Catalyzed Sol Gel Process Research Articles

Synthesis, characterization, and application of silica aerogel thin films prepared via surface derivatization: A comprehensive study on micro-silica nanofilms for enhanced photoelectric conversion efficiency in photovoltaic solar cells

Silica aerogels are nanoporous materials with exceptional optical and physical properties, making them promising candidates to enhance solar cell efficiency as antireflective coatings. This study synthesized hydrophobic silica aerogel thin films under ambient conditions and characterized their porous structure, surface morphology, and optical performance. The films were deposited on monocrystalline silicon solar cells to assess their impact on photovoltaic properties. A two-step acid/base catalyzed sol-gel process was utilized, followed by solvent exchange and surface modification with trimethylchlorosilane. Structural analysis via SEM revealed successful deposition of crack-free films when aging occurred in an ethanol environment. The aerogel displayed considerable specific surface area (115 m2/g), porosity (77.92%) and surface roughness (55-78%) along with a low refractive index (1.05), benefiting light harvesting. Preliminary solar testing showed increased output voltage with a 0.2 mm aerogel coating versus a bare cell. Further IV measurements demonstrated enhanced charge transport and conversion efficiency for the treated cell. The aerogels antireflective and light-trapping effects appear to improve photon absorption. This initial research validates the potential of ambient pressure-synthesized hydrophobic silica aerogels to increase the performance of silicon photovoltaics cost-effectively. Further optimization of film thickness and morphology could realize higher efficiency gains.

Designing multifunctional silica coatings for enhanced broadband antireflection and microfiber contamination sensing

Multifunctional silica coatings find diverse applications in solar energy conversion and pollution monitoring sensors due to their suitability for mass manufacturing. However, the challenge lies in producing robust silica coatings on a large scale with tunable refractive index. This work presents a two-step acid/base catalyzed sol–gel process for synthesizing multifunctional silica coatings with adjustable refractive index. The coatings' porous microstructure allows them to be used as double-layer broadband antireflective coatings and enhances the sensitivity of contamination sensors. The optimized double-layer coatings, designed using computer-aided techniques, demonstrate excellent broadband antireflective performance in the visible regions and high environmental durability. They achieve a maximum transmittance of 99.87% at 591 nm, with an average transmittance of 99.40% in the visible region (400–800 nm) and 98.63% from 400 nm to 1100 nm. Additionally, the coatings exhibit robust abrasion resistance and enhanced surface hydrophobicity with a water contact angle increased from 30° to 126° through HMDS treatment. This work investigated the particle growth mechanism and the relationship between silica nanoparticle microstructure and antireflective coating properties. Furthermore, the coatings' presence of abundant micropores allows successful application onto microfiber contamination sensors, the additional loss increases from 26.40 dB to 37.69 dB over 140 min and decreases to 31.55 dB within one minute, demonstrating rapid adsorption and desorption rates. The work successfully achieves a wide range of adjustable refractive index while maintaining excellent mechanical and optical properties, addressing the traditional trade-off between high porosity and poor mechanical stability. These rationally designed multifunctional silica coatings hold great potential for high-quality broadband antireflection and high sensitivity in microfiber contamination sensing.

Tailoring the Morphology of Monodisperse Mesoporous Silica Particles Using Different Alkoxysilanes as Silica Precursors.

The hard template method for the preparation of monodisperse mesoporous silica microspheres (MPSMs) has been established in recent years. In this process, in situ-generated silica nanoparticles (SNPs) enter the porous organic template and control the size and pore parameters of the final MPSMs. Here, the sizes of the deposited SNPs are determined by the hydrolysis and condensation rates of different alkoxysilanes in a base catalyzed sol-gel process. Thus, tetramethyl orthosilicate (TMOS), tetraethyl orthosilicate (TEOS), tetrapropyl orthosilicate (TPOS) and tetrabutyl orthosilicate (TBOS) were sol-gel processed in the presence of amino-functionalized poly (glycidyl methacrylate-co-ethylene glycol dimethacrylate) (p(GMA-co-EDMA)) templates. The size of the final MPSMs covers a broad range of 0.5-7.3 µm and a median pore size distribution from 4.0 to 24.9 nm. Moreover, the specific surface area can be adjusted between 271 and 637 m2 g-1. Also, the properties and morphology of the MPSMs differ according to the SNPs. Furthermore, the combination of different alkoxysilanes allows the individual design of the morphology and pore parameters of the silica particles. Selected MPSMs were packed into columns and successfully applied as stationary phases in high-performance liquid chromatography (HPLC) in the separation of various water-soluble vitamins.

Synthesis of nanosize zinc oxide through aqueous sol–gel route in polyol medium

BackgroundThis study is aimed to synthesize nanosize zinc oxide by acid catalyzed sol–gel process using zinc nitrate hexahydrate as precursor, aqueous isopropanol as solvent and glycerin for making polyol system. The polyol mediated procedure was employed in combination with calcination induced synthesis of nanoparticles of numerous sizes obtained with the variation in calcination temperature from 500 to 900 ℃. The crystal structure of the prepared samples was characterized by X-ray diffraction analysis (XRD). Infrared spectroscopy (IR) was used to identify the surface hydroxyl groups. Thermal stability was confirmed by differential scanning calorimetry-thermogravimetric analysis (DSC-TGA) whereas field emission scanning electron microscopy (FESEM) was used to study the surface morphology of nanoparticles.ResultsResults revealed the formation of hexagonal wurtzite structure of irregular shaped nanoparticles having size ranging from 50–100 nm. However, the particles combined to form agglomerates of 200–400 nm with the rise in calcination temperature.ConclusionsThese results indicate that nanosize zinc oxide can be synthesized successfully by a simple process comprising of glycerin as a low-cost, non-toxic and eco-friendly polyol followed by calcination at ambient temperatures.

Highly efficient catalytic derived synthesis process of carbon aerogel for hydrogen storage application

For the present work, resorcinol-formaldehyde (R–F) aerogels were synthesized through both acid (nitric acid) and base (sodium carbonate) catalyzed sol-gel process followed by supercritical drying (SCD) as well as ambient pressure drying (APD). RF aerogels were carbonized at high temperatures to form carbon aerogels. The effect of the catalyst type and drying methods on the final characteristics were studied in detail. Microstructural and textural characteristics were evaluated through XRD, SEM, BET, RAMAN, FTIR, and TEM techniques. It was found that the combination of base catalysis and SCD delivered a higher micropore density and more uniform pore distribution. The CAs prepared under such conditions displayed a hydrogen uptake of 0.80 wt% at room temperature and 2.85 wt% at liquid nitrogen temperature (77 K).

Long-Term Performance and Stability of Interlayer-Free Mesoporous Silica Membranes for Wetland Saline Water Pervaporation.

Wetland water is an alternative water resource around wetland areas. However, it is typically saline due to seawater intrusion and contains high natural organic matter (NOM) that is challenging to treat. This study evaluated the stability of interlayer-free mesoporous silica matrix membranes employing a dual acid–base catalyzed sol–gel process for treatment of saline wetland water. The silica sols were prepared under a low silanol concentration, dip-coated in 4 layers, and calcined using the rapid thermal processing method. The membrane performance was initially evaluated through pervaporation under various temperatures (25–60 °C) using various feeds. Next, the long-term stability (up to 400 h) of wetland saline water desalination was evaluated. Results show that the water flux increased at higher temperatures up to 6.9 and 6.5 kg·m−2·h−1 at the highest temperature of 60 °C for the seawater and the wetland saline water feeds, respectively. The long-term stability demonstrated a stable performance without flux and rejection decline up to 170 h operation, beyond which slow declines in water flux and rejection were observed due to fouling by NOM and membrane wetting. The overall findings suggest that an interlayer-free mesoporous silica membrane offers excellent performance and high salt rejection (80–99%) for wetland saline water treatments.

Polyethylenimine wrapped mesoporous silica loaded benzotriazole with high pH-sensitivity for assembling self-healing anti-corrosive coatings

The aim of this work is to develop a self-healing coating doped with pH-sensitive nanocontainers for the active corrosion protection of mild steel. A pH-sensitive carboxyl-functionalized mesoporous silica nanomaterials (MSNs-COOH) was prepared via chemical modification of mesoporous silica nanomaterials (MSNs) which was synthesized in a tetraethyl orthosilicate (TEOS) solution via base catalyzed sol-gel process. Benzotriazole (BTA) molecules were loaded into the internal pores of the prepared MSNs-COOH. Then the BTA-loaded MSNs-COOH were wrapped by the highly branched polyethylenimine (PEI) to obtain the nanocontainers of BTA@MSNs-COOH-PEI. SEM, TEM, DLS, XRD, nitrogen adsorption-desorption isotherms, TGA and FT-IR analyses were employed to characterize the as-prepared nanocontainers. The pH-sensitive releasing property of BTA@MSNs-COOH-PEI was studied using UV–vis spectroscopy, which indicates that the releasing rate of BTA from BTA@MSNs-COOH-PEI can be accelerated under alkaline conditions. Afterwards, a self-healing coating was fabricated based on the epoxy resin primer doped with BTA@MSNs-COOH-PEI which can release BTA inhibitor once localized corrosion occurs. Finally, the active anti-corrosion performance of the as-prepared coating was confirmed by EIS measurements and salt spray tests. The self-healing coating prepared in this work brings a new sight for elaborate design of active anti-corrosion coatings.

Investigation of the Effects of Acid Content and Annealing on the Properties of Nanostructured TiO2 Sol

Titanium dioxide (TiO2) sol was prepared using tetrabutyl titanate as a precursor via an acid catalyzed sol-gel process. Investigation of the effects of acid content and annealing on the properties of nanostructured TiO2 materials. The influence of acid content on the sol density, viscosity, stability and particle size were studied and based on the kinematic viscosity data, Gibbs energies of activation for viscous flow (ΔG*) were also calculated. Furthermore, the prepared samples were characterized using X-ray diffraction (XRD), Fourier transform infrared (FTIR) spectroscopy, scanning electron microscopy (SEM), energy dispersive spectrometer (EDS) and ultraviolet-visible (UV-Vis) spectrophotometer. The results showed that the increase of acid content nearly had no obvious influence on the chemical structure of TiO2 sol. With the increase of annealing temperature, titanium dioxide changes from amorphous phase to crystalline phase, anatase coexists with rutile at 600 °C, sample absorbance increases, and the edge of UV-Vis spectra shows red shift. Ti-O-Ti bond is the main structure of TiO2 sol, and the formed TiO2 molecule has linear structure.

Raspberry-Like Polysilsesquioxane Particles with Hollow-Spheres-on-Sphere Structure: Rational Design, Controllable Synthesis, and Catalytic Application.

Raspberry-like hollow-spheres-on-sphere (HSOS) particles with reactive surfaces, uniform sizes and monodisperse properties were rational designed and fabricated to immobilize gold nanoparticles for the catalytic reduction of 4-nitrophenol. HSOS polysilsesquioxane (PSQ) particles were constructed by an organic alkali catalyzed sol-gel process from trialkoxysilane precursors with stabilized polystyrene (PS) nanoparticles as both a sacrifice template and a Pickering emulsifier. The PSQ particles were fabricated in an ice bath with methyltrimethoxysilane and mercaptopropyltrimethoxysiane as a co-precursor, tetramethylammonium hydroxide (TMAH) as a catalyst, polyvinylpyrrolidone (PVP) and sodium lignosulfonat as co-stabilizers and PS latex as a hard template. The formation mechanism of the hierarchical particles was investigated in detail by the time study through imaging the particles at regular time intervals during the reaction process. Various effect factors on the morphology were studied systematically which showed that the precursor composition, the content of PS, TMAH and PVP are the most important factors. The hierarchical structure combined with the mercaptopropyl groups on both the surface and the skeleton to make it possible to adsorb guest molecules. Au nanoparticles were immobilized on the particles for the catalytic reduction of 4-nitrophenol to 4-aminophenol. The unique PSQ colloids with hollow-spheres-on-sphere extended the family of the hierarchical structures and has shown the potential applications in separations, drug delivery and heterogeneous catalysts.

Effect of water content on the performance and structure of nanosized TiO2 sol

Titanium dioxide (TiO2) sol was prepared using tetrabutyl titanate as a precursor via an acid catalyzed sol–gel process. The influence of water content on the sol density, viscosity, stability and particle size were studied and based on the kinematic viscosity data, Gibbs energies (ΔG*) of activation of the viscous flow was also calculated. Furthermore, the obtained TiO2 materials were characterized by infrared spectroscopy (IR) and X-ray diffraction (XRD) analysis. The results showed that, with the increase of water content, the sol viscosity and zeta potential were increased and the particle size distribution was narrow. When the molar ratio of H2O/Ti reached 4, the prepared sol was transparent, uniform and stable, and the sol average particle size gets the minimum. Ti–O–Ti bond was the primary structure of TiO2 sol and the formed titanium molecules possessed the line-typed structure. The increase of water content nearly had no obvious influence on the chemical structure of sol. The TiO2 gel material was the amorphous state and it turned into anatase type after calcination at 350°C.

Preparation and characterization of nano-AgI/poly-mercaptopropylmethyl-silsesquioxane and investigation of its photo-catalytic activity for Rhodamine B degradation under visible light irradiation

Poly(mercapto-methyl)silsesquioxanes (PMMSQ) were prepared using the base catalyzed sol-gel processing on methyltrimethoxysilane (MTMS) and 3-mercaptopropyltriethoxysilane (MPTES) with 5:5, 4:6 and 3:7 M ratios in mixture of methanol and water. The PMMSQ which prepared with 3:7 M ratio of MTMS:MPTES gives the product by 4:6 ratio, according to the elemental analysis, and it was chosen for grafting silver iodide and it was applied to the photo-catalytic degradation of Rhodamine B in aqueous solution under visible light irradiation. The degradation yield was studied by UV–Vis spectroscopy and the procedure was optimized for the parameters involved such as the amount of catalyst. The stability of the catalyst and the mechanism of the catalytic process were also investigated.

Hierarchical Porosity Tailoring of Sol–Gel Derived Pt/SiO2 Catalysts

Hierarchically porous materials offer the opportunity for catalyst development in regards to improving catalytic performances. In the present work, the combination of latex synthesis, sonochemical reduction and two-step catalysed sol–gel process has been demonstrated to be a versatile method for preparing supported catalysts with tailored hierarchical porosity. This method has been used to prepare porous Pt/SiO2 catalysts with mesopore and macropore size ranges as large as 2–15 nm and 90–400 nm, respectively. These hierarchically porous catalysts presented an excellent catalytic performance for the selective hydrogenation of p-chloronitrobenzene (p-CNB) to p-chloroaniline (p-CAN). Selectivity values up to 100% at 80% conversion of p-CNB and initial reaction rates up to 74.0 molCNB/min molPt were obtained, while a commercial catalyst exhibited both a lower selectivity of 90.8% and a lower initial reaction rate of 47.7 molCNB/min molPt.

NMR Diffusion Study of Ionic Liquids and Ionogels for Use in Lithium Ion Batteries

Solid-state electrolytes have been explored increasingly for use in Li+ batteries on account of their ability to address the safety issues, packaging constraints, and volumetric design concerns associated with liquid electrolytes. Recently, ionogels, pseudo-solid-state electrolytes consisting of an ionic liquid electrolyte confined in a mesoporous inorganic matrix, have attracted interest because of their high ionic conductivity, stability, and solution processability. Due to the complexity of the trapped liquid, the nature of the ion interaction and movement is not well established. Understanding how the ions behave inside the matrix is paramount for increasing the ionic conductivity and Li+ transference number. The literature for these characteristics is lacking in several key areas including, but not limited to, variations in the electrolyte’s Li+ concentration, the choice of silica precursors, and diffusion under different conditions. The ionogel matrix was synthesized using a non-aqueous organic acid catalyzed sol-gel process to form a nanoporous silica matrix around an ionic liquid, BMIM TFSI with variable amounts of LiTFSI added, thus confining the electrolyte. The choice of silica precursors and use of an organic acid allows for a crack free monolith to form under rapid gelation conditions. The silica component maintains a highly porous network with surface areas up to 1300 m2/g and an average pore size of 20nm as measured through N2 adsorption. The ionic liquid (IL) electrolyte component constitutes 75 vol% of the ionogel. Thermal gravimetric analysis shows that the ionogel is thermally stable to 400 oC. Due to the interconnected porosity and large percentage of liquid, conductivities of ̴10-3 S/cm were measured at room temperature for the prepared monoliths using electrochemical impedance spectroscopy (EIS). The degree to which each ion contributes to the total conductivity can be determined by combining the conductivity measurements with self-diffusion measurements obtained by pulsed field gradient nuclear magnetic resonance (PFG NMR) methods. Furthermore the presence of ion pairing or aggregation can be ascertained by direct comparison between the NMR-predicted and EIS-measured conductivity. In this work, the PFG NMR stimulated echo sequence was used to measure the self-diffusion coefficients of the IL cation, Li+, and anion via 1H, 7Li and 19F, respectively, in the IL and ionogel with a concentration of 1M LiTFSI, at variable temperature covering the 0o – 100oC range. Two main confinement effects of all mobile ions in the ionogel are observed (i) a reduction in self-diffusion values of all ions compared to the pure IL; (ii) the presence of a relatively immobile fraction of the ions. Interestingly the effective Li transference numbers defined as D(Li)/[D(Li) + D(BMIM) + D(TFSI)] in the liquid electrolyte and the and ionogel are comparable, with a value of approximately 0.20.

Preparation and characterization of micro-spherical poly-organo-silsesquioxane immobilized ligand systems to support MoO2(acac)2 and investigation of their catalytic properties in epoxidation of alkenes

Poly(chloropropyl-methyl)silsesquioxanes (PCMSQ) were prepared using the base catalyzed sol–gel processing on methyltrimethoxysilane (MTMS) and 3-chloropropyltriethoxysilane (CPTES) with 5:5, 6:4, and 7:3 molar ratios in methanol and water. The PCMSQ with 6:4 molar ratio of MTMS:CPTES, which has the maximum yield, according to the elemental analysis, was chosen and some chlorine atoms of the chloropropyl groups were changed to different amines by refluxing it with ethylenediamine (en), diethylenetriamine (dien), ortho-phenylenediamine (opda), and 2-imidazolidinethion (imt). The amine grafted PCMSQ were then used to support MoO2(acac)2 complex and dien grafted PCMSQ with higher metal content was applied to the epoxidation of cis-cyclooctene with TBHP. The product yields were studied by gas liquid chromatography and the catalytic procedure was optimized for the parameters involved such as the solvent and oxidant. The catalytic activity of this catalyst also was investigated toward epoxidation of some other alkenes. It was also applied to check its reuse ability.

Silica Aerogel as Super Thermal and Acoustic Insulation Materials

Silica aerogels are light weight, nanostructured, and highly porous materials with an open pore structure. Due to their excellent characteristics, such as extremely low thermal conductivity, low density and high porosity, the silica aerogels become promising potential adsorbents, catalysts, thermal insulation, and acoustic absorption materials for environmental purposes. This paper presents the synthesis of a highly flexible polymer modified silica aerogel with the use of a cellulose-methyltriethoxysilane (MTES) precursor in a two-step acid-base catalyzed sol-gel process. The physical properties of the resulting aerogels were characterized by thermogravimetry, scanning electron microscopy, nitrogen adsorption-desorption, contact angle, thermal conductivity measurements, compression testing and Fourier transform infrared spectroscopy. The fabricated aerogel exhibited high flexibility with a Young’s modulus of compression of 0.33 MPa and the density of 0.132 g/cm3. They were hydrophobic in nature and had low thermal conductivity. Preparation of aerogel with solid waste (fly ash/bottom ash) is also discussed. The preliminary results showed that the materials have great potential for environmental application, i.e. enhancement of solid waste recycling rate by converting waste to high value-added materials, super thermal and acoustic insulation materials in green building and removal of oil spilled into surface drainage.

Sol-gel derived flexible silica aerogel as selective adsorbent for water decontamination from crude oil

Oil spills are the most important threat to the sea ecosystem. The present study is an attempt to investigate the effects of sol-gel parameters on seawater decontamination from crude oil by use of flexible silica aerogel. To this goal, methyltrimethoxysilane (MTMS) based silica aerogels were prepared by two-step acid-base catalyzed sol-gel process, involving ambient pressure drying (APD) method. To investigate the effects of sol-gel parameters, the aerogels were prepared under two different acidic and basic pH values (i.e. 4 and 8) and varied ethanol/MTMS molar ratios from 5 to 15. The adsorption capacity of the prepared aerogels was evaluated for two heavy and light commercial crude oils under multiple adsorption-desorption cycles. To reduce process time, desorption cycles were carried out by using roll milling for the first time. At optimum condition, silica aerogels are able to uptake heavy and light crude oils with the order of 16.7 and 13.7, respectively.

Simultaneous Synthesis of Anatase Colloidal and Multiple‐branched Rutile TiO2 Nanostructures

Facile synthesis of titanium dioxide (TiO2 ) nanostructures with controllability over their cystallinity, dimensions, and shape is in demand for diverse optoelectronic applications. Anatase colloidal particles and precipitates of rutile bundles were synthesized simultaneously using HCl catalyzed sol–gel process with titanium tetrachloride as Ti precursor. The crystallinity and the morphology of these two separable TiO2 phases were studied by X‐ray diffraction, Raman spectroscopy, and transmission electron microscopy. The results show that by varying HCl concentration during synthesis, dimensions of colloidal anatase can be tuned from spherical particles with a diameter of 2–5 nm to nanorods of dimension of 4 nm (width) × 14 nm (length). The rutile bundles whose size increased with aging time consisted of multiple branches with elongation along c‐axis. Both anatase nanorods and rutile bundles can be applied as highly efficient photocatalysts or electron conduits.

Development of hydrophobic and optically transparent monolithic silica aerogels for window panel applications

In the present paper, highly transparent, monolithic and hydrophobic silica aerogel monoliths were prepared by using tetraethoxysilane (TEOS) as precursor and methyltriethoxysilane (MTES) as co-precursor with different MTES/TEOS molar ratios (M) by two-step acid–base catalyzed sol–gel process followed by supercritical alcohol drying. The molar ratio of TEOS, ethanol (EtOH), water (0.001 M oxalic acid catalyst) and ammonium hydroxide (1 M NH4OH) was kept constant at 1:5:3.5:3.5 respectively, while the molar ratio of MTES/TEOS (M) was varied from 0 to 0.75. It has been observed that as the M value increases, the gelation time increases. It has been found that lower (0.25) M values resulted in highly transparent (optical transmission >90 % for a 10 mm thick sample at 700 nm wavelength) and negligible volume shrinkage ( 10 % volume shrinkage but excellent hydrophobicity. A good compromise of acceptable optical transmittance (~87 % optical transmission at 700 nm wavelength for a 10 mm thick sample) with negligible volume shrinkage (6 %) were obtained at M = 0.50. The hydrophobicity of the aerogels was tested by measuring the contact angle between a water droplet and silica aerogel surface. The hydrophobicity was confirmed by Fourier transform infra-red spectroscopy and contact angle measurements. the aerogels have been characterized by percentage of volume shrinkage, optical transmittance, scanning electron microscopy, thermal conductivity measurements and thermogravimetric analysis and differential thermal analysis.

Preparation and evaluation of micro and meso porous silica monoliths with embedded carbon nanoparticles for the extraction of non-polar compounds from waters

A novel hybrid micro and meso porous silica monolith with embedded carbon nanoparticles (Si-CNPs monolith) was prepared inside a fused silica capillary (3cm in length) and used as a sorbent for solid-phase microextraction. The hybrid monolithic capillary was synthetized by hydrolysis and polycondensation of a mixture of tetraethoxysilane (TEOS), ethanol, and three different carbon nanoparticles such as carboxylated single-walled carbon nanotubes (c-SWCNTs), carboxylated multi-walled carbon nanotubes (c-MWCNTs), and oxidized single-walled carbon nanohorns (o-SWNHs) via a two-step catalytic sol-gel process. Compared with silica monolith without carbon nanoparticles, the developed monolithic capillary column exhibited a higher extraction efficiency towards the analytes which can be ascribed to the presence of the carbon nanoparticles. In this regard, the best performance was achieved for silica monolith with embedded c-MWCNTs. The resulted monolithic capillaries were also characterized by scanning electron microscopy (SEM), elemental analysis and nitrogen intrusion porosimetry. Variables affecting to the preparation of the sorbent phase including three different carbon nanoparticles and extraction parameters were studied in depth using polycyclic aromatic hydrocarbons (PAHs) as target analytes. Gas chromatography-mass spectrometry was selected as instrumental technique. Detection limits range from 0.1 to 0.3μgL−1, and the inter-extraction units precision (expressed as relative standard deviation) is between 5.9 and 14.4%.

In-situ monitoring of silica shell growth on PS-b-P4VP micelles as templates using DLS

Polystyrene-block-poly(4-vinylpyrdine) (PS-b-P4VP) block copolymer (BCP) was used as a template for the preparation of PS-b-P4VP@SiO2 core-shell particles using an acid catalyzed sol-gel process. The process of silica shell formation and development of shell morphology were studied using a combination of in-situ dynamic light scattering (DLS) and transmission electron microscopy (TEM). The results obtained reveal that shell formation and growth principally involve the following stages: (I) sol assembly around BCP micelles; (II) hydrolysis-condensation reaction accelerated by the protonated P4VP corona of BCP micelles; (III) shell densification; and (IV) shell growth. Present work provides insight into the sol-gel process which takes place in systems containing “reactive” templates, such as protonated PS-b-P4VP micelles, and discloses the mechanism and pathways of silica shell formation. We demonstrate that the whole process can be effectively monitored in-situ using conventional DLS. The results are of significant importance for fabrication of targeted core-shell nanostructures.