Organic‐acid‐catalyzed sol–gel route for preparing poly(methyl methacrylate)–silica hybrid materials

In this study, a series of organic–inorganic hybrid sol–gel materials consisting of a poly(methyl methacrylate) (PMMA) matrix and dispersed silica (SiO₂) particles were successfully prepared through an organic‐acid‐catalyzed sol–gel route with N‐methyl‐2‐pyrrolidone as the mixing solvent. The as‐synthesized PMMA–SiO₂ nanocomposites were subsequently characterized with Fourier transform infrared spectroscopy and transmission electron microscopy. The solid phase of organic camphor sulfonic acid was employed to catalyze the hydrolysis and condensation (i.e., sol–gel reactions) of tetraethyl orthosilicate in the PMMA matrix. The formation of the hybrid membranes was beneficial for the physical properties at low SiO₂ loadings, especially for enhanced mechanical strength and gas barrier properties, in comparison with the neat PMMA. The effects of material composition on the thermal stability, thermal conductivity, mechanical strength, molecular permeability, optical clarity, and surface morphology of the as‐prepared hybrid PMMA–SiO₂ nanocomposites in the form of membranes were investigated with thermogravimetric analysis, differential scanning calorimetry, dynamic mechanical analysis, gas permeability analysis, ultraviolet–visible transmission spectroscopy, and atomic force microscopy, respectively. © 2008 Wiley Periodicals, Inc. J Appl Polym Sci, 2008     

Electrochemical investigations on the corrosion protection effect of poly(vinyl carbazole)‐silica hybrid sol–gel materials

A series of sol–gel derived organic–inorganic hybrid coatings consisting of organic poly (vinyl carbazole) (PVK) and inorganic silica (SiO₂), with 3‐(trimethoxysilyl)propyl methacrylate (MSMA) as coupling agent, were successfully synthesized. First of all, vinyl carbazole (VCz) monomers are copolymerized with MSMA by performing free‐radical polymerization reactions with AIBN as initiator. Subsequently, as‐prepared copolymer (i.e., sol–gel precursor) was further reacted with various feeding content of tetraethyl orthosilicate (TEOS) through organic acid (CSA)‐catalyzed sol–gel reaction to form a series of PVK‐silica hybrid (PSH) sol–gel materials. The as‐synthesized hybrid materials were subsequently characterized by Fourier‐Transformation infrared (FTIR) spectroscopy and solid‐state ²⁹Si NMR. It should be noted that the PVK‐SiO₂ hybrid (PSH) coating on cold‐rolled steel (CRS) electrode with low silica loading (e.g., 10 phr) was found to be superior in anticorrosion property over those of neat PVK based on a series of electrochemical measurements such as corrosion potential, polarization resistance, corrosion current, and electrochemical impedance spectroscopy in 3.5 wt% NaCl electrolyte. The better anticorrosion performance of PSH coatings as compared to that of neat polymer may probably be attributed to the stronger adhesion strength of PSH coatings on CRS electrode, which was further evidenced by Scotch tape test evaluation. Increase of adhesion strength of PSH coatings on CRS electrode may be associated with the formation of Fe–O–Si covalent bonds at the interface of PSH coating and CRS electrode based on the FTIR–RAS (reflection absorption spectroscopy) studies. POLYM. COMPOS., 2012. © 2011 Society of Plastics Engineers     

Ethylene–propylene copolymer/ordered polysilsesquioxane nanocomposites prepared via organic acid‐ or base‐catalyzed binary silica water‐crosslinking reactions

In situ silica sol–gel‐derived organic–inorganic hybrid materials, which comprise a vinyltrimethoxysilane‐grafted ethylene–propylene copolymer (EPR‐g‐VTMS) and n‐hexyltrimethoxysilane (HTMS), were successfully prepared in the presence of an organic acid and base catalyst. Benzenesulfonic acid and aniline were selected as the organic acid and base catalyst, respectively, to examine the progress and effect of progressive changes in the silane water‐crosslinking reaction of EPR‐g‐VTMS/HTMS composites. The water‐crosslinked EPR‐g‐VTMS/HTMS composites were characterized by means of attenuated total reflectance Fourier transform infrared spectroscopy, gel content, solid‐state ²⁹Si cross‐polarization/magic‐angle spinning NMR, wide‐angle X‐ray scattering, tensile strength and field‐emission scanning electron microscopy measurements. These results revealed that the type of catalyst has a substantial influence on the nature of siloxane bonds and eventually the physical tensile properties of the water‐crosslinked EPR‐g‐VTMS/HTMS composites, which can be explained mainly from knowledge of the traditional acid‐ and base‐catalyzed silica sol–gel reaction. Moreover, an in‐depth analysis of the aniline‐catalyzed composites indicated the formation of ladder‐type poly(n‐hexylsilsesquioxane)s and the presence of a highly ordered structure with a thickness equal to the length of two n‐hexyl groups in all‐trans conformation. We demonstrate potential for the future design of highly ordered silicate‐based organic–inorganic hybrid nanocomposites. Copyright © 2009 Society of Chemical Industry     

Preparation and anticorrosive properties of hybrid coatings based on epoxy‐silica hybrid materials

A series of sol‐gel derived organic–inorganic hybrid coatings consisting of organic epoxy resin and inorganic silica were successfully synthesized through sol‐gel approach by using 3‐glycidoxypropyl‐trimethoxysilane as coupling agent. Transparent organic–inorganic hybrid sol‐gel coatings with different contents of silica were always achieved. The hybrid sol‐gel coatings with low silica loading on cold‐rolled steel coupons were found much superior improvement in anticorrosion efficiently. The as‐synthesized hybrid sol‐gel materials were characterized by Fourier‐transformation infrared spectroscopy, ²⁹Si‐nuclear magnetic resonance spectroscopy and transmission electron microscopy. Effects of the material composition of epoxy resins along with hybrid materials on the thermal stability, Viscoelasticity properties and surface morphology were also studied, respectively. © 2009 Wiley Periodicals, Inc. J Appl Polym Sci, 2009     

Effect of baking treatment and materials composition on the properties of bulky PMMA–silica hybrid sol–gel materials with low volume shrinkage

A series of bulky PMMA–silica hybrid sol–gel materials had been successfully prepared through the conventional HCl‐catalyzed sol–gel approach with 2‐hydroxyethyl methyl methacrylate (HEMA) as coupling agent under pumping pretreatment (i.e., exhaustive vacuum evacuation). In this work, the hydroxyl groups of HEMA monomers were first cohydrolyzed with various contents of tetraethyl orthosilicate (TEOS) to afford chemical bonding for the forming silica networks by removal of solvent and byproduct of sol–gel reactions through pumping pretreatment before gelation reactions. Subsequently, the resultant viscous solution was then copolymerized with methyl methacrylate (MMA) monomers at specific feeding ratios by using benzoyl peroxide (BPO) as free‐radical initiator. Eventually, transparent bulky organic–inorganic hybrid sol–gel materials loaded with different silica content were always achieved. The obtained bulky hybrid sol–gel materials were found to be transparent, crack‐free, and of relatively low volume shrinkages even in high silica content. The as‐prepared bulky hybrid sol–gel materials were then characterized through silicon element mapping studies of energy‐dispersive X‐ray (EDX) and transmission electron microscopy (TEM). Effect of heating process at 150°C for 5 h after polymerization and material composition on the thermal properties, mechanical strength, and optical clarity of a series of bulky PMMA–silica hybrid sol–gel materials was investigated and compared by thermogravimetric analysis (TGA), thermomechanical analysis (TMA), hardness test, dynamic mechanical analysis (DMA), and UV–vis transmission spectroscopy, respectively. © 2006 Wiley Periodicals, Inc. J Appl Polym Sci 101: 1151–1159, 2006     

Polyamide–silica nanocomposites: mechanical,morphological and thermomechanical investigations

BACKGROUND: The physical properties of polyamides can be enhanced through incorporation of inorganic micro‐ and nanofillers such as silica nanoparticles. Transparent sol‐gel‐derived organic‐inorganic nanocomposites were successfully prepared by in situ incorporation of a silica network into poly(trimethylhexamethylene terephthalamide) using diethylamine as catalyst. Thin films containing various proportions of inorganic network obtained by evaporating the solvent were characterized using mechanical, dynamic mechanical thermal and morphological analyses. RESULTS: Tensile measurements indicate that modulus as well as stress at yield and at break point improved while elongation at break and toughness decreased for the hybrid materials. The maximum value of stress at yield point (72 MPa) was observed with 10 wt% silica while the maximum stress at break point increased up to 66 MPa with 20 wt% silica relative to that of pure polyamide (44 MPa). Tensile modulus was found to increase up to 2.59 GPa with 10 wt% silica in the matrix. The glass transition temperature and the storage moduli increased with increasing silica content. The maximum increase in the T_g value (144 °C) was observed with 20 wt% silica. Scanning electron microscopy investigation gave the distribution of silica, with an average particle size ranging from 3 to 24 nm. CONCLUSION: These results demonstrate that nanocomposites with high mechanical strength can be prepared through a sol‐gel process. The increase in the T_g values suggests better cohesion between the two phases, and the morphological results describe a uniform dispersion of silica particles in the polymer matrix at the nanoscale. Copyright © 2007 Society of Chemical Industry     

SiO2 reinforced HDPE hybrid materials obtained by the sol–gel method

Novel high density polyethylene (HDPE)/SiO₂ hybrid materials were prepared by the sol–gel process using tetraethoxysilane (TEOS). HDPE and synthesized HDPE‐g‐vinyl trimethoxysilane (VTMS) through melt grafting method was used as the raw material. The structure and thermal, mechanical properties of hybrid materials were investigated by Fourier transform infrared (FTIR) spectroscopy, X‐ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM), simultaneous thermogravimetric (TG), differential thermal analysis (DTA), and tensile tests, respectively. Silica phase in the HDPE‐g‐VTMS hybrids showed a network structure and nano‐scale size. The covalent bonds between organic and inorganic phases were introduced by the HDPE‐g‐VTMS bearing trimethoxysilyl groups, which underwent hydrolytic polycondensation with TEOS. The thermal stability and mechanical properties of HDPE‐g‐VTMS hybrids were obviously improved by embedded silica networks. It was found that the silica content in the HDPE‐g‐VTMS hybrid material was linearly increased with the TEOS dosage. The formation of the HDPE‐g‐VTMS hybrid was beneficial for enhanced mechanical strength and thermal stability, in comparison with the neat HDPE. © 2013 Wiley Periodicals, Inc. J. Appl. Polym. Sci., 2014 , 131, 39891.     

New epoxy/silica‐titania hybrid materials prepared by the sol–gel process

A new type of inorganic‐polymer hybrid materials of epoxy/silica‐titania had been prepared by incorporating grafted epoxy, which had been synthesized by epoxy and tetraethoxysilane (TEOS), with highly reactive TEOS and tetrabutyltitanate (TBT) by using the in situ sol–gel process. The grafted epoxy was confirmed by Fourier transform infrared spectroscopy (FT‐IR) and ¹H‐NMR spectroscopic technique. Results of FT‐IR spectroscopy and atomic force microscopy (AFM) demonstrated that epoxy chains have been covalently bonded to the surface of the SiO₂‐TiO₂ particles. The particles size of SiO₂‐TiO₂ are about 20–50 nm, as characterized by AFM. The experimental results showed that the glass‐transition temperatures and the modulus of the modified systems were higher than that of the unmodified system, and the impact strength was enhanced by two to three times compared with that of the neat epoxy. The morphological structure of impact fracture surface and the surface of the hybrid materials were observed by scanning electron microscopy and AFM, respectively. © 2006 Wiley Periodicals, Inc. J Appl Polym Sci 101: 1075–1081, 2006     

Stabilized dispersions of titania nanoparticles via a sol–gel process and applications in UV‐curable hybrid systems

Organic–inorganic hybrid UV‐curable coatings were synthesized through blending UV‐curable components and stabilized titania sol prepared via a sol–gel process of tetrabutyl titanate (TBT) with three different stabilizers, acetylacetone (Acac), isopropyl tri(dioctyl)pyrophosphato titanate coupling agent (TTPO) and a polymerizable organic phosphoric acid (MAP). The size and the dispersion of titania particle in the UV‐cured organic matrix were dominated by the properties of these stabilizers. A cured hybrid film with titania particle size around 20 nm was obtained when TTPO was utilized as protection agent for the sol. It is interesting that the hardness and flexibility of the photocured hybrid films were improved simultaneously, in contrast to results with neat organic UV‐curable formulations. Copyright © 2006 Society of Chemical Industry     

A comparative study of the preparation and physical properties of polystyrene–silica mesocomposite and nanocomposite materials

In this paper, a comparative study with regard to the preparation and physical properties of as‐prepared polystyrene–silica mesocomposite (PSM) and polystyrene‐silica nanocomposite (PSN) materials is presented. Vinyl‐modified mesoporous silica particles with a wormhole structure were first prepared by doping a sol‐gel metal oxide with an optically active non‐surfactant (dibenzoyl‐L ‐tartaric acid) as a template, followed by template removal through Soxhlet extraction. The as‐prepared silica particles with/without mesopores were subsequently characterized using the Brunauer–Emmett–Teller method and transmission electron microscopy (TEM) and Fourier transform infrared, ¹³C NMR and ²⁹Si NMR solid‐state spectroscopy. A specific feed amount of silica particles was subsequently reacted with styrene monomer by free radical polymerization to yield a series of PSM and corresponding PSN materials. Both as‐prepared composite systems were further characterized using TEM and scanning electron microscopy/energy‐dispersive X‐ray mapping studies. A systematic comparative study of the physical properties of both as‐prepared composite materials clearly illustrated that PSM had effectively enhanced thermal stability, optical clarity and dielectric properties compared to the corresponding PSN counterpart. Evaluation was carried out using thermogravimetric analysis, differential scanning calorimetry, UV‐visible transmission spectroscopy and dielectric constant measurements. Copyright © 2011 Society of Chemical Industry     

Characterization and properties of UV‐curable polyurethane‐acrylate/silica hybrid materials prepared by the sol‐gel process

UV‐curable, transparent hybrid material of urethane‐acrylate resin was prepared by the sol‐gel process using 3‐(trimethoxysilyl)propylmethacrylate (TMSPM) as a coupling agent between the organic and inorganic phases. The effects of the content of acid and silica on the morphology and mechanical properties of UV‐curable polyurethane‐acrylate/silica hybrid (UA‐TMSPM)/SiO₂ materials have been studied. The results of thermogravimetric analysis for the (UA‐TMSPM)/SiO₂ hybrid materials indicated that the thermal stability of the hybrids is greatly improved. It was found that with the increase of HCl content, the interfacial interaction between organic and inorganic phases had been strengthened, as demonstrated by field emission scanning electron microscopy. Without sacrificing flexibility, the hybrid materials showed improved hardness with increasing content of acid and silica. Compared with the pure organic counterpart UA/hexanediol diacrylate (UA/HDDA) system, abrasion resistance of the hybrids improved with increasing acid content, at low silica content. Copyright © 2004 Society of Chemical Industry     

Role of silane coupling agents for performance improvement of poly(vinyl acetate)/tetraethyl orthosilicate hybrid composites prepared by a sol–gel process

Silica based poly(vinyl acetate)/inorganic hybrid composites were prepared via a sol–gel process under acidic conditions. Because the phase behaviour of the hybrids is greatly affected by weak interactions such as hydrogen bonding between organic polymer and inorganic network, two types of silane coupling agent (vinyl trimethoxysilane and 3‐(trimethoxysilyl)propyl methacrylate) were used to introduce specific interactions and to control phase behaviour in the interface between polymer and silica. The interfacial interactions between polymer and inorganic segment in the presence of silane have been investigated by Fourier transform infrared spectroscopy. Thermogravimetric analysis shows that the thermal stability of organic components in the hybrids is enhanced by addition of silane coupling agents. Scanning electron micrographs reveal that silica particles are homogeneously dispersed in the organic matrix as a result of the specific interactions. © 2001 Society of Chemical Industry     

Advanced antistatic/anticorrosion coatings prepared from polystyrene composites incorporating dodecylbenzenesulfonic acid‐doped SiO2@polyaniline core–shell microspheres

We present the preparation of advanced antistatic and anticorrosion coatings of polystyrene (PS) incorporating a suitable amount of dodecylbenzenesulfonic acid (DBSA)‐doped SiO₂@polyaniline (SP) core–shell microspheres. First, aniline‐anchored SiO₂ (AS) microspheres that were about 850 nm in diameter were synthesized using the conventional base‐catalyzed sol–gel process with tetraethyl orthosilicate in the presence of N‐[3‐(trimethoxysilyl)propyl]aniline. SP core–shell microspheres were then synthesized by chemical oxidative polymerization of aniline monomers with ammonium persulfate as an oxidizing agent in the presence of the AS microspheres. The polyaniline shell thickness of the as‐prepared core–shell microspheres was estimated to be about 120 nm. The AS and SP microspheres were further characterized using Fourier transform infrared spectroscopy, scanning electron microscopy (SEM) and transmission electron microscopy. The as‐synthesized DBSA‐doped SP core–shell microspheres were then blended into PS using N‐methyl‐2‐pyrrolidone as solvent and then cast onto a cold–rolled steel (CRS) electrode to obtain antistatic and anticorrosion coatings with a thickness of about 10 µm. The corrosion protection efficiency of the as‐prepared coating materials on the CRS electrode was investigated using a series of systematic electrochemical measurements under saline conditions. The enhanced corrosion protection ability of the PS/SP composite coatings may be attributed to the formation of a dense passive metal oxide layer induced by the redox catalytic effect of the polyaniline shell of the as‐synthesized core–shell microspheres, as evidenced by electron spectroscopy for chemical analysis and SEM observations. Moreover, the PS composite coating containing 10 wt% of the SP core–shell microspheres showed an electrical resistance of about 3.65 × 10⁹Ω cm^?2, which meets the requirements for antistatic applications. Copyright © 2012 Society of Chemical Industry     

A statistical study of poly(ε‐caprolactone) crystallinity in poly(ε‐caprolactone)–silica sol–gel materials and their in vitro calcium phosphate‐forming ability

Composite poly(ε‐caprolactone) (PCL)–silica materials for potential use in orthopaedic applications have been prepared by a sol–gel method using an experimental design approach to investigate the effect of synthesis variables, separately and together, on the physical form of the organic polymer. A combination of differential scanning calorimetry, X‐ray diffraction and Fourier‐transform infrared methods were used to obtain information on the arrangement of the organic polymer in the hybrid material. As our studies investigated the effect of synthesis variables simultaneously, it was possible to establish that the increase of tetraethyl orthosilicate (TEOS)/PCL and HCl/TEOS molar ratios decreased the poly(ε‐caprolactone) crystallinity and provided for a better mixing of the two phases. At a mechanistic level it was possible to show that increase in catalyst content affected the condensation of silicon containing species. In vitro calcium phosphate‐forming ability tests using the static biomimetic method have been carried out on selected PCL–silica sol–gels. In vitro bioactivity was only observed for PCL–silica sol–gel composites with high silica content (30% weight). Changes in catalyst levels had a smaller but still significant effect. Calcium phosphate formation on largely non‐porous surfaces is proposed to occur via the formation of a silica sol–gel layer, and is influenced by the topography and the chemistry of the materials surface. Copyright © 2003 Society of Chemical Industry     

Thermal and optical properties of PMMA–titania hybrid materials prepared by sol‐gel approach with HEMA as coupling agent

A series of sol‐gel derived organic–inorganic hybrid materials consisting of organic poly(methyl methacrylate) (PMMA) and inorganic titania (TiO₂) were successfully synthesized by using 2‐hydroxyethyl methacrylate (HEMA) as coupling agent. In this work, HEMA is first copolymerized with methyl methacrylate monomer at specific feeding ratios by using benzoyl peroxide (BPO) as initiator. Subsequently, the as‐prepared copolymer (i.e., sol‐gel precursor) is then cohydrolyzed with various contents of titanium butoxide to afford chemical bondings to the forming titania networks to give a series of hybrid materials. Transparent organic–inorganic hybrid materials with different contents of titania are always achieved. Effects of the material composition on the thermal stability, optical properties, and morphology of neat copolymer and a series of hybrid materials, in the form of both coating and free‐standing film, are also studied by differential scanning calorimetry, thermogravimetric analysis, UV–Vis transmission spectra, refractometer, and atomic force microscopy, respectively. © 2004 Wiley Periodicals, Inc. J Appl Polym Sci 94: 400–405, 2004     

Synthesis of polymer–inorganic hybrid nanoparticles via radical polymerization initiated by surface‐immobilized photoiniferter

Polymer–inorganic hybrid nanoparticles were prepared through radical photo‐polymerization of methyl methacrylate initiated by N,N‐diethyldithiocarbamyl surface functionalized silica nanoparticles under UV irradiation at ambient temperature. IR analysis and UV spectroscopy confirmed the occurrence of Et₂NCS₂—end groups on the resulting poly(methyl methacrylate), and the morphology of these hybrid nanoparticles was observed directly by means of tapping mode atomic force microscopy (AFM). Copyright © 2003 Society of Chemical Industry     

Study the factors affecting the performance of organic–inorganic hybrid coatings

In this article, a series of hybrid organic–inorganic coatings based on silica‐epoxy composite resins were prepared with the sol‐gel method by using γ‐aminopropyl triethoxysilane as a coupling agent. Especially, the research emphasized on the factors that influenced on the properties of the prepared hybrid coatings. Firstly, epoxy resin was reacted with γ‐aminopropyl triethoxysilane at a specific feeding molar ratio; subsequently, the asprepared sol–gel precursor was cohydrolyzed with tetraethoxysilane (TEOS) at various contents to afford chemical bondings to form silica networks and give a series of organic–inorganic hybrid coatings. They were loaded and cured on steel panels and characterized for FTIR, TGA, DSC, water contact angles (WCA), pencil hardness, surface & three‐dimensional morphological studies, and potentiodynamic polarization tests. The surfaces of the hybrid coatings showed Sea‐Island or Inverting Sea‐Island morphologies at a certain relative content of two components, which made the coatings possess hydrophobic property. Due to the contribution of organic and inorganic components, the prepared hybrid coatings possess a lot of properties such as pencil hardness, thermotolerance, and corrosion resistance. © 2014 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2014 , 131, 41010.     

Synthesis of poly(methylphenylsiloxane)/phenylene‐silica hybrid material with interpenetrating networks and its performance as thermal resistant coating

In this study, poly(methylphenylsiloxane) (PMPS) and phenylene‐silica based hybrid material with interpenetrating networks was prepared by a two‐step sol–gel process. Firstly, in the presence of H₂SO₄, the phenylene‐silica was formed as sol particles with high branching degree by cohydrolysis and condensation of phenylene‐bridged monomer, tetraethoxysilane (TEOS), and hexamethyldisiloxane (MM). Then, the intermediate transformed into gel framework in polymer matrix using alkali catalyst, in order to produce a homogenous hybrid material with interpenetrating networks. The structure of prepared hybrid material was characterized by FTIR and NMR, suggesting that phenylene‐silica framework was imported into polymer matrix and the hybrid products have a much higher network chain density than neat PMPS. The thermogravimetric analysis (TGA) shows that the prepared materials start to degrade at around 490°C. The results of tensile test indicate that the typical PMPS/phenylene‐silica hybrid material has a tensile strength up to 26 MPa and demonstrate a certain degree of flexibility. An increase of phenylene content in phenylene‐silica particles tends to produce hybrid materials with improved thermal stability and tensile strength. The hybrid coating films after calcinating at 350 and 400°C for 2 h exhibit a good mechanical performance on adhesion, impact strength and flexibility. Electrochemical impedance spectroscopy (EIS) measurements show that the investigated films have an extremely high electric resistance (10¹⁰ Ohm·cm²) and a satisfied impermeability to 3.5 wt % sodium chloride solution. © 2012 Wiley Periodicals, Inc. J. Appl. Polym. Sci., 2013     

Nanocomposite coatings via simultaneous organic–inorganic photo‐induced polymerization: synthesis,structural investigation and mechanical characterization

Hybrid sol–gel films were prepared via a simultaneous organic‐inorganic UV‐curing process using a diaryliodonium salt as a superacid photogenerator. In this single‐step procedure, an epoxy functionalized reactive resin mixed with a variable amount of either of two epoxy trialkoxysilane precursors was UV‐irradiated, causing both the initiation of epoxy ring‐opening copolymerization and the catalysis of trialkoxysilyl sol–gel reactions. The concomitant photo‐induced sol–gel process was found to have a significant effect on the two related propagation mechanisms in competition for the oxirane ring‐opening—the active chain‐end and the activated monomer mechanisms—as proved by a systematic examination of the hybrid material microstructure through ²⁹Si and ¹³C solid‐state NMR spectroscopy. The effect of the oxo‐silica network generation on the epoxy reaction kinetics was also evaluated using real‐time Fourier transform infrared spectroscopy upon varying the epoxysilane structure and its concentration. Thermal and dynamic mechanical analyses were systematically performed on these hybrids, by studying thoroughly their structure–property interdependence. Other mechanical characterizations through tribological and scratch tests suggested that the present photopolymer–silica hybrid material provides a powerful tool to tailor mechanical property profiles. Copyright © 2010 Society of Chemical Industry     

Sol–gel process of alkoxysilanes in an elastomer medium

The influence of different mixtures of di‐, tri‐ and tetraalkoxysilanes on the synthesis and character of silica filler particles prepared by a sol–gel reaction in an elastomer medium was investigated. Silica fillers containing organic substituents with basic properties were synthesized in acrylonitrile–butadiene rubber, with and without carboxyl groups, as well as in decane as a suspension medium, which was treated as an elastomer model. ²⁹Si NMR spectroscopy and scanning electron microscopy (SEM) were used to determine the structure of the resulting silica fillers, and their dispersion in the elastomeric medium. Water, alcohol or other polar solvents were not used in the process of creating the silica fillers as it is impossible to introduce them into the elastomer. Copyright © 2005 Society of Chemical Industry