Hydrothermal Synthesis

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4.

9 Hydrothermal Synthesis 105

4.9 Hydrothermal Synthesis

This synthesis method is useful to make a large scale production of nano to micro
size particles. In this technique adequate chemical precursors are dissolved in water
and placed in vessel made of steel or any other suitable metal which can withstand
high temperature typically upto 300 ı C and high pressure above 100 bars. The
vessel, known as autoclave, is usually provided with temperature and pressure
control as well as measuring gauges as illustrated in Fig. 4.32.
It is a very old technique, probably first used by the German scientist Robert
Bunsen, way back in 1839 to synthesize crystals of strontium and barium carbon-
ates. He used a thick glass tube and used temperature above 200 ı C and pressure
more than 100 bars. The technique was later used mostly by geologists and has
become popular amongst nanotechnologists due to the advantages like large yield
and novel shapes and sizes that can be obtained using this technique.
The technique becomes useful when it is difficult to dissolve the precursors at
low temperatures or room temperature. It is also advantageous to use the technique
to grow nanoparticles if the material has a high vapour pressure near its melting
point or crystalline phases are not stable at melting point. The uniformity of shapes
and sizes of the nanoparticles also can be achieved by this technique. Various
oxide, sulphide, carbonate and tungstate nanoparticles have been synthesized by
the hydrothermal synthesis.
Another variation of hydrothermal synthesis technique is known as forced
hydrolysis. In this case usually dilute solutions (10 2 to 10 4 M) of inorganic metal
salts are used and hydrolysis is carried out at rather higher temperatures than 150 ı C.

Fig. 4.32 Photograph of an autoclave set up

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