A method for the preparation of versatile, hydrolytically stable coatings of fused silica capillaries is described. First, the HNO3-pretreated silica surface is reacted with 7-oct-1-enyltrimethoxysilane to form a stable self-assembled alkylsilane monolayer. Secondly, the copolymer of hydroxypropylcellulose and 2-hydroxyethyl methacrylate is statically coated onto a hydrophobized wall. This allows the formation of a highly crosslinked copolymer layer which is tightly bound to the wall surface. Hydrolytical stability in the pH range of 2-10 for several weeks has been demonstrated. The coating generates a low electroosmotic flow at alkaline pH, which can be easily masked by using special buffers. The versatility of this column technology is documented by separations of peptides, glycoproteins and derivatized oligosaccharides.
Mesoporous silica particles of MCM-41 type were synthesized by sol-gel method from tetraethyl orthosilicate (TEOS) in 2-methoxyethanol and deionized water mixture in base conditions at room temperature. Ammonia or sodium hydroxides were used as catalysts and cetyl-trimethylammonium bromide (CTAB) and n-dodecyl-trimethylammonium bromide (DTAB) as structure directing agents. The porosities and the ordered structure have been analyzed using transmission and scanning electron microscopy, small angle neutron and Xray diffraction, nitrogen adsorption, thermal analysis and FTIR spectroscopy. The samples consist of spherical particles of sub-micrometer size, with radially arranged pores. The comparison of the effect of the different surfactants and catalysts shows that by varying the surfactant type and their proportion, the pore sizes can be controlled. As compared to the commonly used ammonia catalyst, the use of NaOH as catalyst results in a much smaller porosity of the as-prepared materials. These materials are not resisting to the heat treatment at 700 ºC used for the template removal, and the ordered porous structure is completely lost.
Details of synthesis and characterization of sol-gel-produced CoFe2O4 nanoparticles embedded in the amorphous SiO2 matrix are presented together with results of an extended magnetization study of these materials. The particle size was found to increase from 6to15nm by varying the temperature of a subsequent annealing from 800to1100°C. All samples exhibited superparamagnetic behavior with values of the blocking temperature TB increasing with the particle size. At temperatures above TB the magnetization curves follow the expected Langevin scaling of M vs H∕T, which is consistent with the formation of the superparamagnetic state. For T<TB, the coercivity field Hc was found to be proportional to T and the frequency-dependent ac susceptibility was found to obey the Néel–Arrhenius law. Both observations are compatible with a model of noninteracting randomly oriented single-domain particles.
Mesoporous silica particles have been synthesized by sol-gel method from tetraethoxysilane (tetraethylorthosilicate, TEOS) and methyltriethoxysilane (MTES), in ethanol and water mixture, at different ratios of the of the silica precursors. Ammonia was used as catalyst at room temperature and hexadecyltrimethylammonium bromide (cetyltrimethylammonium bromide, CTAB) as the structure directing agent. Nitrogen sorption, X-ray diffraction and small-angle neutron scattering gave information on the evolution of the gel structure and pore morphologies in the function of MTES/TEOS molar ratio. Thermogravimetric and differential thermal analysis showed that with addition of MTES the exothermic peak indicating the oxidation of the low molecular weight organic fragments shift to higher temperature. A room-temperature, one-pot synthesis of MCM-41 type materials is presented, in which the variation of the MTES concentration allows to change the hydrophobicity, preserving the specific properties materials, like the ordered pore structure, large specific surface area and high porosity, making them suitable for selective uptake of guest species in drug loading applications. Specifically, the obtained materials had cylindrical pores, specific surface areas up to 1101 m 2 /g and total pore volumes up to 0.473 cm 3 /g. The obtained mesoporous materials are susceptible for further functionalization to improve their selective uptake of guest species in drug delivery applications.
Modification of surfaces with self‐assembled mono‐layers (SAMs) represents a powerful and innovative tool for adjusting physical and chemical properties of surfaces. The adsorption of isomeric molecules with relatively strong and oppositely oriented molecular dipoles, 1,2‐(HS)2‐1,2‐C2B10H10 and 9,12‐(HS)2‐1,2‐C2B10H10, on a flat silver surface is investigated in order to adjust its work function in a desired way. Time‐of‐flight secondary ion mass spectroscopy (ToF‐SIMS) and X‐ray photoelectron spectroscopy (XPS) are used to prove that both isomers (i) chemisorb on a silver surface as thiolates and (ii) exhibit comparable surface densities. Densely packed surfaces of both SAMs are additionally investigated by electrochemical impedance spectroscopy, and effective surface passivation is observed. Co‐deposition of both derivatives is shown to enable effective and fine adjustment of the surface work function value within a range of ∼1 V, which is confirmed by Kelvin probe force microscopy (KPFM). Experimental data indicate faster SAM formation for the former isomer. Contribution of the interface Ag–S bonds to the work function changes is quantified.
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