Synthesis Of Silica Nanospheres Research Articles

Synthesis of Silica Nanoparticles for the Manufacture of Porous Carbon Membrane and Particle Size Analysis by Sedimentation Field‐Flow Fractionation

Silica nanoparticles were synthesized by emulsion polymerization by mixing ethanol, ammonium hydroxide, water, and tetraethyl orthosilicate. An apparatus was designed and assembled for a large‐scale synthesis of silica nanospheres, which was aimed for uniform mixing of the reactants. Then sedimentation field‐flow fractionation (SdFFF) was used to determin the size distribution of the silica nanoparticles. SdFFF provided mass‐based separation where the retention time increased with the particle size, thus the size distribution of silica nanoparticles obtained from SdFFF appeared more accurate than that from dynamic light scattering, particularly for those having broad and multimodal size distributions. A disk‐shaped porous carbon membrane (PCM) was manufactured for application as an adsorbent by pressurizing the silica particles, followed by calcination. Results showed that PCM manufactured in this study has relatively high surface area and temperature stability. The PCM surface was modified by attaching a carboxyl group (PCM‐COOH) and then by incorporating silver (PCM‐COOH‐Ag). The amount of COOH group on PCM was measured electrochemically by cyclic voltammetry, and the surface area, pore size, pore volume of PCM‐COOH‐Ag by Brunauer–Emmet–Teller measurement. The surface area was 40.65 and reduced to 13.02 after loading a COOH group then increased up to 30.37 after incorporating Ag.

Synthesis of silica nanospheres with Ni2+-iminodiacetic acid for protein separation

Silica (SiO2) nanospheres (NSs) with immobilized metal ligands have been prepared for the affinity separation of proteins. First, SiO2 NSs were prepared by controlled hydrolysis of tetraethoxysilane in a basic aqueous-ethanol solution. Then through reaction of iminodiacetic acid (IDA) with 3-glycidoxypropyltrimethoxysilane and immobilization of them onto the surfaces of above SiO2 NSs, novel affinity adsorbents with IDA chelating groups were obtained. After chelating Ni2+ ions, the SiO2–IDA–Ni2+ NSs were applied to separate his-tagged proteins directly from the mixture of lysed cells. The SiO2–IDA–Ni2+ NSs present negligible nonspecific protein adsorption and high protein binding ability (28.3 mg/g).

Synthesis and Size Characterization of Silica Nanospheres Using Sedimentation Field-Flow Fractionation (SdFFF)

Silica nanoparticles were synthesized by a conventional emulsion polymerization by mixing ethanol, ammonium hydroxide, water and tetra ethyl orthosilicate (TEOS). A new reaction apparatus was assembled for a large scale synthesis of silica nanospheres in the laboratory, which was designed for uniform mixing of the reactants. The apparatus was equipped with a disc type agitator with six rectangular propellers. The new apparatus allowed high reproducibility in terms of the mean size and the size distribution of the silica nanoparticles with the relative standard deviation of less than about 6%. Sedimentation field-flow fractionation (SdFFF) was employed for determination of the size distribution of the silica nanoparticles. SdFFF provided size-based separation of the silica nanoparticles, with the retention time increasing with the size. When SdFFF analysis was repeated three times for the same sample, the standard deviation was less than 4%, showing reliability of SdFFF in size measurement. SdFFF seems to provide more accurate size distribution than DLS, particularly for those having broad and multimodal size distributions. Change in the agitation speed resulted in significant change in the mean diameter of the silica nanoparticles. Agitation speed of 400 rpm in 3 L reaction vessel yielded silica particles of about 100 nm in diameter, while at 200 rpm in 1 L vessel yielded those of about 500 nm.

Synthesis of silica nanosphere from homogeneous and heterogeneous systems

Silica nanosphere was synthesized using homogeneous and heterogeneous systems, respectively. In homogeneous system, silica spheres were synthesized without cetyltrimethylammonium bromide (CTABr), which gave bimodal particle size and lower yield (77%). To improve the yield, CTABr was added and found that the yield was very high (100%). The particle was in nm range, but the particle sizes are bimodal. To avoid it, reaction in heterogeneous system using CTABr was carried out. Nanosized silica sphere with uniform size (yield, 94%) was observed. Homogeneous system contains a mixture of ethanol, water, aqueous ammonia and tetraethylorthosilicate (TEOS). In the case of heterogeneous system, only ethanol was absent.

A New Insight into the Mechanistic Study on Synthesis of Silica Nanospheres

The physicochemical characteristics (SEM, N2 adsorption, FT-IR, MASNMR) of samples from kinetics (10 min, 20 min, 30 min, 1 h and 3h) of hydrolysis of tetraethyl orthosilicate (TEOS) gives new insight into the synthesis of nanosphere. The particle sizes are increased with time, however, the surface areas decreased. FT-IR investigation reveals the presence of high intensed silanol groups of 960 cm-1 at 10 min, which reduced on progress of the reaction time. This suggests the partial hydrolysis and condensation of alkoxy groups in TEOS. 29Si MASNMR analysis shows the presence three different silica species(Q4, Q3 and Q2) in 10 and 20 min samples. The intensity of Q2 species decreases with time and other species concentration were increased.