Low-temperature synthesis of nano-sized metal molybdate powders

Nanocrystalline metal molybdate [i.e., AMoO₄ where A=Ca(II), Co(II),Cu(II), Ni(II), and Zn(II)] powders have been prepared from the complete evaporation of a polymer-based metal-complex precursor solution. The precursor solution was constituted of the metal ions that were in aqueous solution through complexation with ethylene diamine tetraacetic acid (EDTA) in the presence of diethanolamine (DEA), and a polymeric reagent, which was an aqueous solution mixture of sucrose and polyvinyl alcohol (PVA). Complete dehydration of the precursor solution generated a voluminous mesoporous carbon-rich precursor mass, heat treatment (at temperatures ≤500°C) of which resulted in the respective metal molybdate phase. The average diameter of the particles from transmission electron microscopy and X-ray diffraction studies ranged between 15 and 40 nm.     

Hydrothermal synthesis of nanoplates assembled hierarchical h-WO3 microspheres and phase evolution in preparing cubic Zr(Y)O2-doped tungsten powders

Three-dimensional hierarchical h-WO₃ and doping tungsten powders have recently attracted considerable attention because of their superior sensing properties and refined grains, respectively. In this article, we report a facile hydrothermal hydrogen reduction process for preparing hierarchical h-WO₃ microspheres that self-assemble with nanoplates. Meanwhile, the phase evolution process and evolution mechanisms during the conversion of h-WO₃ to W are systemically investigated. Results indicate that the highly homogeneous h-WO₃ microspheres are uniformly covered with ultrafine ZrY₂(OH)₁₀ micelles, which fully transform into m-WO₃ and cubic Zr(Y)O₂ after calcination at 600?°C. Microspheres possessing different pore diameters and containing nanosized particles can be obtained by adjusting the hydrogen reduction process. These phase evolution process can provide reasonable guidance for preparing tungsten oxide with high electrochemical properties and ultrafine tungsten powders. The h-WO₃ microspheres with an average size of 3?μm consist of nanoplates and the tungsten powders doped with 1.0?wt% Zr(Y)O₂ have a mean particle size of approximately 1.4?μm. Comparative test results indicate that the addition of 1.0?wt% Zr(Y)O₂ can promote the formation of low-degree particle agglomerates.     

Hydrothermal synthesis of chromium dioxide powders and their characterisation

Chromium dioxide (CrO₂) powders have been synthesised by decomposing CrO₃ and Cr₂O₅ powders under hydrothermal conditions in the temperature range of 300–500°C and pressure range of 250–1200 bars. Oxides of antimony and iron have been used as modifiers to induce acicular morphology. A novel method of using alkali metal salts such as chlorides and carbonates as mineralisers produces CrO₂ with superior magnetic characteristics. The particle size distributions have been correlated with the magnetic properties of the materials. The products obtained have properties rendering them useful for magnetic recording applications.     

Hydrothermal synthesis of surface-modified iron oxide nanoparticles

We synthesized surface-modified iron oxide nanoparticles in aqueous phase by heating an aqueous solution of iron sulfate (FeSO₄) at 473 K with a small amount of either n-decanoic acid (C₉H₁₉COOH) or n-decylamine (C₁₀H₂₁NH₂), which is not miscible with water at room temperature. Transmission electron microscopy showed that the addition of n-decanoic acid or decylamine changed the shape of the obtained nanoparticles. X-ray diffraction spectra revealed that the synthesized nanoparticles were in α-Fe₂O₃ or Fe₃O₄ phase while Fourier transform infrared spectroscopy and thermogravimetry indicated the existence of an organic layer on the surface of the nanoparticles. In the synthetic condition, decreased dielectric constant of water at higher temperature increased the solubility of n-decanoic acid or n-decylamine in water to promote the reaction between the surface of iron oxide nanoparticles and the organic reagents. After the synthesis, the used organic modifiers separated from the aqueous phase at room temperature, which may help the environmentally benign synthesis of surface-modified metal oxide nanoparticles.     

Hydrothermal synthesis of oriented MnS nanorods on anodized aluminum oxide template

High-density aligned MnS nanorods with a narrow length distribution were prepared on an anodized aluminum oxide (AAO) template under a hydrothermal condition. MnS nanomaterials with different shapes were obtained using different precursor concentrations in the reaction solution. The porous surface of the AAO template and the precursor concentrations may play key roles in the initial nucleation stage of growing oriented MnS nanorods.     

纳米粉体制备8YSZ电解质工艺性能研究

实验研究了纳米粉体制备8YSZ电解质的固相烧结过程。根据阿基米德原理测瓷体密度；通过测定烧结前后瓷片尺寸，求出烧结线收缩；采用四端电极法测瓷体的电导率；使用扫描电子显微镜(SEM)观测样品微观形貌，并探讨了YSZ纳米粉体烧结的动力学过程。由于纳米颗粒尺寸较细、粒度分布均匀、无硬团聚和很好的球形度，使得烧结温度大幅度降低。实验表明，最佳烧结温度为1450℃，此时材料致密，相对密度在97％以上；气孔含量少、晶粒均匀，电导率高，1000℃时为0．162Ω^-1cm^-1，是理想的高温电解质材料。     

Hydrothermal synthesis of transition metal oxide nanomaterials in HEPES buffer solution

Various transition metal oxide (Co₃O₄, Mn₃O₄ and ZnO) nanostructures were readily synthesized in HEPES buffer solution (200 mmol/L, pH 7.40) via a simple hydrothermal method. The products were characterized by powder X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), selected area electron diffraction (SAED) and energy dispersive X-ray spectroscopy (EDX). It was found that the morphologies of the as-obtained transition metal oxide nanostructures were affected by the reaction temperature, HEPES/metal salt molar ratio and metal precursor. HEPES with two free nitrogen atoms (piperazine group) and terminal hydroxyl groups plays a critical role as a reactant and surfactant to prevent the transition metal oxide nanomaterials from aggregation.     

水热法制备ZST微波陶瓷粉体

采用水热法制备了(Zr0.8Sn0.2)TiO4粉体,并借助于XRD、SEM、热分析等手段对反应后的结晶粉末进行了表征.实验结果表明,粉末性能受反应溶液pH值的影响显著.随着pH值的增大,晶粒的生长更加充分,完整.反应后的晶粒粒度为纳米尺度,表面活性大,有利于烧结.烧结温度在1260-1320℃之间,比传统固相法制备的ZST陶瓷烧结温度降低了300多度.     

The flowability of fine powders in reduced gravity conditions

The extrapolation of Qian’s semi-theoretical relationship for the transition between cohesive and non-cohesive powder fluidization behavior into regions of low gravity is studied and a validation experiment employing fluidization is discussed. The fluidization experiment utilized fine glass and alumina powders in a fluidized bed and was flown onboard NASA’s reduced gravity aircraft. The transition region between cohesive and non-cohesive behavior is determined for the glass and alumina powders at gravity levels of 1.8, 1.0, 0.38, and 0.16 g. The results are compared to Qian’s model and show fair agreement. The fluidization experiment limitations are discussed and a rotating drum experiment that will reduce the experiment uncertainty, provide quantifiable results, and is suitable for flight onboard NASA’s reduced gravity aircraft is proposed. The rotating drum technique determines the characteristic frequency of the powder’s center of area to detect avalanching. The concept is validated by comparing the characteristic frequency obtained from analyzing a cohesive powder to the characteristic frequency obtained from analyzing a flowable powder.     

Hydrothermal synthesis of titanate nanowire arrays

A simple templateless synthesis strategy for titanate nanowire arrays was developed by employing hydrothermal reactions. Hydrothermal treatment of metallic titanium powder with H₂O₂ in a 10 M NaOH solution produced a new sodium titanate compound, Na₂Ti₆O₁₃·xH₂O (x ∼ 4.2), as arrays of nanowires of lengths up to 1 mm. The nanowires were characterized by using XRD, SEM, TGA, and TEM. The nanowires have exceptionally large aspect ratios of 5000 or higher, and they can form arrays over a large area of 2 × 3 cm². Investigations on the reaction products in varied conditions indicate that the array formation requires simultaneously controlled formation and crystal growth rates of the Na₂Ti₆O₁₃·xH₂O phase.     

Hydrothermal synthesis of fine perovskite PbTiO3 powders with a simple mode of size distribution

Perovskite phase PbTiO₃ powders were hydrothermally synthesized so as to be fine and homogeneous in physico-chemical properties. Such powders are currently used in the fabrication of electronic ceramic components. The powders were successfully synthesized using a strong alkali as catalyst. Borderline synthesizing conditions, such as temperature and time, were established and their effects on geometrical properties, like mean particle size were determined. Polyacrylamide as an additive was found to be effective for the synthesis of the powders with a simple mode of particle-size distribution.     

Hydrothermal growth of zirconia nanobars on zirconium oxide

Zirconia nanorods and nanoparticles were grown hydrothermally starting from zirconium monoxide powder. The process was performed in an autoclave using NaOH as a mineralizer at nominal concentrations 15 M, 20 M and 25 M, and at a temperature of 200 °C for 1 week. The samples were characterized by high resolution transmission electron microscopy, showing that the nanorod diameter spanned from 25 to 200 nm and their length from a few hundred nm up to 2 μm. X-ray photoelectron spectrometry showed that after the treatment all the material was zirconium (IV) oxide, as confirmed by X-ray diffraction and selected area electron diffraction. The latter showed that the nanobars were in the monoclinic phase and the nanopowders in the tetragonal one.     

Hydrothermal synthesis of highly pure brookite-type titanium oxide powder from aqueous sols of titanate nanosheets

Hydrothermal synthesis of brookite-type titanium dioxide was examined using aqueous sols of titanate nanosheets, which were prepared with Ti[OCH(CH₃)₂]₄ and N(CH₃)₄OH by a bottom-up process in aqueous solutions. Highly pure brookite powders were yielded at hydrothermal temperatures as low as 120 °C and N(CH₃)₄OH/Ti[OCH(CH₃)₂]₄ molar ratios greater than 2. Although titanate nanosheets are formed at N(CH₃)₄OH/Ti[OCH(CH₃)₂]₄ ≥ 0.4, the addition of excess N(CH₃)₄OH was critical in forming highly pure brookite powders. Excess N(CH₃)₄⁺ caused the precipitation of layered titanates, which were formed by stacking titanate nanosheets. Additionally, the crystal nucleation of brookite occurred in the precipitates. Then, the adsorption of titanate nanosheets on brookite particles caused the particles to transform into rod-like shapes elongated along the c-axis. The adsorbed titanate nanosheets were structurally converted into brookite under the influence of the underlying brookite crystal. Despite having a rough surface, the resulting brookite particles were single crystal-like. Moreover, the use of any tetraalkylammonium hydroxides other than N(CH₃)₄OH did not yield brookite. The addition of N(CH₃)₄OH to the reaction sols yielded precipitates of small titanate nanosheets. The morphology of the titanate nanosheets could have a significant influence on brookite crystallization.     

Hydrothermal synthesis of fibrous lead titanate powders

A fibrous lead titanate (PbTiO₃) powder with light-yellow colour has been prepared by hydrothermal synthesis. The influences of Pb/Ti ratio (0.3 to 1.0) in the mixture and reaction time on the formation of fibrous PbTiO₃ under hydrothermal conditions have been investigated. The preferable conditions for preparing fibrous perovskite-type PbTiO₃ from fibrous potassium titanate are that the Pb/Ti ratio is 1.0, reaction temperature 150 °C and time 72 h. The particles of fibrous powder of perovskite type are usually less than 2 m in diameter and more than 50 m in length. The fibrous morphology is essentially unchanged up to about 650 °C, but it disappeared after heating to 1000 °C.     

水热法合成PZT粉体的研究

以硝酸铅、氧氯化锆、钛酸四丁酯为反应物前躯体,氢氧化钾为矿化剂,采用水热法合成PZT粉体.系统研究了反应温度、反应时间、矿化剂浓度和引入表面活性剂聚乙烯醇(PVA)对PZT晶体生长的影响.通过XRD和SEM对粉体进行了表征,探索出制备PZT粉体的最佳条件,研究结果表明:在KOH浓度为2 mol/L、180℃反应12 h的条件下可制备得到粒径约为1μm,粒径均匀,晶体发育完整的钙钛矿结构的PZT粉体;在该反应体系中加入适量PVA时得到了棒状纤维结构的粉体.     

葡萄糖基炭微球的制备与结构表征

以葡萄糖为碳源制备炭微球,考察了原料浓度、反应时间和反应温度对所得炭微球形貌和产率的影响,并测定了其表面官能团的种类和数量。结果表明,葡萄糖浓度为0．5mol／L、反应温度为180℃、反应时间为7h的条件下制备了粒径300nm左右、分数性较好的炭微球。所得炭微球表面合有丰富的羟基、羰基、羧基等含氧官能团,采用联碱中和法定量测定了上述官能团的含量。     

超细氧化铝粉体的表面改性研究

利用两种硅烷偶联剂、三种钛酸酯偶联剂对Al2O3粉体颗粒表面有机改性,比较了不同偶联剂对颗粒表面的改性效果,结果表明硅烷偶联剂未能对粉体表面进行有效的有机改性.红外光谱分析证实了偶联剂NTC401在Al2O3粉体表面进行了化学吸附,而偶联剂JSC和CT136在Al2O3粉体表面主要发生物理吸附.电镜照片说明,经NTC401改性的Al2O3粉体粒子之间的团聚得到了有效改善,而经JSC和CT136改性的Al2O3粉体粒子之间的团聚未得到改善.机理分析认为中心钛原子六配位的结构能够有效阻止颗粒团聚.     

SiC超细粉制备机理研究

以蒸馏水为研磨介质,采用行星式球磨机对平均粒径约为10μm的SiC粉料进行了球磨,对球磨粉料进行酸洗除铁及水洗,制备出平均粒径为351.5nm的SiC超细粉料,详细分析了粉料制备过程中的物理化学变化与机理.结果发现:粗分散体系长时间球磨所得超细粉体溶液形成胶体分散系,体系固相含量增加,颗粒平均最小间距减小,颗粒间的范氏引力倍增,易形成团聚体;超细粉料胶体溶液在酸洗过程中产生了硬团聚,主要是由于Fe2+氧化水化成为Fe(OH)3胶桥,将超细粉料钳住所致;另外,测试溶液接近SiC等电点时亦会导致颗粒团聚.酸洗去除胶桥、调解溶液pH值可有效消除团聚.     

BaMoO4粉体的水热法制备及发光性能研究

利用水热法制备出了不同形貌的白钨矿结构的BaMoO4粉体材料,样品的结构、形貌及光致发光性能利用XRD、Raman、FESEM和PL谱进行了表征,探讨了工艺参数对BaMoO4材料形貌的影响。通过调整反应温度、反应pH值和表面活性剂CTAB浓度可以调控BaMoO4材料的形貌,得到了棱锥状、多面体及树枝状等形貌的BaMoO4材料。BaMoO4样品的室温光致发光谱是由发光中心在约540nm处的单一绿光组成,样品的形貌不同发光强度不同。