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1
Sol-Gel Technology and Solid State Reaction
Prepared by:
Adnan Majeed
2
Table of contents
Introduction
Sol and Gel
Sol gel process
Factors influencing sol-gel process
Applications
Advantages
Limitations
3
Introduction
• Sol gel processing designates a type of solid material synthesis,
performed in a liquid and at low temperature.
• It’s a typical nanotechnology. Because all gel products contain
nanoparticles or nanocomposites.
• Synthesis schemes used depends on initial precursors.
4
5
Sol and Gel
Sol is a stabledispersionof colloidalparticlesor polymers ina solvent.
Consist of liquidwithcolloidalparticleswhichareno dissolved,butdo not
sediment.
Gel is a three dimensional continous network which encloses liquidphase.
6
7
Suspension of finesolidparticles or liquid droplets in a gas.
Aerogel
Drying is performed atsupercriticalconditions, network structuremay be retained
and a gel withlargepores may be found.
Xerogel
Gelis dried by evaporation ,capillaryforceswillresultinshrinkage, the gel network
collapse.
Aerosol
8
Xerogel
Aerogel
9
Sol gel process
 Hydrolysisandcondensationofmolecule
 Gelation
 Ageing
 Drying
 Firing
 Densification
10
Factors influencing sol-gel process
• Parameters influencing hydrolysis
• Typeand amount ofcatalyst
• Parameters influencing condensation
• Type ofprecursor
• pH
• Type ofsolvent
11
Applicationsof Sol-Gel Technology
• Optical and photonic applications
• Mechanical applications
• Biomedical application
• Bioreactors
• Chemical Applications
• Electronic applications
• Thermal applications
12
 Can produce thin bond-coating to provide excellentadhesion between the
metallic substrate andthe top
 Can produce thick coating to provide corrosion protection performance.
 Can easily shape materials into complexgeometries in a gel state.
 Can producehigh purityproducts.
Advantages
13
 Can havelow temperature usually200-600°C.
 Can providea simple,economicand effectivemethod to
produce high quality coatings.
 Through sol-gel processing, homogeneous, high-purity
inorganic oxide glasses can be made.
14
Weakbonding
High permeability
Difficulty in controlling porosity
Substratedependency
Limitations
15
Solid-state reaction
• The solid-state reaction route is the most widely used
method for the preparation of polycrystalline solids from a
mixture of solid starting materials.
• The factors on which the feasibility and rate of a solid state
reaction depend include, reaction conditions, structural
properties of the reactants, surface area of the solids,
their reactivity and the thermodynamic free energy change
associated with the reaction.
16
Outline of the experimental procedure
Reagents
• These are the solid reactants from which it is proposed
to prepare a solid crystalline compound.
• The selection of reactant chemicals depends on the
reaction conditions and expected nature of the
product.
• The reactants are dried thoroughly prior to weighing.
• As increase in surface area enhances the reaction
rate, fine grained materials should be used if possible.
17
• After the reactants have been weighed out in the required amounts, they
are mixed.
• For manual mixing of small quantities, usually an agate mortar and
pestle are employed.
• Sufficient amount of some volatile organic liquid –
preferably acetone or alcohol – is added to the mixture to aid
homogenization.
• This forms a paste which is mixed thoroughly. During the process of
grinding and mixing, the organic liquid gradually volatilizes and has usually
evaporated completely after 10 to 15 minutes.
Mixing
18
• For the subsequent reaction at high temperatures, it is necessary to
choose a suitable container material which is chemically inert to
the reactants under the heating conditions used.
• The noble metals, platinum and gold, are usually suitable.
• Containers may be crucibles or boats made from foil.
Container material
19
• The heating program to be used depends very much on
the form and reactivity of the reactants.
• In the control of either temperature or atmosphere, nature
of the reactant chemicals are considered in detail.
• A good furnace is used for heat treatment.
Heat treatment
20
The product materials are analyzed using various
characterization techniques such as X-ray
diffraction (XRD), scanning electron microscopy
(SEM), transmission electron microscopy (TEM), etc.
Analysis
Thank you
21

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Sol gel method and solid state reactions

  • 1. 1
  • 2. Sol-Gel Technology and Solid State Reaction Prepared by: Adnan Majeed 2
  • 3. Table of contents Introduction Sol and Gel Sol gel process Factors influencing sol-gel process Applications Advantages Limitations 3
  • 4. Introduction • Sol gel processing designates a type of solid material synthesis, performed in a liquid and at low temperature. • It’s a typical nanotechnology. Because all gel products contain nanoparticles or nanocomposites. • Synthesis schemes used depends on initial precursors. 4
  • 5. 5 Sol and Gel Sol is a stabledispersionof colloidalparticlesor polymers ina solvent. Consist of liquidwithcolloidalparticleswhichareno dissolved,butdo not sediment. Gel is a three dimensional continous network which encloses liquidphase.
  • 6. 6
  • 7. 7 Suspension of finesolidparticles or liquid droplets in a gas. Aerogel Drying is performed atsupercriticalconditions, network structuremay be retained and a gel withlargepores may be found. Xerogel Gelis dried by evaporation ,capillaryforceswillresultinshrinkage, the gel network collapse. Aerosol
  • 9. 9 Sol gel process  Hydrolysisandcondensationofmolecule  Gelation  Ageing  Drying  Firing  Densification
  • 10. 10 Factors influencing sol-gel process • Parameters influencing hydrolysis • Typeand amount ofcatalyst • Parameters influencing condensation • Type ofprecursor • pH • Type ofsolvent
  • 11. 11 Applicationsof Sol-Gel Technology • Optical and photonic applications • Mechanical applications • Biomedical application • Bioreactors • Chemical Applications • Electronic applications • Thermal applications
  • 12. 12  Can produce thin bond-coating to provide excellentadhesion between the metallic substrate andthe top  Can produce thick coating to provide corrosion protection performance.  Can easily shape materials into complexgeometries in a gel state.  Can producehigh purityproducts. Advantages
  • 13. 13  Can havelow temperature usually200-600°C.  Can providea simple,economicand effectivemethod to produce high quality coatings.  Through sol-gel processing, homogeneous, high-purity inorganic oxide glasses can be made.
  • 14. 14 Weakbonding High permeability Difficulty in controlling porosity Substratedependency Limitations
  • 15. 15 Solid-state reaction • The solid-state reaction route is the most widely used method for the preparation of polycrystalline solids from a mixture of solid starting materials. • The factors on which the feasibility and rate of a solid state reaction depend include, reaction conditions, structural properties of the reactants, surface area of the solids, their reactivity and the thermodynamic free energy change associated with the reaction.
  • 16. 16 Outline of the experimental procedure Reagents • These are the solid reactants from which it is proposed to prepare a solid crystalline compound. • The selection of reactant chemicals depends on the reaction conditions and expected nature of the product. • The reactants are dried thoroughly prior to weighing. • As increase in surface area enhances the reaction rate, fine grained materials should be used if possible.
  • 17. 17 • After the reactants have been weighed out in the required amounts, they are mixed. • For manual mixing of small quantities, usually an agate mortar and pestle are employed. • Sufficient amount of some volatile organic liquid – preferably acetone or alcohol – is added to the mixture to aid homogenization. • This forms a paste which is mixed thoroughly. During the process of grinding and mixing, the organic liquid gradually volatilizes and has usually evaporated completely after 10 to 15 minutes. Mixing
  • 18. 18 • For the subsequent reaction at high temperatures, it is necessary to choose a suitable container material which is chemically inert to the reactants under the heating conditions used. • The noble metals, platinum and gold, are usually suitable. • Containers may be crucibles or boats made from foil. Container material
  • 19. 19 • The heating program to be used depends very much on the form and reactivity of the reactants. • In the control of either temperature or atmosphere, nature of the reactant chemicals are considered in detail. • A good furnace is used for heat treatment. Heat treatment
  • 20. 20 The product materials are analyzed using various characterization techniques such as X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), etc. Analysis