Synthesis of Tin Oxide Nanoparticles by Sol-gel method

Titanium dioxide (TiO2) is a semiconducting transition metal oxide material. It can be used in solor cells,
chemical sensors, self-cleaning surfaces, and environmental purification, etc. Photocatalytic activity of
TiO2 is one of the most distinctive features. It can be exist in lab crystalline and amorphors forms and
exists in three crystalline polymorphs; anatase, rutile and brookite. There are are many methods to
synthesize TiO2 such as conventional solid state route, hydrochemical, sorochemical, etc. Among then,
Sol-gel method is the promising route for synthesis of powders for photocatalytic materials.

Requirements:

(1) Titanium isopropoxide (Ti(OCH(CH3)2)4)

(2) Citric acid monohydrate (CC3H5O(CO)3H3H2O)
(3) Nitric acid
(4) Ammonium hydroxide
(5) Deionized water
(6) Ice bath
(7) Oven
(8) Muffle furnace
(9) Filter paper, beaker, pH paper, conical flask, etc.

Characterization technique XRD, SEM

Experimental procedure
(1) 1.0m of NH4OH solution is added to titanium isopropoxide (TiO(H(CH 3)2)4) is an ice bath at
10Ċ to titanic acid [ Ti(OH)4] .
(2) Then, it is dissolved in nitric acid to form titanyl nitrate [TiO(NO 3)2]
(3) To adjust pH value of the solution, deionized water containing 0.3m Titanium isopropoxide
and 1.0m NH4OH is added.
(4) After adjusting pH range 2-6, white precipitate sol is obtained.
(5) Then it is washed, filtered and dried in an oven at 80Ċ for 2h.
(6) Then, the resulting gel is calcined in muffle furnace at 400Ċ and 800Ċ for 2h.
(7) Then, it is characterized by XRD, &SEM.

Conclusion
At pH 2-6,
(a) Calcination Temperature 400Ċ, 2h
TiO2-> anatase structure
At pH 2-4
(b) Calcination Temperature 600Ċ, 2h
TiO2-> multiphase of anatase and rutile structure

=>The TiO2 particles are highly agglomerated and irregular in shape with particle sizes in the
range of 0.1-0.5µm.
=>When pH values and calcination temp: is increased from 2->6 and 400Ċ to 800Ċ respectively
the size of both rutile and anatase phases increased