MS512

Sol-Gel Nano Materials and Process
Prof. Byeong-Soo Bae

Dept. of Materials Sci. & Eng.
bsbae@kaist.ac.kr
I.
II.
III.
IV.
Introduction
Chemistry of Precursors Solutions
Sol-Gel Process of Silica
Sol-Gel Process of Complex Oxides
(Ferroelectrics)
V. Sol-Gel Process of Hybrid Materials
VI. Sol-Gel Process of Mesoporous
Materials
Text:
1.
2.
A. C. Pierre, Introduction to Sol-Gel Processing, Kluwer Academic

Publisher, 1998
C. J. Brinker, G. W. Scherer, Sol-Gel Science, Academic Press,
1990
MS512 Nano Technology
I. Introduction
Sol-gel Processing
Sol-gel processing is a wet chemical route to synthesis of a colloidal suspension of solid
particles or clusters in a liquid (sol) and subsequently to formation of a dual phase material of
a solid skeleton filled with a solvent (wet gel) through sol-gel transition (gelation). When the
solvent is removed, the wet gel converts to a xerogel through ambient pressure drying or an
aerogel through supercritical drying. Thin (~ 100 nm), uniform and crack-free films can be
readily formed on various materials by dip, spin, or spray-coating; thick films can be obtained
by multiple coatings.
In the sol preparation, the precursors (either organic or inorganic) undergo two chemical
reactions: hydrolysis and condensation or polymerization, typically with acid or base as
catalysts, to form small solid particles or clusters in a liquid (either organic or aqueous
solvent). The solid particles or clusters are so small (1~1,000 nm) that gravitational forces are
negligible and interactions are dominated by van der Waals, coulombic and steric forces. Sols
are stabilized by an electric double layer, or steric repulsion, or their combination.
Colloid: a suspension in which the dispersed
phase is so small ( 1~1000 nm) that gravitational

forces are negligible and interactions are dominated by short-range forces, such as Van der Waals
attraction and surface charges.
Sol: a colloidal suspension of solid particles in a liquid .

Gel: a solid network filled with a second phase of colloidal dimensions, either liquid or gas that
also forms a three dimensional inter-connected network.
Gelation: also called sol-gel transition that begins with the formation of solid fractal aggregates that
grow until they extends throughout the sol.
Xerogel: a gel in which the solvent has been removed by evaporation at an ambient environment.
Aerogel: a gel in which the solvent has been removed by supercritical drying. An aerogel typically
has a porosity >75% and a BET surface area > 1000 m2/g.
Supercritical drying: a process of removing the liquid from the pores of wet gel above the
critical temperature and critical pressure.
Precursor: a starting compound for preparation of a colloid (or sol). It consists of a metal or
metalloid element surrounded by various ligands. It includes inorganic salts and organic compounds.
Hydrolysis: a chemical reaction in which hydroxyl groups become attached to the metal atom
by replacing the ligands in the precursor.
Condensation (or polymerization): A process that hydroxyl groups merge to form metaloxygen-metal bonds, while releasing a water molecule, resulting in formation of solid particles or
clusters through combining monomers, growth of particles or clusters, and linking of particles or
clusters into chains and networks that extend through the sol.
Steric force: a repulsion which results from polymers adsorbed to the interacting surfaces.
The physical basis of the steric repulsion is a combination of a volume restriction effect arising
from the decrease in possible configurations in the region between the two surfaces and an
osmotic effect due to the relatively high concentration of adsorbed polymers in the region
between the two surfaces as they approach one another.
Electric double layer: forms at the vicinity of a solid particle in a sol. When a solid
submerges into a liquid, the surface will be electrically charged and subsequently an electric
double layer forms due to the combination of coulombic, entropic and other specific forces. When
two particles approach each other, as soon as the double layers overlap, a repulsive electrostatic
force arises to prevent two solid particles to aggregate so that the sol is stabilized.
Sol-gel processing is a simple technology in principle but has required considerable effort to
become of practical use. Sol-gel enables materials to be mixed on an atomic level and thus
crystallization and densification to be accomplished at a much low temperature. However, a true
atomic level homogeneity in a multiple component system is an endeavor; the difficulty arises
from the fact that the chemical reactivity varies greatly from precursor to precursor. Precursor
modification and step-wise partial hydrolysis are the common approaches to homogeneity in
multiple component systems.
The advantages of the sol-gel process in general are high purity, homogeneity, and low
temperature. For a lower temperature process, there is a reduced loss of volatile components and
thus the process is more environmental friendly. In addition, some materials that cannot be made
by conventional means because of thermal and thermodynamical instability, can be made by this
process. The sol-gel process has many applications in synthesis of novel materials. Examples
include aerogels used in space crafts to capture stellar dust, xerogels as matrix in biosensors, and
high power laser materials.
Alkoxides:M(OR)n
M= Si,Ti,Zr,Al
R= -CH3, -CH2CH3
H ydrolysis
OR
RO
M
OR
OR
OR
2O
RO
OH
ROH
OR
Condensation
OR
RO
OR
OH + RO
OR
OR
OR
RO
OR
OR
O
OR
OR
OR
+ ROH
OR
RO
M
OR
OR
OH + HO
OR
OR
OR
RO
OR
O
OR
OR OR
+ HOH
Definitions of Sol-Gel Process

Alkoxide Sol-Gel
Dislich - Procedure to prepare the multicomponent oxides that are homogeneous at the
atomic level
should include the colloidal coprecipitates of hydroxides and oxyhydrates
restrict to the gels synthesized from metal alkoxides
Coloidal Sol-Gel
Segal Production of inorganic oxides either from colloidal dispersion or from the
metal alkoxides
non-oxides such as nitrides and sulfides, and organic-inorganic hybrids
Colloidal route used to synthesize ceramics with an intermediate stage including a sol
and/or gel state
Production of inorganic oxides either from colloidal dispersion or from the metal
alkoxides
Chemical processing to synthesize ceramics glasses, and hybrids from wet
chemicals
Inorganic Polymerization
Solution
Sol
Monomer
Dimer
O
O
O
O
O
O
O
O
Oxide
O
O
M
O
O
O
O
Oligomer
O
O
M
O
M
O
O
O
O
O
Solid
M
O
O
O
O
O
O
O
Colloid
O
O
O
O
Gelation
O
O
O
O
O
O
Sintering
Drying
Gel
Processing of Sol-Gel Materials

Powders
Monoliths
Coatings and Thin Films

Porous Materials and Aerogel
Fibers
Melting and Sol-Gel Process for Glass Fabrication
Advantages and Disadvantages of Sol-Gel Process

Advantages
Disadvantages
High purity from raw materials
High cost of raw materials
Good homogeneity from raw materials
Large shrinkage during processing
Low processing temperature
Residual fine pores and hydroxyls
Good shape ability
Health hazards of organic solution
Production of new composition glasses
Easily cracking during the drying stage

Long processing times
Characteristics of Sol-Gel Process

D Low temperature process of fine ceramics and glasses
D Bottom-up fabrication from chemicals
D Aqueous-based chemistry and process
D Immobilization & encapsulation over wide range of
sizes, chemistries and functions
D Mild & easily controlled conditions
D Molecular level dispersion
Fabrication of Sol-Gel Optical Fiber Preform
Sol-Gel Coatings on Display
Antiglare
Li
1.0% of incident light

<Interference effect>
gh
t
Silica layer
AR layers
CCoonnddu
uccttiivv
ee layer
Glass
Phosphor
Preparation of Nano Materials by Sol-Gel Processing
Solution
<100
C
Sol
<100
C
Wet
gel
<150
C
Dry
gel
<500
C
Heated
gel
<1200
C
Glass,
Ceramics
Porous gels
Pores
Organic molecules
Gels dispersed
with organic
molecules
Organic polymer
Inorganicorganic
composites
Gels
dispersed with
inorganic or
metal particles
Inorganic network
Glass
Ceramics
Particles
Grains
II. Chemistry of Precursors Solutions

Precursor Solution
Chemical Precursor
Chemical reactant which contain the cation M present
in the final inorganic sol or gel
Metallic salts - MmXn, eq) AlCl3
C2H5)3
Metal alkoxides M(OR)n, eq) Al(O
Organometalic compounds
Solvents
Water
Non-aqueous solution
Protic solvent
Aprotic solvent
Acidic solvent
Basic solvent
Amphoretic solvent
Hydrolysis of Metal Salts Solution

Ions Solvation
Dissolution is solution
MX Mz+ + Xz- in the solution
oxo ligand(O2-)
Cation solvation
Solvatation shell [M(H2O)N]Z+
Hydrolysis
Deprotonation of a solvated metal cation

Aquo ligand H2O hydroxo ligand(OH-)or an
Formation of Hydroxo Ligands

Solvated metal: an acid, Water: Lewis base
[M(OH2)N]Z+ + hH2O [M(OH)(OH2)N-1](z-1) + + H3O+
acid + Lewis base conjugates base conjugated acid
[M(OH)h(OH2)N-h] aquo-hydroxo complex
Formation of Oxo Ligands

Deprotonation of an hydroxo ligand
[M(OH)(OH2)N-1](Z-1)+ + hH2O [MOh(OH2)N-h] (Z-h)+ + hH3O+
acid+
Lewis base conjugated base + conjugated acid
[MO(OH2)N-1]z-2 aquo-oxo ligand complex
[M(OH2)N]Z+ + hH2O [M(OH)(OH2)N-1](z-1) + + H3O + hH2O [MOh(OH2)N-h] (Z-h)+ +

+
hH
: [MO H ]Z+
h=03O
N
2N
aquo-ion
0<h<N :
[M(OH)X(OH2)N-x](Z-X)+
(N-Z): M(OH)
h=N
hydroxo-aquo
N]
hydroxo
complex complex
N<h<2N : [MOX(OH)N-x](N+X-Z)oxoh=2N
hydroxo
(2N-Z)-complex
: [MON]
oxo-ion
Condensation of Metal Salt Solution

Condensation and Polymerization
Hydroxo ligand (M-OH) ol bridge (M-OH-M) oxo bridge (M-O-M)
Condensation by Olation
For the low charge cations dissociative SN1 mechanism
-M-OH + -M- M-OH-MH2OM -M- + H2O
For the higher charge cations nucleophilic addition reaction AN
-M-OH + -M-OH M-OH-M-OH
For the transition elements associative SN2 mechanism
Condensation by Oxolation
For the low charge cations dissociative SN1 mechanism
-M-OH + -M- M-OH-MH2OM -M- + H2O
For the higher higher charge cations nucleophilic addition reaction AN
-M-OH + -M-OH M-OH-M-OH
For the transition elements associative SN2 mechanism
Alkoxide Precusors
Alkoxides:M(OR)n
M= Si,Ti,Zr,Al
R= -CH3, -CH2CH3
Hydrolysis of Metal Alkoxides

Hydrolysis
Alkoxy group (OR) Hydroxo(OH) or Oxo(O) ligands
(1) Nature of alkoxy group
(2) Nature of solvent
(3) Concentration in solvent
(4) ) Water to alkoxide molar ratio rw = [H2O]/
[alkoxide]
(5) temperature
Formation of Hydroxo Ligands

M(OR)z + H2O M(OH)(OR)z-1 + ROH
Hydrolysis of Silicon Alkoxide
Acidic solution (pH < 2.5)

- Negatively charged particles
- [H3O]+ attack the oxygen in alkoxy group
Basic solution (pH > 2.5)

- Positively charged particles
- OH- attacks the Si in alkoxides
Formation of Oxo Ligands

Lewis base
Water vapor
Condensation of Metal Alkoxides

Condensation by Olation
SN2 nucleophilic substitution mechanism
Condensation of Oxolation
Transfer of the H to an OR ligand
Transfer of the H to an OH group
Condensation of Silicon Alkoxides
Acidic solution (pH < 2.5)

- Two step SN2 type mechanism condensation
- Protonation of silanol group
- Hydrolysis is faster than condensation
- Linear polymer
Basic solution (pH > 2.5)
- Deprotonation of silanol group
- Condensation is faster than hydrolysis
- Dense solid
Precursor Mixing
Mixing Two Alkoxides
Double alkoxides
- Mixing two alkoxides in same non-aqueous solvent
Simultaneous hydrolysis of simple alkoxides
- Simultaneous refluxing in solvent
Matching the hydrolysis rates of different alkoxides
- Partially hydrolyzed Si(OR)4 and Al(OR)3
Mixing Two Metal Salts

Mixing a Alkoxide with a Metal Salt
III. Sol-Gel Process of Silica
1 Aqueous Silicate
Kinetics of hydrolysis and condensation
is slower
Polymerization at pH 2 - 7
Proportional to [OH-]
3-D gel network by aggregation
Hydrolysis with water
Polymerization above pH 7 - 10
Stable sol
Particle growth rather than aggregation
Thermal decomposition
Polymerization below pH 2
Proportional to [H+]
Metastable
1 Silicon Alkoxide Sol-Gel

hydrolysis
Si- OR + H 2 O
Si- OH + R OH
estrification
alcohol conden sation

S i- O- Si
S i- O R + HO- S i
alcoholysis
+ R OH
water con den sation

S i- O H + HO- Si
Si- O- Si
hydrolysis
+ H 2O
Precursor Solution
Silicon alkoxide + water + alcohol + catalyst
H2O:Si molar ratio (r) 1~ over 50
Concentrations of acids or bases 0.01 ~ 7 M
Precursor Molecules
Tetraalkoxysilanes
Si(OR)4 :
TEOS(tetraethoxysilane),
TMOS(tetramethoxysilane)
Organoalkoxysilanes
RnSi(OR)3 :
MTMS(Metyltrimethoxysilane),
DMDMS(Dimetyldimethoxysilane)
Molecular Building Blocks

Hexamethoxydisiloane
Octamethoxytriethoxtsilane
Methoxylated cubic
octamer - Silsiquioxane
1 Hydrolysis of Silicon Alkoxides
Effects of Catalyst
H2O/Si Ratio (r)
1 Steric and Inductive Effects

Effects of Solvents
Protic solvent enhance hydrolysis
1 Condensation of Silicon Alkoxides

Effect of Catalyst
on
Minimum at about pH 1.5

Maximum at intermediate pH
Acid catalyzed
condensation (pH<2)
protonated silanol
Base catalyzed
condensation (pH>2)
deprotonated silanol
Steric and Inductive

Effects
Acidity of silanol higher

pH IEP
Basicity of silanol lower
pH IEP
In acid-catalyzed,
steric effects > inductive
effects
Effects of
Prof.Solvent
Byeong-Soo Bae
Protic solvent acid-
1 Structural Summary
Low pH Condition
Hydrolysis rate > condensation rate

Cluster-cluster growth network structure
High pH Condition
Unhydrolyzed monomers
Monomer-monomer growth - particles
Intermediate pH Condition
Minimum hydrolysis rate rate limiting
General Condition
Acid catalyzed, low water system drawing fiber

Acid catalyzed, high-water system bulk gels
Base catalyzed, high-water system particles
IV. Sol-Gel Process of Complex Oxides
Solution Process of Electo or Optical Ceramics
Sol-Gel Ferroelectrics
Lead
Titanium
Zirconium
Metallorganic Precursors
Metal alkoxides
Zr n-propoxide [Zr(OC3H7)4]
Ti isopropoxide [Ti(OCH(CH3)2)4]
Ethoxides, Butoxides
Inorganic or organic salts
La nitrate
Pb acetate
Alcohol or Water
Gelation Control
Firing Additives
Viscosity Adjustment
Precursor Solution
Solvents
Primary solvent - stablization
Chemical modifiers
-methoxyethanol, acetic acid glycol
Chelating agents
- -diketone (acetylacetone)
Secondary solvent
Ethylene glycol, propanol, methanol or water
Control in viscosity, pH, surface tension
Dipping,Spraying
or Spin Coating
Drying and Organic
Removal
280-400C
Multilayer
Coatings
Crystallization
400-700 C
Preparation of Ferroelectric Solutions

Alcohol-Based Solution
Pb acetate trihydrate, Ti isopropoxide, Zr n-propoxide
2-methoxyethanol + 2-methoxyethanol/water
Change to methoxides and partial hydrolysis
Water-Based Solution

Acetic acid + water, propanol, glycols
MOD Solution
Pb acetate, Ti acetylacetonate, Zr acetate
Pb 2-ethyl hexanonate, Ti isopropoxide, Zr tetra-n-butoxide
Water + methanol, hexane
Thermal decomposition
Fabrication of Ferroelectric Films
Sr metal
2-Methoxyethanol
Nb(OC2H5)5
Ba metal
2-Methoxyethanol
Distillation
Distillation
Ti isopropoxide
2-Methoxyethanol
2-Methoxyethanol
In dry N2 gas
Refluxing (12h)
Refluxing
0.4M precusor solution
0.1M SBN sol
Coating
Coating
Iteration
Iteration
Drying
Drying
Heat Treatment
for Crystallization
Heat Treatment
for Crystallization
Preparation of Stable Solution

Dilution
2-methoxyethanol + 2-methoxyethanol/water
Change to methoxides and partial hydrolysis
Chemical Modification and Complexation
Acetic acid + water, propanol, glycols
Surface Modification of Nanoparticles
Stablization of particles
IV. Sol-Gel Process of Hybrid Materials

size
mm
/
/
/
/
/
/
(FRP,FRC,FRM)
Nanocomposite
Physical
hybridization
1nm
Nanohybrid
1
hybridization
Class I (Nanocomposite)
D Organic dyes embedded in sol-gel matrix
Organic dyes, inorganic ions or molecules + silica, aluminosilicate, zirconia, titania
fluorescence, photochromic, non-linear optical properties
D Inorganic particles embedded in a polymer

Inorganic particles + polymer blend
D Organic monomers embedded in sol-gel matrices

Polymerizable organic monomer + sol-gel inorganic matrices
Polymerization
Sol-gel
D Polymers filled with in-situ generated inorganic particles

Inorganic particle formation by sol-gel reaction in a polymer matrices
Sol-gel
Polymerization
D Simultaneous formation of interpenetrating organic-inorganic networks

Alkoxides functionalized by liable plymerizable group
Polymerization
Sol-gel
D Obtension of ordered organic-inorganic structures

Insertion of organic molecules polymers into an anisotropic inorganic network
Build anisotropic inorganic particles using organic molecules and self assembled aggregates
Sol-gel
Class II (Nanohybrids)
D Organically modified silicon alkoxides
Sol-gel
D Polyfunctional alkoxysilanes
RxSi(OR)4-x
Polymerization
(RO)3Si-R-Si(OR)3
Sol-gel
D Alkoxysilanes functionalized by polymers (RO)3Si-Polymer-Si(OR)3

Sol-gel
D Surface modification by organoalkoxysilanes
Polymerization
D Template building blocks

Polymerization
D Ordered hybrid materials

Self-assembly of molecular units on surface hydroxyl groups
Hybrids from Sol-Gel Process of Organoalkoxysilanes

RnSi(OR)4-n
Network modifier ( R' : unreactable)
Network former ( R' :polymerizable)

O
methyl, ethyl
CnH2n+1-Si(OR)3
H2 C
phenyl
Si(OR)3
amino
H2N-(CH2)3-Si(OR)3
epoxy
O-(CH2)3-Si(OR)3
methacrylate
mercaptopropyl
HS-(CH2)3-Si(OR)3
H2 C
fluoro
CF3-(CF2)n-(CH2)2-Si(OR)3
R
CH-O-(CH2)3-Si(OR)3
vinyl
C Si(OR)3
H
=O
=
Si,Ti,Zr,...
R modifier
inorganic
R entrappe
d
molecul
e
Modification
Functionalization
organic
polymeric
chain
Crosslinking
Sol-Gel Hybrid Materials (HYBRIMER)

D
Organic Modification
Heterometal Network
Polymer Network
Silica Network
Compensation of
Characteristics
Y Hard and Stable
Y Soft and Flexible
Y Easy Process
Y Cheap
D Functionalization
Y Modification Y
New function
D Transparency
Y Optical materials
Y Functional coating
ORMOCER,
ORMOCER, CERAMER,
CERAMER, POLYCERAM,
POLYCERAM,
Hybrid
Hybrid Sol-Gel
Sol-Gel Glass,
Glass, Hybrid
Hybrid Polymer,
Polymer,HYBMRIMER
HYBMRIMER
Characteristics of HYBRIMER
D Transparency
D Functionality
D Compensation of Characteristics
D Modulation & Tunability of Characteristics
D Easy Process & Fabrication
D High Thermal & Chemical Stability
D Easy Encapsulation with Better Compatibility
Transparency of HYBRIMER
D Hybrids of molecular level
D Coloration by doping of dyes or colloids
D Application of optics, display, and coatings
Compensation of Characteristics
Ref.: Fraunhofer ISC

D Compensation of Polymer and Glass Properties
Polymers
Glass
Refractive index
1.40 - 1.65
1.35 1.95
Dielectric Constant
Low
High
dn/dT (10-7)
-140 to -85
-8 to 6
Thermal Expansion
150 to 700
-10 to 160
Youngs Modulus (Mpa)
1 -10
4 -130
Thermal Stability
90 -250
450 -950
Hardness
Low
High
D Mechanical Properties
Silica/PDMS HYBRIMER
Functionality of HYBRIMER
D Hydrophilic and Hydrophobic Coatings
Optical Application of HYBRIMER

D Solid state dye laser materials
D Rare-earth emission materials
D Nonlinear optical and photorefractive materials
D Photochemical hole burning materials
D Photochromic materials
D Optical sensor matrials
D Optical waveguide materials
Functionality of HYBRIMER
D NLO Chromophore HYBRIMER
Unpoled
Unpoled
Polymers
Sol-Gel
Si(OEt)3
(OEt)3Si
Hybrids
NLO
NLO
Si
Si
Si
O
NL O
SiO
O Si
(b
)
(c
)
O Si
Si
O
O
Si
Si O
NL
O O
O O
O
Si
Si
O
ON Si
LO
Si
NL
O
NL
O
NLO
O O
Si O
O
NLO
Si
(a
)
O
NL
NL O
O
NLO
O
O
OSi
O
Si
Si
Si
O
O
Si
Si
Hybrids
NLO
Si
Poled
Poled
Polymers
Sol-Gel
HCl / DMF
- CH3OH
- H2O
O
O
heating around Tg
electric field on
cooling
electric field off
SHG
EO
wave length change

Frequancy Doubling
spatial, wave front

Spatial Light Modulators
EO
amplitude, wave form

E-O Modulators
Silica vs. Polymer for Waveguide Materials

PPoollyy
SSiillii
FHD,CVD
ccatemp
a
High
Difficult,Expensive.
Lower
High
High
Low
Not
Not
Stress
Process
Absorption
Mechanical
Thermal
Spin-on
mLow
etemp.
rr
m
e
Easy, Cheap
Versatile
Low
Low
Low
Thermo-optics
Design
Functionality
Versatile
Polarization
dependence
Anisotropy
High
Versatile
Advantages of HYBRIMER Waveguide

Silica Waveguide
Manipulation of refractive index in a broad range
Easy fabrication
Easy incorporation of inorganic/organic doponts
HYBRIMER Waveguide
Thick films without cracks
Hydrogen bonding to stabilize
organic dopants
Photoimprinting, Easy
process
Sol-Gel Silica Waveguide

Manipulation of refractive index

in a broad range
Thermally and chemically
stable
Hardness for end facet
polishing
Polymer Waveguide
Micro-Patterning in HYBMRIMER by Photo-polymerization

Photo -i nitiator
UV
Selective etching
developing
R'=CH3;C2H4OH
= - C3 H6OOC -
Fabrication of waveguides
Encapsulation & Immobilization in HYBRIMER

D Entrapment of biomolecules and chemical species in porous structure
D Better compatibility in organic environments
D Applications in biosensor, bioreactors, chemical sensor, catalysis
VI. Sol-Gel Process of Mesoporous Materials

Micelle Structure
Spherical micelle
Cylindrical micelle
Lamellar micelle
Inverse micelle
Ordered Mesoporous Materials

Hexagonal packing of cylindrical micelles
Cubic packing of spherical micelles
Planar packing of micellar micelles
Hexagonal
Cubic
Cubic
Lamellar
Fabrication Procedure
Micellar rods with a surfactant micelles in a hexagonal array add inorganic
precursor solution in a polar solvent array of hollow oxide cylinders organic
heart elimination by washing or by calcination
Micelles with inorganic precursor solution
Surfactants
Alkyl-ammonium halide (cationic surfactant)

[CnH2n+1N(CH3)3]X- , X=Cl or Br Cetyltrimethylammonium bromide (CTAB)
Poly(oxyethylene) non-ionic surfactant [n-alkylpolyethylene glycol ethers]
CH3(CH2)n-1(OCH2CH2)mOH = CnEOm
Brij 56, C16H33(OCH2CH2)10OH
Poly(ethylene oxide)-block-poly(propylene oxide)-block-poly(ethylene

oxide)
Pure Silicate Composition

Liquid Crystal Templating Mechanism
Silica source TEOS, Ludox, fumed silica, sodium silicate
Alkyltrimethylammonium halide surfactant - cetyltrimethylammonium bromide (CTAB)
Base - sodium hydroxide or tetramethylammonium hydroxide (TMAOH)
Water
Silicate Rod Assembly
Silicate Layer Puckering
Charge Density Matching
Folding Sheets
Silicatropic Liquid Crystals
General Liquid Crystal Templating Mechanism: Electrostatic Mechanism
Applications
Catalysis
- High Surface Areas and Thermal Stability

Sorption and Separation
Inclusion of Nanostructured Materials
Optical Applications
- Dye Inclusion
- Nanocrystals (Quantum Dots)
- Organometallic Complexes
- Polymer Inclusions
- NLO and Laser Materials
- Photochromic Materials
Chemical Sensors
Insulator Materials
Low k Materials
Hydrogen Storage and Electrode Materials
- Carbon Nanotubes

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Sol-Gel Nano Materials and Process

Prof. Byeong-Soo Bae

A. C. Pierre, Introduction to Sol-Gel Processing, Kluwer Academic

Prof. Byeong-Soo Bae

MS512 Nano Technology

Prof. Byeong-Soo Bae

MS512 Nano Technology

Colloid: a suspension in which the dispersed

phase is so small ( 1~1000 nm) that gravitational

Sol: a colloidal suspension of solid particles in a liquid .

Prof. Byeong-Soo Bae

MS512 Nano Technology

Prof. Byeong-Soo Bae

MS512 Nano Technology

Prof. Byeong-Soo Bae

MS512 Nano Technology

Prof. Byeong-Soo Bae

MS512 Nano Technology

Definitions of Sol-Gel Process

Prof. Byeong-Soo Bae

MS512 Nano Technology

Prof. Byeong-Soo Bae

MS512 Nano Technology

Processing of Sol-Gel Materials

Coatings and Thin Films

Prof. Byeong-Soo Bae

MS512 Nano Technology

Melting and Sol-Gel Process for Glass Fabrication

Prof. Byeong-Soo Bae

MS512 Nano Technology

Advantages and Disadvantages of Sol-Gel Process

High purity from raw materials

High cost of raw materials

Good homogeneity from raw materials

Large shrinkage during processing

Low processing temperature

Residual fine pores and hydroxyls

Good shape ability

Health hazards of organic solution

Production of new composition glasses

Easily cracking during the drying stage

Prof. Byeong-Soo Bae

MS512 Nano Technology

Characteristics of Sol-Gel Process

Prof. Byeong-Soo Bae

MS512 Nano Technology

Fabrication of Sol-Gel Optical Fiber Preform

Prof. Byeong-Soo Bae

MS512 Nano Technology

Sol-Gel Coatings on Display

1.0% of incident light

Prof. Byeong-Soo Bae

MS512 Nano Technology

Preparation of Nano Materials by Sol-Gel Processing

Prof. Byeong-Soo Bae

MS512 Nano Technology

II. Chemistry of Precursors Solutions

MS512 Nano Technology

Hydrolysis of Metal Salts Solution

Deprotonation of a solvated metal cation

Formation of Hydroxo Ligands

Prof. Byeong-Soo Bae

MS512 Nano Technology