Synthesis of micrometer-sized silica-stabilized polystyrene latex particles

Micrometer-sized silica-stabilized polystyrene latexes have been readily prepared by alcoholic dispersion polymerization using a 13 or 22 nm commercial alcoholic silica sol as the sole stabilizing agent. These resulting surfactant-free polystyrene particles have relatively narrow particle size distributions and contain surprisingly low levels of silica (相似文献   

Separation and identification of synthetic dysstuffs by thin-layer electrophoresis and its application in the forensic analysis of liquors

Summary The excessive demand for alcoholic drinks has resulted in the preparation of fakes and created a problem for their identification. Dyestuffs have been added to alcoholic liquors and the separation of these dyestuff mixtures into their various components has been the subject of study by thin-layer electrophoretic techniques on silica gel-G plantes. 10 dyestuffs commonly used in liquors and beverages have been resolved into their components. The migration distances of the separated coloured zones in five electrolytes, either basic or acidic, have been recorded. The technique was found to be particularly suitable for distinguishing fake samples from genuine ones.     

Polystyrene-silica nanocomposite particles via alcoholic dispersion polymerization using a cationic azo initiator

Submicrometer-sized polystyrene-silica nanocomposite particles have been prepared by alcoholic dispersion polymerization of styrene using commercial alcoholic silica sols of 13 or 22 nm diameter as the sole stabilizing agent. The key to the formation of colloidally stable nanocomposite particles is the selection of a cationic azo initiator (use of nonionic or anionic initiators leads either to the formation of silica-stabilized polystyrene latex particles with very low silica contents or to the precipitation of polystyrene, respectively). Neither surface modification of the silica sol nor the addition of surfactant or polymeric stabilizers is required for successful nanocomposite syntheses. The purified polystyrene-silica nanocomposite particles have relatively narrow particle size distributions, with mean diameters ranging from 331 to 464 nm as judged by disk centrifuge photosedimentometry. Thermogravimetric analyses indicated mean silica contents of 13-26 wt. %, depending on the synthesis conditions. Calcination of the polystyrene-silica nanocomposite particles leads to the formation of hollow silica shells, which indicates a well-defined core-shell morphology for the original nanocomposite particles.     

Sol–gel synthesis of silica containers using a corrosion inhibitor,catamine AB,as a templating agent

It has been shown that silica container particles containing a large amount (~1 g/g of SiO₂) of a corrosion inhibitor, catamine AB, can be obtained, with the inhibitor being loaded at the stage of the sol–gel synthesis of the particles by using catamine micelles as a template. Being introduced into an H₂S-containing aggressive aqueous medium, such containers protect rather efficiently carbon steel from hydrogen-sulfide corrosion and hydrogenation. The protection effect seems to be realized via not only the release (desorption) of catamine AB molecules from the containers, but also the adsorption of the products of gradual dissolution of silica matrix on the surface of metal being protected.     

Restraint of stress in fabricating the large areas of crack-free porous silica films in the presence of composite polydimethylsiloxane

To present a new method of fabricating the large areas of crack-free porous silica films by introduction of composite polydimethylsiloxanes (PDMS). We employed two kinds of side-chain polyether modified by PDMS terminated with Si–CH₃ and Si–OC₂H₅ groups in preparation of large areas of porous silica films. The porous film presents a mesopore structure with a porosity of 58.0 %, which is fit for thermal-isolating layer applied in pyroelectric devices. The stress evolution on gel-to-ceramic film conversion has been investigated. The results reveal that a slow decrease in tensile stress before 250 °C and a slow increase after 250 °C can be observed, which is closely related to the alteration of chemical composition in the heat-treatment process. It is clear that the stress has been restrained with the addition of composite PDMS.     

Sol–Gel Synthesis of SiO<Subscript>2</Subscript> Containers Using Micelles of an Anionic Corrosion Inhibitor as a Template and the Prospects of Creation Protective Coatings Based on Them

It has been shown that silica container particles can be loaded with large amounts of an anionic corrosion inhibitor, sodium N-oleyl sarcosinate, at the stage of the sol?gel synthesis of the particles by using its micelles as a template. When incorporated into paint and varnish coatings, such containers efficiently protect low-carbon steel and D16 aluminum alloy from corrosion under severe conditions of neutral salt spray.     

Corrosion protection enhancement effect by mixed silica nanoparticles of different sizes incorporated in a sol–gel silica film

We demonstrate an enhancement of corrosion protection by sol–gel silica film including mixed silica nanoparticles of 10 and 50 nm. Low-temperature silica films were prepared by sol–gel dip-coating method, followed by a thermal annealing at 200 °C. Importantly, film with mixed particles exhibits lower corrosion current density and slower loss of film resistance during the immersion in electrolyte solution, showing an improved corrosion protection over the film with 50 nm particles. The improved corrosion protectability of the mixed particles comes from the suppressed diffusion of ionic species by a close packing of 10 nm particles.     

Electrochemical noise generated during the stress corrosion cracking of sensitized alloy 690

Electrochemical noise in current has been used to monitor the stress corrosion cracking (SCC) susceptibility of alloy 690 sensitized at 700 °C during 48 h in sodium thiosulfate at 90 °C. At 48 h of aging, the specimen failed by SCC and the corrosion current pulses had high intensity and low frequency, and were associated with the nucleation and propagation of stress corrosion cracks during slow strain rate tests. When the alloy was immune to SCC, the observed corrosion current pulses had a much higher frequency and lower intensity, indicating either uniform corrosion or passivation. The type of transients observed do not indicate the mechanism responsible for the observed embrittlement, but only the cracking initiation or propagation process.     

Mechanochemical Effects in Processes of Corrosion of Metals

Mechanochemical effects have been investigated in the processes of corrosion of bent plates of unalloyed and high-alloy steel in aqueous solutions of sulfuric and hydrochloric acids. Special attention was paid to the strain sign effect discovered recently and caused by the existence of a surface stress in solids. The use of the weight method and the hydrogen method of corrosion control has yield well consistent results confirming the existence of the mechanochemical effect of the strain sign even under condition of the starting corrosion cracking. The domination of corrosion on the concave side gives evidence of the negative sign of surface stress at the steel/solution boundary, which can be explained by the formation of the electrical double layer.     

Two layered silica protective film made by a spray-and-dip coating method on 304 stainless steel

The silica coating has attracted much attention because of its superior corrosion resistance with almost no harm to human health and to the environment. In this study, a two layered silica film was tried to get an enhanced corrosion resistance. The silica film was prepared on the hairline finish 304 stainless steel surfaces by-a-spray- and subsequent-dip-coating process. The spray coating solution was prepared by mixing sodium silicate solution, silica colloid, tetraethyl orthosilicate (TEOS), methyltriethoxysilane (MTES), ethanol, and distilled water. Then the solution was sprayed onto the stainless steel surface, and was dried and heat treated. The dip coating solution was prepared by a simple mixing of TEOS and acidic water into ethanol, and the prior spray coated sample was dipped into the solution. The outer dip coated layer was intended to cover spray coated rough and porous layer and hence to enhance the corrosion resistance. A homogeneous and crack free surface was successfully obtained after the dip coating. The prepared silica film was characterized using scanning electron microscopy, potentiodynamic polarization scan, and electrochemical impedance spectroscopy. The two layered film showed an enhanced corrosion resistance. The enhancement was attributed to a protecting effect of the dip coated layer where the diffusion of ionic species was successfully impeded.     

SiO2纳米粒子对溶胶凝胶涂层性能的影响

在高强钢表面制备了防护性溶胶凝胶涂层,并研究了不同浓度二氧化硅纳米粒子的加入对于涂层形貌、耐蚀性和硬度的影响。采用扫描电子显微镜(SEM)和电子能谱(EDS)观察了涂层的微观结构和成分;采用显微硬度计测试了涂层的硬度;采用电化学方法研究了二氧化硅纳米粒子的浓度对于涂层耐蚀性能的影响;采用傅里叶红外光谱研究涂层的化学结构,进而探讨了二氧化硅纳米粒子对于涂层的强化机理。结果显示涂层加入二氧化硅纳米粒子的最佳浓度为500 mg.L-1,此条件下的涂层表面均匀致密,有较高的硬度并且在3.5%NaCl溶液中体现出较好的耐蚀作用。纳米粒子在溶胶中反应形成活性羟基基团并与硅烷发生反应生成空间网状结构,从而强化涂层。     

Preparation and Structure of Microporous Silica Membranes

Silica sols have been prepared in an alcoholic solution by hydrolysis and condensation of TEOS (tetra-ethyl-ortho-silicate) molecules as a function of water and nitric acid concentration. The polymers are intended as precursors for ceramic, gas separation membranes. These molecules show fractal behavior as determined by SAXS (Small Angle X-ray Scattering). Microporosity of dried and calcined silica polymers is determined by N₂-adsorption at 77 K. Fractal dimension and porosity increase with increasing acid concentration. Both the sol structure and the drying kinetics determine the porosity values. N₂-adsorption isotherms are not very suitable for the determination of pore size distributions of microporous silica.     

Electrochemical behaviour of SiO2 sol-gel coatings on stainless steel

SiO₂ coatings onto stainless steel substrates have been prepared by sol-gel in order to study the performance and mechanism of attack in different corrosive solutions. The electrochemical behaviour of the samples has been evaluated by Electrochemical Impedance Spectroscopy using NaCl and HCl as electrolytes. Comparative tests have been performed on samples with one and two silica layers as well as on uncoated ones. SiO₂ coatings produce no important protection of stainless steels subjected to electrochemical corrosion. This behaviour may be explained by micropores and microcracks produced during the coating sintering.     

Cerium hybrid silica coatings on stainless steel AISI 304 substrate

AISI 304 Stainless Steel is widely used in different industrial fields because of its mechanical and corrosion properties. However, its tendency to corrosion in presence of halide ions limits the applications. One strategy to improve the corrosion resistance is the use of coatings barriers containing corrosion inhibitors in their formulation. The lanthanides present attractive green and corrosion properties for the substitution of chromates, which are the most common substances used as corrosion protection. However, these compounds are highly toxic, and an intense effort is being undertaken to replace them. Cerium is a good alternative because of its relatively low cost and abundance. It fulfils the basics requirements for being considered an alternative inhibitor: the ions form insoluble hydroxides and they present low toxicity. Inorganic and hybrid sol-gel coatings have been developed to increase the corrosion resistance of metals and they provide an excellent vehicle for the incorporation of secondary phases including particles and metal ions as cerium ions. The aim of this work was to study the influence of the incorporation of cerium ions in hybrid silica sol-gel coatings deposited on AISI 304 stainless steel as substrate as a potential replacement of chromate treatments. This system should combine the barrier protection effect of silica coating with the corrosion inhibitor effect of the cerium ions inside the coatings. After 7 days of immersion in NaCl, coated substrates showed lower current densities than the bare steel, although the coatings produced from Ce (III) salts experience a slight weakening in time and those obtained from Ce (IV) chemicals evidence an enhance in the coating performance, probably due to the plugging of corrosion products in the defective areas of the film.     

Structure of a new phenol aldehyde from the leaves of Eucalyptus viminalis

A new terpenoid phenol aldehyde has been isolated from an alcoholic extract of the leaves of the ribbon eucalyptus by column chromatography on silica gel, and on the basis of the results of¹H and¹³C NMR spectroscopy and mass spectrometry the structure of 4-[1-(3,5-diformyl-2,4,6-trihydroxyphenyl)-3-methylbutyl]-ledol is proposed for it. The relative configurations of the substituents in the terpenoid moiety of the molecule have been determined. All-Union Scientific-Research Institute of Medicinal Plants and Production Association, Moscow. Translated from Khimiya Prirodnykh Soedinenii, No. 6, pp. 789–795, November–December, 1991.     

Structure of a new phenol aldehyde from the leaves of Eucalyptus viminalis

A new terpenoid phenol aldehyde has been isolated from an alcoholic extract of the leaves of the ribbon eucalyptus by column chromatography on silica gel, and on the basis of the results of¹H and¹³C NMR spectroscopy and mass spectrometry the structure of 4-[1-(3,5-diformyl-2,4,6-trihydroxyphenyl)-3-methylbutyl]-ledol is proposed for it. The relative configurations of the substituents in the terpenoid moiety of the molecule have been determined.All-Union Scientific-Research Institute of Medicinal Plants and Production Association, Moscow. Translated from Khimiya Prirodnykh Soedinenii, No. 6, pp. 789–795, November–December, 1991.     

Stress dependence of paramagnetic point defects in amorphous silicon oxide

Room-temperature red cathodoluminescence (CL) emission (R band) arising from the paramagnetic point-defect population present in amorphous silicon oxide (SiOx) has been characterized with respect to its shift upon applied stress, according to a piezo-spectroscopic (PS) approach. The R band (found at around 630 nm) originates from nonbridging oxygen hole centers (NBOHC; Si-O*) generated in the presence of oxygen-excess sites. It is shown that reliable stress assessments can be obtained in silica glass with a relatively high spatial resolution, provided that appropriate spectroscopic procedures are developed to precisely extract from the CL spectrum the shift upon stress of the R band, isolated from other partly overlapping bands. Macroscopic and microscopic PS calibration procedures are shown to lead to consistent results on silica materials with different chemical characteristics and, thus, with different intrinsic defect populations. In addition, quantitative calibrations of both electron probe size and luminescence emission distribution within the electron probe are given. As an application of the PS technique, the magnitude of the residual stress piled up (mainly due to a thermal expansion mismatch) at a sharp silica/silicon interface has been characterized by taking into account the gradient in defect population developed as a function of distance from the interface. In the Results and Discussion section, brief comments are offered regarding the possible impact of highly spatially resolved stress assessments in silica glass upon the development of new materials and advanced electronic devices.     

Silica Sol-Gel Coatings on Metals Produced by EPD

The objective of this work has been to combine the sol-gel method and the electrophoretic deposition (EPD) process to prepare thick coatings onto metallic substrates. Two different routes were used for preparing the sol-gel silica suspensions. On one hand, silica particulate sols were obtained by basic catalysis of alkoxides and alkylalkoxides. On the other, silica suspensions were prepared by adding a commercial colloidal silica sol to an organic-inorganic acid catalysed silica sol. The properties of the suspension and the physical parameters associated to EPD (current density, potential, electric field and deposition time) were studied. Crack-free deposits up to 20 m were obtained after drying and crack-free glass-like coatings of 12 m after sintering at 500°C for 30 minutes. The electrochemical behaviour of these coatings was evaluated by potentiodynamic methods, showing an excellent behaviour against corrosion.     

Alcoholic Solvent Effect on Silica Synthesis—NMR and DLS Investigation

The solvent effect on the synthesis of silica particles has been elucidated through the examination of hydrolysis rate and particle growth by 29Si NMR and Dynamic Light Scattering studies, respectively, in various alcoholic solvents. Kinetic data obtained from the NMR experiments indicate that the rate of hydrolysis is fastest in 1-butanol and the rates follow an unusual order of 1-butanol > methanol > ethanol > 2-propanol > 1-propanol. This order of the rates of hydrolysis is rationalized with two opposing factors, steric hindrance reducing the rate and decrease of hydrogen bonding enhancing the rate. The final particle size increases as the alcohol molecular weight increases. This might be due to decrease in polarity of the alcohols.     

Titania nanoparticles synthesis in mesoporous molecular sieve MCM-41

Nanocrystalline titanium oxide (TiO(2)) is one of the most useful oxide material, because of its widespread applications in photocatalysis, solar energy conversion, sensors and optoelectronics. The control of particle size and monodispersity of TiO(2) nanoparticles is a challenging task. The use of MCM-41, an inorganic template of uniform pore size (2-10 nm), can overcome this difficulty and produce stable nanoparticles of uniform size and shape. Here, we demonstrate the synthesis of titania nanoparticles inside the pores of silica based MCM-41 forming a TiO(2)/Si-MCM composite. Composites are formed in the alcoholic medium by incipient wetness impregnation method. Titania particles of average 3 nm size are obtained. Effect of silica and titania precursors on the quality of nanoparticles has been investigated. The characterization of titania-MCM-41 composites has been carried out using a variety of techniques like UV-vis absorption spectroscopy, X-ray diffraction, FT-IR spectroscopy, X-ray photoelectron spectroscopy, transmission electron microscopy and photoluminescence spectroscopy. It has been found that the titania particles are co-ordinated with Si-MCM by SiOTi covalent bond.