Initial stages of tin electrodeposition from sulfate baths in the presence of gluconate

Tin electrodeposition in its initial stages in acid sulfate/gluconate baths was studied with varying tin and gluconate concentrations using potential-controlled electrochemical techniques. The deposit morphology was observed by scanning electron microscopy (SEM). A comparison with tin electrodeposition from acid sulfate baths in the absence of gluconate was also carried out. Use of a highly acidic bath leads to nonuniform deposits, even in the presence of gluconate; at pH 4 deposits are uniform, brilliant and suitable for finishing applications. Tin crystallites have a well defined morphology which depends on bath agitation conditions. In the absence of agitation, the crystallites have the same tetragonal shape as in a sulfate bath without gluconate.     

釉上金红颜料的研制

采用液相反应法研制了釉上金红颜料，给出了颜料和熔剂配方及其制备方法。     

Solvent-free oxidation of benzyl alcohol with oxygen using zeolite-supported Au and Au–Pd catalysts

The oxidation of benzyl alcohol to benzaldehyde has been investigated in the absence of solvent using zeolite-supported Au and Au–Pd catalysts. Three zeolites were investigated, ZSM-5, zeolite β and zeolite Y, and these were contrasted with the titanoslicalite TS-1 and TiO₂ as supports. For the Au catalysts the best results are obtained with zeolite β as the support and the conversions were comparable or better than those observed with TiO₂ in terms of turn over frequencies. However, the selectivities observed with the acidic zeolites were lower than the non-acidic TS-1 and TiO₂. This is due to the subsequent reaction of benzaldehyde via acid catalysed reactions to give benzyl benzoate and its dibenzyl acetal, and, in some cases dibenzylether. Initial catalysts were evaluated with a gold loading of 2 wt% and increasing this to 4 wt% showed the expected increase in activity, indicating that there is scope to improve the performance of these catalysts. The most active catalysts were prepared by impregnation and catalysts prepared by deposition precipitation were considerably less active. Introduction of Pd into the catalyst improved the activity without significantly affecting the selectivity.     

Structural analysis of Au/Mg(OH)2 during deactivation by Debye function analysis

Using a Debye function analysis, the presence of icosahedral and face centered cuboctahedral gold in a 1 1 ratio has been found in freshly prepared Au/Mg(OH)₂ catalyst. The results support earlier studies which suggest the icosahedral form to be more stable at small nanometer sizes. Interactions between the gold and the Mg(OH)₂ support appear to be weak, with the gold rapidly coagulating over a period of three months. Re-analysis of the aged sample shows the gold to be mainly in the form of truncated decahedra.     

Au/ZnO and Au/Fe2O3 catalysts for CO oxidation at ambient temperature: comments on the effect of synthesis conditions on the preparation of high activity catalysts prepared by coprecipitation

The preparation of Au/ZnO and Au/Fe₂O₃ catalysts using two coprecipitation methods is investigated to determine the important factors that control the synthesis of high activity catalysts for the oxidation of carbon monoxide at ambient temperature. In particular, the factors involved in the preparation of catalysts that are active without the need for a calcination step are evaluated. The two preparation methods differ in the manner in which the pH is controlled during the precipitation, either constant pH throughout or variable pH in which the pH is raised from an initial low value to a defined end point. Non-calcined Au/ZnO catalysts prepared using both methods are very sensitive to pH and ageing time, and catalysts prepared at a maximum pH = 5 with a short ageing time (ca. 0–3 h) exhibit high activity. Catalysts prepared at higher pH give lower activity. However, all catalysts require a short operation period during which the oxidation activity increases. In contrast, the calcined catalysts are not particularly sensitive to the preparation conditions. Non-calcined Au/Fe₂O₃ catalysts exhibit high activity when prepared at pH ≥ 5. Calcined Au/Fe₂O₃ prepared using the controlled pH method retain high activity, whereas calcined catalysts prepared using the variable pH method are inactive. The study shows the immense sensitivity of the catalyst performance to the preparation methods. It is therefore not surprising that marked differences in the performance of supported Au catalysts for CO oxidation that are apparent in the extensive literature on this subject, particularly the effect of calcination, can be expected if the preparation parameters are not carefully controlled and reported.     

Ni-ZrO2纳米复合电铸层抗高温氧化性能的研究

通过间歇式抗高温氧化实验,建立了纯镍电铸层和N i-ZrO2纳米复合电铸层高温氧化动力学模型,分析了电铸层表面和横截面的形貌,测定了电铸层的组织结构。结果表明,N i-ZrO2纳米复合电铸层抗高温氧化性能明显优于纯镍铸层,复合电铸层表面生成的氧化膜晶粒细小且致密,并且该氧化膜较薄,产生的内应力较小,与复合电铸层的黏附性较好。     

Single-phase gold/palladium catalyst: The nature of synergistic effect

The liquid phase oxidation of glycerol with oxygen has been studied using mono and bimetallic catalysts based on Au and Pd metals supported on activated carbon, in order to study the effect of the metal on the distribution of the products and on activity of catalysts. It was found that by using bimetallic catalysts (Au–Pd) a strong synergistic effect was shown. By using a preformed nucleating centre we were able to obtain a single alloyed phase, which allowed us to address the synergistic effect to the presence of alloyed Au/Pd. The advantage of using this latter catalyst lies not only in the high activity but also in a prolonged catalyst life. Although a partial leaching of palladium and assembling of the particles have been revealed by ICP and HRTEM respectively, activity after 10 re-cycles decreased less than expected (about 10%).     

微生物脱砷预处理难冶含砷金矿提金的研究

用化能自养的氧化铁硫杆菌和氧化硫硫杆菌，对河北半壁山含砷金精矿进行了公斤级的预处理氧化脱砷实验．在细菌预处理反应器中的连续和批式脱砷实验表明，目前选育的菌种是有效的．严格控制工艺条件，可以在4天左右便脱砷率高于80％．后续氰化提金实验证实，金的总回收率可达90％以上．用微生物脱砷预处理难冶含砷金矿有金浸出率高、便于固定浸出的砷、免除对环境污染的优点，是有很好应用前景的处理难冶含砷金矿的技术路线．     

适用于摩托车零件的多层镍电镀工艺

概括目前我国摩托车零件电镀所用镀层组合，对照有关金属覆盖层的国家标准，认为摩托车零件应用多层镍组合，并提供了工艺配方。     

Reforming of methane with carbon dioxide over supported bimetallic catalysts containing Ni and noble metal: I. Characterization and activity of SiO2 supported Ni–Rh catalysts

Cobalt catalysts supported on silica aerogel have been prepared using sol–gel chemistry followed by drying under supercritical ethanol conditions. Three different loadings of cobalt were synthesized: 2, 6, and 10% by weight. Transmission electron micrographs indicate that the metallic cobalt exists as discrete particles 50–70 nm in diameter for the 2 and 6% loadings. The 10% catalyst shows long needles of cobalt. BET and BJH measurements indicate that the catalysts retain the silica aerogel properties of high surface area (∼800 m²/g), large pore volume (∼5 cm³/g), and an average pore diameter in the mesoporous regime (∼25 nm). The catalysts were evaluated for Fischer–Tropsch activity in a laboratory-scale packed bed reactor. All three catalysts were active with the 10% Co catalyst achieving more than 20% CO conversion which corresponds to a rate of 1.53 g CO per g-cat per hour. The catalysts were selective for the C₁₀₊ hydrocarbons with more than 50% of the carbon contained within this fraction. A significant portion of the C₉–C₁₅ hydrocarbon product was observed as 1-olefins which reflects the enhanced mass transport within the very porous aerogel support.