Influence of preparation method on structural and magnetic properties of nickel ferrite nanoparticles

Nickel ferrite nanoparticles of very small size were prepared by sol-gel combustion and co-precipitation techniques. At the same annealing temperature sol-gel derived particles had bigger crystallite size. In both methods, crystallite size of the particles increased with annealing temperature. Sol-gel derived nickel ferrite particles were found to be of almost spherical shape and moderate particle size with a narrow size distribution; while co-precipitation derived particles had irregular shape and very small particle size with a wide size distribution. Nickel ferrite particles produced by sol-gel method exhibited more purity. Sol-gel synthesized nanoparticles were found to be of high saturation magnetization and hysteresis. Co-precipitation derived nickel ferrite particles, annealed at 400??C exhibited superparamagnetic nature with small saturation magnetization. Saturation magnetization increased with annealing temperature in both the methods. At the annealing temperature of 600??C, co-precipitation derived particles also became ferrimagnetic.     

Study on preparation of NiOOH by a new catalytic electrolysis method

The present paper reports a new catalytic electrolysis method to prepare NiOOH. KMnO₄ is proposed as a catalyst to play the role of electron-transfer medium in the electrolysis preparation of NiOOH for the first time. Through the self-redox reaction of KMnO₄, the highly efficient electron-transfer process between the electrolyte and the electrode of the spherical Ni(OH)₂ is realized, thus resulting in a high electrolytic efficiency and short electrolysis time. The mechanism of catalytic electrolysis is preliminarily discussed. The experimental results show that the electrode prepared with the NiOOH powders by catalytic electrolysis offers a discharge capacity of 267 mAh g⁻¹ at a current density of 120 mA g⁻¹ and exhibits good cycling performance.     

Influence of Fe catalytic doping on the properties of TiO2 nanoparticles synthesized by microwave method

The present work focus on the development of an effective process for undoped and Fe doped TiO₂ powders production by microwave technique. The influence of Fe doping on the structure, phase, vibrational bands and optical properties of TiO₂ were discussed. The X-ray diffraction patterns of nanoparticles revealed a preferentially oriented (101) anatase phase for TiO₂ and transforms to rutile TiO₂ with Fe doping. Fourier transform infrared spectra analysis confirmed the phase transformation from anatase to rutile TiO₂ with Fe doping. The UV–visible spectra showed the increase in absorption band with Fe doping when compared with undoped TiO₂ nano particles, and optical band gap decreased slightly with Fe doping. SEM micrographs revealed spherical shaped grains of TiO₂ with high homogeneity, with a subsequent reduction in the agglomeration of particles with Fe doping suggesting its potential application for better photo catalytic activity.     

Influence of the preparation method on the physicochemical properties of tolbutamide/cyclodextrin binary systems

Tolbutamide (TBM) was found to form an inclusion complex with beta cyclodextrin (beta-CD) in solution and in solid state. Inclusion complex formation between tolbutamide and beta-cyclodextrin in aqueous solution was studied by phase solubility and spectral shift methods. The apparent stability constant Ks calculated by these techniques, in water, were estimated as 195.7 and 236.5 M(-1), respectively. The phase solubility studies revealed a B(S)-type diagram with an inclusion complex of 1:2 molar ratio. The solid inclusion complexes of TBM and beta-CD were prepared at a molar ratio of 1:2 by kneading, coprecipitation, freeze-drying, and spray-drying methods. In addition, the physical mixture was prepared. Characterization of TBM: beta-CD inclusion was performed using differential scanning calorimetry (DSC), Raman spectroscopy, and X-ray diffractometry and by application of a so-called ether wash method. All the inclusion systems investigated led to a significant improvement in the dissolution over free TBM, and the dissolution rate of the active material was observed to be independent of the preparation method.     

Influence of preparation method on hydroxyapatite porous scaffolds

Hydroxyapatite (HA) is extensively used in medical applications as an artificial bone because of its similarity to the natural components of human bones and for its excellent biocompatibility. The porous structure of HA ceramics is more generally used as a scaffold. Many techniques, which are performed under fluid system, have been applied to fabricate HA porous scaffolds. In this work, polymeric sponge technique was employed in the preparation of HA slurry appropriated for porous ceramic fabrication. Effort for strength improvement was made on porous HA ceramic in several aspects. The effect of HA/water, binder/plasticizer ratios and dispersant content on the rheological properties of HA suspension in combination with the addition of SiC and SiO₂ on the compressive strength of porous bodies were investigated and discussed.     

催化裂化原位降硫助剂的制备及其性能研究

采用溶胶-凝胶法制备具有介孔结构的降硫基质材料，选择具有降硫选择性的活性元素对合成的基质材料进行改性处理，考察不同的改性方法对制得的催化裂化原位降硫助剂性能的影响，并对基质材料和降硫助剂的结构进行表征。采用美国进口的ACE-R小型催化裂化评价装置将降硫助剂与催化裂化催化剂匹配进行性能评价，在不改变原催化裂化产品分布和产品性质的同时，降低原料的总硫含量，总硫降低可达40％以上。     

影响硫化镉/碲化镉性能的关键制备技术探讨

CdTe多晶薄膜具有接近理想光谱响应状态的禁带宽度(1.45eV)和高达10-5cm-1的光吸收系数,是较具前途的光伏材料,而CdTe薄膜太阳能电池由于具有低的制造成本和高的转换效率,使其成为最具发展前途的薄膜太阳能电池。CdS和CdTe膜层的质量对CdTe薄膜太阳能电池的性能有很大影响,如何完善CdS和CdTe的制备技术,获得高质量的膜层,引起了广泛关注。笔者综述了影响CdS和CdTe质量的关键制备因素,提出了一些新的制备方法。     

络合剂对溶胶凝胶制备纳米铜及其催化性能影响

为研究络合剂对纳米铜粉体的制备及其催化性能的影响,分别以柠檬酸、葡萄糖为络合剂,采用溶胶-凝胶法制备纳米铜.考察了两种络合剂对制备过程以及产物结构的影响,通过催化苯氧化合成苯酚的反应考察制得的纳米铜粉的催化性能.研究表明:葡萄糖为络合剂制得的纳米铜(G-Cu)平均粒径较小(30 nm),比表面积为5.203 m2/g,在催化苯制苯酚反应时,具有较高的苯转化率(50.30%),但对苯酚的选择性较差;而柠檬酸为络合剂制得的纳米铜(C-Cu)平均粒径为55 nm,比表面积19.517 m2/g,催化苯转化率为21.95%,选择性为38.46%.此外,通过对溶胶凝胶法制备机理分析可知,在形成的胶体结构中,柠檬酸和葡萄糖中的羧基和羟基分别与铜离子进行配位.     

A cost-effective preparation method of Ba-hexaaluminate nanoparticles for catalytic combustion of methane

The rod-like hexaaluminate nanoparticles have been prepared by using the alumina sol as the (NH₄)₂CO₃ co-precipitation precursor and supercritical drying (SCD) method. Formation of the final hexaaluminate likely occurs via diffusion of the Ba²⁺ ions into the δ-Al₂O₃ matrix. Only Ba-hexaaluminate phase (alumina-rich phase) is observed in the hexaaluminate products. Since the network of the aerogel has a higher stability than that formed by using aluminum nitrate, leading to the decrease in the mobility of aluminum at high calcination temperature, which plays a significant role in maintaining high surface area and pore structure.     

Influence of preparation method on the performance of ternary blended cements

This paper examined the feasibility of preparing high performance gap-graded blended cements by adding fine and coarse supplementary cementitious material (SCM) fractions into commercial Portland cement, and the efficiency of SCMs in gap-graded blended cements and interground blended cements were comparatively evaluated. The results show that the particle size distribution of gap-graded blended cements was much closer to a Fuller distribution, due to the intentional addition of fine and coarse SCMs, resulting in a higher initial packing density. As granulated blast furnace slag (GBFS) was mainly arranged in the fine fraction of the gap-graded blended cements, its efficiency was increased dramatically, contributing to 43.5% of the total measured hydration products. As a result, gap-graded blended cement pastes presented a homogeneous and dense microstructure due to “grain size refinement” and “pore size refinement”, therefore their setting times were decreased significantly, and both early and late strengths were increased remarkably in comparison to the interground blended cements investigated in this study.     

KOH活化处理碳纳米管对其负载非晶态NiP催化性能的影响

经KOH活化处理和未经活化处理的碳纳米管分别用于负载非晶态NiP合金.以苯加氢为探针反应,研究了KOH活化处理温度和时间对碳纳米管的性质及其负载非晶态NiP催化剂活性的影响.研究结果表明:碳纳米管经KOH处理可以提高其负载非晶态NiP催化剂的催化活性,催化剂活性随活化温度升高和活化时间延长而增加.由于KOH处理改变了碳纳米管的微观结构,增加了其比表面积,所以非晶态NiP在碳纳米管上更易沉积分散,其负载的非晶态NiP合金催化剂的催化活性较高.     

Influence of preparation conditions on superconducting properties of Bi-2223 thin films

We report electrical transport properties of Bi₂Sr₂Ca₂Cu₃O_10+x (Bi-2223) superconducting thin films fabricated by pulsed-laser deposition on SrTiO₃ substrate. The aim of the study was to investigate the influence of preparation conditions such as deposition temperature (T _S), annealing time (t _A) and deposition rate (r). A critical temperature (T _c) as high as 110 K and critical current density (J _c) of 6·2 × 10⁶ A/cm² at 20 K were obtained for T _S = 760°C, t _A = 4 h and r = 1·5 Å/s. We also investigated the effect of Li doping on Bi-2223 thin films. Li intercalation results in high resistive onset transition temperature and the resistivity shows broadening in magnetic field that increases with field. The large broadening of resistivity curve in magnetic field suggests that this phenomenon is directly related to the intrinsic superconducting properties of the copper oxide superconductors. The sudden drop in J _c at relatively low magnetic field (H < 0·5 tesla) is due to the effect of Josephson weak-links at the grain boundaries.     

Influence of lanthanum addition on preparation and powder properties of cobalt phosphates

Transition metal phosphates are used as inorganic pigments; however, these materials had a weak point for acid and base resistance. Because lanthanum phosphate is insoluble in acidic and basic solution, the addition of lanthanum cation was tried to improve the acid and base resistance of cobalt phosphate pigment. The lanthanum doped cobalt phosphates were prepared from phosphoric acid, cobalt nitrate, and lanthanum nitrate solution. The additional effects of lanthanum cation were studied on the chemical composition, particle shape and size distribution, specific surface area, color, acid and base resistance of the precipitates, and their thermal products.     

Influence of co-catalyst on growth of carbon nanotubes using alcohol catalytic CVD method

This paper describes the influence of a co-catalyst on growth of carbon nanotubes (CNTs) by alcohol catalytic chemical vapour deposition (ACCVD) method. Silicon wafers covered with thermal oxide or polycrystalline diamond thin film were used as substrates. Ni thin film supported with Al, Cu or Ti was used as a catalyst. The films were deposited by pulsed laser deposition technique. Comparison of the various types of the co-catalyst (Al, Cu, Ti) leads to the conclusion that Cu co-catalyst is suitable for producing very thin single wall carbon nanotubes (SWCNTs) and combination of Al and Ni provide a good condition to the catalytic growth of CNTs. In addition, we observed also the influence of the various diffusion barriers (thermal oxide and polycrystalline diamond) on growth of CNTs. Prepared samples were analysed by Raman spectroscopy (RS) and scanning electron microscopy (SEM).     

A novel preparation method for porous noble metal/ceramic catalytic membranes

Adsorption at liquid/solid interface has been explored to prepare catalytically active ceramic membranes. Boehmite sol maintains its dynamic stability in the pH range of 3.5–4. Adsorption of metal salt on the sol particles can only be performed in the above pH range, but the adsorption can still be optimized by proper choice of ligand. Therefore, the effect of the ligands (NH₃, Cl^–, EDTA) on the adsorption of the noble metal ions (Pd(II), Pt(II), Pt(IV) and Rh(III)) as a function of pH on -Al₂O₃ particles was studied. Thus the noble metal complexes which can significantly adsorb in the above pH range were found. Using the complexes, the noble metal ion modified boehmite sols were synthesized. Then by the sol-gel process, the porous noble metal/ceramic cataytic membranes were prepared. The membranes were further characterized by N₂ adsorption-desorption, scanning electron microscopy (SEM), transmission electron microscopy (TEM) and SEM-WDX (wave dispersion of X-ray). The H₂ and N₂ permeation through these membranes at elevated temperatures was also measured. Based on the above experiments, the novel technique can produce the mesoporous catalytically active ceramic membranes without any defects and with a uniform dispersion of the active materials in the coating.     

Influence of the method of preparation on Yb2O3 hydration

Preliminary studies have shown that in order to achieve the complete removal of the uptaken CO₂ and H₂O from a ytterbium oxide aged in air, thermal activation up to 1173 K is required. Parallel studies have shown that bulk hydration of Yb₂O₃ does occur, the CO₂ acting as a kinetic inhibitor. The above results refer to a Yb₂O₃ prepared in our laboratory from hydroxicarbonate-like phases. In the present work, the influence of the preparation method on the hydration process is examined, by extending the study to two additional samples, a standard commercial one and another obtained by calcining a ytterbium oxalate. It is shown that the intensity of the hydration reaction depends strongly on the method of preparation. Certain applications of 4f oxides, such as their use as transition metal supports, involve thermochemical processes which may alter drastically the initial texture of the ytterbia from the oxalate. It makes this sample less useful although its initial specific surface area is high.     

溶胶-凝胶法制备ZnO薄膜及其性能研究

使用溶胶-凝胶法在P型Si(100)衬底上成功地制备了具有c轴择优取向性和高可见光透射率的多晶ZnO薄膜.通过XRD、SEM以及PL光谱等分析,表明:所制备的是结晶良好的ZnO薄膜,表面均匀致密,薄膜晶粒尺寸大约在15～60 nm,颗粒平均直径大约为38nm.由透射谱可知,制备的ZnO薄膜在可见光区域内薄膜的平均透射率在85%以上;由光致发光谱可知,室温下可观察到显著的紫外光发射,说明具有较好的光学性质.