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Hydrothermal Method

The document summarizes several methods for synthesizing novel inorganic solids: 1) Hydrothermal synthesis involves heating reactants in a closed vessel called an autoclave above water's boiling point, allowing for crystal nucleation and growth. It can produce nanomaterials not stable at high temperatures. 2) Chemical vapor deposition involves chemical reactions of gaseous precursors on a heated substrate, forming a dense deposit. Reactant gases flow into a reaction chamber where they adhere and react on the substrate. 3) Intercalation involves inserting guest molecules between layers of a lattice, forming intercalation compounds like graphite intercalated with potassium that increases the interlayer spacing.

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74 views16 pages

Hydrothermal Method

The document summarizes several methods for synthesizing novel inorganic solids: 1) Hydrothermal synthesis involves heating reactants in a closed vessel called an autoclave above water's boiling point, allowing for crystal nucleation and growth. It can produce nanomaterials not stable at high temperatures. 2) Chemical vapor deposition involves chemical reactions of gaseous precursors on a heated substrate, forming a dense deposit. Reactant gases flow into a reaction chamber where they adhere and react on the substrate. 3) Intercalation involves inserting guest molecules between layers of a lattice, forming intercalation compounds like graphite intercalated with potassium that increases the interlayer spacing.

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avni vats
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© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
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NOVEL INORGANIC

SOLIDS
PRESENTATION
PREPARED BY : SONIYA PRASAD
COURSE : B.SC CHEMISTRY (H)
ROLL NO : 21/76004
HYDROTHERMAL METHOD
 The hydrothermal method involves heating the reactants
in a closed vessel, an autoclave with water. The
autoclave is usually constructed from thick stainless
steel withstand the high pressures and is fitted with
safety valves. It may be lined with non reactive
materials such as Teflon. The autoclave is heated, the
pressure inside increases and the water remains liquid
above its normal boiling temperature of 373K so called
‘superheated water’. These conditions in which the
pressure is raised above the atmospheric pressure and
the temperature is raised above the boiling temperature
of water are known as hydrothermal conditions.
HYDROTHERMAL METHOD
Mechanism of hydrothermal method :
 Synthesis of nanomaterials by hydrothermal method is a
crystallisation process directly from solutions that usually
involves two steps : crystal nucleation and subsequent growth.
 Nucleation occurs when the solubility of the solute exceeds
its limit in the solution i.e, when the solution become
supersaturated.
 The reaction is irreversible,the solute precipitates into clusters
of crystals that grow to macroscopic size.
 Following nucleation, the crystals grow sequentially or
concurrently via a series of processes involving the
incorporation of growth units, which have the same
composition as crystal entities but posses the same or
different structures from the bulk solution into existing crystal
entities and causing increased sizes.
 These different processes can be roughly categorized
into four steps – transport of units through solution,
attachment of units to surface, movement of units on
surface and attachment of units to growth sites.
Advantages :
1. Hydrothermal synthesis can generate nanomaterials
which are not stable at elevated temperatures.
2. Nanomaterials with high vapor pressures can be
produced with minimum loss of materials.
3. These methods are more environment friendly.
4. It creates large sized and high quality crystal and
nanoparticles.
Disadvantages :
5. High cost of equipment.
CHEMICAL VAPOR DEPOSITION
 chemical vapor deposition can be defined as the
deposition of a solid on a heated surface from a
chemical reaction in the vapor phase. It belongs to the
class of the vapor transfer processes which is atomistic
in nature.
 Chemical vapor deposition results from the chemical
reaction of gaseous precursors at a heated substrate to
yield a fully dense deposit.
Instrumentation
Working
 A pre defined mix of reactant gases and dilute inert
gases are introduced at a specified flow rate into the
reaction chamber.
 The gas molecules move to the substrate and adhere.
This is called adsorption.
 The reactant get absorbed on the surface of the substrate.
 The gas molecules chemically react forming a solid that
adheres to the surface i.e, the reactants undergo chemical
reactions with the substrate to form the film.
 The gaseous by products of the reactions are removed
from the surface called desorption and evacuated from
the reaction chamber.
 During the process of chemical vapor deposition , the
reactant gases not only react with the substrate material
at the surface but also in gas phase in the reactor’s
atmosphere.
 Reactions that takes place at the surface are known as
heterogeneous reactions.
 Heterogeneous reactions selectively occur on the heated
surface of the substrate where they create a good quality
films.
ADVANTAGES :
1. It can be applied to a wide variety of base materials
including gases, ceramics and metals.
2. It can be used for coating or freestanding structures.
3. Materials can be deposited with high purity.

DISADVANTAGES :
4. The precursors needed to be volatile at near room
temperature.
5. The by products of CVD reactions can also be
hazardous.
6. CVD precursors can also be highly toxic, explosive or
corrosive.
INTERCALATION METHOD
The solids produced by the reversible
insertion of guest molecules into lattices
are known as intercalation compounds.
GRAPHITE INTERCALTED
COMPOUNDS
 Potassium vapor reacts with graphite above the
melting temperature of potassium , it forms a
golden compound KC8 .
 potassium ions sit between the graphite layers
and the inter layer spacing is increased by
200pm.
 Addition of small amount of KO2 to the molten
potassium results in the formation of a double
layer of potassium atoms between the graphite
layers and a formula close to KC4.
THANK YOU

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