碳酸铝铵热分解制备α-Al2O3超细粉

研究了以硫酸铝铵和碳酸氢铵为原料合成碳酸铝铵的工艺条件．在实验条件范围内，将硫酸铝铵溶液以低于1．2L．h－1的速度加入到碳酸氢铵溶液中，可合成碳酸铝铵；在其它操作条件下，获得的产物为γ－AlOOHγ－AlOOH升温过程中的物相变化次序为：γ－AlOOH→γ－Al2O3→δ－Al2O3→θ－Al2O3→α－Al2O3;而碳酸铝铵的相变次序为：碳酸铝铵→无定型Al2O3→θ－Al2O3→α－Al2O3碳酸铝铵转变为θ－Al2O3和α－Al2O3的温度均比γ－AlOOH低约100℃γ－AlOOH在1200℃煅烧1h方可完全转变为α－Al2O3，其颗粒尺寸为150um；粉体经1450℃、2h烧结相对密度为84.46％；而碳酸铝铵在1100℃煅烧1h就可完全转变为α-Al2O3，其颗粒尺寸为70um，粉体在相同的烧结条件下相对密度可达97.80％     

掺Er3+勃姆石(γ-AlOOH)凝胶高温烧结相变

采用溶胶-凝胶法(sol—gel)制备掺0-20mol％Er^3 勃姆石(γ-AlOOH)凝胶，X射线衍射和差热分析法研究掺Er^3 ：γ—AlOOH凝胶在950-1400℃烧结的相变过程．结果表明：Er^3 的掺杂降低α相的生长速度，抑制Al2O3的θ→α相变，推迟相变结束温度50-70℃，Er-Al-O系化合物Al10Er6O24和ErAlO3相的析出取决于掺Er^3 浓度和烧结温度．在较高烧结温度下，ErAlO3相由掺1-5mol％Er^3 ：Al2O3中析出；Al10Er6O24相则在掺5-20mol％Er^3 ：Al2O3中析出，随着烧结温度的升高，在全部掺Er^3 ：Al2O3中析出．ErAlO3相促进θ→α相变的形核，α相形核起始温度可提前30-50℃，但对α相生长影响不大．Al10Er6O24相对θ→α相变没有显著影响．     

Fe(OH)3凝胶两步法水热制备均分散针形铁红胶粒

本文以Fe（OH）3凝胶为初始物，研究了成核温度、pH值以及Sn4 离子对水热合成针形α－Fe2O3粒子形貌的影响．实验证明，一定浓度的Fe（OH）3凝胶先在50～80℃成核，而后加入晶体成长剂，并调节pH值后入釜在150～170℃，短时间可转化为均匀针形α－Fe2O3粒子．解决了实验结果重现性差这一关键问题．使用TEM及XRD对结果进行了表征．     

Al2O3和Y2O3包覆的SiC复合粒子制备

本文利用非均匀成核法,将Al（OH）3和Y（OH）3均匀地包匿在SiC粒子表面,制备出被覆Al2O3和Y2O3的SiC复合粒子．包覆Al（OH）3的SiC粒子,其等电点IEP的pH=3．4移至pH=7.3,再用Y（OH）3包覆表面被覆Al（OH）3的SiC复合粒子后,其等电点IEP又从pH=73移至pH=8.6左右．并且表面包覆的SiC粒子,其水悬浮液流变性质发生了变化．经盐酸滴定表明,涂层物质的包覆率可达95％以上．     

叶腊石及其粉末基本性质和工艺性能

叶腊石为晶体结构，属层状硅酸盐矿物，其晶体结构是每一结构单位层由上下二层（Si—O）四面体层中间夹一层（Al—O，OH）八面体层组成。结构式为Al2[Si4O10]（OH）2，实验式为Al2O3·4H2O，理论化学成分为Al2O3 28．3％，SiO2 66．7％，H2O 5．0％，自然界很少见到纯叶腊石，往往有各种杂质伴生。[第一段]     

水热法制备纳米级片状氧化铝

本文以Al2(SO4)3·18H2O和氨水为原料,采用水热法制得六角形片状的γ-Al2O3,研究了不同pH值对前驱体产物AlOOH形貌的影响,并采用XRD、SEM、TG-DSC等分析手段对所得产物的物相、形貌以及晶相转变过程进行了表征。结果表明,pH值对产物的形貌起决定性的作用,所制得的片状γ-AlOOH前驱物的粒径为50~150nm、厚度为10~20nm。将片状γ-AlOOH前驱物在600℃下焙烧4h,可得到保持原有六角形状、且尺寸基本一致的片状γ-Al2O3。     

基于第一性原理研究H2O分子在双相TiAl合金表面的吸附行为

为研究电场作用对H2O分子在γ-TiAl和α2-Ti3Al表面的吸附行为影响,采用第一性原理方法对H2O分子在γ-TiAl（111）和α2-Ti3Al（0001）表面不同吸附位置的吸附能、态密度、几何结构、电荷布局进行分析。结果发现,H2O分子在γ-TiAl（111）和α2-Ti3Al（0001）表面上的top Ti位置吸附最为稳定,但电场更容易促进H2O分子与α2-Ti3Al（0001）表面的相互作用,即α2-Ti3Al更易与H2O分子发生反应,从而优先形成Ti的致密氧化膜,致使α2-Ti3Al被保护。探究γ-TiAl和α2-Ti3Al单相具有相同溶解速度的条件,对提升双相（γ-TiAl和α2-Ti3Al相）TiAl合金电解加工表面质量具有十分重要的意义。     

多孔γ-Al2O3过渡膜的结构与性能研究

采用溶胶－凝胶技术，在多孔Al2O3载体上制备了一层适合于涂覆分离膜的γ-Al2O3多孔过渡膜。通过XRD与DTA－TG等测试手段研究了γ-Al2O3凝胶膜在热处理过程中的物理化学变化；通过TEM、SEM分析与泡点法研究了多孔膜的微观结构。实验结果表明：实验中制备的γ-Al2O3膜具有择优取向的特点；γ-Al2O3过渡膜的最可几孔径为0．38μm左右，厚度为4μm，薄膜的渗透性能测试结果表明，材料对H2与N2气的最大分离系数α＝3．30。     

pH对水合Al2O3纳米流体的稳定性和导热性的影响

利用两步法制备了Al2O3水合纳米流体，测试了不同pH值下，不同体积分数的～203纳米流体的zeta电位和导热系数，研究pH值对Al2O3．H20纳米流体稳定性和导热性的影响，实验结果表明：对不同体积分数的Al2O3纳米流体，pH存在一个优化值对应zeta电位的绝对值最大，而电位的绝对值越大，纳米颗粒在流体中分散稳定性越好，因此对Al2O3纳米颗粒来说，要得到稳定分散的纳米流体pH值应在8～9之间为最佳；同样随着pH的变化，也存在一个最优值对应于Al2O3纳米流体的导热系数增加到一个最大的值，并且导热系数随纳米粒子体积分数增加而增大。实验结果表明纳米流体的稳定性和导热性与pH有密切的关系，此结论与文献[6]和[13]中的结论一致。     

Sol-gel法合成纳米羟基磷灰石的热力学分析

对水溶液中合成羟基磷灰石时的Ca-P2O5-H2O系和Ca(OH)2-H3PO4-H2O系进行了热力学分析,绘出了磷酸及各磷酸根离子分布系数与pH值的关系图和Ig[Ca]T同pH值的关系图,并得出了合成纳米HAP的合适条件.     

Magnetic coupling in La0.67Ca0.33MnO3/La0.67Sr0.33CoO3/La0.67Ca0.33MnO3 sandwiches

La_0.67Ca_0.33MnO₃ (LCMO)/La_0.67Sr_0.33CoO₃ (LSCO)/LCMO trilayer films are fabricated on single-crystal substrates NdGaO₃ (110) and the interlayer coupling are investigated. Compared with LCMO single layer, sandwiches showed the enhanced metal-insulator transition temperature of LCMO layers. The magnetoresistance is dependent on spacer thickness and the peak value dramatically decreases when LSCO layer is thick enough because of shorting by the LSCO layer. The magnetic coercivity H_C shows a nonmonotonic behavior with changing spacer layer thickness and the waist-like hysteresis indicates that there is an indirect exchange coupling between the top and bottom LCMO layers across the spacer layer.     

Varistor properties of ZnO-Pr6O11-CoO-Cr2O3-Y2O3-In2O3 ceramics

The varistor properties of the ZnO-Pr₆O₁₁-CoO-Cr₂O₃-Y₂O₃-In₂O₃ ceramics were investigated for different concentrations of In₂O₃. The increase of In₂O₃ concentration slightly increased the sintered density (5.60-5.63 g/cm³) and slightly decreased the average grain size (3.4-2.9 μm). The breakdown field increased from 6023 to 14822 V/cm with increasing concentration of In₂O₃. The nonlinear coefficient increased from 17.6 to 44.6 for up to 0.005 mol%, whereas the further doping caused it to decrease to 36.8. In₂O₃ acted as an acceptor due to the donor concentration, which decreases in the range of 1.02 × 10¹⁷ to 0.24 × 10¹⁷/cm³ with increasing concentration of In₂O₃.     

Microstructures of YBa2Cu3O7/La0.7Ca0.3MnO3 and La0.7Ca0.3MnO3/YBa2Cu3O7 bi-layers grown on (001)LaAlO3

Epitaxial YBa₂Cu₃O₇/La_0.7Ca_0.3MnO₃ (YBCO/LCMO) bi-layers and La_0.7Ca_0.3MnO₃/YBa₂Cu₃O₇ (LCMO/YBCO) bi-layers were grown on (001)LaAlO₃ by pulsed laser deposition, and their microstructures were compared by transmission electron microscopy investigation. In the YBCO(100 nm)/LCMO(150 nm) bi-layers, the LCMO layer consists of columnar grains of ~ 17 nm in diameter and contains mixed orientation domains of [100]_c, [010]_c and [001]_c. The YBCO layer is totally c-axis oriented and the YBCO lattices are tilted − 2.5° to + 2.5° as they grew on the rough surfaces of LCMO columnar grains. For the LCMO(140 nm)/YBCO(140 nm) bi-layers, the LCMO/YBCO interface is sharp and flat. The initial 12-nm thickness of the YBCO layer is composed of c-axis oriented domains, and the upper part of YBCO layer is [100] oriented. The LCMO layer was predominantly [001]_c oriented while [100]_c-oriented domains were occasionally observed.     

Nanocrystallization of SrBi2Nb2O9 from glasses in the system Li2B4O7---SrO---Bi2O3---Nb2O5

Transparent glasses in the system (100−x)Li₂B₄O₇–x(SrO---Bi₂O₃---Nb₂O₅) (10≤x≤60) (in molar ratio) were fabricated by a conventional melt-quenching technique. Amorphous and glassy characteristics of the as-quenched samples were established via X-ray powder diffraction (XRD) and differential thermal analyses (DTA) respectively. Glass–ceramics embedded with strontium bismuth niobate, SrBi₂Nb₂O₉ (SBN) nanocrystals were produced by heat-treating the as-quenched glasses at temperatures higher than 500 °C. Perovskite SBN phase formation through an intermediate fluorite phase in the glass matrix was confirmed by XRD and transmission electron microscopy (TEM). Infrared and Raman spectroscopic studies corroborate the observation of fluorite phase formation. The dielectric constant (_r) and the loss factor (D) for the lithium borate, Li₂B₄O₇ (LBO) glass comprising randomly oriented SBN nanocrystals were determined and compared with those predicted based on the various dielectric mixture rule formalism. The dielectric constant was found to increase with increasing SBN content in LBO glass matrix.     

Syntheses of hollandite type Rb2Cr8O16, K2Cr2V6O16 and K2V8O16

Hollandite-type compounds, Rb₂Cr₈O₁₆, K₂Cr₂V₆O₁₆ and K₂V₈O₁₆, were synthesized under high P-T conditions up to 1200°C and 7GPa. The structural refinement using a single crystal of Rb₂Cr₈O₁₆ confirms that the structure is similar to that of K₂Cr₈O₁₆. Magnetic measurements indicate that Rb₂Cr₈O₁₆ is ferromagnetic below 295K, K₂Cr₂V₆O₁₆ paramagnetic down to 77K and K₂V₈O₁₆ has susceptibility anomaly at 175K. These compounds are all semiconductive and show discontinuities in temperature-resistivity curves at points corresponding to magnetic anomalies.     

PbSbBiS4-Sb2S3 and PbSbBiS4-Bi2S3 joins in the PbS-Sb2S3-Bi2S3 system

Phase equilibria along the PbSbBiS₄-Sb₂S₃ and PbSbBiS₄-Bi₂S₃ joins of the PbS-Sb₂S₃-Bi₂S₃ system have been studied for the first time using differential thermal analysis, X-ray diffraction, microstructural analysis, microhardness tests, and density measurements, and the phase diagrams of the joins have been mapped out. The joins are shown to be pseudobinary with limited series of terminal solid solutions. The solid solutions are p-type semiconductors.     

Structural study of Sr0.3Ba0.7Nb2O6 and La0.030Sr0.255Ba0.700Nb2O6 ceramic systems

Sr_0.3Ba_0.7Nb₂O₆ (SBN) and La_0.030Sr_0.255Ba_0.700Nb₂O₆ (LSBN) ceramic compounds have been prepared using the traditional ceramic method at two different calcination temperatures (900 and 1000 °C) and later sintered both at 1400 °C. A study of the effects of the calcination temperatures and La substitution on the morphological, compositional, and structural properties of SBN and LSBN is presented using scanning electronic microscopy (SEM), energy dispersive spectroscopy (EDS), and X-ray diffraction (XRD) analysis. From Rietveld refinement processes, the XRD patterns were interpreted to evaluate such effects in the structural parameters and the site occupation factors of the heavy metals and oxygen atoms. The effect of the incorporation of La resulted in a 0.25% cell contraction and turned out to be higher than the 0.08% dilation effect produced by the increase of calcination temperature. The La ion with similar effective ionic radius and higher electronegativity is incorporated into the structure occupying the A₁ site just like the Sr ions in the SBN compound. Differences in the site occupation factors between the SBN and LSBN samples lead to substantial changes in the physical properties such as temperature of relative dielectric constant maximum, relative dielectric constant, and dielectric loss, correlated with the distortion and the relative orientation of the oxygen octahedra.     

Vapour-liquid equilibria in the ternary mixtures N2---CH4---C2H6 and N2---C2H6---C3H8

A systematic study was performed with mixtures consisting of N₂, CH₄, C₂H₆ and C₃H₈, to investigate experimentally phase equilibria and caloric properties and to test the accuracy of thermodynamic correlations. The first part of this Paper reports results of T---p---x---y measurements on ternary systems in the range 20 < p < 120 bar and 140 < T < 220 K. The results are compared with data calculated by generalized equations of state.     

The effect of Bi1.5Zn0.5Nb0.5Ti1.5O7 cover layer on the dielectric and tunable properties of Ba0.6Sr0.4TiO3/Bi1.5Zn0.5Nb0.5Ti1.5O7 bilayered thin films

Bi_1.5Zn_0.5Nb_0.5Ti_1.5O₇ (BZNT) thin films with different thicknesses as cover layers were deposited on the Ba_0.6Sr_0.4TiO₃ (BST) thin films on the Pt/Ti/SiO₂/Si substrates by radio frequency magnetron sputtering method. The microstructure, surface morphology, dielectric and tunable properties of BST/BZNT heterogeneous bilayered films were investigated as a function of the thickness of BZNT films and the effect of BZNT films on the asymmetric electrical properties of BST/BZNT bilayered films was discussed. It was found that BZNT cover layer significantly improved the leakage current and the dielectric loss, and the dielectric constant and tunability of BST/BZNT bilayered thin films simultaneously decreased with the increasing thickness of BZNT films. The BST/BZNT bilayered thin film with a 50 nm BZNT cover layer gave the largest figure of merit (FOM) of 33.48 with the upper tunability of 55.38%. The asymmetric electrical behavior of BST/BZNT bilayered films is probably related to an internal electric field caused by built-in voltages at Pt/BST and BZNT/Au interfaces.     

静电纺丝法制备的Co0.6Ni0.3Cu0.1Fe2O4和Co0.6Ni0.3Zn0.1Fe2O4纳米纤维的结构及磁性能

采用静电纺丝技术制备出表面光滑、直径均匀的Co_(0.6)Ni_(0.3)Cu_(0.1)Fe_2O_4/PVP和Co_(0.6)Ni_(0.3)Zn_(0.1)Fe_2O_4/PVP纳米纤维前驱丝,经500~900℃煅烧后得到Co_(0.6)Ni_(0.3)Cu_(0.1)Fe_2O_4和Co_(0.6)Ni_(0.3)Zn_(0.1)Fe_2O_4纳米纤维。用TG-DSC、XRD、SEM及VSM现代测试分析手段对Co_(0.6)Ni_(0.3)Cu_(0.1)Fe_2O_4和Co_(0.6)Ni_(0.3)Zn_(0.1)Fe_2O_4纳米纤维的结构、形貌及磁学性能进行测试表征。结果表明:在空气气氛中经500~900℃煅烧后可得到纯尖晶石相、结晶度良好的纳米纤维或短纤维;当温度为700℃时,Co_(0.6)Ni_(0.3)Cu_(0.1)Fe_2O_4和Co_(0.6)Ni_(0.3)Zn_(0.1)Fe_2O_4纳米纤维的形貌细长而光滑且直径相对均匀,大约为80nm;此时Co_(0.6)Ni_(0.3)Cu_(0.1)Fe_2O_4纳米纤维则保有较高的剩磁比(M_r/M_s)及矫顽力,分别为0.56和1 088.87Oe。在500℃、600℃、700℃、800℃、900℃煅烧后,Co_(0.6)Ni_(0.3)Zn_(0.1)Fe_2O_4纳米纤维的饱和磁化强度分别比Co_(0.6)Ni_(0.3)Cu_(0.1)Fe_2O_4纳米纤维增大了14.5%、7%、16%、10.7%、8%,而矫顽力则分别降低了38%、51%、50%、46%、46.7%。两种纳米纤维的饱和磁化强度及矫顽力存在差异,为CoNi铁氧体在电磁方面的应用提供了很好的参考。