Sodium chloride dendrite columns in (GC)2

Summary A method is described for roughening the surface of sodalime glass capillaries by depositing sodium chloride dendrites on the inner wall. The sodium chloride layer improves the wettability of the wall and shows favourable adsorption properties. For apolar and polar stationary phases coating efficiencies of 60 to 85% are attained.     

Surface analysis of sol-gel coatings on glass by secondary neutral mass spectrometry

Secondary neutral mass spectrometry (SNMS) has been used to profile coatings of the systems SiO₂ and 65SiO₂.20TiO₂.15ZrO₂ (STZ). The coatings have been deposited on float glass and heat insulating glass by dip coating from alkoxide solutions. The microporous gel coatings have been densified by heat treatment. The SBM method (separate bombardment mode) has been applied to characterize the systems and the HFM method (high frequency mode) to check for matrix effects in the SBM depth profiles. Both methods show sodium diffusion from the float glass substrate into the STZ coating and no significant sodium diffusion into the SiO₂ coating. Measurements of the coatings on the heat insulating glass indicate that the SnO₂ interlayer acts as a diffusion barrier. The diffusion of sodium from the float glass substrate into the STZ coating during consolidation has been analyzed by SBM-SNMS. The sputtering rate decreases with increasing consolidation. Due to large differences between sputtering rates of the substrate and of the microporous coatings, the calibration of sodium intensities from time to depth at the interface has not been possible. However, a correlation between the final temperature of heat treatment and the depth of the Na₂O depletion in the substrate surface under the coating can be obtained.     

Atomic force microscopy of coated glasses

Atomic force microscopy has been used to investigate the topology of alkoxide gel dip coatings on different substrates. Results of SiO(2) - TiO(2) - ZrO(2) (STZ) coatings are presented on float glass, on polished fused silica, on commercially coated insulating flat glass, and on PtRh. Consolidated STZ coatings display the so-called glass pattern with ripples equal or less than 2 nm high. The same pattern is seen on partially dense STZ coatings, as soon as the surface is stiff enough for scanning, and also on the bottom of a 50 nm deep sputtering crater in the consolidated coating. The vitreous STZ coating on the fire side of the float glass is as flat as the float glass itself. It has the same tendency to contamination. 100 nm wide and 50 nm deep polishing grooves on fused silica have been filled up with the 80 nm thick coating, only dips of a few nm remain. The trenches between the SnO(2) crystallites on the insulating flat glass were filled up and the roughness of the substrate was partially reduced. PtRh sheet remained rough even after the coating. On the partially densified STZ coating, sputtering generates a grained surface.     

A new surface roughening method for glass capillary columns. Sodium chloride deposition from suspension

A method is described for roughening the surface of glass capillary columns for subsequent coating with polar stationary phases. A suspension of sodium chloride, obtained by addition of a saturated solution of sodium chloride in methanol to 1,1,1-trichloroethane, is passed through the column at velocities of 1–5 cm/s. During passage of the suspension, particles of sodium chloride deposit spontaneously on the column wall. The amount of sodium chloride deposited on the column wall is a function of the volume of the suspension passed through and of the contact time of the suspension and the column wall. Ultimately the amount of sodium chloride per unit surface area approaches a maximum. Columns covered with this maximum amount of sodium chloride were prepared with high reproducibility and coated with a number of polar stationary phases. Various factors that influence the stability of the suspension and the deposition of sodium chloride are discussed and minimum requirements are given. A theoretical model is proposed for the mechanism of deposition of sodium chloride particles on the glass wall.     

Atomic force microscopy of coated glasses

Atomic force microscopy has been used to investigate the topology of alkoxide gel dip coatings on different substrates. Results of SiO₂ – TiO₂ – ZrO₂ (STZ) coatings are presented on float glass, on polished fused silica, on commercially coated insulating flat glass, and on PtRh.· Consolidated STZ coatings display the so-called glass pattern with ripples equal or less than 2 nm high. The same pattern is seen on partially dense STZ coatings, as soon as the surface is stiff enough for scanning, and also on the bottom of a 50 nm deep sputtering crater in the consolidated coating.· The vitreous STZ coating on the fire side of the float glass is as flat as the float glass itself. It has the same tendency to contamination. 100 nm wide and 50 nm deep polishing grooves on fused silica have been filled up with the 80 nm thick coating, only dips of a few nm remain. The trenches between the SnO₂ crystallites on the insulating flat glass were filled up and the roughness of the substrate was partially reduced. PtRh sheet remained rough even after the coating.· On the partially densified STZ coating, sputtering generates a grained surface.     

Application of polyaniline/sol-gel derived tetraethylorthosilicate films to an amperometric lactate biosensor.

The electrochemical entrapment of polyaniline (PANI) onto sol-gel derived tetraethylorthosilicate (TEOS) films deposited onto indium-tin-oxide (ITO) coated glass has been utilized for immobilization of lactate dehydrogenase (LDH). The performance of these sol-gel/PANI/LDH electrodes has been investigated as a function of the lactate concentration, applied potential, pH of the medium and interferents. The amperometric response of the electrodes under optimum conditions exhibited a linear relationship from 1 mM to 4 mM. An attempt has been made to extend the linearity up to 10 mM for lactate by coating an external layer of polyvinyl chloride (PVC) over the sol-gel/PANI/LDH electrodes with a correlation coefficient of 0.89. These sol-gel/PANI/LDH electrodes have a response time of about 60 s, a shelf life of about 8 weeks at 0-4 degrees C and have implications in a lactate biosensor.     

Polystyrene film-coated glassware: a new means of reducing metal losses in trace metal speciation

A recently developed process for coating a glass surface with polystyrene (PS) film, by use of a simple chemical process has been used to reduce trace metal adsorption by cell components. The glass coating is a two-step procedure consisting of covalent attachment of vinyl-terminated PS to Si atoms on the glass surface then adsorption of PS from solution to create a stable PS film. To assess the quality of the coating we used anodic stripping voltammetry to study the adsorption of lead and cadmium ions in coated and untreated glass cells. In both short and long-term (24 h) experiments we observed that the amount of metal adsorbed was considerably less for the PS film-coated glass cell than for the uncoated cell. Further experiments showed that metal desorption is faster and metal contamination after cleaning is significantly lower for the coated cells. The PS film was, moreover, stable over a period of 6 months within the pH range 3.5–9.     

Inhibiting surface crystallization of amorphous indomethacin by nanocoating

An amorphous solid (glass) may crystallize faster at the surface than through the bulk, making surface crystallization a mechanism of failure for amorphous pharmaceuticals and other materials. An ultrathin coating of gold or polyelectrolytes inhibited the surface crystallization of amorphous indomethacin (IMC), an anti-inflammatory drug and model organic glass. The gold coating (10 nm) was deposited by sputtering, and the polyelectrolyte coating (3-20 nm) was deposited by an electrostatic layer-by-layer assembly of cationic poly(dimethyldiallyl ammonium chloride) (PDDA) and anionic sodium poly(styrenesulfonate) (PSS) in aqueous solution. The coating also inhibited the growth of existing crystals. The inhibition was strong even with one layer of PDDA. The polyelectrolyte coating still permitted fast dissolution of amorphous IMC and improved its wetting and flow. The finding supports the view that the surface crystallization of amorphous IMC is enabled by the mobility of a thin layer of surface molecules, and this mobility can be suppressed by a coating of only a few nanometers. This technique may be used to stabilize amorphous drugs prone to surface crystallization, with the aqueous coating process especially suitable for drugs of low aqueous solubility.     

刚果红交联聚乙烯醇薄膜／K^＋交换玻璃光波导检测氯化氢气体

用环氧氯丙烷为交联剂合成了刚果红(CR)交联聚乙烯醇(PVA)CR-PVA敏感试剂.用匀胶机将其做成薄膜固定在钾离子交换玻璃光波导表面,研制出一种光波导氯化氢气体传感器.CR-PVA薄膜碱式结构的最大吸收波长在600 nm以下,对波长为632.8 nm的激光吸收很弱;薄膜与酸性气体发生反应后强烈吸收波长在632.8 nm附近的导波或消失波;检测输出光强度的变化,即能够测出酸性气体浓度.测试结果表明,本传感器对低浓度HCl气体有快速响应,且对1.6～192 mg/m3范围内有良好的线性响应;SO2、NO2气体的浓度大于18000 mg/m3时才有响应,而对于高、低浓度H2S气体均无响应.     

Improvements in the performance of etched glass capillary columns

Summary The surface of hydrogen chloride etched, glass capillary columns can be rendered less active by heating at 400°C for 3 hours in a stream of dry nitrogen prior to coating. The reduction of surface activity is probably caused by loss of water from surface silanol groups to produce siloxide bridges. In addition, such treatment almost halves the bleed rate of columns coated with OV 101 silicone oil stationary phase at 280°C and causes no deterioration in the wetting properties of the etched glass surface.     

The preparation of thick-film glass capillary columns

A detailed method for the routine preparation of glass capillary columns is presented. The method consists of coating a glass tube with quartz powder prior to pulling the tube into a capillary. The inner surface of the capillary consists of an even distribution of quartz particles fused to the walls. This surface has been found readily deactivated by standard procedures and ideal for the preparation of thick-film glass capillary columns. The method has been thoroughly tested in two independent laboratories to ensure that the procedures described are reproducible.     

Recyclable hydrophilic-hydrophobic micropatterns on glass for microarray applications

A novel method for fabricating recyclable hydrophilic-hydrophobic micropatterns on glass chips is presented. TiOx patterns (100-2000 microm) were sputtered on glass chips via a through-hole mask. The patterned chips were then vapor-coated with fluoroalkylsilane, for example, (heptadecafluoro-1,1,2,2-tetrahydrodecyl)triethoxysilane (FTES) to form a hydrophobic coating layer. The fluoroalkyl chain of FTES film on TiOx patterns was photocleaved under UV irradiation, exposing the fresh hydrophilic TiOx patterns. The resulting chip could be used multiple times by repeating the coating and photocleaving processes with negligible deterioration of the hydrophobic FTES film coated on glass. If desired, bare glass patterns could also be generated by removing the TiOx patterns with KOH. The patterned glass chips have been successfully used for microarray fabrication.     

Advanced sol–gel coatings for practical applications

One of the features of the sol–gel techniques is closeness to the industrial applications. Another feature is the variation of shapes of obtained materials like bulk, fiber, coating film, powder and so on. Among them, the author has focused on research of the sol–gel coatings on various substrates for practical applications as well as the fundamental research under the collaboration with industry. In this review, results of such research will be presented. These include (a) protective coating on metal sheets, (b) micropatterning on glass substrates, (c) water-repellant coating on windshields, (d) colored coating on glass bottles for easy recycling, (e) superhydrophobic and superhydrophilic coating on glass plates, and (f) anti-reflective coating on glass lenses for cameras. Some were highly successful, and some were not, of course. The author also contributed to the foundation of The Japanese Sol–Gel Society in 2003. The activities of The Society in these 8 years are introduced.     

Measurement of molecular transport in poly(vinyl chloride) by the step response technique

Sorption and diffusion of methane and 1-butene in poly(vinyl chloride) (PVC) powder have been investigated by the step-response method using gas chromatography. The sorption equilibrium constant of 1-butene was lower than that of chlorine, despite the higher critical temperature of 1-butene, while the sorption of methane was negligibly small at temperatures much higher than critical. The diffusivity of 1-butene in PVC showed a discontinuous dependence on temperature at the glass transition point, suggesting that the micro-Brownian motion of the polymer chain enhances the diffusivity at the higher temperature. Below the glass transition temperature, the diffusivity of 1-butene in PVC showed a lower value than has been measured for other smaller molecules such as chlorine and hydrogen chloride.     

孔雀石绿－聚氯乙烯膜涂层玻璃电极的研制

本文报道了孔雀石绿－聚氯乙烯膜涂层玻璃电极的研制及其应用。该电极是将孔雀石绿敏感的聚氯乙烯膜涂敷于ｐＨ玻璃电极表面而制得。所制电极具有制作简单，使用方便，响应灵敏度高，选择性好等优点。能够直接用于孔雀石绿的测定。本文将该电极应用于催化电位法分析，测定了几种环境水样中亚硝酸根的含量，结果满意。     

One-pot electrosynthesis of polyglycine-like thin film on platinum electrodes as transducer for solid state pH measurements

The anodic oxidation of concentrated glycine based aqueous electrolyte on smooth platinum electrode leads to a strongly grafted polyglycine-like coating on the surface in an irreversible way. Due to the proton affinity towards amino groups of polyglycine (PG), the electrodeposited thin film was used as receptor for solid potentiometric pH sensor. In order to reach local pH measurement, we developed miniaturized microelectrodes on glass substrate thanks to photolithography process. We used silver chloride on silver as the reference electrode. The couple (silver chloride, PG based platinum electrode) of microelectrodes gives linear potentiometric response vs. pH in the range [2-12], reversibly and with a sensitivity of 52.4 mV/pH (for 1 mm electrode size). PG based pH electrode is compared to other organic polymer based pH receptor such as linear polyethylenimine (L-PEI), polyaniline (PANI) and glass membrane.     

Effect of pulse Nd-YAG laser beam interaction on annealing of nanopowder ITO using spin-on-glass

The effect of pulse Nd-YAG laser on structural and electrical properties of ITO thin film on glass by spin coating process was evaluated. It was found that the beam interaction of pulse laser energy has a significant effect on crystallization, conductivity and optical properties of ITO. Laser irradiation with a wavelength of 1,064 nm and energy of 8–40 J are employed. The conventional X-Ray diffraction studies show the peak intensities of (211), (222), and (440) planes increased by using Nd-YAG laser treatment and prove the crystallization of ITO nanoparticle. Due to absorption of millisecond pulse laser, the resistivity of ITO coating on glass substrate which was annealed at 350 °C, reduced by a factor of 100, and a resistance of less than 0.6 kΩ has been achieved.     

不同色浆质量分数的水性聚氨酯涂料对聚氯乙烯表皮低温爆破性能的影响

本文制备了一系列不同色浆质量分数的水性聚氨酯涂料,并将其喷涂在汽车仪表板聚氯乙烯(PVC)表皮的背面形成复合材料。 用旋转流变仪表征了涂料的粘度以评价其喷涂性能;用差示扫描量热仪表征了材料的玻璃化转变温度(T_g);利用万能材料试验机表征了材料在-30 ℃条件下的拉伸性能及抗撕裂性能;用动态热机械分析仪表征了材料的损耗比随温度的变化。 结果表明:不同色浆质量分数的涂料都能喷涂,含有涂层材料PVC表皮在-30 ℃低温爆破性能与涂层材料的T_g、低温拉伸性能、抗撕裂性能的关系并不大,而与涂层材料的阻尼性能直接相关。 材料的阻尼性能越好,其低温爆破性能越好。     

Development of Water-Repellent Glass Improved Water-Sliding Property and Durability

A water-repellent glass with high water-sliding property using FAS for the hydrophobic material has been developed. It had been thought that the sliding property of FAS was inferior to PDMS. But it was found that the sliding angles of the surfaces coated with FAS were affected by coating condition. And the glass on which fluorinated alkyl groups oriented toward normal direction of the surface had almost equal water-sliding property to the one coated with PDMS. Furthermore its durability against wiper abrasion and outside weathering was much higher than that with PDMS. And XPS analysis was carried out to confirm the orientation of fluorinated alkyl groups on the developed water-repellent glass. This kind of water-repellent glass was adopted as commercial automotive windows.     

氧化锌薄膜/锡掺杂玻璃光波导元件及其对氯苯的气敏性研究

建立了玻璃光波导气敏元件检测氯苯气体的方法.采用浸渍-提拉法将ZnO敏感膜固定在锡掺杂玻璃光波导表面,研制出了检测氯苯气体的ZnO薄膜/锡掺杂玻璃光波导气敏元件,并用该玻璃光波导气敏元件对挥发性有机气体进行了检测.实验结果表明,在室温下,气敏元件对氯苯气体有明显的响应,而对相同浓度的其它挥发性有机气体的响应相对较小,对...