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Synthesis and Application of Nano-Sized SiO2 to Textiles: a Review

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 Research: Nano-Sized Silica

Synthesis and Application of Nano-

Sized SiO2 to Textiles: a Review
By B.H. Patel and P.N. Patel, Department of Textile Chemistry, The Maharaja
Sayajirao University of Baroda, Gujarat, India
1. Introduction Abstract
The chemical compound silicon dioxide, also Silica remains the most important component for the development of glass for windows,
known as silica (from the Latin silex), is an drinking glasses, beverage bottles and home-care products. In this article we have reported
oxide of silicon with the chemical formula methods of synthesis of nano-sized silica and their application to textiles for achieving
SiO2. It has been known for its hardness since multi-functional fabric properties.
antiquity. Silica is most commonly found in
nature as sand or quartz, as well as in the cell Keywords: Nano Silica, Synthesis, Hydrophobic, Filler, Fire retardant
walls of diatoms. Silica is manufactured in
several forms, including fused quartz, crystal, ‡3ODVPDHQKDQFHGFKHPLFDOYDSRXU (eg. sodium oxide, potassium oxide, lead(II)
fumed silica, colloidal silica, silica gel, and deposition using TEOS at about 400°C oxide, zinc oxide, or mixtures of oxides form-
aerogel. Si (OC2H5)4 + 12 O2 → SiO2 + 10 H2O ing silicates and glasses as the Si-O-Si bonds
+ 8 CO2 in silica are broken successively. As an exam-
2. Chemistry ple, the reaction of sodium oxide and SiO2 can
Silica is the common name for materials ‡3RO\PHUL]DWLRQRIWHWUDHWK\ORUWKRVLOLFDWH produce sodium orthosilicate, sodium silicate
composed of silicon dioxide (SiO2) and occurs (TEOS) at below 100°C using amino acid and glasses, dependent on the proportions of
in crystalline and amorphous forms. Crystal- as catalyst. Pyrogenic silica (sometimes reactants:6
line silica exists in multiple forms. Quartz and, called fumed silica or silica fume), which
more specifically a-quartz, is a widespread is a very fine particulate form of silicon 2 Na2O + SiO2 → Na4SiO4
and well-known material. Upon heating, a- dioxide, is prepared by burning SiCl4 in an
quartz is transformed into b-quartz, trydimite oxygen rich hydrocarbon flame to Na2O + SiO2 → Na2SiO3
and cristobalite. Porosil is the family name for produce a “smoke” of SiO2:
porous crystalline silica. Quartz exists in natu- SiCl4 + 2 H2 + O2 → SiO2 + 4 HCl (0.25–0.8) Na2O + SiO2 → glass
ral and synthetic forms, whereas all porosils
are synthetic. Amorphous silica, silica gel, is produced by Examples of such glasses have commercial
Amorphous silica can be divided into natu- the acidification of solutions of sodium silicate significance, eg. soda lime glass, borosilicate
ral specimens (eg. diatomaceous earth, opal to produce a gelatinous precipitate that is glass and lead glass. In these glasses, silica is
and silica glass) and human-made products.1,2 then washed and then dehydrated to produce termed the network former or lattice former.
Silicon dioxide is formed when silicon is colourless, microporous silica. Quartz exhibits With silicon at high temperatures, gaseous
exposed to oxygen (or air). A very shallow a maximum solubility in water at temperatures SiO is produced.
layer (approximately 1 nm or 10 Å) of so- about 340°C. This property is used to grow
called native oxide is formed on the surface single crystals of quartz in a hydrothermal SiO2 + Si → 2 SiO (gas)
when silicon is exposed to air under ambient process where natural quartz is dissolved in
conditions. Higher temperatures and alterna- superheated water in a pressure vessel which 3. Methods for Synthesis of
tive environments are used to grow well-con- LVFRROHUDWWKHWRS&U\VWDOVRI²NJFDQ Nano-Sized SiO2
trolled layers of silicon dioxide on silicon, for EHJURZQRYHUDSHULRGRI²PRQWKV7KHVH
example at temperatures between 600° and crystals are a source of very pure quartz There are several methods for creating
1200°C, using so-called dry or wet oxidation for use in electronic applications. Fluorine nanoparticles, including both attrition and
with O2 or H2O, respectively. The depth of reacts with silicon dioxide to form SiF4 and O2 pyrolysis. In attrition, macro- or micro-scale
the layer of silicon replaced by the dioxide is whereas the other halogen gases (Cl2, Br2, I2) particles are ground in a ball mill, a planetary
44% of the depth of the silicon dioxide layer react much less readily.6 ball mill, or other size-reducing mechanism. In
produced.3 pyrolysis, vaporous precursor (liquid or gas)
Silicon dioxide is attacked by hydrofluoric is forced through an orifice at high pressure
Alternative methods used to deposit a layer acid (HF) to produce hexafluorosilicic acid: and burned. The resulting solid is air classified
of SiO2 include:4 to recover oxide particles from by-product
SiO2 + 6 HF → H2SiF6 + 2 H2O
gases.8
‡/RZWHPSHUDWXUHR[LGDWLRQ²ƒ& HF is used to remove or pattern silicon Initial development of new crystalline materi-
of silane dioxide in the semiconductor industry. als was based on nanoparticles generated by
SiH4 + 2 O2 → SiO2 + 2 H2O Silicon dioxide dissolves in hot concentrated evaporation and condensation (nucleation and
alkali or fused hydroxide: growth) in a sub-atmospheric inert-gas envi-
‡'HFRPSRVLWLRQRIWHWUDHWK\O ronment (Gleiter 1989; Siegel 1991, 1994).9,10
SiO2 + 2 NaOH → Na2SiO3 + H2O
RUWKRVLOLFDWH7(26DW²ƒ& Various aerosol processing techniques have
Si(OC2H5)4 → SiO2 + 2 H2O + 4 C2H4 Silicon dioxide reacts with basic metal oxides been reported to improve the production yield

MAY 2012 35
Research: Nano-Sized Silica

of nanoparticles (Uyeda 1991, Friedlander nanoparticles by gelation, precipitation and of nano silica have been reported. F. Teng
1998).11,12 These include synthesis by com- hydrothermal treatment (Kung and Ko 1996).28 HWDOREWDLQHGPRQRGLVSHUVHG&G6²6L22.
bustion flame (Zachariah 1994, Calcote and Size distribution of semiconductor, metal and Core-shell particles ranging from nanometres
.HLO$[HOEDXP3UDWVLQLV13 metal-oxide nanoparticles can be manipulated ²QPWRPLFURPHWUHV²—PZHUH
SODVPD5DRHWDO14 laser ablation by either dopant introduction (Kyprianidou- prepared in situ in the nonionic reverse micro-
%HFNHUHWDO chemical vapour con- Leodidou et al. 1994)29 or heat treatment emulsions.32 L.M Lee et al have reported that
GHQVDWLRQ.HDUHWDO16 spray pyrolysis :DQJHWDO30 Better size and stability the micrometre-sized hollow silica particles
(Messing et al. 1994); electrospray (de la control of quantum-confined semiconductor ZHUHV\QWKHVLVHGE\VRO²JHOUHDFWLRQLQZDWHU
Mora et al. 1994);18 and plasma spray (Berndt nanoparticles can be achieved through the use in-oil (W/O) emulsion, as the viscosity of water
HWDO19 RILQYHUWHGPLFHOOHV*DFRLQ)RUVROJHO droplets in W/O emulsion was controlled with
Additional silica-nanoparticle synthesis processing, the development of continu- polyethylene glycol (PEG) or polyvinyl pyr-
techniques include sonochemical process- ous processing techniques based on present rolidone (PVP).33
ing, cavitation processing, microemulsion knowledge of batch processing has yet to be Xinqi Chen and Rodney S. Ruoff prepared
processing and high-energy ball milling. In addressed for economical scale-up production the SiOx nanowire and nanocoils by the
sonochemistry, an acoustic cavitation process of nanoparticles. Other related sol-gel issues simple catalyst-free thermal chemical vapour
nanoparticle was formed at extremely high concern the cost of precursors and the recy- deposition method. Where the nanowire and
temperature gradient and pressure (Suslick et cling of solvent. Overall, sol-gel processing is nanocoils were synthesised ranged from 20nm
al. 1996)20 The technique can be used to pro- attractive for commercial scale-up production. WRQPDQGOHQJWKXSWR—PDWƒ&WR
duce a large volume of material for industrial 1200°C temperature.34 J.Y. Lao and J.G. Wen
applications. In hydrodynamic cavitation, silica 3.1 Chemical Method reported that amorphous SiOx nanotubes in
nanoparticles are generated through creation The sol-gel process is a wet-chemical WKHUDQJHQPWRQPZHUHV\QWKHVLVHG
and release of gas bubbles inside the sol-gel technique (also known as chemical solution by the thermal evaporation method in pres-
solution (Sunstrom et al. 1996).21 deposition) widely used recently in the fields ence of germanium dioxide.
The microemulsions approach has been used of materials science and ceramic engineering. N. Venkatathri prepared silica nanoparti-
IRUV\QWKHVLVRIPHWDOOLF.LVKLGDHWDO22 Such methods are used primarily for the fab- cles with sizes ranging from 100-400nm by
semiconductor (Kortan et al. 1990; Pileni et al. rication of materials (typically a metal oxide), hydrolysis of tetraethyl ortho silicate in ethyl
1992),23,24 silica (Arriagada and Osseo-Assave starting from a chemical solution (sol, short alcohol.36 Deepika et al reported that when
 magnetic and superconductor (Pillai for solution) which acts as the precursor for an silica-gold core-shell (SiO2@Au) nanoparticles
HWDO26 nanoparticles. The technique is integrated network (or gel) of either discrete were created by the Citrate method, Borohy-
useful for large-scale production of nanopar- particles or network polymers. dride method, and a combination Citrate and
ticles using relatively simple and inexpensive Typical precursors are metal alkoxides and Borohydride methods, the size of the core
KDUGZDUH+LJJLQV Finally, high-energy metal chlorides, which undergo hydrolysis and (SiO2) nanoparticle was founded to be ~260
ball milling is the only top-down approach for polycondensation reactions to form either a nm and the size of shell (Au) nanoparticle was
silica nanoparticle synthesis. The technique, network ‘elastic solid’ or a colloidal suspen- ~20 nm. P. K. Jal, et al prepared silica na-
which is already a commercial technology, has VLRQRUGLVSHUVLRQ²DV\VWHPFRPSRVHGRI noparticles by the precipitation method within
been considered dirty because of contamina- discrete (often amorphous) submicrometre WKHaQPUDQJHZKHUHWKHVRGLXPVLOLFDWH
tion problems from ball-milling processes. particles dispersed to various degrees in a or silicon alkoxide or halide gets converted
Major efforts in nanoparticle synthesis can host fluid. Formation of a metal oxide involves to a polymeric network of gel form.38 De et
be grouped into two broad areas: gas-phase connecting the metal centres with oxo (M-O- al patented a method of silica synthesis by
synthesis and sol-gel processing. Among all M) or hydroxo (M-OH-M) bridges, therefore precipitation, where, to acidified water (pH is
the synthesis techniques discussed above, generating metal-oxo or metal-hydroxo poly- ²DONDOLPHWDOVLOLFDWHVROXWLRQDQG+2SO4
gas-phase synthesis is one of the best tech- mers in solution. Thus, a gel-like diphasic sys- were added simultaneously.39
niques with respect to size monodispersity, tem is formed containing both a liquid phase /HHHWDOUHSRUWHGWKHDQDHUR²VRO²JHO
typically achieved by using a combination of and a solid phase. In the case of the colloid, a technique for production of silica powders
rigorous control of nucleation-condensation significant amount of fluid may need to be re- with high specific areas (>400m2 gï) by a
growth and avoidance of coagulation by diffu- moved initially for the gel-like properties to be nonpyrolytic aerosol process.40 Concentrated
sion and turbulence as well as by the effective recognised. Centrifugation and sedimentation ammonia solution in ethanol and water was
collection of nanoparticles and their handling processes are used for phase separation. Re- also used for the hydrolysis and condensation
afterwards. Alternatively, inert silica encapsula- moval of the remaining liquid (solvent) phase of tetraethoxy silane to prepare monodis-
tion of nanoparticles by gas-phase reaction requires a drying process and, afterwards, a persed silica with low surface area by using the
and by oxidation in colloidal solution has been thermal treatment, or firing process, is often SFB method.41
shown to be effective for metallic nanoparti- necessary in order to favour further polycon- Many methods have also been reported for
cles (Andres et al. 1998). However, gas-phase densation and enhance mechanical proper- the preparation of pure nano-silica particles
synthesis is generally a low-production-rate ties and structural stability via final sintering, by the sol-gel technique. A simple technique
process (typically in the 100 milligrams per densification and grain growth.31 reported for the preparation of porous silica
hour range).13 is the selective leaching of clay minerals with
Sol-gel processing is a wet chemical-synthesis 3.2 Other Methods acid.42 Janet et al43 prepared porous silica gels
approach that can be used to generate Recently many methods for the preparation with high surface area from tetraethylotho-

36 INTERNATIONAL DYER
silicate and polyacrylic acid of high molecular methods, mainly owing to facility, versatil- properties in fabric.
weight in acidic media by a sol-gel method. ity, purity, homogeneity and modifications
Ikeue et al44 presented the synthesis of self- of material properties by changing synthesis 4.1 Application to Textiles
standing porous silica thin films with different parameters. The mean pore size, the intercon-
pore structures by a solvent evaporation meth- nectivity and the pore-size distributions can 4.1.1 Super Hydrophobic - Biomi-
od. Jian-Feng et al reported a novel method be controlled by changing the molar ratio of metic - Self Cleaning - Lotus Effect
for the synthesis of porous hollow silica nano water/precursor, type of catalyst or precursor, The hydrophobicity of a surface is determined
particles (PHSNP) by employing nanosized temperatures of gelation, drying, and stabilisa- by the contact angle. The higher the contact
calcium carbonate as a template. The PHSNP tion. Moreover, the sol-gel technique is inex- angle, the higher the hydrophobicity of a
had a uniform, spherical hollow structure with pensive and the silica nanoparticles produced surface. Surfaces with a contact angle < 90°
DGLDPHWHURI²QPDQGZDOOWKLFNQHVVRI are non-toxic materials. are referred to as hydrophilic and those with
approximately10nm, as well as a surface area an angle >90° as hydrophobic. Some plants
RIP2/g. 4. Application of Nano-Sized show contact angles up to 160° and are called
Bogush and Zukoski46 obtained monodis- SiO2 VXSHUK\GURSKRELFPHDQLQJWKDWRQO\²
persed silica particles having sizes rang- of a water drop’s surface is in contact. Plants
ing from 40nm to several micrometres by Silica is used primarily in the production of with a double-structured surface like the lotus
controlled hydrolysis of tetraethylortho-silicate glass for windows, drinking glasses, beverage FDQUHDFKDFRQWDFWDQJOHRIƒZKHUHDV
(TEOS) in ethanol, followed by condensa- bottles, and many other uses. The majority of a droplet’s actual contact area is only 0.6%.
tion (polymerisation) of the dispersed phase optical fibres for telecommunications are also All this leads to a self-cleaning effect. Dirt
material. Also, the Sung Kyoo Park prepared made from silica. It is a primary raw material particles with an extremely reduced contact
silica nanoparticles from tetraethylortho- for many white-ware ceramics such as earth- area are picked up by water droplets and are
silicate (TEOS) dissolved in ethanol by using enware, stoneware and porcelain, as well as thus easily cleaned off the surface. If a water
a semi-batch process in order to control the industrial Portland cement. Silica is a common droplet rolls across such a contaminated
particle properties. Ryu48 had also prepared additive in the production of foods, where it surface the adhesion between the dirt particle,
amorphous silica by oxidation of silicon. Janet is used primarily as a flow agent in powdered irrespective of its chemistry, and the droplet
et al49 had produced porous silica gels with foods, or to absorb water in hygroscopic is higher than between the particle and the
high surface areas from tetraethylothosilicate applications. It is the primary component of surface. As this self-cleaning effect is based on
and polyacrylic acid of high molecular weight diatomaceous earth, which has many uses, the high surface tension of water, it does not
LQDFLGLFPHGLDE\WKHVRO²JHOPHWKRG3RURXV ranging from filtration to insect control. It is work with organic solvents.
silica glass was prepared through sol-gel also the primary component of rice-husk ash, Some nanotechnologists have developed
processing using tetramethylorthosilicate which is used, for example, in filtration and treatments, coatings, paints, roof tiles, fabrics
(TMOS) as a precursor, with HNO3 and HF as cement manufacturing. and other surfaces that can stay dry and clean
catalysts. Thin films of silica grown on silicon wafers themselves in the same way as the lotus leaf.
Brinker et al had prepared a nanosol by hy- via thermal oxidation methods can be quite This can usually be achieved using special
drolysis of the precursor material. The precur- beneficial in microelectronics, because of its fluorochemical or silicone treatments on struc-
sors were either inorganic metal salts or metal high chemical stability. In electrical applica- tured surfaces or with compositions contain-
organic compounds such as metal alkoxides or tions, it can protect the silicon, store charge, ing micro-scale particulates. Water droplets
acetylacetonate. These hydroxides are mostly block current, and even act as a controlled on taro leaf with lotus effect (upper), and taro
unstable in higher concentrations and there- pathway to limit current flow. A silica-based OHDIVXUIDFHPDJQLILHG²LVRQHPLOOLPHWUH
fore tend to undergo subsequent condensa- aerogel was used in the Stardust spacecraft to span) showing a number of small protrusions
tion reactions. The condensation reactions collect extraterrestrial particles. Silica is also (lower).
lead to the formation of particles with sizes used in the extraction of DNA and RNA, due to
in the nanometre range. Hydrolysis can be its ability to bind to the nucleic acids under the Easy Care Finish
carried out under acidic as well as alkaline presence of chaotropes.
conditions. As hydrophobic silica, it is used as a Hydrophobic surface can be produced mainly
Hua Zou et al have reported that nanosilica defoamer component. In hydrated form, in two ways:
powder is mainly produced by the fuming it is used in toothpaste as a hard abrasive ‡%\FUHDWLQJDURXJKVWUXFWXUHRQD
method and the precipitation method in to remove tooth plaque. In its capacity as hydro phobic surface
industry. Fumed silica is a fine, white, odour- a refractory, it is useful in fibre form as a ‡%\PRGLI\LQJDURXJKVXUIDFHXVLQJPDWHULDO
less and tasteless amorphous powder. It is high-temperature thermal-protection fabric. with low surface free energy.
manufactured by a high-temperature vapour In cosmetics, it is useful for its light-diffusing Both these approaches have been used to give
process in which SiCl4 is hydrolysed in a flame properties and natural absorbency. Colloidal a hydrophobic finish to textile substrates.
of oxygen-hydrogen according to the reac- silica is used as a wine- and juice-fining agent. Fluorocarbon finishes constitute an important
tion: In pharmaceutical products, silica aids powder class of hydrophobic finishes. Fluorocarbons
flow when tablets are formed. Finally, it is used are a class of organic chemicals that contain a
SiCl4+2H2+O2 → iO2+4HCl as a thermal-enhancement compound in the perfluoroalkyl residue in which all the
The sol-gel technique presents many process- ground-source heat-pump industry. Finally it hydrogen atoms have been replaced by fluo-
ing merits for several material-production is used in textiles to achieve multi-functional rine, resulting in very high thermal stability and

MAY 2012 37
Research: Nano-Sized Silica

low reactivity. These chemicals considerably which creates a protective layer that impedes the glass-transition behaviour of the polymer
reduce the surface tension. The critical surface oxygen penetration and creates an insulating matrix is controversial, since Tg of polymer
WHQVLRQëFRI²&)LV1P layer between the heat and the fuel. Phospho- nanocomposites varies for a variety of
Fluorocarbon finishes are dispersions of per rus compound is one of the best materials for reasons, such as filler size, filler loading and
fluorinated acrylates, having comonomers. forming char. The flame-retardant characteris- dispersion conditions.
Durable fluorocarbon finishes have reactive tics of epoxy resins have been demonstrated
methanol or epoxy groups that may react to to improve with nanoscale phosphorus-con-
form a cross-linked network that may also be- taining epoxy/silica hybrids, obtained via the &RQFOXVLRQV
come covalently bonded to the surface of the sol-gel process. The synthesis of materials whose properties
fibres. These finishes form low-energy films can be controlled and altered at the atomic
that protect the fibres in the treated fabrics. Thermal Protective Finish level is a challenging task. Thus, nano-sized
SiO2 particles have a great future because of
Flame Retardant Finish Thermal properties are the properties of their ability to form ideal links between
materials that change with temperature. They molecular and solid-state chemistry. It has
A fire retardant is used to make materials are studied by thermal analysis techniques, been found that silicon-carbon bonds are
harder to ignite by slowing decomposition and which include DSC, TGA, DTA, dielectric stable. Silicon-containing moieties can be
increasing the ignition temperature. It func- thermal analysis, etc. Generally, the incorpora- included in a number of sites in organic
tions by a variety of methods, such as absorb- tion of nanometre-sized inorganic particles molecules and can start the formation of
ing energy away from the fire or preventing into the polymer matrix can enhance thermal varied polymers. It can further lead to the
oxygen from reaching the fuel. stability by acting as a superior insulator and formation of solid materials such as silicides,
Polymer nanocomposites for flame-retardant mass transport barrier to the volatile products oxides, and thermomechanical ceramics.
applications are attractive, and the nanoscale generated during decomposition. Its potential was explored recently in order to
silica particle is a new type of nanoparticle for Meanwhile, the incorporation of nanometre- use organo-silicon compounds as potential
flame-retardant nanocomposites. The flam- sized inorganic particles such as silica is very metal organic precursors. The incorporation
mability behaviour of a polymer is defined on effective in decreasing the CTE of the polymer of nanometre-sized inorganic silica particles
the basis of several processes or parameters, matrix. Studies on the effect of silica filler ad- has been used to give a hydrophobic finish to
such as burning rates, spread rates, ignition dition on polymer glass-transition temperature textile substrates and also to enhance thermal
characteristics, etc. An important characteristic show a wide variety of behaviours. The effect stability as well as impart a flame-retardant
of the fire retardant is the formation of char, of the nano fillers in polymer composites on finish to the textiles. ID

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'RURWD1DSLHUVNDHWDO¶7KHQDQRVLOLFDKD]DUGDQRWKHUYDULDEOHHQWLW\3DUWLFOHDQG)LEUH·7R[LFRORJ\
6XQJJ\X/HH¶(QF\FORSHGLDRIFKHPLFDOSURFHVVLQJ·&5&3UHVV,6%1
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3LOODL93.XPDU0-+RX3$\\XEDQG'26KDK¶3UHSDUDWLRQRIQDQRSDUWLFOHVRIVLOYHUKDOLGHVVXSHUFRQGXFWRUVDQGPDJ-
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