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1
A
M. Sc. Research Project Report on
Supported Silver Nanoparticles: Synthesis,
Characterization and Catalytic Studies
Submitted by,
Mr. Aamer S.K.R.
Under the guidance of,
Dr. Sagar D. DelekarAssistant Professor,
Department of Chemistry,
Dr.Babasaheb Ambedkar Marathwada University, Aurangabad
Sub-campus Osmanabad 413 501 (M.S.) India
2011-2012
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Objectives
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Synthesis of supported silver nanoparticles
using Chemical reduction method.
Characterization of synthesized catalyst by various
spectroscopic methods such as XRD, FT-IR, TEM,
EDAX and UV-Visible measurement
catalytic activity of supported Silver NPs for
reduction of aromatic nitro compounds
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Why Silver?
Nobel Metal,
Low cost
Antimicrobial activity
Electrical conductivity-High
light response occur in the visible regime
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Methodology
4
Sol-gel
Electrochemical Deposition
Laser
Chemical reduction
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Chemical Reduction Method
Advantages: Able to generate special shaped nanoparticles
Low temperature synthesis
Simpler technology
The lower cost
Less instrumentation
Self assembling
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5mL 0.001 M Silver Nitrate+
6mL 0.01M Dextrose
Reduced Silver
10mL 0.009M SDS solution
Colloidal Silver Nanoparticles
Colloidal Silver NPs
+
TiO2 NPs
Silver supported
TiO2 Nanocatalyst
Synthesis Route
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Characterization
UV-Visible Spectroscopy
X-Ray Diffraction (XRD) Studies
Transmission Electron Microscopy (TEM)
Energy Dispersive X-Ray Analysis (EDAX)
Fourier Transmission- Infrared Spectroscopy (FT-IR)
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Results and discussion
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200 300 400 500 600 700 800
0.0
0.1
0.2
0.3
0.4
0.5
Ag NPs
Ab
sorbance
Wavelength (nm)
Figure 1A: UV- Visible spectra of colloidal Silver Nanoparticles.
UV-VISIBLE STUDIES
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300 400 500 600 700 800
0.0
0.1
0.2
0.3
0.4
0.5
0.6
0.7
0.8
0.9
c
b
a
a= after 1 monthb= after 2 month
c= after 3 month
Absorbance
Wavelength (nm)
Figure 1B: UV-Vis Spectrum of Silver Nanoparticles
for stability measurements
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300 400 500 600 7000.0
0.2
0.4
0.6
0.8
1.0
b
a
Ab
sorbance
Wavelength nm
a-Ag-TiO2
b-TiO2
Figure 1C: UV-Visible spectra of Supported Silver Nanoparticles
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X-RAY DIFFRACTION STUDIES
20 40 60 800
2000
4000
6000
8000
10000
(400)
b
a
(312)
(215)
(220)
(116)
(204)
(105)
(200)
(004)
(101)
(111)In
tensity(A.U
.)
a- Ag-TiO2[JCPDS#22-1272]
b- TiO2[JCPDS#03-0939]
Figure 2: XRD patterns of TiO2and Ag supported TiO2 nanoparticles.
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TRANSMISSION ELECTRON
MICROSCOPY
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Figure 3a: TEM image of
pure TiO2 NPs
Figure 3b: TEM image of
Ag supported TiO2 NPs.
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ENERGY DISPERSIVE X-RAY
ANALYSIS
Figure 4: EDAX pattern of 1 mole% Ag supported TiO2 NPs
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FOURIER TRANSMISSION
INFRARED SPECTROSCOPY
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4000 3500 3000 2500 2000 1500 1000
0.30
0.35
0.40
0.45
0.50
0.55
0.60
0.65
0.70
0.75
0.80
0.85
0.90
0.95
1.00
1.05
1.10
1098
1066
1226
1216
a
b
Transm
ittance%
Wavenumber (cm-1
)
Figure 5: FT-IR spectra of pure SDS and SDS capped NPs:
a) Pure SDS; b) SDS Capped Silver NPs
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CATALYTIC ACTIVITY
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Reduction of 4-nitrophenol to 4-aminophenol using
silver NPs supported on TiO2 as catalysts
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250 300 350 400 450 500
0.0
0.1
0.2
0.3
e
dc
b
a
Ab
sorbance
Wavelength (nm)
a= 4NP
b= 4NP+NaBH4
c= 10mind= 20min
e= 30min
Figure 6: UV-Visible spectra of catalytic study of reduction of 4-NP to 4-AP.
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Conclusions
Successful synthesis of silver NPs by chemical
reduction method.
Simplicity and stability
Supported silver NPs on TiO2 have been best materials
for the reduction of aromatic nitro compounds.
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