Transcript Slide 1

Examination of mechanical stability and gas sensor application
of (As2S3)100-x(AgI)x chalcogenide glasses
INA
K. Kolev1*, T. Petkova1, C. Popov2
1
2
Institute of Electrochemistry and Energy Systems (IEES), Bulgarian Academy of Sciences
Institute of Nanostructure Technologies and Analytics (INA), University of Kassel, Germany
EXPERIMENTAL SET–UP
MOTIVATION
 Development of new transduction principles in the sensoric technique
 Search for new sensitive materials
 New sensors with improved sensitivity, selectivity and reliability
MFC-1
Flow Chamber
Electronic Sensor
Analyte 1
MFC-2
carrier
gas
Different functionalization
layers for diverse gases
sensor
inlet
Electronics
acquisition
card
valves
Analyte 2
MFC-3
Mass-flow
controllers
outlet
PC
SORPTION PROPERTIES
 Fabrication process – complementary metal-oxidesemiconductor (CMOS) technology
64.480
64.475
64.470
25 %
8%
17 %
33 %
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Water
Methanol
Isopropanol
Acetone
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64.455
54 %
64.450
0
 Integration of transducer, actuator and read-out in one unit
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14
21
28
35
42
49
56
63
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water
methanol
ethanol
isopropanol
acetone
ammonia
20
15
Resonance frequency, kHz
 Cantilever sensors – a miniature version of a microbalance
Resonance frequency shift, Hz
Resonance frequency, kHz
CANTILEVER–BASED
CHEMICAL GAS SENSORS
25
64.485
10
5
acetone in
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0
70
0
10
20
30
40
50
10
20
30
40
50
100
120
Response time, s
60
Concentration, vol%
Resonance frequency, kHz
 Decrease of the resonance frequency with addition of mass, i.e.
by sorption of gas molecules
THEORETICAL BASIS of
STRESS INVESTIGATION
 K – spring constant of the cantilever
64.485
64.480
64.475
acetone out
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64.465
64.460
 1 – resonance frequency before exposure
0
16mm
20
40
60
80
Response time, s
16mm
8mm
4.6mm
5mm
3mm
4mm
4mm
2mm
6mm
123
5 67 4
 2 – resonance frequency after exposure
8.5mm
4mm
STRESS MEASUREMENTS
7mm
150
Stoney's equation:
s 
D2
ESi
6 (1   ) R
1
d
Initial stress
Stress after 3 Months relaxation
Focus on frame
Mechanical Stress, MPa
SURFACE and MORPHOLOGY
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0
Time, min
K  1
1 
  2 
m 
2  2
4   1  2 
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Focus on beam
s - film stress
d - film thickness
ESi - Young's modulus of the substrate
 - Poisson's ratio of the substrate
D - thickness of the substrate
R - curvature radius of the bending
L2 + h2
R
2h
L, h - length and deflection
of the cantilever beam
cantilever, deflection determined
by optical microscopy
h
h
compressive
tensile
d
tensile stress
0
compressive stress
-50
-100
-150
5
10
15
20
25
30
AgI content, %
D
h
50
0
Dcant
L
100
CONCLUSIONS
The surface and morphology analysis of the thin films shows that films are uniform, homogeneous, featureless
and smooth both on surface and in depth
 The magnitude and the sign of the stress are functions of the film composition and structure as well as of the
mechanical and thermomechanical properties.
 The bigger tensile stress of the samples with 5 % at. AgI can be related to initial incorporation of atoms with larger
atomic radius into As2S3 pyramidal structure.
 As AgI amount increases Ag atoms occupy the microvoids and thus the glass density enhances and the structure
stabilizes. This densification and stabilization of the structure leads to weakening of the tensile stress and change in
the sign of the mechanical stress to compressive in the samples with 25 and 30 % at. of AgI.
Resonating cantilevers functionalized with amorphous (As2S3)90(AgI)10 film were exposed to vapors of different
analytes, including water, VOC and ammonia, in order to study the sorption properties of the chalcogenide coating.
 The highest sensitivity was observed towards acetone, the analyte with one of the highest molecular weight and
with the lowest dipole moment among the tested analytes.
The authors gratefully acknowledge the financial support of the European
Social Fund (Program “Development of human resources”) under
contract BG051PO001/07/3.3-02/58/17.06.2008).
 The sensor acted primarily as a microbalance distinguishing the vapors by the difference in their molecular weight
with physisorption as main mechanism.
 The short response and recovery times together with the linear increase of the response signals with the analyte
concentration make the investigated As-S-Ag films a promising candidate for gas sensitive elements.