Unique commercial applications of the sol-gel process in Japan

Two unique commercial applications of the sol-gel process in Japan are presented. One application involves alkoxide-derived nanometer-sized silica particles used in the final polishing of silicon wafers for the fabrication of integrated circuits. The particles are cocoon-like in shape and have almost replaced conventional abrasives because of the advantages over spherical particles of similar size in terms of obtaining high polishing efficiency for good surface finish. The other application concerns the treatment of paper with an alkoxide solution for water repellent and oil resistance properties, which leads to new products for disposable tableware or cooking ware for microwave oven use.     

Synthesis and structural characterization of amorphous nano-sized SiBONC ceramic powders via polymer pyrolysis

SiBONC ceramic powders have been prepared via a polymer pyrolysis route using silicon tetrachloride (SiCl₄), benzaldehyde (PhCHO), boron trichloride (BCl₃) and aniline (PhNH₂) as starting materials. Fourier transform infrared spectra (FT-IR), X-ray photoelectron spectroscopy (XPS), X-ray diffraction (XRD), and transmission electron microscopy (TEM) were performed to investigate the structural characteristics of the polymer precursor and the ceramic powders. The SiBONC ceramic powders in spherical shape with a mean diameter of 50 nm are amorphous and composed of B-N, Si-O, Si-C, and SiON_x groups. The SiBONC ceramic powders were sintered at 1700 °C to a dense material which still remained amorphous.     

Microhardness of N-Vinylpyrrolidone Modified Glass-Ionomer Cements

ABSTRACT

The water soluble N-vinylpyrrolidone (NVP) monomer was used to prepare poly(N-vinylpyrrolidone-co-itaconic acid-co-acrylic acid) glass-ionomer copolymers, using a free-radical polymerization process. NVP modified terpolymer was mixed with glass powders from four commercial glass ionomer systems. Microhardness from the set cement was measured and compared to several commercial glass-ionomer systems. The Knoop hardness number (KHN) values were recorded on polished specimens conditioned for 48 hours and 7 days. One-way analysis of variance and Tukey-Kramer tests were used to determine the significant differences among the materials tested in each group. Among the four commercial cements, Ketac-Molar (KM) showed the highest value and α-Silver (AS) snowed the lowest value in KHN. Fuji II (F2) and α-Fil (AF) showed much the same values in KHN. At the same P/L ratio, NVP modified glass-ionomers showed higher KHN values than the AS, similar to the AF and F2, and lower than the KM. The effect of P/L ratios was evident and highest KHN values for each group were basically presented by the one with a higher P/L ratio. Higher P/W ratio did not improve the KHN for the AS and KM group, but improved the F2 group.     

聚氨酯/环氧树脂IPN复合抛光材料的制备及性能研究

本研究采用聚氨酯与环氧树脂(PU/EP)作为胶黏剂形成互穿网络(IPN),以无机磨料和稀土抛光剂为分散相,通过一定的成型工艺制备成复合抛光材料。通过固化前后的红外光谱,分析了PU、EP两者之间的反应;热重分析表明PU/EP IPN复合抛光材料的耐热性能比纯的PU和EP有显著提高;体视显微镜照片显示该复合抛光材料具有微孔结构;力学及应用性能研究显示当胶黏剂含量为25%时性能最佳;且在PU/EP=2时,抛光后的玻璃透光率保持原有的97%,且耐磨性得到大幅度提高。     

Effect of calcination temperature on the textural properties of 3 mol% yttria-stabilized zirconia powders

Zirconia-based ceramics have been commonly used in many different technological fields. This kind of materials have consequently received a great deal of attention. The main goal of this study was to investigate the effect of the calcination temperature on the morphological and textural properties of 3 mol% yttria-stabilized zirconia powders (3YSZ). Scanning electronic microscopy (SEM), nitrogen adsorption isotherms, thermogravimetry-differential scanning calorimetry (TG-DSC), X-ray diffraction (XRD) and Fourier transform infrared (FT-IR) spectroscopy have been used with such an aim. Once the 3YSZ powders were dried at 100 °C they were subjected to calcination at 300, 500 or 700 °C. The calcination temperature noticeably influences the surface and textural properties of the 3YSZ powders. Textural parameters appear to be closely related to the removal of the alcohol used in the sol-gel synthesis procedure. The largest values of specific surface area and pore volumes correspond to samples prepared at 100 and 500 °C (i.e., 161 and 62 m²/g). In the first case, this fact is attributable to the removal of residual water and alcohol occluded within the powder particles whereas in the second case it may be due to the elimination of gases produced during the calcination stage.     

A new approach for the removal of protein impurities from purified biologicals using combinatorial solid-phase ligand libraries

The removal of last impurity traces from a purified protein is generally called polishing. It is an important step in downstream processing since protein impurities may generate undesirable side effects when the preparation is intended for research, diagnostic and more importantly therapeutic applications. Polishing is generally achieved by using orthogonal separation methods to previous steps, the most common being gel permeation chromatography. In spite of its polishing effectiveness, this technique suffers from a poor separation capacity and modest productivity as a result of low speed. Other approaches, for instance, based on anion exchange or on hydrophobic chromatography, that may be optimized for a given process cannot be used as generic methods. This document reports for the first time the use of a combinatorial solid-phase peptide library as a general method for the removal of impurity traces. Several examples of impurity trace removal are reported; starting material is either a pure protein spiked with serum proteins or with Escherichia coli extracts or current purified proteins still containing a small percentage of impurities. Among polished proteins are recombinant human albumin expressed in Pichia pastoris and human transferrin purified from whole plasma. This new method is used in neutral or even physiological pH and ionic strength conditions, with a remarkable capability to remove impurities. The process is as rapid as current adsorption chromatography procedures usable for the removal of a large number of protein impurities, with each one present in small amounts, such as host cell proteins.     

In situ ellipsometry of surface layer of non-metallic transparent materials during its finish processing

For modern technology applications it is important to develop non-contact methods of control of the modification of dielectric materials surface layer. The aim of the work is to determine the level of roughness changes in the surface layer of non-metallic material, optical glass BK-7, and to control it by in situ ellipsometry. The probing light spot was formed at a second (lower) reflective surface of the plate being studied during its mechanical processing at direct observation of these changes. The fine mechanical polishing was carried out for 2 hours by using the grinding-polishing machine installed directly on the sample table of ellipsometer LEF-3M. The angle of light incidence was close to 70 degree. The ellipsometric parameters, were determined within the mechanically processed area. For this purpose, the probing light beam passed two times through the sample and then returned to the initial (air) medium, where its polarization state was studied. The polarized beam falls on lower plate surface polished by conventional technology using grinding-polishing CeO₂-based instrument “Aquapol” (grain size 1 micron). The time dependences of the ellipsometric parameters during the surface layer treatment were studied. In these dependences the tendency of changes of ellipsometric parameters indicates the surface roughness enhancement.     

Function of liquid and tool wear in ultrasonic bound-abrasive polishing of fused silica with different polishing tools

The recently proposed fixed-abrasive polishing process was revisited, but this paper focuses mainly on the potential influence of various liquids and the different kinds of pellets on the polishing process as well as the wear of pellet in ultrasonic assisted and conventional processes. The results show that using liquids is helpful in improving surface quality and lowering surface roughness. In particular, the surface roughness is improved sharply for pore-free pellet, from >80 nm to <1 nm (avg.) and the polishing process smoothly proceed that otherwise will hardly progress without liquids. However, the liquids do not necessarily always improve polishing process. There is an optimal volume for a specific polishing process. Moreover, the wear of pellet was also evaluated as well. The results suggest that applying ultrasonics can effectively alleviate the wear loss of pellet and increase the “G-ratio” of polishing process.     

Crystal and magnetic structure of single-crystal La<Subscript>1-x</Subscript><Emphasis Type="Bold">Sr</Emphasis><Subscript>x</Subscript><Emphasis Type="Bold">MnO</Emphasis><Subscript>3</Subscript><Emphasis Type="Bold">(x ≈ 1/8)</Emphasis>

A neutron powder diffraction (NPD) study on the crystal and magnetic structure of a crushed La_1-xSr_xMnO₃ (x ≈ 1/8) single crystal has been performed. The sample belongs to orthorhombic (Pnma, O) above the Jahn-Teller (JT) transition temperature (T_JT) and monoclinic (P12₁/c1, M^′) in the JT regime. We have also refined the NPD data below the charge/orbital ordering (CO/OO) temperature (T_CO/OO) with a monoclinic (P12₁/c1, M^′′) model because the experimental resolution was insufficient to clearly identify a triclinic structure. The refined lattice parameters show an obvious breathing-mode distortion between T_CO/OO and T_JT, accompanied by a large deviation of the monoclinic angle β from 90°, signifying a very strong cooperative JT distortion. A ferromagnetic (FM) moment of 3.43(5)μ _B/Mn besides an A-type antiferromagnetic (A-AFM) moment of 0.54(2) μ _B/Mn is directed mainly along the b axis in P12₁/c1 symmetry at 5 K. With increasing temperature, the A-AFM domains transform into FM ones above ~100 K and the FM spin orientation turns from the b to the c axis in crystallographic b-c plane below T_c = 187(1) K. The magnetization measurements show typical anomalies around T_CO/OO and T_JT. The measured saturation moment of 3.9(1)μ _B/Mn at 70 kOe and 5 K is well consistent with the sum 3.97(5)μ _B/Mn of the refined FM and A-AFM moments at 5 K, implying the A-AFM spins are aligned in field direction at 70 kOe. The applied magnetic field can affect the paramagnetic insulating (PMI) state in the range of magnetic polarons. Based on the size of JT distortion and the bond-valence sums (BVS’s), the CO/OO phenomenon is being discussed.     

ICP-AES测定铂金饰品抛光灰中铂、钯、金和银

提出一种 ICP- AES快速测定铂金饰品抛光灰中铂、钯、金、银的分析方法。 5 g样品经灰化处理后 ,王水提取 ,直接测定 ,该方法的检出限 Pt、Pd、Au、Ag分别为 4 6 .5、4 2 .3、10 .4和 5 .1ng·m L-1。回收率为94 .2 %— 10 3.5 %之间。相对标准偏差为 2 .8%— 4 .4 %。