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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. Delekar


Assistant 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
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

Methodology
Sol-gel
Electrochemical Deposition

Laser
Chemical reduction

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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Synthesis Route
5mL 0.001 M Silver Nitrate + 6mL 0.01M Dextrose

Colloidal Silver NPs + TiO2 NPs

Reduced Silver
Silver supported TiO2 Nanocatalyst

10mL 0.009M SDS solution

Colloidal Silver Nanoparticles

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)

Results and discussion

UV-VISIBLE STUDIES
0.5

Ag NPs
0.4

Absorbance

0.3

0.2

0.1

0.0

200

300

400

500

600

700

800

Wavelength (nm)

Figure 1A: UV- Visible spectra of colloidal Silver Nanoparticles.


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0.9 0.8 0.7 0.6

a= after 1 month b= after 2 month c= after 3 month

Absorbance

0.5 0.4 0.3 0.2 0.1 0.0 300 400 500 600 700

b a
800

Wavelength (nm)

Figure 1B: UV-Vis Spectrum of Silver Nanoparticles for stability measurements


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1.0 a-Ag-TiO2 b-TiO2

0.8

Absorbance

0.6

0.4

0.2

b a

0.0 300

400

500 Wavelength nm

600

700

Figure 1C: UV-Visible spectra of Supported Silver Nanoparticles


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X-RAY DIFFRACTION STUDIES


(101)
10000 a- Ag-TiO2 [JCPDS#22-1272] b- TiO2 [JCPDS#03-0939] 8000

Intensity (A.U.)

6000 b

(004)

(105) (400)

4000 a 2000

(200)

(204)

(116) (220)

(111)

(215)
80

0 20 40

60

Figure 2: XRD patterns of TiO2 and Ag supported TiO2 nanoparticles.


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(312)

TRANSMISSION ELECTRON MICROSCOPY

Figure 3a: TEM image of pure TiO2 NPs


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Figure 3b: TEM image of Ag supported TiO2 NPs.

ENERGY DISPERSIVE X-RAY ANALYSIS

Figure 4: EDAX pattern of 1 mole% Ag supported TiO2 NPs


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FOURIER TRANSMISSION INFRARED SPECTROSCOPY


1.10 1.05 1.00 0.95 0.90 0.85 0.80 0.75 0.70 0.65 0.60 0.55 0.50 0.45 0.40 0.35 0.30 4000 3500 3000 2500 2000
-1

Transmittance %

1226 1098
a
1500

1216
1000

Wavenumber (cm )

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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

Reduction of 4-nitrophenol to 4-aminophenol using silver NPs supported on TiO2 as catalysts


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0.3

a= 4NP b= 4NP+NaBH4 c= 10min d= 20min e= 30min

Absorbance

0.2

d
0.1

c b

0.0 250 300 350 400 450 500

Wavelength (nm)

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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