individuals
Specificity
Temporal response
Ease of designing assay protocols
Protocol robustness
Of the marker for the dysfunction
Of the sensor for the marker
Of the sensor system, including
reagents
V.R. Rao: rrao@ee.iitb.ac.in

IIT Bombay

12

Temporal Variations of Markers


Time
(hrs)

Trop.I
(ng/ml)

CKMB
(ng/ml)

Myo.
(ng/ml)

Normal 0.02-.4

0 .1- 7

20-92

0.4

200

0.8

900

12

10.4

30

50

24

22

60

40

48

14

18

40

72

9.3

39

A: early release of myoglobin or CKMB isoforms after AMI;


B: cardiac troponin after AMI; C: CK-MB after AMI;
D: cardiac troponin after unstable angina.
IIT Bombay

Heart-type fatty acid binding protein


(hFABP)

European Journal of Cardio-thoracic Surgery 19 (2001) 859-864

IIT Bombay

13

Conventional Approaches
Sequential assays for enzymatic activity
Immunoassays:
ELISA (Enzyme Linked ImmunoSorbant
Assay)
Radioimmunoassay
Immunoprecipitation

Chromatography (!)
Electrophoresis for separating isomers
and then looking for activity (for lab
(skilled labor, time consuming))
V.R. Rao: rrao@ee.iitb.ac.in

IIT Bombay

Our approach
Biosensor array based on microfabricated
sequential assay systems
General approach is to use affinity sensors
Use direct affinity sensors:
Affinity cantilevers
EIS capacitors
Conducting polymer devices

V.R. Rao: rrao@ee.iitb.ac.in

IIT Bombay

14

A Review on Cantilever Sensors

Surface Stress

Temperature changes

Resonant Frequency

Surface stress changes detected of the order of 106N/m


Measure temperature changes down to 105 K
Mass change estimations in the atto- to zepto-gram (1021 g)
Silicon based materials, Reliability & Optical Detection
Anja Boisen et. al., Cantilever-like micromechanical sensors, IOP Rep. Prog. Phys.
74 (2011) 036101 (30pp)

IIT Bombay

tensile

compressive

In 1909, Stoney developed a theory to measure surface


stress/elastic strain of a thin film deposited onto a sheet of
metal. Modified Stoneys formula:

Fundamental understanding still lacking on the origin of surface stress


Anja Boisen et. al., Cantilever-like micromechanical sensors, IOP Rep. Prog. Phys.
74 (2011) 036101 (30pp)
IIT Bombay

15

What happens when reactions occur on


the Cantilever surface? ..1

Binding of molecules to sensor surface


leads to changes like:
Conformational changes or physical
steric crowding
Changes in surface charge
Changes in molecular density in sensing
layer
Configurational entropy changes
Changes in Intermolecular energetics
Covalent attachments
Wu et al, Origin of nanomechanical cantilever motion generated from biomolecular interactions,
PNAS,February 13, 2001 vol. 98 no. 4, 15601564

IIT Bombay

Source of Cantilever surface stress ..2


Kinetic analysis of binding reaction:
It is a reversible reaction
Gibbs free energy as it is a function of enthalpy and entropy
changes of the reaction, G= H - T S
The driving force in antigenantibody binding originates from an
increase in the entropy of solvent molecules displaced from the
interface upon complexation (i.e. it is entropy-driven).

Thermodynamic analyses have suggested that a considerable number of


antigenantibody interactions are enthalpy-driven, i.e. they make
favourable enthalpy changes with some opposition from the negative
entropy contribution to association.
Hydrogen bonds contribution: In addition to the direct antigenantibody
hydrogen bonds, solvent-mediated hydrogen bond formation drives the
interaction. Water molecules in the solvent form hydrogen bonds with
both antigen and antibody.
Anja Boisen et al, Cantilever-like micromechanical Sensors, 2011 Rep. Prog. Phys. 74,
036101

IIT Bombay

16

Resonant Frequency Changes

Bimetallic Cantilever tip deflection:

IIT Bombay

iSens Functional Architecture


Disposable part
Sample

Input Filter

Reactor

Reagent

Biosensor
Array

Signal
Conditioning
+
Display

Control + Processing
Electronics

IIT Bombay

17

iSens Prototype
Reference

Myoglobin

Reference

CK-MB

1.5 cm

Drain

Analyte

Plastic
Silicon/SU8

IIT Bombay

3 cm

Poly Si (Piezoresistor)
Cantilever/EIS/CP
Contacts
Analyte (serum)
V.R. Rao: rrao@ee.iitb.ac.in

IIT Bombay

Biosensor Array: Affinity


Cantilevers-1
Based on resonating
structure 0r deflection:
Attachment changes
mass or stiffness of
resonating structure
and thence resonant
frequency
Attachment changes
the surface stress
leading to a bending of
the cantilever

Antibodies

Mirror

Silicon
Picture courtesy: Anja Boisen
et.
al., IOP Rep. Prog. Phys. 74
(2011) 036101 (30pp)

Cantilever Video

G.F.=(R/Ro)/
IIT Bombay

18

Polymer Microcantilevers
Displacement Z

3L2 1

Et 2

Polymer considered : SU-8


Advantages of SU-8
Lower Young's modulus (40 X lower compared to
Si based materials!)
(5 GPa)
Schematic of microcantilever sensor

Inexpensive fabrication process & Ease in patterning


Compatibility for integrating sensor with CMOS & other micro fluidic components
Relatively stress free nature of the deposited film.
N.Kale et al., (IEEE/ASME) Journal of Microelectromechanical Systems (J-MEMS), Dec. 2006
M. Joshi et al., IEEE/ASME Journal of Microelectromechanical Systems (J-MEMS), Vol. 20, No. 3, June 2011
IIT Bombay

Polymer Microcantilevers -Piezoresistive


transduction
R
4
K
s
R
Eh

K
sensitivity
E
Piezoresistive layers

Gold

-strain gauge.
-K 2.
-Easy to
incorporate.
- Lower
sensitivity.
J. Thaysen et al.,
IEEE MEMS Conference
2002.

Poly Silicon
-Piezoresistive
-K > 20 (dependent
on material
optimization)
-Low Temperature
deposition methods
like HWCVD.
- Stiffness increase
- Smaller SNR
IEEE J-MEMS, 2009
IIT Bombay

SU-8/nanoparticle (or
nanowire) Composites

-Piezoresistive
-K 90
-Spin coatable
- Compatible with
SU-8
- Does not affect the
overall stiffness
- Good sensitivity
- Suffers from
Reproducibility
Nanotechnology, 2011
IIT Bombay

OFET/TFT
Embedded
Cantilevers

-Piezoresistive
- K>200
- Spin coatable
- Lower stiffness
- Good Sensitivity
- Better
homogeniety
IEEE J-MEMS, 2011
IIT Bombay
IIT Bombay

19

SU8/Poly-Si/SU8 Cantilevers for detecting


Myoglobin

R/R (K/E) (4ss t )


Low Youngs Modulus E (5 GPa) of SU-8
High Gauge Factor K (20) of polysilicon

SU-8 processing: simple and low cost


Immobilization on SU-8: Surface
modification by novel ammonia cracking
process (patented process)

N.Kale et al., (IEEE/ASME) Journal of Microelectromechanical Systems (J-MEMS), Dec. 2006


M.Joshi et al., Journal of Micromechanics and Microengineering Dec 2010
M.Joshi et al., (IEEE/ASME) Journal of Microelectromechanical Systems (J-MEMS), , June
2011
V.R. Rao: rrao@ee.iitb.ac.in

IIT Bombay

Hot-Wire CVD Cluster Tool for Low-Temperature


poly/nitride Deposition
Gas
Manifold

MFC

Exhaust
line
LLTC

Filament
Assembly
Shaft

Reactor
Slit
Valve
H2/NH B2H6
3

Gate Valve
View Port

Pirani Gauge

Nitin S. Kale et al., (IEEE/ASME) Journal of Microelectromechanical Systems (J-MEMS), Volume


18, Feb. 2009
IIT Bombay

20

HWCVD Polysilicon as a
Piezoresistor
Gauge Factor defined as
G.F.=(R/Ro)/
High gauge factor of polysilicon (K~30) as compared to that of
metal (K~2)
Gauge factor of polysilicon depends on
Grain size
Doping concentration
Doping type
Texture
Above factors dependent upon hot-wire process parameters like
substrate temperature, hydrogen dilution and boron flow
V.R. Rao: rrao@ee.iitb.ac.in

IIT Bombay

Hotwire CVD Polysilicon as


Piezo
HWCVD poly conductivity
as a function of temp

Calibration for glass substrate

IIT Bombay

21

Low-temp HWCVD piezo-poly for SU8/nitride


Cantilevers
Experimental

G.F.=(R/Ro)/

Experimental

Experimental

N.Kale et al., Proc. of the 8th IEEE Conference on Nanotechnology (IEEE NANO 2008),
August 18-21, 2008, USA

IIT Bombay

HWCVD Films for Polymer


Bio-MEMS

Crystallinity (intensity of <111>


peak) increases with polysilicon film
thickness.

Grain size determined from


X-ray data, using Scherrers
formula

IIT Bombay

22

HWCVD Films for Polymer BioMEMS


Glass
RMS
roughness
: 1.8 nm

HWCVD films deposited on SU-8/Glass show a


clear <111> peak while the ones on glass show a
high amorphous content

SU-8 on
glass
RMS
roughness
:
0.58 nm
IIT Bombay

HWCVD Film Optimization

XRD of polysilicon films


deposited on SU-8 coated
silicon substrate with different
hydrogen dilution

Variation of gauge factor and grain size


for polysilicon films deposited on SU-8
coated glass and bare glass substrate
with different hydrogen dilution
IIT Bombay

23

Low-temp HWCVD piezo-poly for SU8/nitride


Cantilevers
Experimental

G.F.=(R/Ro)/

Experimental

Experimental

N.Kale et al., Proc. of the 8th IEEE Conference on Nanotechnology (IEEE NANO 2008),
August 18-21, 2008, USA

IIT Bombay

SU8-Polysilicon-SU8 Process Flow &


Characterization

Nitin S. Kale et al., (IEEE/ASME) J-MEMS, Vol. 18, Feb. 2009

M. Joshi et al., Journal of Micromechanics and Microengineering, vol. 20 (2010) 125007.


IIT Bombay

24

First demonstration of SU-8/Polysilicon/SU-8


Cantilever

Straight cantilevers: Optimized process conditions


Measured Resonant Frequency: ~40 KHz, Spring Constant: 0.25
N/mt

N.S. Kale et al., (IEEE/ASME) Journal of Microelectromechanical Systems (J-MEMS) Feb., 2009
IIT Bombay

Polymer Microcantilevers -Piezoresistive


transduction
R
4
K
s
R
Eh

K
sensitivity
E
Piezoresistive layers

Gold

-strain gauge.
-K 2.
-Easy to
incorporate.
- Lower
sensitivity.
J. Thaysen et al.,
IEEE MEMS Conference
2002.

Poly Silicon
-Piezoresistive
-K > 20 (dependent
on material
optimization)
-Low Temperature
deposition methods
like HWCVD.
- Stiffness increase
- Smaller SNR
IEEE J-MEMS, 2009
IIT Bombay

SU-8/nanoparticle (or
nanowire) Composites

-Piezoresistive
-K 90
-Spin coatable
- Compatible with
SU-8
- Does not affect the
overall stiffness
- Good sensitivity
- Suffers from
Reproducibility
Nanotechnology, 2011
IIT Bombay

OFET/TFT
Embedded
Cantilevers

-Piezoresistive
- K>200
- Spin coatable
- Lower stiffness
- Good Sensitivity
- Better
homogeniety
IEEE J-MEMS, 2011
IIT Bombay
IIT Bombay

25

Polymer Cantilevers with embedded Carbon Black


particles

Appl. Phys. Lett. 88, 113508 (2006); L.


Gammelgaard,
P. A. Rasmussen et al., TU Denmark

CB/Polymer composite conducts for CB


concentration above percolation threshold

Conduction due to tunneling between two


aggregates : R/R due to change in
tunnel distance upon application of strain

Expected to be highly sensitive


V.R. Rao: rrao@ee.iitb.ac.in

IIT Bombay

Variability issues with Polymer Nano-composites

V.R. Rao: rrao@ee.iitb.ac.in

IIT Bombay

26

Polymer Nano particle composite


SU-8/Carbon Black Composite Nano-indentation Characterization

Scanned images of a set of Berkovich indent at the SU-8 surface

Schematic of load displacement curve


Oliver Pharr method to extract H and E

Load Vs indentation depth for different loads


IIT Bombay

Polymer Nano particle composite


SU-8/Carbon Black Composite :Characterization

Youngs Modulus of the composite as a function


of CB vol %

1. Parallel mixing model:

Hardness of composite as a function of CB vol %.

2. Guth-Smallwood equation for modulus

Seena et al., Nanotechnology , 22 (2011) 295501

IIT Bombay

27

SU-8 cantilevers with embedded Carbon Black Nano


particles
Parameter

Value

Cantilever
length

250m

Width

120m

Upper SU-8
thicknes
s

400nm

Lower SU-8
thicknes
s

1.8m

Die area

3.4mmX
1.5mm

Thinnest polymer
cantilevers with
embedded Nanoparticles

Fabrication of the devices IIT Bombay 6 mask process

Seena.V. et al., Pro. of the 5 th International Workshop on Nanomechanical


Cantilever Sensors, May 19 - 21, 2008,Mainz, Germany 2008
IIT Bombay

Highly sensitive self standing SU-8


cantilevers with embedded CB

Seena V. et al., Solid State Sciences (Elsevier), Volume 11, Issue 9, September 2009

IIT Bombay

28

Packaged Polymer Composite Cantilever Dies


Packaging: CMET PUNE
Microcantilever
Die

Package

SEM of the released SU-8/CB


microcantilever

Package Lid with


Integrated Heater

Inlet

Outlet

IIT Bombay

Development of Polymer composite


microcantilever sensor

Characterization

Resonance frequency was measured using Polytek Laser Doppler Vibrometer


(collaboration with Prof. Rudra Pratap, IISc)

Electromechanical characterization

V. Seena et al., 23rd IEEE International


Conference on MEMS (MEMS 2010)
Resonance Frequency =38.9 kHz

IIT Bombay

29

Electromechanical Characterization of SU-8 cantilevers with


embedded CB composite
Parameter

SU-8/CB/SU- SU-8/Au/SU-8
8
cantilever
cantilever

Deflection
sensitivity
[ppm]

1.1/nm

0.3/nm

Surface stress
sensitivity
[N/m] -1

7.6*10-3

1.3*10-2

These cantilevers are expected to


provide R/R of 10s of ppm for a
typical antibody-antigen interaction
[5mN/m]
Surface stress sensitivity: ~8 ppm/ (mN /mt)
Resonant frequency: 22 KHz
Spring constant: 0.4 N/mt
IIT Bombay

Noise in Polymer Composite Cantilevers

Higher noise levels compared to SU8-Au-SU8.


Estimated minimum detectable surface stress ~ 39 mN/m

IIT Bombay

30

ZnO Nanowire Embedded Strain Sensing


Cantilever

(a) Silicon dioxide grown on a silicon wafer (b) First encapsulation layer of SU-8 (c)
Patterned Cr/Au layer for contact. (d) Pattering of ZnO seed layer (e) Vertical
Growth of ZnO Nanowire (f) Bottom encapsulation layer of SU-8. (g) Pattering of
SU-8 anchor layer.
IIT Bombay

Low Youngs modulus of polymer and the high strain sensitivity of ZnO
nanowires, resulting out of the high surface area
Vertical ZnO nanowire grown using a low temperature (95 C) solution
based hydro-thermal method.
Measured Surface stress sensitivity: 128 ppm/nm.
Resonant Frquency: 30.4 KHz
Prasenjit Ray, V. Ramgopal Rao, ZnO Nanowire Embedded Strain Sensing Cantilever: A New
ultra-sensitive Technology Platform, To be published in J-MEMS, 2013

IIT Bombay

31

Polymer Microcantilevers -Piezoresistive


transduction
R
4
K
s
R
Eh

K
sensitivity
E
Piezoresistive layers

Gold

-strain gauge.
-K 2.
-Easy to
incorporate.
- Lower
sensitivity.
J. Thaysen et al.,
IEEE MEMS Conference
2002.

Poly Silicon
-Piezoresistive
-K > 20 (dependent
on material
optimization)
-Low Temperature
deposition methods
like HWCVD.
- Stiffness increase
- Smaller SNR
IEEE J-MEMS, 2009
IIT Bombay

SU-8/nanoparticle (or nanowire)


Composites

-Piezoresistive
-K 90
-Spin coatable
- Compatible with
SU-8
- Does not affect the
overall stiffness
- Good sensitivity
- Suffers from
Reproducibility
Nanotechnology, 2011
IIT Bombay

OFET/TFT
Embedded
Cantilevers

-Piezoresistive
- K>100
- Spin coatable
- Lower stiffness
- Good Sensitivity
- Better
homogeniety
IEEE J-MEMS, 2011
IIT Bombay
IIT Bombay

Organic Transistor/TFT as a Strain Amplifier

Pentacene or ZnO

IIT Bombay

32

Polymer microcantilever with integrated OFET


[B] Design and Fabrication of CantiFET
6
5
Geometrical details of CantiFET
Parameter

(A)

Value

1. Cantilever length

340 m

2. Cantilever width

170 m

3. Cantilever overall thickness

1.9 m

4. Die area

Reference and
measurement
cantilevers

4 mm X 4 mm
D

Layer details of CantiFET


Layer No

Material

Thickness

1. Cantilever first layer

SU-8

1 m

2. Gate

Cr/Au

5nm/ 80 nm

3. Gate Dielectric

SU-8

900 nm

4. Source/ Drain

Cr/Au

5nm/ 80 nm

Pentacene

40-50 nm

5 .Organic semiconductor

(B)

Drain Pentacene Source


Gate Dielectric SU-8
Gate
Structural SU-8

(A) Planar and (B) Cross sectional schematic of CantiFET device

IIT Bombay

Polymer microcantilever with integrated OFET


[B] Design and Fabrication of CantiFET
6
Device designs
6
Objective : To understand the anisotropic
nature of strain sensitivity

of pentacene

Current direction parallel to strain

Current direction perpendicular to strain

Current direction both parallel and perpendicular to


strain

Current direction at 450 angle to the strain

IIT Bombay

33

Polymer microcantilever with integrated OFET


[B] Design and Fabrication of CantiFET
6
Process flow
7

Concept
Source, drain and gate
contact pads open on
top side through OFET
on the bottom side

Sacrificial layer

SU-8 2002 structural layer

Source Drain contact of Cr/Au

Contact Pad and Gate


electrode of Cr/Au

Thick SU8 pattering as anchor layer

Gate dielectric

Release of the device


from the silicon

IIT Bombay

Organic CantiFETs realized at IIT Bombay

V.Seena et al., IEEE/ASME Journal of MEMS (J-MEMS) , April 2012

IIT Bombay

34

Polymer microcantilever with an integrated OFET


6
9

CantiFET Deflection Characterization


IIT Bombay

Polymer microcantilever with integrated OFET


[Characterization of CantiFET

7
Average strain , on pentacene layer 0in a rectangular microcantilever,
Lp
1
L Z nr k Z
2L

EI
L : Beam length
Lp : length of strain sensitive layer
Znr : distance of strain sensitive
layer from neutral axis
Z : the vertical deflection
k : the stiffness of the cantilever given by,
E : Youngs modulus
I : the moment of inertia.

3EI
L3

For CantiFET structure,


Lp = L, and Znr = h (thickness of
cantilever) 3h Z

4 L3

The sensitivity, [(I/I)/nm]:15.6 ppm for 1 nm of deflection.

V.Seena et al., IEEE/ASME Journal of MEMS (J-MEMS) , April 2012

IIT Bombay

35

Polymer microcantilever with integrated OFET


Characterization of CantiFET
1/f noise characterization

7
1

Noise spectral density showed a 1/f 1.72 dependence


Drain current noise level at Vgs= Vds = -5V : 0.64 pA/Hz

Min. surface stress sensitivity: 0.17 mN/m


IIT Bombay

Al- Doped ZnO thin-film transistor embedded micro-cantilever


as a piezoresistive sensor

(a) Sacrificial layer (b) SU-8 2002 structural layer (c) Contact Pad and
Gate electrode of Cr/Au (d) Gate dielectric (e) Source Drain contact of
Cr/Au (f) Thick SU8 pattering as anchor layer (g) Release of the device
from the silicon wafer
RF sputter deposit a 50 nm AZO thin film
IIT Bombay

36

ZnO TFT on a Cantilever as a Strain Amplifier

Channel Semiconductor:
Al doped ZnO
ZnO

IIT Bombay

Measured surface stress


Sensitivity: 116 ppm/nm
of deflection
Prasenjit Ray, V.Ramgopal Rao,
Al- Doped ZnO thin-film transistor
embedded micro-cantilever as a
piezoresistive sensor,
accepted, APL, 2013

IIT Bombay

37

Polymer Microcantilevers -Piezoresistive


transduction
R
4
K
s
R
Eh

K
sensitivity
E
Piezoresistive layers

Gold

-strain gauge.
-K 2.
-Easy to
incorporate.
- Lower
sensitivity.
J. Thaysen et al.,
IEEE MEMS Conference
2002.

SU-8/nanoparticle (or
nanowire) Composites

Poly Silicon
-Piezoresistive
-K > 20 (dependent
on material
optimization)
-Low Temperature
deposition methods
like HWCVD.
- Stiffness increase
- Smaller SNR
IEEE J-MEMS, 2009
IIT Bombay

-Piezoresistive
-K 90
-Spin coatable
- Compatible with
SU-8
- Does not affect the
overall stiffness
- Good sensitivity
- Suffers from
Reproducibility
Nanotechnology, 2011
IIT Bombay

OFET/TFT
Embedded
Cantilevers

-Piezoresistive
- K>100
- Spin coatable
- Lower stiffness
- Good Sensitivity
- Better
homogeniety
IEEE J-MEMS, 2011
IIT Bombay
IIT Bombay

Cantilever Systems for


Cardiac Diagnostics
Cantilever Platform: Low cost, Highly
Sensitive, Field Deployable
Bio-functionalization
System Level Integration

V.R. Rao: rrao@ee.iitb.ac.in

IIT Bombay

38

Cantilever Systems for


Cardiac Diagnostics
Cantilever Platform: Low cost, Highly
Sensitive, Field Deployable
Bio-functionalization

System Level Integration

V.R. Rao: rrao@ee.iitb.ac.in

IIT Bombay

Selective Immobilization Surface


Treatment

Immobilization chamber
IIT Bombay

39

SU-8 chemical structure: Effect of Ammonia Treatment in


HWCVD

(a) before ammonia treatment

(b) after treatment

By cleaving the CO bond of the epoxy group, an amino group can


get attached to one of the carbon atoms (verified with XPS)
M.Joshi et al., Biosensors and Bioelectronics, vol. 22, no.11,pp. 2429-2435, May 2007
IIT Bombay

Antibody Immobilization
Cantilevers (Dry)

on

Silicon

Nitride

and

SU-8

Surface modification: Top surface of silicon nitride and SU-8


cantilever modified in Hot Wire CVD setup (Dry)
Linker attachment- Dip in 1% aqueous solution of homo-bifunctional
agent (glutaraldehyde) for 30 minutes
Antibody immobilization- Incubation of Human Immunoglobulin
(HIgG) for one hour
Blocking of non-specific binding sites- Blocking of unsaturated
aldehyde sites and non-specific adsorption sites by dipping in BSA for
one hour
Identification of grafted antibody layer- Incubation of FITC tagged
goat anti HIgG for 1 hour
IIT Bombay

40

Process steps in Silanization and Antibody Immobilization on


SiO2 surface

IIT Bombay

Steps in Antibody Immobilization


Silanization
(grafting of silane layer)

BSA treatment **

Linker attachment (Glutaraldehyde)

Rinsing with PBS


Grafting Antibody Layer
(HIgG/anti-Mb)

Rinsing with PBS

Antigen (anti HIgG/Mb) binding

Rinsing with PBS

[HIgG]: 0.1 mg/ml; [anti-HIgG]: 0.05 mg/ml


Rinsing with PBS**

[anti-Mb]: 0.5 mg/ml; [Mb]: 0.5 mg/ml


IIT Bombay

41

ANTIBODY IMMOBILIZATION RESULTS

SiO2

a)

Si3N4

b)

SU-8

Micrograph of silanized surface


patterned on silicon and treated with
HIgG followed by FITC tagged goat
anti-HIgG

a) Micrograph of silanized SU-8 cantilever


treated with HIgG followed by FITC tagged
goat anti-HIgG
b) Unmodified SU-8 surface showing self
fluroscence property
IIT Bombay

SU-8/Carbon black/ SU-8 cantilevers

Before Antibody Immobilization

After Antibody Immobilization


IIT Bombay

42

Antibody Immobilized SU-8/SiN-poly-SiN Cantilevers


Using Dry silanization protocol involving HWCVD

Fluorescence microscope images of FITC tagged antiHIgG


antibodies immobilized on a nitride/poly/nitride cantilever
bio-functionalized by the process of dissociated ammonia
treatment

SU-8 with immobilization after the


HWCVD surface treatment

M. Joshi et al., Applied Surface Science, Vol.253,No.6, pp.3127-3132, January, 2007


IIT Bombay

Cantilever Systems
Cantilever Platform: Low cost, Highly
Sensitive, Field Deployable
Bio-functionalization
System Level Integration

V.R. Rao: rrao@ee.iitb.ac.in

IIT Bombay

43

Cantilever Systems
Cantilever Platform: Low cost, Highly
Sensitive, Field Deployable
Bio-functionalization

System Level Integration

V.R. Rao: rrao@ee.iitb.ac.in

IIT Bombay

Liquid Cell Module


create a reaction chamber
environment for cantilever
sensors such that sensing
time and SNR can be
reduced along with the
miniaturization of overall
system.
we have developed a liquid
cell for oxide/poly/nitride
and SU-8 cantilevers: using
PDMS
IIT Bombay

44

Fabrication Flow of PDMS


Liquid Cell

IIT Bombay

PDMS Liquid Cell


Specifications:

Base material: Poly-dimethyl-siloxane (PDMS)


elastomer
Fabrication: Simple MEMS
fabrication processes
(optical Lithography,
Plasma treatment, etc.)

Volume: 10-20 L

Advantages: Biocompatible, easily


patternable, surfacemodification easy,
transparent

IIT Bombay

45

Integration of the Cantilever with


the Liquid Cell
SiO2 cantilever-die:
1. Plasma treatment (50W, 30 secs.) of the oxide
surface and the liquid cell surface (surfaces to be
adhered)
2. Heat treatment at 800 C
On SU-8 cantilever-die:
1. Applying semi-cured PDMS on both the surfaces
(SU-8 and liquid cell)
2. Heat treatment at 800 C
IIT Bombay

Cantilever-Liquid Cell Integration:


Selective Immobilization

Top View

IIT Bombay

46

Cantilever+Flow Cell

Cantilever Characterization Set-up


Explosive
Vapor
Generato
r

Gas Outlet

Key Features:

R/R Measurement
Circuitry
(Wheatstone
Bridge)

433MHz RF
Transceiver
16-bit
Microcontroller

Power
Management

24-bit
ADC
(Delta
Sigma)

LCD

Inside the Wireless Cantilever


Characterization System.
Specifications:
Range of R: 40K to 1M
Sensitivity: 0.7mV/ppm
Power supply: 12V batteries
Supply current: <100mA

Reliable R measurement down to 2


ppm
Half/Full bridge configuration of
cantilevers
Compensation for R mismatch
Precision performance
Graphic LCD and in-built signal
generator (version 2)
High resolution acquisition using 24-bit
ADC (version 2)
Adjustable gain and sensitivity
Easy calibration
Rechargeable battery operated system
Low cost

Sudip Nag et al., "An Ultra-sensitive R/R Measurement System for Biochemical Sensors using Piezoresistive
Micro-Cantilevers", 31st Annual International Conference of the IEEE Engineering in Medicine and Biology
Society (EMBC'09), Minneapolis, Minnesota, USA, 2nd - 6th September, 2009

IIT Bombay

Cantilever Characterization System


Reference
Cantilever
(piezoresistor R)
Voltage Reference

R
Buffer

Programmable Gain
Amplifier

24-bit ADC

Data Out
(To Microcontroller)

Measuring Cantilever
(piezoresistor
RR)

Wheatstone Bridge based R/R measurement system


Neena et al., Current Excitation Method for R Measurement in Piezo-Resistive Sensors
with a 0.3-ppm Resolution IEEE Transactions on Instrumentation & Measurement,

March 2012

Neena et al. Piezoresistive 6-MNA Coated Microcantilevers with Signal Conditioning Circuits
for Electronic Nose Applications, ASSCC, 2012
IIT Bombay

47

The Best reported Cantilever Characterization


Till date: IITB

IIT Bombay

Specifications of the Cantilever


Characterization System
Range of R
Range of R
Sensitivity *
Resolution*
Sampling Time
Actuating signal
Power Supply
PCB Size

:
:
:
:
:
:
:
:

1K to 2M
0.3 ppm to 2000 ppm
~1.2mV/ppm
~2ppm
0.25 seconds
DC, 1.5V
+3V DC, 11mA (with RF)
33mm 17mm 15mm

Neena et al., Current Excitation Method for R Measurement in Piezo-Resistive Sensors


ith a 0.3-ppm Resolution IEEE Transactions on Instrumentation & Measurement, March 2012
Neena et al. Piezoresistive 6-MNA Coated Microcantilevers with Signal Conditioning Circuits
for Electronic Nose Applications, ASSCC, 2012
IIT Bombay

48

Bio-ICAS
Photo of SC_IITB_2

IIT Bombay

Bio-ICAS, Recent Measurement Results of INA in


SC_IITB_2
DC current=5.5 A

Post-layout
simulation

Measurement

19.98 dB

19.52dB

115 dB

107dB

up to 40mV
(pp)

up to 40mV (pp)

Input-referred voltage noise


density (with chopper)

88nV/Hz at
5Hz

50nV/Hz at
5Hz

Input-referred voltage noise


density (without chopper)

2V/Hz at 5Hz

Input common-mode voltage


range

0.6 to1.2V

0.7 to1.2V

Linearity (w.r.t. common-mode


input voltage)

+/- 1.6%

Linearity (w.r.t. diff. input voltage)

+/- 1.5%

Specification
Voltage Gain
CMRR
Input Diff. Voltage Range

Optimal design
for ultra lowpower
consumption in
0.18 um CMOS
process.
At least 50%
power reduction
maintaining high
CMRR and low
input noise,
compared to
latest reported
designs in higher
technology
nodes. IIT Bombay

49

Exploratory Sketches - iSens

IIT Bombay

CAD Packaging of Components

IIT Bombay

50

A polymer composite cantilever based iSens Prototype


for cardiac Diagnostics

IIT Bombay

Ver-2 for Hospital Trials:


iSens Working prototype built jointly with NanoSniff Technologies Pvt. Ltd.

IIT Bombay

51

Cantilever Characterization with antibodyantigen interactions

Myoglobin
Detection

PBS

IIT Bombay

R Experiments ( Rf Ri )
Myoglobin Anti Myoglobin

IIT Bombay

52

R Experiment using FABP Anti FABP

IIT Bombay

Only FABP ( No Anti - FABP )

IIT Bombay

53

R Experiment using spiked serum ( with FABP )

IIT Bombay

Proposed Technology
iSens technology has the following pros &
cons
Benefits: Simple procedure, low cost, fast
response
Possible to integrate with CMOS technologies
Disadvantages: Unproven new technology

The system should be adaptable to new


international standards for cardiac
diagnostics
V.R. Rao: rrao@ee.iitb.ac.in

IIT Bombay

54

An Ultra-sensitive Piezo-resistive
Polymer Cantilever Technology
iSens: A point of care system for Cardiac Diagnostics

Explosive Detection
Technology Enables for Web enabled Cardiac
monitoring
System-in-Package solutions
IIT Bombay

Explosive DetectionChallenges ..1

Important factors for analysis and detection:


Specific Functional Group
Elemental Composition

Explosives under purview


TNT (2,4,6-TriNitroToluene)
RDX (hexahydro-1,3,5-trinitro-1,3,5-triazine)
PETN (PentaErythritol TetraNitrate)

IIT Bombay

55

Explosive DetectionChallenges ..2


Popular
Name

Chemical
Formula

Decomposition
Temp. (oC)

Molecular
Mass (g/mol)

Density at
20C (g/cm3)

Vapor
Pressure
at 25oC (torr)

TNT

C7H5N3O6

240

227.13

1.654

~ 6.0 x 10-6

RDX

C3H6N6O6

170

222.12

1.820

~ 5.0 x 10-9

PETN

C5H8N12O4

190

316.14

1.773

~ 1.5 x 10-8

Currently available sensor systems suffer from several problems, viz. cost, size,
sensitivity, selectivity
IIT Bombay

Explosive Detection: Challenges ..3


Chemical Composition

- Diversity in chemical composition.


- High Nitrogen density is not unique to explosives.
Plastics like Melamine, Polyurethane and Nylon too
have comparable nitrogen densities.

Very low vapour pressures: TNT (13 ppbv), RDX


(0.0084 ppbv) at 300 K.

Deliberate Concealment: Shape can be easily changed


by moulding techniques; densities too are variable.
IIT Bombay

Dual Degree 1st Stage

56

Different Approaches: IIT-B


Introduction
The Challenges in Explosive Detection
Current Worldwide status
IIT-B Explosive Detection Approach based on
Cantilever Deflection
Deflagration (jointly with Prof. S.Mukherji, Bio-school, IIT-B)
Organic Sensors (OFETs)
Florescence Quenching Prof. Anil Kumar, Chemistry, IIT-B
Pattern Recognition
Surface Plasmon Resonance/ Evanescent wave based optical

detection (Prof. S.Mukherji, Bio-school, IIT-B)

Orthogonality in package for reduced false positives


IIT Bombay

Cantilever based Explosive Detection @


IIT Bombay
Surface coatings
(a) 4-mercaptobenzoic acid
(4-MBA)
(b) Fluoroalcohol
polysiloxane polymer
(SXFA)
(c) Porphyrin
coating on cantilevers
(d) 6-Mercaptonicotinic Acid
[6- MNA]
(e) Other proprietary coatings

Electrical Transduction
IIT Bombay

57

MEMS Pre-concentrator

IIT Bombay

Microcantilever Experimental Setup for


explosive vapor detection
Schematic of the experimental
set up for explosive experiments

Experimental set up

Vapor generator with an


MFC and 3 way valves for
controlling Nitrogen and
explosive gases

Signal conditioning
circuit and a PTFE gas
flow cell containing
cantilever.

Vapor Generator
developed in TBRL
Data acquisition

IIT Bombay

58

Functionalization of Polymer Microcantilevers


for Explosive Detection
Selective coating for Explosives
4-MBA
SXFA
Sputtering of 5nm of Ti and
SXFA in Chloroform is applied
30nm of Au.
selectively on the cantilevers
Cantilevers are dipped in 6mM
solution of 4 -MBA* for 24 hours
Cant#

f (kHz) after Ti/AU


coating

f (kHz) after 4-MBA

100

79.5

Curvature of the
Cantilever after 4-MBA
coating

IIT Bombay

Polymer nanocomposite microcantilever sensor


(a)

(b)

1 2mm to 6mm
conversion
(3) Incorporation of smaller PTFE gas flow cell 1
for microcantilevers
8
Nozzle:

10 mm diameter
PTFE flow cell

Faster response with smaller flow cell

(b) Effect of nitrogen flow rate

1/31/2013

IIT Bombay

59

IIT Bombay

Air Flush

IIT Bombay

60

Piezo-resistive detection of explosives with


composite polymer microcantilevers

RDX & TNT: ppb level of detection routinely possible with these
micro-cantilever systems now !

IIT Bombay

Flow rate from MFC


Temperature
Duration of dry
N2 purging before
starting the
experiment

Functionalization

IIT Bombay

61

Flow rate from


MFC
Temperature
Duration of dry
N2 purging
before starting
the experiment
Functionalization

IIT Bombay

Flow rate from MFC


Temperature
Duration of dry
N2 purging before
starting the
experiment

Functionalization

IIT Bombay

62

Microcantilever Response to test samples


A: Benzophenone
B: Diphenyl Acetic Acid
C: TNT
D: Dihydrocholestrol
E: 3,4-Dimethoxy-2,5dimethyl ester of thiophene
F: diol diester of thiophene
G: m-Dinitrobenzene

H: 1-Chloro-2,4dinitrobenzene
I: 3,5-dinitrobenzoic acid

IIT Bombay

Microcantilever sensor for explosive vapor


detection
Experimental set up
Vapor generator

Flow cell integrated with the


Cantilever PCB.

Microcantilever PCB connected to a


signal conditioning circuit

6 ppt of RDX on 4-MBA coated

cantilevers creates a surface stress of


roughly 30 mN/m

0.36 mV/ppb of TNT in our


poly.comp. Cantilevers highest
reported
IIT Bombay

63

Explosive Detector Prototype for RDX/TNT developed


@ IIT Bombay

Seena et al., IOP Nanotechnology , 22 (2011) 295501


IIT Bombay

IIT Bombay

64

IIT Bombay

HEMRL test report for the Cantilever sensors developed at IIT Bombay
D = Detected; ND = Not Detected
S No

Composition

HMX
NG (Nitroglycerine)
NC (Nitrocellulose)
C-4
RDX
PEK
LTPE
TNT
Composition B
Tetryl
Prima Cord
Sheet Explosive
PETN
ANFO
Ammonium Nitrate
SEMTEX
TATP
EGDN
KClO4
KClO3
PBX

Cantilever based systsem


with proprietary surface
coatings

FIDO (Response)

Cantilever based Flourescence based


2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
21

D
D
ND
D
D
D
D
D
D
D
D
D
D
ND
D
D
D
D
D
D
D

D
D
D
ND
D
D
D
D
D
D
D
D
D
D
D
D
ND
ND
ND
ND
NDIIT Bombay

65

E-Dog (s) to Sniff out Explosives

An ultra-sensitive
(parts-per-billion
level)
nano-electromechanical
sensor

A rechargeable
Li-Po battery

Wireless
Transmission
Module

A real dogs nose 100 to 10 Million times more sensitive than humans. In
laboratory tests dogs were able to detect 1 to 2 parts billion routinely and in some
cases 500 parts per trillion, below the detection limit of any available equipment today.
IIT Bombay

Approaches to address
selectivity
Selectivity through coatings
Antibodies for explosives !!
Cantilever Arrays
Orthogonality in package
Photo-thermal cantilever response
with Pyroelectric materials
MEMS Pre-concentrator

IIT Bombay

66

Microcantilever sensor for explosive vapor


detection
Explosive detection- further approches
Use of dehumidification technique at the inlet of the sensor unit.
eg. A zeolite membrane
Functionalizing microcantilevers using molecules having the Host-Guest
properties
1. Calixerines (A wide class of cyclic oligomers)
Aromatic rings constitute cup shaped cavity.
Deposited or immobilized onto solid surfaces.
Inherit appropriate pre-organization of the host molecule,

since the calixarene macrocycle is shaped like a

conical basket, where it possesses a lower rim

and an upper rim


2. Metallated Porphyrins
Microcantilever arrays with different coatings on individual cantilevers and
perform a pattern recognition.
Bringing orthogonality to sensing.
IIT Bombay

Miniaturized wireless explosive detector

Packaged flow cell for explosive detection

PCBs for wireless explosive detector

Fully automated and stand off detection

Packaging: CMET PUNEE

IIT Bombay

67

IIT Bombay

Piezoelectric Cantilevers
Transduction applications
Energy Scavenging

Piezoelectric Photo-patternable Polymer


Composites
- ZnO
- Various multiferroic materials

Multiferroic materials

Self

powered
wireless Sensor
Networks

Mrunal A. K et al., "Electrical Actuation and Readout in a Nano-electro-mechanical Resonator


based on a Laterally Suspended Zinc Oxide Nanowire ", Nanotechnology, Vol. 23 (2012) 025501
Prashanthi et al., A Novel Photo-Plastic Piezoelectric Nanocomposite for MEMS Applications,
IEEE/ASME Journal of MEMS(J-MEMS), April 2012
Prashanthi et al"Local piezoelectric response of ZnO nanoparticles embedded in a
photosensitive polymer", Physica Status Solidi RRL 6, No. 2, 77-79 (2012)
M. Kandpal et al., Photopatternable nano-composite (SU-8/ZnO) thin films for piezo-electric
applications, Appl. Phys. Lett. 101, 104102 (2012)
IIT Bombay

68

Piezo-electric SU8 polymer composite


cantilevers out of ZnO nanoparticles

Prashanthi et al., IEEE/ASME Journal of MEMS (J-MEMS), April, 2012


Manoj et al., Applied Physics Letters, September 2012

IIT Bombay

Piezo-electric SU8 polymer composite cantilevers


out of ZnO nanoparticles contd

Prashanthi et al., Physica Status


Solidi RRL, Feb 2012
Prashanthi et al., IEEE/ASME Journal
of MEMS (J-MEMS) , April 2012
Manoj et al., Applied Physics Letters,
Sept 2012
IIT Bombay

69

ZnO-SU8 Polymer Composite Cantilevers for


Energy Scavenging applications

Piezoresponse (pm)

Response recorded by placing the


cantilever on a speaker
250
200
150
100
50
(b)

0
0

4
6 IIT Bombay
8
10
Voltage (V)

Development of Novel Multiferroic materials


for MEMS Applications
Coexistence of magnetic & ferroelectric
ordering in a certain range of temperature
Presence of coupling between two order
parameters (M-E effect) offers an
additional degree of freedom in device
designing
Tremendous application potential in the
area of MEMS and non-volatile memories
Jointly with Prof. V.R.Palkar & Dr. Prashanthi K., IIT Bombay
IIT Bombay

70

Material studies
1. Inducing ferromagnetism in antiferromagnetic BiFeO3 without disturbing its
ferroelectricity by means of doping at Bi sites (Bi 0.6La0.1Dy0.3FeO3)
2. Removal of La from Dy modified BFO system (bulk and thin films) leads to
reduction in the leakage current and improvement in ferroelectric
properties
enhancement in the magnetic properties by one order of magnitude
3. Magnetic anisotropy develops non-linearly with the thickness of the films

correlated to internal stress developed during growth process

4. Effect of permanent magnetic field and electric field on the dielectric


response of the BDFO thin films at GHz frequencies

The coupling between two phenomenon has been observed at

microwave frequencies
1. V.R.Palkar et al., Journal of Material Research, Vol.22, 2068-2073 (2007)
2. K Prashanthi et al., Solid State Communications, Vol.149, 188-191 (2009)
3. V.R.Palkar et al., Journal of Physics D: Applied Physics, Vol.41, 045003 (2008)
4. V.R. Palkar et al., Journal of Material Research, Vol.22, 2179-2184 (2007)
IIT Bombay

Co-existence and coupling of Ferroelectricity and


Magnetism at Macroscopic as well as at Microscopic Level

Very small magneticfield can induce


large electric
polarization

Coexistance of Ferroelectric
and Magnetic Properties at
Macro as well as Microscopic
Level

We are not aware of a


prior observation of an
electric-field-induced
magnetic hysteresis in
the magnetic domain
structure

Coupling Between Ferroelectric and


Magnetic Properties at Macro as well as
Microscopic Level

V. R. Palkar et al., Applied Physics Letters, Vol. 93, 132906 (2008)

IIT Bombay

71

MEMS Devices Using a Novel Multiferroic BDFO System


Bulk
Micromachining

Two-mask process

with contacts

Si<100> wafer

Step 2: BDFO deposition by


PLD
Step 3: Patterning of BDFO
using lithography and BDFO
etching

Step 4: Etching of Si to
release the cantilever
IIT Bombay

Microfabrication Process for BDFO cantilevers with gold as


top electrode
Step 1: RCA cleaned Si
wafer

Step 2: Deposition
of BDFO by PLD

Step 3: Patterning of
BDFO using lithography
(mask1) followed by
etching of BDFO in 5:1
BHF

Step 5: Patterning of
Cr/Au using
lithography (mask 2)
followed by Au/Cr
etching
Step 6: Bulk etching of
silicon using TMAH to
release the cantilevers

Silicon

BDFO

Cr

Step 4: Deposition
of Cr/Au layers by
sputtering

Gold

40um
200-500um

IIT Bombay

72

IIT Bombay

Dr. Prashanthi & Prof. Palkar

IIT Bombay

73

First Generation Handheld Device for detection


of TNT and RDX at Room Temperature
SIDE VIEW

Sub ppt sensitivity


Highly selective
10 prototypes
Available for field trials

TOP VIEW

Anilkumar, IITB
&
BIGTEC Labs
IIT Bombay

3-D Wireless Networked Sensor


Systems

iSens: A point of care system for Cardiac Diagnostics

Sensors for Security & Environmental Applications


- Explosive Detection
Technology Enablers for Web enabled Cardiac
monitoring

IIT Bombay

74

Silicon Locket

Low power ASIC based Fabricated & working fine


Low cost SU8 Accelerometer Motion artifacts
Undergoing field trials in hospitals
TCS-Industry partner

Lead investigator: Prof. D.K.Sharma & colleagues from Bio-school


V.R. Rao: rrao@ee.iitb.ac.in

IIT Bombay

A miniaturized 3 channel 12 lead


ECG unit

V.R. Rao: rrao@ee.iitb.ac.in

IIT Bombay

75

A modular 3 channel 12
lead ECG unit

Lead investigator: Prof. D.K.Sharma


V.R. Rao: rrao@ee.iitb.ac.in

IIT Bombay

ASIC for Silicon Locket

V.R. Rao: rrao@ee.iitb.ac.in

IIT Bombay

76

Future Plans for SiLoc ASIC

V.R. Rao: rrao@ee.iitb.ac.in

IIT Bombay

Motion Artifacts

V.R. Rao: rrao@ee.iitb.ac.in

IIT Bombay

77

First demonstration of polymer


based Accelerometer @IIT-B

20m

Optical and SEM micrographs of a structure with a seismic mass


supported by four beams attached to an anchoring region.
V.R. Rao: rrao@ee.iitb.ac.in

IIT Bombay

Low cost polymer accelerometers for


integration with the ECG electrodes

V.R. Rao: rrao@ee.iitb.ac.in

IIT Bombay

78

Polymer Composite Microaccelerometer


First time demonstration of Piezoresistive polymer MEMS
accelerometer.
Low temperature processing..
Simpler Process Flow
Improvement in sensitivity due to the lower Youngs modulus
of structural Polymer.
Smarter designs aiming for any type of application or
performance improvement can be easily implemented due to
the micromachining potential of the polymer using standard
UV lithography, e-beam lithography, laser, X-Ray,
Microsteriolithography etc.

IIT Bombay 157

Polymer Composite Microaccelerometer

Seena et al., Unpublished

IIT Bombay

79

Characterization of Polymer Composite


Microaccelerometer
using Polytek Laser Doppler vibrometer

Displacement =4.13nm
f = 13.9 kHz

Resonance Frequency
IIT Bombay

Polymer Composite Microaccelerometer


400

reldisp
Linear Fit of Data2_reldisp
Slope = 25

reldisp
Linear Fit of Data2_reldisp

350

Displacement of proof mass (nm)

Displacement of proof mass (nm)

Slope = 47.49
300
250
200
150
100
50

0
0

0.05

0.10

0.15

0.20

0.25

Acceleration (g)

Relative displacement of proof mass Vs


Input acceleration, device response at
f resonant = 10.01 kHz for a<0.3g

Acceleration (g)

Relative displacement of proof mass Vs Input


acceleration, device response at
f resonant = 10.01 kHz for a>1g

Seena et al., "A Novel SU-8 Composite Piezo-resistive MEMS Accelerometer to be


published

IIT Bombay 160

80

12 lead heart monitor with a


thermal printer
The unit is battery operated.
It has a user interface with a pictorial
guide for attachment for for any one
of the 12 standard ECG leads.
This allows a minimally trained person
to take an ECG, which has obvious
advantages in a rural setting.
ECGs can be collected by a eld
operator with printouts and then
examined at the hospital by a doctor.

This is a portable ECG unit with a printer, which can be easily


carried by a doctor in a briefcase
V.R. Rao: rrao@ee.iitb.ac.in

IIT Bombay

Realization of handheld Polymer


micro-cantilever Sensor Systems
Polymer Cantilever technology highly
suitable for low-cost disposable
Identify an application
health-care applications
The high sensitivity offered by this
technology helps build sensors for
cardiac marker detection & for
Develop the technology
detecting explosives in the vapor phase
down to the low ppt level
Simple instrumentation & low cost
Product Realization
(piezo-resistive measurements) enable
development of wire-less sensor
networks for environmental/ security
applications
Low Temperature Processes (max 100
Commercialization
deg C) Integration with CMOS Post processing for CMOS
V.R. Rao: rrao@ee.iitb.ac.in

IIT Bombay

81

Angel Funded by Priaas investments, R&D Funding by ICICI


SPREAD
16 people currently employed in NanoSniff including 5
Ph.D.s
Three Products: OmniCant TM , Explosive Detector, iSens
OmniCant launched in August 2012
Setting up of manufacturing facilities
sales@nanosniff.com

V.R. Rao: rrao@ee.iitb.ac.in

IIT Bombay

IIT Bombay

82

IIT Bombay

Ver-2 for Hospital Trials:


iSens Working prototype built jointly with NanoSniff Technologies Pvt. Ltd.

IIT Bombay

83

Technology Transfers from CEN, IIT Bombay


Beagle Bigtech Industries, Bangalore
(Prof. Anilkumar, Chemistry)
Surface Plasmon Resonance
(Prof. S.Mukherji, DBSE)
A Detection system for E.coli and other waterborne bacteria
(Prof. S.Mukherji, DBSE)

Ultra Low voltage Devices & High Voltage I/O Devices


(Prof. V.Ramgopal Rao, EE)
Silicon Locket (Prof. D.K.Sharma, EE)

IIT Bombay

Prototypes/Products in the CEN@IIT-B

Portable ECG Monitor

Silicon Locket

D.K.Sharma & team

D.K.Sharma & team

Explosive Detector

PolySense Aqua

BEAGLE

Anilkumar

Portable SPR System

A.Q.Contractor
S.Mukherji

IIT Bombay
Explosive wireless sensor node

84

Thank You

IIT Bombay

Approaches to address
selectivity
Selectivity through coatings
Antibodies for explosives !!
Cantilever Arrays
Orthogonality in package
Photo-thermal cantilever response
with Pyroelectric materials
MEMS Pre-concentrator

IIT Bombay

85

More than Moore Era of CMOS Scaling


Spintronics,
Molecular
Electronics
Etc. s

Adapted from Evolution scenario for III-V/Ge devices on Si platform through (Takagi et al., ICSICT, 2010
pp.50-53, 2010)
IIT Bombay

Pentace/P3HT etc.

IIT Bombay

86

Organic Transistor Platform for Sensing


Applications
(a) Radiation sensing

A radiation study is carried out on OFETs to


see the effect of ionizing radiation
A P3HT based OFET is exposed to 60Co
radiation (1 krad/min) for different time span
Change in the characteristics of the OFETs are
observed after each radiation dose
A control sample is also characterized at the
same time to see the effect of degradation in
ambient
IIT Bombay

OFET Sensor Degradation


with Radiation

H. N. Raval, et al., Determining Ionizing Radiation using Sensors Based on Organic Semiconducting
Material, Applied Physics Letters, Feb 2009
IIT Bombay

87

Off-current and Current


Ratio

IIT Bombay

OFET array Based Personal Dosimeter


Applied for patent
PCT Application
filed
US patent is being
filed
Working with BARC
Device
Details

OFF
curren
t (Ioff)
(A)
1.77e-8

ON
current
(Ion)
(A)
1.98e-6

Mobilit
y
(cm2/V
s)
1.38e-3

Threshold
Voltage
(V)
-6.48

Ion/Ioff

Single

Radiation
Dose
(Gy)
0

OFET

10

2.34e-7

2.88e-6

7.83e-4

7.75

12.3

Sensor

30

3.48e-7

3.10e-6

7.13e-4

11.01

8.89

3- OFETs
Connected
In Parallel

0
10

1.4e-7
7.56e-7

6.36e-6
7.67e-6

1.38e-3
7.68e-4

-5.63
5.96

45.3
10.1

30

1.12e-6

8.45e-6

7.41e-4

8.35

8.42

H.N.Raval, V.Ramgopal Rao, IEEE EDL, Accepted, 2010,

112

IIT Bombay
H.N.Raval et al., IEEE EDL, 2009, pp. 484 486.

88

(b) OFETs for Explosive Detection


a

-6

VGS= 0 to -20 V
Before Exposure
After Exposure

-10

Drain Current IDS (A)

Drain Current IDS (A)

-12

Before Exposure
After Exposure

-3

-6

-2

-4

-1

-2

-10

-20

-30

-40

Drain Voltage VDS (V)

R.S. Dudhe, et al. Appl. Phys. Lett., 93,


2008, 263306
R.S.Dudhe, et al.,
Sensors and
Actuators A: Physical, Vol. 148, 2010,
pp.158.
Sandeep G. Surya et al.,, ",, Sensors &
Actuators B: Chemical (Elsevier), 2012

VGS= 0 to -20 V

-4

-8

-5

0
0

-10

-20

-30

-40

Drain Voltage VDS(V)

V.R. Rao: rrao@ee.iitb.ac.in

IIT Bombay

OFET Passivation

Nitride passivation layers for polymer electronics


S.P. Tiwari et al., Organic FETs with Hot-wire CVD (HWCVD) Silicon Nitride as a Passivation and Gate
Dielectric Layer, Volume 516, Issue 5, Pages 770-772, Thin Solid Films, 2008
V.R. Rao: rrao@ee.iitb.ac.in

IIT Bombay

89

(c) OFETs for CO Sensing

To be published in
APL

V.R. Rao: rrao@ee.iitb.ac.in

IIT Bombay

IIT Bombay

90

CO Sensing with Polymer Composite Cantilevers

IEEE Trans. On Nanotechnology , July 2012

IIT Bombay

Some Research Directions

Circuit Design for Energy Scavenging applications (Sub 0.3 V operation)


Device-circuit co-design (o/p resistance issues in piezo-electric MEMS
devices and its impact for circuit design) (series-parallel connection of
MEMS piezoelectric devices)
Low frequency Vibration Energy Harvesting (Devices, circuits, analysis)
Modeling polymer composite piezo-electric cantilevers/Size/shape effects
Asymmetric immobilization for Cantilevers
Novel piezo-resistive platforms
Self powered ICs/Sensor systems
MEMS-CMOS co-design
MEMS-Organic electronics integration
Circuit design with organic electronics
OFET Sensors
Pattern recognition approaches/algorithms
Use of MEMS Switches to reduce CMOS Standby power/System level
modeling
Sensors for Agricultural applications (Precision farming)
Ultra low power Micro-pumps for air & liquid handling (sensor networks)
Other cantilever based sensors
IIT Bombay
V.R. Rao: rrao@ee.iitb.ac.in

91

B. K. Chakravarthy
Industrial Design Centre, IIT Bombay

Students/Post-docs:

Seena, Nitin Kale, Manoj Joshi, Sheetal Patil,

Prashanthi, Abhinav Prasad, Deepika Reddy, Dilip


Agarwal, Sudip Nag, Naveen Kadayinti, Neena,
Avil Fernandez, Sahir Gandhi, Gaurav Chatterjee,

Faculty Collaborators:

S.Mukherji (Immobilization), Dept. of Bio-Sciences & Engg.


D.K.Sharma (Instrumentation): Dept. of Electrical Engineering

Anilkumar (Surface coatings), Dept. of Chemistry


M.Shojaei (ASIC Design); Dept. of Electrical Engineering
P.R.Apte (Fabrication): Dept. of Electrical Engineering
C.P.Rao (Calixerines): Dept of Chemistry
M. Ravikanth (Porphyrins): Dept of Chemistry
Prita Pant (Nano-indentation): Dept. of Metallurgy & Mat.Sci.
V.R.Palkar (Multi-ferroics), Dept. of Electrical Engg.
B. K. Chakravarthy (Prototype-development) Industrial Design Centre
Amit Agarwal (Micro-fluidics), Dept. of Mechanical Engineering
T.Kundu (photo-thermal), Dept of Physics
IIT Bombay
Funding from NPSM, DIT,V.R.
NPMASS,
DST
Rao: rrao@ee.iitb.ac.in

Initial Explosive Detector Prototypes

IIT Bombay

92

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