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Unit-II

Synthesis
 Synthesis of ceramic powders and nanoparticles,
 sintering and grain growth mechanisms
Synthesis of Ceramic Powders

Conventional Ceramic Synthesis Route Wet-Chemical Route

• Generally Micron Size Particles • Nano-Size Particles


• As reaction is between particles • Reaction is at atomic or
• Could be made into submicron size molecular level
using high energy ball milling
(Planetary Ball milling)
• Thermodynamic and Kinetic factors are
important in in solid state reaction
Conventional Ceramic Synthesis Route Vs Wet-Chemical Route
• Both the chemical and mechanical methods have their own advantages and disadvantages.

• The mechanical method is successful for a large-scale production of bulk ceramic


powders at its low cost and easy adaptability.

• In conventional solid-state method, high temperature and heating for prolonged time
makes successful the particles coarse.

• Fine powders mainly prepared by chemical process have an improved homogeneity;


densifications and the chemical precursors used in this process can easily be refined to
increase the purity.

• However, in many cases, the chemical routes generally involve complex techniques
when compared to the conventional solid-state methods
Conventional Ceramic Synthesis Route
Direct reaction between solids wont react at room temperature High Temp. are required to react

Schematic of Solid State reaction in mixed powders


Synthesis of NaFe(SO4)2, a cathode material for Na ion batteries by standard
ceramic synthesis route

DST-SERB project
Wet-Chemical (Nano) Methods
Sol-Gel Synthesis
General schematic of the co-precipitation method
Wet-Chemical (Nano) Methods
1:1
Synthesis of NaFe(SO4)2, a cathode material for Na ion batteries by Wet-Chemical
route

DST-SERB project
1. Mechanical attrition
(Ball milling)
2. Lithography

1. Sol-gel
2. Chemical vapor
deposition (CVD)
TOP-down approach-Ball milling
Chemical Vapour deposition (CVD)
RF Plasma Synthesis

• Utilizes the plasma generated RF


coils
• Starting material is contained in a
pestle in a evacuated chamber
• The metal is heated above its
evaporation temperature using
high voltage RF coils, wrapped
around the evacuated system
• He gas is then allowed to enter
the system, forming a high
temperature plasma in the region
of the coils
• The metal vapour nucleates on
the He gas atoms and diffuses up
to a colder collector rod, where
nanoparticles are formed
Thermolysis
Nanoparticles can be made by decomposing solids at high temperatures having metal cation and
molecular anions or metal organic compounds. This process is called as thermolysis