VISVESWARAYA TECHNOLOGICAL UNIVERSITY

DAYANANDA SAGAR COLLEGE OF ENGINEERING

DEPARTMENT OF CHEMICAL ENGINEERING

TITLE:
SYNTHESIS AND CHARACTERIZATION OF NANOCOMPOSITE AND
ITS APPLICATIONS

KUMAR SHIVESH PROJECT GUIDE: Prof. DEEPA H. A.

NISSIM JACOB
TRISHA MAJUMDER 1

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 Introduction
 Objectives of the project
 Methodology
 Synthesis of Titanium dioxide nanoparticle
 Synthesis of Copper Oxide nanoparticle
 Synthesis of CuO-TiO2 nanocomposite
 Characterization
 Application
 Results and Discussion.
 Conclusion
 References
 Acknowledgement

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What is nanotechnology?
Nanotechnology is the ability to control or manipulate materials on the atomic scale to
create structures that have novel properties and functions because of their size, shape or
composition.
What are nanoparticles?
Nanoparticles are particles between 1 and 100 nanometers in size. In nanoparticles,a
particle is defined as a small object that behaves as a whole unit with respect to its
transport and properties.
Nano Crystalline metal oxides and composites have attracted continuous attention
due to their versatile applications in optical devices, sensors, catalysis, photo catalysis.

What is a solar cell?

A solar cell or photovoltaic cell is an electrical device that converts the energy of light
directly into electricity by the photovoltaic effect which is a physical and chemical
phenomenon.
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 To synthesize the nano -metal oxides and
their composites .
 To characterize the synthesized nano metal
oxides and composites for the required
physical and chemical properties such as
size, morphology,band gap engineering.
 To test , estimate and enhance the optical
properties such as photo conductivity, by
fabrication of Dye Synthesized Solar Cell.

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 Procurement of Chemicals.
 Synthesis of nano-metal oxide and its composite
 Characterization of the Synthesized nano composites by
SEM XRD and UV spectroscopy.
 Fabrication of Dye-Synthesized Solar Cell.

CuO nanoparticle TiO2 nanoparticle CuO-TiO2 Solar cell

nanocomposite
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 In the present work,TiO2 nanoparticles were prepared by solution combustion
synthesis treatment of solution of a titanium precursor with water and fuel
 Titanium tetra butoxide was a starting reagent for TiO2 synthesis.

Fig 1: Titanium Tetra-butoxide

 An aqueous solution was prepared in a petridish by taking 6 ml of the titanium
tetra-butoxide and 24 ml of 1:1 Nitric acid.
 The aqueous solution of titanium was then mixed with 2.8 grams of Glycine.
Glycine acts a fuel thus acts as an aid for combustion.

Fig 2: Titanium tetra butoxide+1:1 HNO3 + Glycine

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 The solution was then put into the hot air furnace where the entire content is
charred at about 400 ˚C .
 The charred matter was then cooled and it was scrapped out into a crucible
 The crucible was again kept in hot air oven for about two hours at a high temp
about 550˚C
 The sample was allowed to cool inside the furnace for about 10-12 hours.
 The calcinated sample was then grounded carefully to obtain TiO2 of
nanoparticle size range as shown in fig 3.
 .
All the reagents used are of analytical grade


 Fig 3: TiO2 Nanoparticles

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 The synthesis of the CuO nanocrystals was formed by thermal
decomposition, which was prepared by precipitation of Cu(NO3)2 .
3H2O with fuel in aqueous solution.
 The CuO powders of different sizes and shapes were synthesized
by controlling technological parameters (such as the reaction
temperature/time, Cu:fuel molar ratio and initial concentration of
the copper precursor) .
 In present process, 5 grams of copper nitrate was taken in a clean
and dry petri dish and dissolved with 15 ml of distilled water and
stirred until a clear blue solution is obtained.
 The aqueous copper solution was then mixed with 2.8 grams of
glycine and 15 ml of distilled water followed by gentle stirring..
 The entire solution was then ignited at about 400˚C until the entire
content transforms into a black powder

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 The precipitate was then scrapped out carefully and then grounded into fine
powder
 The synthesized copper oxide nanoparticle is as shown in fig 4.

Fig 4: CuO Nanoparticle

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 The synthesis of CuO-TiO2 nanocomposites is briefly summarized as follows.
PART 1
 Stoichiometric amount i.e 6 ml of titanium tetra butoxide as the starting reagent,
24 ml of 1:1 nitric acid was taken in Perti dish (I) and titanium solution was
prepared as shown in fig 6.
 This solution was in the form of a coagulated gel type matrix which has to be
grounded using glass rod until uniform size.

Fig 5: Titanium Tetrabutoxide Fig 6: Petridish containg Titanium

Tetra-butoxide and 1:1 Nitric
Acid

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PART 2:
 In another Petri dish (II) 5grams of copper nitrate trihydrate was taken which was
dissolved in 15 ml distilled water.
 To this 2.8 grams of glycine and 15 ml of distilled water was added which acts
like a fuel for combustion.
 This entire mixture was stirred well and poured into Petri dish (I). As shown in fig
7.

Fig 7: Petridish containing both Titanium and Copper precursor.

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PART :3
 The solution was then heated in a hot air oven for 10-15 minutes
until the entire content is charred with dissipation of smoldering
gases.
 The charred content was then allowed to cool and then carefully
scrapped into a clean and dry crucible as shown in fig 5.
 The crucible was then calcinated in a hot air oven at temp about
550˚C for two hours to obtain homogenous single phase end
product.
 After calcination the entire content was allowed to cool for about
10-12 hours.
 The entire content of the crucible was then grounded manually until
a fine textured end product was obtained as shown fig 6.
 The grounded end product was transferred into clean and dry
sample bottles.
 All the chemicals that were used for this synthesis are strictly of
analytical grade and was used without further purification.

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 SYNTHESIS OF CuO-TiO2 NANOCOMPOSITE

FIG 8: Crucible containing charred nanocomposite

FIG 9:Pesel and Motar containing final CuO/TiO2 nanocomposite

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 Scanning electron microscope(SEM) analysis
 X-ray diffraction (XRD)analysis
 Ultra- Violet Spectroscopy ( UV) analysis

X- Ray diffraction SEM UV-Spectroscopy

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 Element Weight % Atomic % Net Int. Error % Kratio
CK 12.29 21.27 40.12 10.01 0.0561

OK 46.99 61.05 105.36 11.62 0.0535

TiK 40.72 17.67 891.63 1.93 0.3623

1(a) SEM image for TiO2 (b) EDAX image for TiO2 Nanoparticle

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 Element Weight % Atomic % Net Int. Error % Kratio
CK 22.59 51.00 30.22 12.50 0.0594

OK 12.58 21.33 44.66 12.00 0.0319

CuK 64.83 27.67 454.87 2.61 0.6031

2(a) SEM image of CuO (b) EDAX image of CuO Nanoparticle

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 Element Weight % Atomic % Net Int. Error % Kratio
OK 31.16 61.32 73.35 11.69 0.0552

TiK 28.17 18.52 449.81 2.66 0.2705

CuK 40.67 20.16 268.92 3.17 0.3755

3(a) SEM image for TiO2-CuO Nanocomposite (b) EDAX image for TiO2-CuO
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Counts
10-80-TiO2

1500

O2 Ti1

1000

500

O2 Ti1

O2 Ti1
O2 Ti1

O2 Ti1

O2 Ti1

O2 Ti1
O2 Ti1
O2 Ti1
0
20 30 40 50 60 70

Position [°2θ] (Copper (Cu))

Fig 4a:TiO2 nanoparticle X-Ray Diffraction

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Counts
10-80-Cu O

4000

Cu2 O1
3000

Cu1 O1; Cu2 O1

2000

Cu1 O1

Cu1 O1

Cu2 O1

Cu1 O1; Cu2 O1

Cu2 O1

Cu2 O1
1000

0
20 30 40 50 60 70

Position [°2θ] (Copper (Cu))

Fig 4b:CuO Nanoparticle X-Ray diffraction

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Counts
10-80 -TiO2CuO

O2 Ti1
2000

O2 Ti1; Cu1 O1
1000 Cu1 O1

O2 Ti1

O2 Ti1; Cu1 O1

O2 Ti1; Cu1 O1
Cu1 O1
O2 Ti1

O2 Ti1

Cu1 O1

Cu1 O1

Cu1 O1
Cu1 O1

Cu1 O1

O2 Ti1

O2 Ti1

Cu1 O1
0
20 30 40 50 60 70

Position [°2θ] (Copper (Cu))

Fig 4c:TiO2-CuO Nanocomposite X-Ray diffraction

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 UV/Vis spectrum of various samples
2

1.8

1.6

1.4

1.2
Absorbannce

0.8

0.6

0.4

0.2

0
200
212
224
236
248
260
272
284
296
308
320
332
344
356
368
380
392
404
416
428
440
452
464
476
488
500
512
524
536
548
560
572
584
596
608
620
632
644
656
668
680
692
Wavelength
TiO2 TiO2-CuO

Fig 5: UV-Spectroscopy for CuO, TiO2, TiO2-CuO

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The working principle of a DSSC is explained in figure below :

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 FABRICATION OF DYE SYNTHESIZED SOLAR
CELL:
 Synthesized TiO2 nanoparticles and TiO2-CuO nanocomposites were
separately coated on the conductive side of the fluorine tin oxide
coated glass plates.
 These glass plates were then treated with natural dye(majorly
consisting of anthocyanin) and electrolyte.
 The solar cell was completed by binding it with a carbon coated
fluorine tin oxide coated glass plate.
 Both the TiO2 coated dye synthesized solar cell and TiO2-CuO coated
dye synthesized solar cell was then tested for their conductivity using
a multi-meter.
 The conductance of the solar cells were evaluated. .
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 TiO2 coated TiO2-CuO coated
semiconductor elctrode semiconductor electrode
and counter electrode and counter electrode

TiO2 coated TiO2-CuO coated

completed solar completed solar cell
cell

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PARAMETERS TiO2 COATED SOLAR TiO2-CuO COATED
CELL SOLAR CELL

VOLTAGE 0.35 V 0.387V

BAND GAP 3.17 eV 2.85 eV

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 TiO2, CuO nanoparticles and TiO2-CuO nanocomposite were synthesized using
Combustion Synthesis method
 Synthesized nanoparticles and their composites were characterized using SEM,XRD,
UV Spectroscopy.
 The Band Gap Energy for TiO2-CuO nanocomposite was found to be 2.85 eV while for
TiO2 it was 3.17 eV which indicates that CuO–TiO2 has better ability of light absorption
when compared with TiO2.
 Dye sensitized solar cells were fabricated with TiO2 and TiO2-CuO nanocomposite and
their performances were compared.
 The voltage for TiO2 was found to be 0.25V where as for the TiO2-CuO nano composite
it was 0.39V. This clearly states the TiO2-CuO composite has better photo conductance
than TiO2

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[1] A.Kopp Alves et al., Novel synthesis and characterization of Nano structured Materials,Engineering
materials,DOI : 10.1007/978-3-642-412752_2,Verlag Berlin (2013).
[2]. Patil, K.C., Mimani,T., Solution Combustion Synthesis of Nanoscale Oxides and their composites,
Mater. Phys. Mech 4, 134 - 137 (2001) .
[3]. Kingsley, J.J , Patil , K.C., A Novel Combustion Process for the Synthesis of Fine Particle α – alumina
and related Oxide Materials, Mater. Lett. 6, 427 - 432 (1998) .
[4]. Claudia Longo , Macro. A., A Successful Combination of Materials ,Institituto de Quimica Universida
de Estadual de Campinas, Brazil (2002) .
[5]. Smestad, GP, Gratzel, M. (1998) Demonstrating electron transfer and nanotechnology: A natural dye-
sensitized nano crystalline energy converter. Journal of Chemical Education, 75 (6), 752-756.
[6]. Bailey, M., Park, J., Dhirani, A. (2002) Natural Dye-Sensitized Nanocrystalline Solar Cell. Department
of Chemistry,University of Toronto.
7]. How to build your own solar cell (http://www.solideas.com/solrcell/english.html), A Nano crystalline
dye-sensitized solar cell DIY.
[8]. Smestad, GP & Grätzel, M. (1998). Demonstrating electron transfer and nanotechnology: A natural dye-
sensitized nano crystalline energy converter. Journal of Chemical Education, 75 (6), 752-756.
[9]. Takechi, K., Muszynski, R., Kamat, PV. Fabrication procedure of dye-sensitized solar cells
(http://www.nd.edu/~pkamat/pdf/solarcell.pdf) .
[10]. O’Regan, B &Grätzel, M. (1991) A low-cost, high-efficiency solar cell based on dyesensitized
colloidal TiO2 films. Nature, 353 (6346), 737-740.
[11]. Gratzel. M (2005) , Solar Energy Conversion by Dye Sensitized Photovoltaic cells , Inorganic 27
Chemistry , Volume 4 , 6841 – 6851.

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THANK YOU

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We would like to express our profound gratefulness to Prof. Deepa
H.A., Assistant Professor, Department of Chemical Engineering
and Dayananda Sagar College of Engineering for guiding us all the
way till the end of the project.
We are deeply in debt to our honorable Principal and to our HOD
Dr.R. Ravishankar, who have cooperated whole heartedly for the
completion of our project.
We are equally thankful to Head of Department, and Staff Members of
the Chemical Engineering, Chemistry Department of M.S.
Ramaiha College of Engineering for providing us necessary
guidance.
We also express our gratitude and thanks to Staff Members (Teaching
and Non-teaching ) of the Chemical Engineering Department of
Dayananda Sagar College of Engineering, and Dr. K.S. Anantha
Raju, Chemistry Department of Dayananda Sagar College Of
Engineering for their support which led to successful completion of
the project.

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