Ceramic Powder
Synthesis
Solid State
Synthesis
Wet- Chemical
methods
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Ceramic Powder Synthesis: Solid State vs. Wet-Chemical Methods, Study notes of Inorganic Chemistry
An in-depth comparison between solid state and wet-chemical methods for the synthesis of ceramic powders. It covers various techniques such as ball milling, co-precipitation, polymer precursor method, combustion synthesis, and sol-gel process. The document also discusses the advantages and limitations of each method, including particle size control, energy requirement, and reactivity. It is a valuable resource for students and researchers in the field of ceramic materials science.
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2018/2019
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Ceramic Powder
Synthesis
Solid State
Synthesis
Wet- Chemical
methods
Solid-State
Synthesis
Oxide or Carbonate
precursors
Mixin
g
Calcinati
on
Phase
Identification
Ball
milling
Ceramic
Powder
Advantages of Wet-Chemical
methods
Low phase formation temperature
Produce highly pure ceramic powders
Control over particle size, size distribution and
particle shape
Ceramic powders produced have high reactivity
and therefore sinter at low temperatures.
Produce soft agglomerate and can be easily
deagglomerated
CO-PRECIPITATION
Mixture of metal ion solution
Spraying in to a bath of precipitating agent*
Filtration and washing of the precipitate Drying Calcination Deagglomeration
* Precipitating agents: NH
4
OH, NH
4
CO
3 or Oxalic acid ondition for co-precipitation olubility product of the precipitate should be very low he solubility product of constituent precipitate must be similar
Homogeneous Precipitation
Metal ion solution + Urea
or HMT
Heati
ng
Precipita
te
Filtration/washing
Drying
Calcinati
on
Ball milling
NH
2
-CO-NH
2
+ H
2
O 2NH
3
- CO 2 (CH2) 6 N 4 + H 2 O 4 NH3 + 6 H-CHO
Advantages
Produce monodisperse particles Produce spherical particles
Polymer Precursor
Method
Metal ion solution +
Polymer
Heati
ng
G
el
Calcinat
ion
Ball
milling
Ceramic
powder
COMBUSTION SYNTHESIS
Aqueous metal nitrate solution + Fuel ( urea or glycine) Heating ( 400 – 500 o C) Combustion Deagglomeration Nanocrystalline powder Advantages:
Low reaction time
(^) Nanocrystalline powder (^) High surface area Foamy zirconia ash obtained after combustio
AUTO COMBUSTION METHOD
Metal nitrate + Citric acid Heating Resin Auto ignition Ash Calcination Deagglomeration Nanocrystalline powder
CALCULATON OF AMOUNT OF FUEL FOR COMBUSTION
Valancy Balance Method The reducing valancy of metal ion = its charge Reducing valancy of carbon = + Valancy of nitrogen = Reducing valancy of hydrogen = + Oxidizing valancy of oxygen =- For the reaction 0.8 La(NO 3 ) 3 .6 H 2 O + 0.2 Sr(NO 3 ) 3 + Cr(NO 3 ) 3 .9H 2 O+ n NH 2 - CH 2 -COOH La0.8Sr0.2CrO 3 0.8[+3+(0+-2x3)3]+ 6(+1x2-2)]+0.2[+2+(0+-2x3)2]+ [+3+(0+-2x3)3+9(+1x2-2)] +n[0+1x2+4+1x2+4-2x2+1=
SPRAY
DRYING
Laboratory model spray dry
Metal salt
solution
Spray
dying
Calcinat
ion
Ball
milling
Ceramic
Powder
SEM of ceramic powder prepared by
POWDER
CHARACTERIZATION
- Powder density
- Surface area
- Particle size
- Morphology
DETERMINATION OF DENSITY
Weight of Sp. Gravity Bottle = W Weight of the bottle filled with water = W Weight of bottle + powder = W Weight of bottle + powder + Water = W4 (Stage 4) Weight of powder = W3-W Volume of bottle = W2-W Volume occupied by water in stage 4 = W4-W Volume of powder = Volume of bottle – Volume occupied by water = (W2-W1)- (W4-W3) Density = Mass /volume =W3-W1/(W2-W1)-(W4-W1)