Electrodeposition of Au/nanosized diamond composite coatings

Ultra-dispersed diamond UDD particles were codeposited in gold matrix coatings from a sulphite electrolyte, changing bath load and key operating parameters. The influence of electrolyte pH, current density and bath load on current efficiency, particle co-deposition, surface morphology and microhardness of composite coatings was investigated. UDD incorporation is mainly affected by bath load; however, particle embedding is specifically sensitive to electrolyte pH and deposition current density. The maximum mass fraction of carbon in the coating, about 0.55%, is obtained by depositing from ultrasonically pre-treated electrolytes with UDD concentration 20 g l⁻¹, pH 9.5 and 3 mA cm⁻² . Au/UDD composites are characterised by an increased microhardness and improved wear resistance. When compared to pure gold coatings which are notoriously weak, Au/UDD electrodeposits from sulphite electrolytes represent a significant improvement. Presented at the 4th Baltic Conference on Electrochemistry, Greifswald, 13–16, 2005     

Sustainable and rapid preparation of nanosized Fe/Ni-pentlandite particles by mechanochemistry

In recent years, metal-rich sulfides of the pentlandite type (M₉S₈) have attracted considerable attention for energy storage applications. However, common synthetic routes towards pentlandites either involve energy intensive high temperature procedures or solvothermal methods with specialized precursors and non-sustainable organic solvents. Herein, we demonstrate that ball milling is a simple and efficient method to synthesize nanosized bimetallic pentlandite particles (Fe_4.5Ni_4.5S₈, Pn) with an average size of ca. 250 nm in a single synthetic step from elemental- or sulfidic mixtures. We herein highlight the effects of the milling ball quantity, precursor types and milling time on the product quality. Along this line, Raman spectroscopy as well as temperature/pressure monitoring during the milling processes provide valuable insights into mechanistic differences between the mechanochemical Pn-formation. By employing the obtained Pn-nanosized particles as cathodic electrocatalysts for water splitting in a zero-gap PEM electrolyzer we provide a comprehensive path for a potential sustainable future process involving non-noble metal catalysts.

A sustainable and rapid mechanochemical method for the preparation of bimetallic nanosized pentlandite particles as cathode material is developed and tested within zero-gap PEM cells.     

Effect of the displacement reaction on the composition of the magnetic layer in electrodeposited layered nanostructures Co-Cu/Cu and Ni-Cu/Cu

Methods of stripping voltammetry, quartz microgravimetry, and x-ray-fluorescence analysis are employed to explore the copper displacement process on thin electrodeposited layers of pure cobalt and nickel and on deposits of these metals with inclusions of copper. The displacement reaction proceeds at a considerable rate on cobalt in the sulfate and sulfosalicylate solutions and virtually does not proceed on nickel in both the sulfate or sulfate-chloride solutions. An estimate of the rate of the copper displacement reaction following a change in the concentration of copper ions in the solution and in the pH of the sulfosalicylate solution is given. A decrease in the contact exchange rate is facilitated by a decrease in the concentration of copper ions in solution and their participation in the formation of complexes.     

Structure and properties of nanosized coatings deposited onto polymers

Results of studies aimed at developing a new approach to measuring stress-strain properties of nanosized solids (strength, yield stress, and the value of plastic deformation at uniaxial tension) are generalized. This approach is based on the analysis of the parameters of microrelief arising upon the deformation of polymer films with thin coatings. It is demonstrated for the first time that the stress-strain properties of aluminum coatings deposited onto Lavsan substrates depend on the level of stresses in the substrate, the value of its deformation, and the thickness of the coating. The evolution of these parameters is related to the strain hardening of metal and the effect of nanostructuring of crystalline materials in the range of small thicknesses. When precious metal (Au, Pt) nanosized films are deposited onto polymers by ion-plasma sputtering, in the course of metal deposition, polymer surface layers interact with cold plasma. Stress-strain properties of polymer surface layers modified by plasma are quantitatively estimated for the first time. The model is proposed that makes it possible to take into account the contribution of the properties of precious metal and plasma-modified polymer surface layer to the strength of the coating.     

Alloy Formation and Strength of Ni-Cu Interaction in Ni-Cu/ZnO Catalysts

A series of Ni-Cu/ZnO catalysts were prepared and studied by temperature-programmed reduction. The results show that after reduction a Ni-Cu alloy formed; the strength of Ni Cu interaction depends on the Ni-Cu ratios, the higher the Cu/Ni ratio, the stronger the Ni-Cu interaction. This phenomenon was attributed to the donation of electrons from the d band of Cu to that of Ni, increasing the bonding strength.     

Cu对Ni-Cu/SiO2催化1,4-丁炔二醇加氢性能的影响

采用超临界干燥法和等体积浸渍法制备了不同Ni/Cu比例的Ni-Cu/SiO₂双金属催化剂,利用ICP、BET、XRD、H₂-TPR、H₂-TPD、NH₃-TPD等手段对催化剂进行了结构表征,考察了不同Ni/Cu比例对催化剂结构以及1,4-丁炔二醇加氢性能的影响.结果表明,少量Cu的引入不仅能够提高Ni活性物种的分散性,而且Ni-Cu双金属间的相互作用改善了NiO物种的还原性能及氢活化能力,有利于氢和1,4-丁炔二醇在活性位点的快速转化.在反应温度50℃,氢压1 MPa,反应时间3 h的加氢评价条件下,Ni/Cu比为3：1时,15Ni5Cu/SiO₂催化材料不仅可以实现BYD的完全转化,而且能够有效降低难分离副产物2-羟基四氢呋喃的含量,具有最优的加氢活性和对1,4-丁烯二醇及1,4-丁二醇的选择性.     

Two triazole-based metal-organic frameworks constructed from nanosized Cu20 and Cu30 wheels

Two metal-organic frameworks constructed from nanosized Cu(20) and Cu(30) wheels have been obtained under hydrothermal conditions based on 1,2,3-triazole and 1-H-1,2,3-benzotriazole, respectively. Crystal structure analysis shows that their differences in the size and nuclearity of Cu(20) and Cu(30) wheels are attributed to the steric effect of ligands.     

Characteristics of electrodeposition of composite coatings based on nanosized molybdenum disulfide and copper

Voltammetry was used to study the charge state of molybdenum disulfide nanoparticles in single-layer aqueous dispersions obtained by hydration of LiMoS₂. MoS₂ nanoparticles were shown to have a negative charge. Nanodispersed MoS₂ can be used to deposit Cu-MoS₂ coatings. The influence of some deposition parameters (electrolyte composition, current mode) on the coating composition was determined.     

Special features of preparation of nanosized zirconium diboride powders of various dispersity

Products of the zirconium powder reaction with amorphous boron in a Na₂B₄O₇ ionic melt at 650–850°C and those of the ZrCl₄ reaction with NaBH₄ at 300–725°C have been studied by means of X-ray diffraction, scanning electron microscopy, X-ray photoelectron spectroscopy, thermogravimetry, and elemental analysis. At temperature ≥750°C, single-phase ZrB₂ with the particle size of 60–80 nm is formed in a Na₂B₄O₇ ionic melt, whereas the ZrB₂ powder obtained via the reaction of ZrCl₄ with NaBH₄ at temperature ≥575°C consists of particles differing in the shape, some of which are close to spherical with diameter of 10–35 nm.     

Electrolytic preparation of a reduced ninhydrin reagent for amino acid analysis

Summary A flow-through electrolysis using a column electrode was applied to the preparation of a reduced ninhydrin reagent suitable for a highly reproducible and sensitive determination of amino acids. Non-reduced ninhydrin solution, which could be stably stored for long duration even in contact with atmospheric oxygen, was fed at a constant flow rate of 0.25 ml min^–1 into the flow-through electrolysis cell, whereby ninhydrin was reduced to hydrindantin. The hydrindantin content in the reagent (presumably 1.61 mol%) was sufficiently constant for the subsequent quantitative reaction of the amino acids being eluted from the HPLC system. The electrolytically prepared reagent was practically identical with those prepared by chemical reduction.

---

Elektrolytische Herstellung von reduziertem Ninhydrinreagens für die AminosÄureanalyse

     

Ni-Cu/CeO2催化剂上乙醇水蒸气重整反应

 研究了Ni-Cu/CeO2催化剂在乙醇水蒸气重整反应中的催化性能. 以具有高比表面积的CeO2为载体,用沉积沉淀法制备了一系列不同担载量的Ni, Cu双组分催化剂,采用X射线衍射、程序升温还原和透射电子显微镜对催化剂的晶相组成、还原性能和形貌进行了表征. 结果表明, CuO, NiO和CeO2的相互作用明显改善了NiO的分散. 适量CuO的加入使NiO分散度增大,颗粒明显变小,从而使催化剂具有更好的催化性能,但过多CuO的加入反而降低了催化剂的活性. Ni和Cu的催化性能差异较大, Ni具有优异的断裂C-C键性能,在低温下即可实现乙醇的完全转化,而在高温区则具有很好的甲烷重整性能,可获得很高的氢气产率; Cu在低温区倾向于使乙醇脱氢生成乙醛以及进一步脱羰基生成丙酮,在高温区也具有一定的乙醇裂解性能.     

Facile preparation of superhydrophobic coatings by sol-gel processes

Different organic/inorganic compositions and deposition methods were used to prepare superhydrophobic surfaces using metal alkoxides and the sol-gel process. Both surface roughness and composition had to be adjusted in order to obtain very high contact angles and low contact angle hysteresis as a necessary requirement for superhydrophobicity. Multilayer samples with a fluorinated organic-inorganic top layer showed water contact angles of about 157 degrees with low hysteresis (2 degrees ). Water drops rolled easily off their surface at a tilt angle as low as 4 degrees .     

甲烷部分氧化制合成气在Ni,Cu及Ni-Cu合金上的DFT研究

基于密度泛函理论(DFT)的DMol3量子力学计算程序模块应用于合金体系,通过与N i(111)和Cu(111)的比较,研究了N iCu(111)上甲烷部分氧化制合成气的活性.计算结果显示,Cu的加入导致H2在N iCu(111)的脱附能垒低于H2在N i(111)上的脱附能垒,CO的吸附热变化不大.此外,还考察了甲烷解离的过程,发现Cu的加入对速控步骤的活化能影响不大.     

A novel process for preparation of hybrid nanosized neodymium oxybromide and neodymium oxide

Russian Journal of General Chemistry - A novel process to prepare hybrid nanosized neodymium oxybromide and neodymium oxide from neodymium(III) nitrate hexahydrate has been developed. The...     

Preparation and properties of fibrous sorbents with grafted nanosized organosiloxane coatings containing complexing aminomethylenephosphonic ligands

We have modified fibrous sorbents with the organosiloxane coating containing aminomethylenephosphonic ligands at silicon atoms. The so prepared materials efficiently absorb ions of some transition metals from solutions in aqueous hydrochloric acid.     

Ni-Cu/ZnO双金属催化剂催化CO加氢反应

ｉＣｕ／ＺｎＯ双金属催化剂催化ＣＯ加氢反应王亚权（天津大学化工学院一碳化工国家重点实验室，天津３０００７２）关键词镍，铜，氧化锌，负载型催化剂，双金属催化剂，一氧化碳，加氢分类号Ｏ６４３一种金属担载在载体上，可以产生多种相互作用，如金属载体强相互...     

Electrochemical preparation of thin rhenium-tellurium coatings from chloride-borate electrolyte

The kinetics and mechanism of cathode electrodeposition of thin Re-Te films from a chloride-borate electrolyte containing NH₄ReO₄, TeO₂, HCl, and H₃BO₃ were studied. The region of potentials in which rhenium is electrodeposited together with tellurium was determined by cyclic voltammetry. The combined electrodeposition of rhenium and tellurium occurred with minor depolarization due to the energy liberated during the formation of the Re-Te alloy.     

活性炭基水解催化剂的制备及其脱硫性能的研究

分别通过溶胶-凝胶法、浸渍法制备Cu/活性炭(AC)水解催化剂,考察了不同制备方法对水解脱硫性能的影响。利用XRD、BET、SEM等对载体及催化剂进行表征,分析了预处理对AC表面性质及不同制备方法对脱硫效率的影响,并探讨了水解脱硫的机理。结果表明,浸渍法所制备的水解催化剂活性优于溶胶-凝胶法制备的催化剂,在通过预处理增大了AC的比表面积、丰富了AC的孔道结构的基础上,浸渍法能均匀地将活性组分分散在载体表面及其孔道中,而溶胶-凝胶法制备的催化剂活性组分主要覆盖在载体的表面,不能有效进入孔道内,造成脱硫效率下降。在反应温度80℃、羰基硫浓度1.33g/m~3、空速1500h~(-1)、氧化铜质量分数为5%时,浸渍法制备的水解催化剂具有较高的硫容,可达29mg S/g。     

不同Ti/Ba比钛酸钡纳米粉体及其陶瓷的制备和介电性能研究

采用溶胶-凝胶(Sol-gel)法制备了不同Ti/Ba比的钛酸钡纳米粉体及其陶瓷。通过XRD、SEM和TEM对钛酸钡粉体及陶瓷进行了表征,并测试了陶瓷的介电性能,研究了Ti/Ba比对陶瓷微观结构和介电性能的影响。结果表明:通过溶胶-凝胶工艺制备的纳米粉体主要为立方相钛酸钡,平均粒径约19~33 nm:随Ti/Ba比的增加,钛酸钡纳米粉体平均粒径呈先稍递减后增大的趋势,当粉体平均粒径大于30 nm吋,四方相在混合相中所占比例逐渐增大;Ti/Ba=1.01~1.03时,陶瓷中异常长大的晶粒较多,室温介电常数降低;1300℃烧结2 h的Ti/Ba=1.04的钛酸钡陶瓷具有较好的介电性能。