Sol–gel process

In materials science, the sol–gel process is a method for producing solid materials from small molecules.
The method is used for the fabrication of metal oxides, especially the oxides of silicon (Si) and titanium
(Ti). The process involves conversion of monomers into a colloidal solution (sol) that acts as the precursor
for an integrated network (or gel) of either discrete particles or network polymers. Typical precursors are
metal alkoxides.

Contents
Stages
Particles and polymers
Polymerization
Sono-Ormosil
Pechini process
Nanomaterials
Applications
Protective coatings
Thin films and fibers
Nanoscale powders
Biomedical
Opto-mechanical
Medicine
See also
References
Further reading
External links

Stages
In this chemical procedure, a "sol" (a colloidal solution) is formed that then gradually evolves towards the
formation of a gel-like diphasic system containing both a liquid phase and solid phase whose morphologies
range from discrete particles to continuous polymer networks. In the case of the colloid, the volume fraction
of particles (or particle density) may be so low that a significant amount of fluid may need to be removed
initially for the gel-like properties to be recognized. This can be accomplished in any number of ways. The
simplest method is to allow time for sedimentation to occur, and then pour off the remaining liquid.
Centrifugation can also be used to accelerate the process of phase separation.

Removal of the remaining liquid (solvent) phase requires a drying process, which is typically accompanied
by a significant amount of shrinkage and densification. The rate at which the solvent can be removed is
ultimately determined by the distribution of porosity in the gel. The ultimate microstructure of the final
component will clearly be strongly influenced by changes imposed
upon the structural template during this phase of processing.

Afterwards, a thermal treatment, or firing process, is often

necessary in order to favor further polycondensation and enhance
mechanical properties and structural stability via final sintering,
densification, and grain growth. One of the distinct advantages of
using this methodology as opposed to the more traditional
processing techniques is that densification is often achieved at a
much lower temperature.
Schematic representation of the
The precursor sol can be either deposited on a substrate to form a different stages and routes of the
film (e.g., by dip-coating or spin coating), cast into a suitable sol–gel technology
container with the desired shape (e.g., to obtain monolithic
ceramics, glasses, fibers, membranes, aerogels), or used to
synthesize powders (e.g., microspheres, nanospheres).[1] The sol–gel approach is a cheap and low-
temperature technique that allows the fine control of the product's chemical composition. Even small
quantities of dopants, such as organic dyes and rare-earth elements, can be introduced in the sol and end up
uniformly dispersed in the final product. It can be used in ceramics processing and manufacturing as an
investment casting material, or as a means of producing very thin films of metal oxides for various
purposes. Sol–gel derived materials have diverse applications in optics, electronics, energy, space,
(bio)sensors, medicine (e.g., controlled drug release), reactive material, and separation (e.g.,
chromatography) technology.

The interest in sol–gel processing can be traced back in the mid-1800s with the observation that the
hydrolysis of tetraethyl orthosilicate (TEOS) under acidic conditions led to the formation of SiO2 in the
form of fibers and monoliths. Sol–gel research grew to be so important that in the 1990s more than 35,000
papers were published worldwide on the process.[2][3][4]

Particles and polymers

The sol–gel process is a wet-chemical technique used for the fabrication of both glassy and ceramic
materials. In this process, the sol (or solution) evolves gradually towards the formation of a gel-like network
containing both a liquid phase and a solid phase. Typical precursors are metal alkoxides and metal
chlorides, which undergo hydrolysis and polycondensation reactions to form a colloid. The basic structure
or morphology of the solid phase can range anywhere from discrete colloidal particles to continuous chain-
like polymer networks.[5][6]

The term colloid is used primarily to describe a broad range of solid-liquid (and/or liquid-liquid) mixtures,
all of which contain distinct solid (and/or liquid) particles which are dispersed to various degrees in a liquid
medium. The term is specific to the size of the individual particles, which are larger than atomic dimensions
but small enough to exhibit Brownian motion. If the particles are large enough, then their dynamic behavior
in any given period of time in suspension would be governed by forces of gravity and sedimentation. But if
they are small enough to be colloids, then their irregular motion in suspension can be attributed to the
collective bombardment of a myriad of thermally agitated molecules in the liquid suspending medium, as
described originally by Albert Einstein in his dissertation. Einstein concluded that this erratic behavior
could adequately be described using the theory of Brownian motion, with sedimentation being a possible
long-term result. This critical size range (or particle diameter) typically ranges from tens of angstroms
(10−10  m) to a few micrometres (10−6  m).[7]

Under certain chemical conditions (typically in base-catalyzed sols), the particles may grow
to sufficient size to become colloids, which are affected both by sedimentation and forces of
 gravity. Stabilized suspensions of such sub-micrometre spherical particles may eventually
result in their self-assembly—yielding highly ordered microstructures reminiscent of the
prototype colloidal crystal: precious opal.[8][9]
Under certain chemical conditions (typically in acid-catalyzed sols), the interparticle forces
have sufficient strength to cause considerable aggregation and/or flocculation prior to their
growth. The formation of a more open continuous network of low density polymers exhibits
certain advantages with regard to physical properties in the formation of high performance
glass and glass/ceramic components in 2 and 3 dimensions.[10]

In either case (discrete particles or continuous polymer network) the sol evolves then towards the formation
of an inorganic network containing a liquid phase (gel). Formation of a metal oxide involves connecting the
metal centers with oxo (M-O-M) or hydroxo (M-OH-M) bridges, therefore generating metal-oxo or metal-
hydroxo polymers in solution.

In both cases (discrete particles or continuous polymer network), the drying process serves to remove the
liquid phase from the gel, yielding a micro-porous amorphous glass or micro-crystalline ceramic.
Subsequent thermal treatment (firing) may be performed in order to favor further polycondensation and
enhance mechanical properties.

With the viscosity of a sol adjusted into a proper range, both optical quality glass fiber and refractory
ceramic fiber can be drawn which are used for fiber optic sensors and thermal insulation, respectively. In
addition, uniform ceramic powders of a wide range of chemical composition can be formed by
precipitation.

Polymerization
The Stöber process is a well-studied example of polymerization
of an alkoxide, specifically TEOS. The chemical formula for
TEOS is given by Si(OC2 H5 )4 , or Si(OR)4 , where the alkyl
group R = C2 H5 . Alkoxides are ideal chemical precursors for
sol–gel synthesis because they react readily with water. The
reaction is called hydrolysis, because a hydroxyl ion becomes
attached to the silicon atom as follows:

Si(OR)4 + H2O → HO−Si(OR)3 + R−OH

Depending on the amount of water and catalyst present,

hydrolysis may proceed to completion to silica: Simplified representation of the
condensation induced by hydrolysis of
Si(OR)4 + 2 H2O → SiO2 + 4 R−OH
TEOS.

Complete hydrolysis often requires an excess of water and/or the

use of a hydrolysis catalyst such as acetic acid or hydrochloric
acid. Intermediate species including [(OR)2 −Si−(OH)2 ] or [(OR)3 −Si−(OH)] may result as products of
partial hydrolysis reactions.[1] Early intermediates result from two partially hydrolyzed monomers linked
with a siloxane [Si−O−Si] bond:

(OR)3−Si−OH + HO−Si−(OR)3 → [(OR)3Si−O−Si(OR)3] + H−O−H

or

(OR)3−Si−OR + HO−Si−(OR)3 → [(OR)3Si−O−Si(OR)3] + R−OH

Thus, polymerization is associated with the formation of a 1-, 2-, or 3-dimensional network of siloxane
[Si−O−Si] bonds accompanied by the production of H−O−H and R−O−H species.

By definition, condensation liberates a small molecule, such as water or alcohol. This type of reaction can
continue to build larger and larger silicon-containing molecules by the process of polymerization. Thus, a
polymer is a huge molecule (or macromolecule) formed from hundreds or thousands of units called
monomers. The number of bonds that a monomer can form is called its functionality. Polymerization of
silicon alkoxide, for instance, can lead to complex branching of the polymer, because a fully hydrolyzed
monomer Si(OH)4 is tetrafunctional (can branch or bond in 4 different directions). Alternatively, under
certain conditions (e.g., low water concentration) fewer than 4 of the OR or OH groups (ligands) will be
capable of condensation, so relatively little branching will occur. The mechanisms of hydrolysis and
condensation, and the factors that bias the structure toward linear or branched structures are the most critical
issues of sol–gel science and technology. This reaction is favored in both basic and acidic conditions.

Sono-Ormosil
Sonication is an efficient tool for the synthesis of polymers. The cavitational shear forces, which stretch out
and break the chain in a non-random process, result in a lowering of the molecular weight and poly-
dispersity. Furthermore, multi-phase systems are very efficient dispersed and emulsified, so that very fine
mixtures are provided. This means that ultrasound increases the rate of polymerisation over conventional
stirring and results in higher molecular weights with lower polydispersities. Ormosils (organically modified
silicate) are obtained when silane is added to gel-derived silica during sol–gel process. The product is a
molecular-scale composite with improved mechanical properties. Sono-Ormosils are characterized by a
higher density than classic gels as well as an improved thermal stability. An explanation therefore might be
the increased degree of polymerization.[11]

Pechini process
For single cation systems like SiO2 and TiO2 , hydrolysis and condensation processes naturally give rise to
homogenous compositions. For systems involving multiple cations, such as strontium titanate, SrTiO3 and
other perovskite systems, the concept of steric immobilisation becomes relevant. To avoid the formation of
multiple phases of binary oxides as the result of differing hydrolysis and condensation rates, the entrapment
of cations in a polymer network is an effective approach, generally termed the Pechini Process.[12] In this
process, a chelating agent is used, most often citric acid, to surround aqueous cations and sterically entrap
them. Subsequently, a polymer network is formed to immobilize the chelated cations in a gel or resin. This
is most often achieved by poly-esterification using ethylene glycol. The resulting polymer is then
combusted under oxidising conditions to remove organic content and yield a product oxide with
homogeneously dispersed cations.[13]

Nanomaterials
In the processing of fine ceramics, the irregular particle sizes and shapes in a typical powder often lead to
polydisperse (non-uniform) packing morphologies that result in packing density variations in the powder
compact. Uncontrolled flocculation of powders due to attractive van der Waals forces can also give rise to
microstructural heterogeneities.[15][16]

Differential stresses that develop as a result of non-uniform drying shrinkage are directly related to the rate
at which the solvent can be removed, and thus highly dependent upon the distribution of porosity. Such
stresses have been associated with a plastic-to-brittle transition in consolidated bodies,[17] and can yield to
crack propagation in the unfired body if not relieved.

In addition, any fluctuations in packing density in the compact as it

is prepared for the kiln are often amplified during the sintering
process, yielding heterogeneous densification.
Some pores and
other structural defects associated with density variations have been
shown to play a detrimental role in the sintering process by
growing and thus limiting end-point densities. Differential stresses
arising from heterogeneous densification have also been shown to
result in the propagation of internal cracks, thus becoming the
strength-controlling flaws.[18][19][20][21][22]

It would therefore appear desirable to process a material in such a Nanostructure of a resorcinol-

way that it is physically uniform with regard to the distribution of formaldehyde gel reconstructed from
components and porosity, rather than using particle size small-angle X-ray scattering. This
distributions which will maximize the green density. The type of disordered morphology is
containment of a uniformly dispersed assembly of strongly typical of many sol–gel materials.[14]
interacting particles in suspension requires total control over
particle-particle interactions. Monodisperse colloids provide this
potential.[8][9][23]

Monodisperse powders of colloidal silica, for example, may therefore be stabilized sufficiently to ensure a
high degree of order in the colloidal crystal or polycrystalline colloidal solid which results from
aggregation. The degree of order appears to be limited by the time and space allowed for longer-range
correlations to be established. Such defective polycrystalline structures would appear to be the basic
elements of nanoscale materials science, and, therefore, provide the first step in developing a more rigorous
understanding of the mechanisms involved in microstructural evolution in inorganic systems such as
sintered ceramic nanomaterials.[24][25]

Applications
The applications for sol gel-derived products are numerous.[26][27][28][29][30][31] For example, scientists
have used it to produce the world's lightest materials and also some of its toughest ceramics.

Protective coatings

One of the largest application areas is thin films, which can be produced on a piece of substrate by spin
coating or dip-coating. Protective and decorative coatings, and electro-optic components can be applied to
glass, metal and other types of substrates with these methods. Cast into a mold, and with further drying and
heat-treatment, dense ceramic or glass articles with novel properties can be formed that cannot be created
by any other method. Other coating methods include spraying, electrophoresis, inkjet[32][33] printing, or roll
coating.

Thin films and fibers

With the viscosity of a sol adjusted into a proper range, both optical and refractory ceramic fibers can be
drawn which are used for fiber optic sensors and thermal insulation, respectively. Thus, many ceramic
materials, both glassy and crystalline, have found use in various forms from bulk solid-state components to
high surface area forms such as thin films, coatings and fibers.[10][34] Also, thin films have found their
application in the electronic field[35] and can be used as sensitive components of a resistive gas sensors.[36]
Nanoscale powders

Ultra-fine and uniform ceramic powders can be formed by precipitation. These powders of single and
multiple component compositions can be produced on a nanoscale particle size for dental and biomedical
applications. Composite powders have been patented for use as agrochemicals and herbicides. Powder
abrasives, used in a variety of finishing operations, are made using a sol–gel type process. One of the more
important applications of sol–gel processing is to carry out zeolite synthesis. Other elements (metals, metal
oxides) can be easily incorporated into the final product and the silicate sol formed by this method is very
stable.

Biomedical

Another application in research is to entrap biomolecules for sensory (biosensors) or catalytic purposes, by
physically or chemically preventing them from leaching out and, in the case of protein or chemically-linked
small molecules, by shielding them from the external environment yet allowing small molecules to be
monitored. The major disadvantages are that the change in local environment may alter the functionality of
the protein or small molecule entrapped and that the synthesis step may damage the protein. To circumvent
this, various strategies have been explored, such as monomers with protein friendly leaving groups (e.g.
glycerol) and the inclusion of polymers which stabilize protein (e.g. PEG).[37]

Other products fabricated with this process include various ceramic membranes for microfiltration,
ultrafiltration, nanofiltration, pervaporation, and reverse osmosis. If the liquid in a wet gel is removed under
a supercritical condition, a highly porous and extremely low density material called aerogel is obtained.
Drying the gel by means of low temperature treatments (25-100 °C), it is possible to obtain porous solid
matrices called xerogels. In addition, a sol–gel process was developed in the 1950s for the production of
radioactive powders of UO2 and ThO2 for nuclear fuels, without generation of large quantities of dust.

Opto-mechanical

Macroscopic optical elements and active optical components as well as large area hot mirrors, cold mirrors,
lenses, and beam splitters all with optimal geometry can be made quickly and at low cost via the sol–gel
route. In the processing of high performance ceramic nanomaterials with superior opto-mechanical
properties under adverse conditions, the size of the crystalline grains is determined largely by the size of the
crystalline particles present in the raw material during the synthesis or formation of the object. Thus a
reduction of the original particle size well below the wavelength of visible light (~500 nm) eliminates much
of the light scattering, resulting in a translucent or even transparent material.

Furthermore, results indicate that microscopic pores in sintered ceramic nanomaterials, mainly trapped at the
junctions of microcrystalline grains, cause light to scatter and prevented true transparency. it has been
observed that the total volume fraction of these nanoscale pores (both intergranular and intragranular
porosity) must be less than 1% for high-quality optical transmission, i.e. the density has to be 99.99% of the
theoretical crystalline density.[38][39]

Medicine

Unique properties of the sol–gel provide the possibility of their use for a variety of medical
applications.[40][41][42] A sol–gel processed alumina can be used as a carrier for the sustained delivery of
drugs and as an established wound healer. A marked decrease in scar size was observed (http://irc.ifmo.ru/e
n/88677/isu_viewnews/972/First_biocomposite_for_wound_healing_and_scar-size_decreasing_based_on_
sol%E2%80%93gel_alumina.htm) because of the wound healing composite including sol–gel processed
alumina. A novel approach (http://irc.ifmo.ru/en/88677/isu_viewnews/1075/New_generation_of_trombolyt
ic_drugs.htm) to thrombolysis treatment is possible by developing a new family of injectable composites:
plasminogen activator entrapped within alumina.

See also
Coacervate, small spheroidal droplet of colloidal particles in suspension
Freeze-casting
Freeze gelation
Mechanics of gelation
Random graph theory of gelation
Liquid–liquid extraction

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Further reading
Colloidal Dispersions, Russel, W. B., et al., Eds., Cambridge University Press (1989)
Glasses and the Vitreous State, Zarzycki. J., Cambridge University Press, 1991
The Sol to Gel Transition. Plinio Innocenzi. Springer Briefs in Materials. Springer. 2016.

External links
International Sol–Gel Society (http://www.isgs.org/)
The Sol–Gel Gateway (http://www.solgel.com/)

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