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SYNTHESIS OF CERAMICS

KESHAV SINGLA CH8227 HARSHITA GUPTA CH8218

The synthesis of ceramic nanoscale particles have received considerable attention in view of potential because of unique properties and materials. The numerous applications of ceramic nanopowders have encouraged researchers to explore physical and chemical methods for their synthesis. METHODS OF SYNTHESIS 1.PHYSICAL METHODS 2.CHEMICAL METHODS

INTRODUCTION

1. PHYSICAL METHODS Vapour Condensation. Spray Pyrolysis. Thermochemical Decomposition. 2. CHEMICAL METHODS Sol-gel Technique. Reverse Microemulsions Method. Mechanochemical Synthesis. Precipitation of Solutions. Chemical synthesis of preceramic polymers.

VAPOUR CONDENSATION METHOD


STEP 1 : Metallic nanopowder condensed under a inert convection gas(argon or helium). Supersaturated metal vapours obtained in the chamber. STEP 2: Powder oxidised by introducing oxygen in the chamber. Nanoparticles collected on the surface cooled by liquid nitrogen. The post-oxidation is a critical method and it should be done slowly. Due to highly exothermic reaction, particle heats upto 1273 K for very short time(1sec) resulting in agglomeration into large particles. So a subsequent annealing process is required to complete the oxidation.

STE

VAPOURISATION METHODS
1.Thermal evaporation:
Different types of heat sources are used to produce supersaturated vapours. Preparation of nanoparticles by supersaturated vapours produced by thermal evaporation was first established in 1930 to first prepare nanoparticles of elements. Oxides were later prepared by the same method by introducing oxygen into the metal vapour.

2.Sputtering :

Has advantages over thermal evaporation method. Can be used for wide variety of materials . Stable and easily controlled method. Both DC and RF magnetron sputtering are used to prepare nanoparticles and nano clusters.

Evaporation source consists of a sputter source with a sputter target positioned normal to the cold surface axis. Example-Nanoparticles of ZrO2 are produced using a sputter source that has a zirconium target of 75mm diameter positioned 100mm from the cold surface. Metal oxide ceramics can be prepared in two ways: 1. Metal particles prepared by DC sputtering using an argon atmosphere are allowed to react with oxygen. 2. Second method involves reactive RF sputtering of a metal target using Ar/O2 gas mixtures. Oxygen should be continuously added to the sputter chamber to replace the amount consumed. The second method is preferable since it avoids high temperature particle agglomeration that normally occurs during postoxidation.

3. Laser methods

Laser evaporation is achieved by focussing a high energy pulsed laser onto the metal target of interest. The temperature at the focusing point can exceed 10000K and can vaporise any substance. The hot metal atoms are then allowed react with oxygen or ammonia inside the chamber to form vapor phase metal oxide metal nitride molecules. Oxides like ZnO, SiO2, TiO2, ZrO2, Al2O3 and MgO. Advantages include versatility, ease of performance and high purity products. Disadvantage is high production cost and difficulty in scaling up. Operating temperature is limited by the choice of source material and as a result the technique cannot be used for a wide variety of materials.

SPRAY PYROLYSIS
Spray pyrolysis is another useful method for synthesis of high purity homogeneous ceramic powders. The technique is also called solution aerosol thermolysis, evaporative decomposition of solutions, plasma vaporisation of solutions and aerosol decomposition. The starting material is chemical precursor mainly salts in solution, sol or suspension form. The process involves the generation of aerosol droplets by atomisation of starting solution. The droplets generated undergo evaporation with solute condensation within the droplet. This is followed by drying, thermolysis of precipitate particle at higher temperature to produce micro-porous particles. Various techniques like pressure, two fluid, ultrasonic and electrostatic atomisers can be used for atomisation.

Flame or Thermochemical Decomposition


Flame processes have been widely used to synthesize nanosize powders of ceramic materials. This is another type of gas condensation technique, with starting material being a liquid chemical precursor. The process is referred to as chemical vapor condensation(CVC). Chemical precursors are vaporized and then oxidized in a combustion process using a fuel- oxidant mixture such as propane-oxygen or methane-air. The flame usually provides a high temperature( 1200-1300 K), which promotes rapid gas phase chemical reactions. Flame process are used industrially to produce commercial quantities of ceramic particles like silica, titina etc. This is because of the low cost of production as compared to all other methods. The disadvantage of flame synthesis is that the control of particle size, morphology and phase composition is difficult and limited.

Several types of flame reactors have been used. One example is the recent development of a lowpressure flat flame combustion reactor. Advantages of this method are an increased production rate and the fact that pyrolysis and condensation occur in gas phase, which precludes impurity entrainment from the reactor walls. Nanoparticles of several ceramic oxides have been successfully prerared using this reactor, including TiO2,

CHEMICAL METHODS
There are five different types of chemical methods used in synthesis of ceramic nanoparticlesSOL-GEL METHOD REVERSE MICROEMULSION OR MICELLE METHOD PRECIPITATION FROM SOLUTIONS MECHANOCHEMICAL METHODS CHEMICAL SYNTHESIS OF PRECERAMIC POLYMERS

1.SOL GEL METHOD


Its a wet chemical technique for synthesis. Used to prepare metal oxides by hydrolysis of metal precursors mainly alkoxides in an alcoholic solution resulting in the formation of hydroxide. Condensation of hydroxide molecules by elimination of water leads to formation of a network of hydroxide molecules. So a gelatin forms and a dense porous gel is achieved. removal of solvent and drying of gel results in ultra fine powder of metal hydroxide. Since process starts with a nanosized unit and undergoes reactions on nanoscale , result is nanomaterials. Example-its used to produce porous

Sol gel process


Hydrolysis and drying are two key factors that determine the properties of final product. Hydrolysis rate depends on the electonegativity of metal atom, steric hindrance of alkoxy groups and molecular structure of the alkoxide. This process is mainly useful to prepare metal oxides but nonoxides can be prepared by using organometallic precursors. Sol gel process offers several advantages over other techniques for synthesising nanopowders of metal oxide ceramics.These include production of ultrafine porous powders and homogeneity of product at molecular level.

2. REVERSE MICROEMULSION OR MICELLE METHOD


It is one of the recent promising routes to nanocrystalline materials. Surfactants dissolved in organic solvents form spherical aggregates called reverse micelles.In the presence of water,the polar head groups of surfactant molecules organize themselves around small water pools ,leading to dispersion of aqueous phase in the continuous oil phase. Reverse micelles are used to prepare nanoparticles by using a water solution of reactive precursors that can be converted to insoluble nanoparticles.

Nanoparticle synthesis inside the micelles can be achieved by various methods including hydrolysis of reactive precursors and precipitation reactions of metal salts.Solvent removal and subsequent calcinations leads to final product. Surfactants like pentadecaoxyethylene nonyl phenyl ether(TNP-35), poly nonyl phenol ether(NP5) etc are used Parameters affecting the particle size distribution are: Concentration of precursor in the micelle. Mass of aqueous phase in the microemulsion. Advantages of this method arePreparation of very small particles Ability to control the particle size. Disadvantages areLow production yields. Need to use large amounts of liquids.

3. PRECIPITATION FROM SOLUTION (WET CHEMICAL SYNTHESIS)

It is one of the conventional methods for preparing nanoparticles of metal oxide ceramics. The process involves dissolving a salt precursor usually a chloride, oxychloride or nitrate , eg-AlCl3 to make Al2O3. The corresponding metal hydroxides usually form and precipitate in water on addition of a base such as sodium hydroxide or ammonium hydroxide. The resulting chloride salts are then washed away and hydroxide is calcined after filtration and washing to obtain the final oxide powder. The method is useful in preparing ceramic composites of different oxides by co-precipitation of corresponding hydroxides in same solution. Disadvantage of this method is the difficulty in controlling the particle size distribution. Fast and uncontrolled precipitation often takes place ,resulting in large particles.

4. CHEMICAL SYNTHESIS OF PRECERAMIC POLYMERS


This method involves the use of molecular precursors that facilitate the synthesis of nanomaterials containing phase of desired composition. Using chemical reactions to prepare the preceramic polymer overcomes the limitation of low production yields of physical methods. This method is useful in preparing non-oxide ceramics such as silicon carbide and silicon nitride. Metal carbides and metal nitrides are obtained by pyrolysis of polymers containing appropriate metal like silver or aluminium and carbon or nitrogen(preceramic polymers).

ExampleSilicon carbide and silicon nitride are the most important ceramic nanomaterials prepared via this route. They are synthesised by pyrolysis of polycarbosilanes and polysilazanes at temperatures between 1273 and 1473 K.

5. MECHANO-CHEMICAL METHODS

Mechanochemical synthesis involves mechanical activation of solid state displacement reactions. The process is used to make nanoparticles of ceramics like Al2O3 and ZrO2. It involves the milling of precursor powders to form a nanoscale composite structure that react during milling and subsequent heating. Eg-nanoparticles of Al2O3 prepared by milling AlCl3 with CaO powdere. A nanocomposite of CaO particles embedded within AlCl3 matrix is obtained. Subsequent heating at 573K led to nanoparticles of -Al2O3 within a CaCl2 matrix . The by-product CaCl2 can be removed by washing.

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