固相反应法制备Nd:YAG透明陶瓷

以Y(NO3)3和NH3·H2O为原料,并在Y(NO3)3溶液中添加少量(NH4)2SO4,采用沉淀法制备出化学组成为Y2(OH)5(NO3)·nH2O的先驱沉淀物.先驱沉淀物在1100℃下煅烧4h,得到了平均粒径为60nm的氧化钇原料粉体.Y2O3粉体与Al2O3、Nd2O3超细粉球磨混合后,采用固相反应工艺,经1700℃真空烧结5h,制备出透明的NdYAG陶瓷,同时对NdYAG透明陶瓷的光学性能进行了研究.     

共沉淀法制备YAG超细粉及透明陶瓷

研究了共沉淀法制备YAG透明陶瓷的工艺。采用Al(NO3)3和Y(NO3)3的混合溶液为母盐,以碳酸氢铵为沉淀剂,采用共沉淀法制备了化学组成为Y2(CO3)3·nH2O+NH4AlO(OH)HCO3的碳酸盐先驱沉淀物。使用透射电镜和X射线衍射对先驱沉淀物的形貌及煅烧过程的相转变进行了研究。结果表明先驱沉淀物在900℃煅烧2h后完全转变为YAG相。1100℃煅烧后得到的YAG粉体具有良好的烧结性能。使用0.5%(质量分数)的TEOS(正硅酸乙酯)作为烧结添加剂,1700℃真空烧结5h后,得到了透明YAG烧结体。     

硫酸盐共沉淀法制备YAG粉体及透明陶瓷

以自制Y2(SO4)3和NH4Al(SO4)2·12H2O混合溶液为母盐,碳酸氢铵为沉淀剂,采用共沉淀法制备了以YAG相为主要成分的混合粉体.研究表明,先驱体化学成分为[NH4AlO(OH)HCO3]·0.3[Y2(CO3)3·2H2O].先驱体经1200℃、2h煅烧,pH=7.2时产物以YAG相为混合粉体的主要成分,pH=8.5时Y2O3为主要成分.在较低温度下(低于1500℃),以硫酸盐为母盐制备的YAG混合粉体烧结性低于同样条件下硝酸盐为母盐合成的粉体烧结性.1100℃煅烧2h后合成的YAG混合粉体(pH=7.2),经1700℃真空烧结5h,获得了完全透明的YAG陶瓷,可见光区的最大透光率约为60%.     

溶胶-凝胶法制备纳米Y2O3粉体

为了改善Y2O3粉体的分散性,提高其烧结活性,试验以三乙醇胺和氨水为凝胶剂,利用溶胶-凝胶方法合成了纳米级Y2O3粉体,采用差热/热重、X射线衍射、透射电镜研究了前驱体的组成、前驱体在不同的煅烧温度下的物相变化以及煅烧粉体的分散性.结果表明,前驱体的组成为Y2(OH)5.14(NO3)0.86H2O,在500℃保温2h可直接生成立方相的Y2O3,煅烧至1000℃保温2h得到了结晶度高、分散性好、平均粒径为50nm、近球形的YO纳米粉体;三乙醇胺的加入有利于提高YO粉体的分散性.     

不同酸化条件下水热合成V2O5粉末的结构和电化学性能

为了研究酸化条件对V2O5粉末结构和电化学性能的影响,利用HNO3和H2C2O4酸化NH4VO3溶液,经水热和后续热处理制备了V2O5粉体。利用X射线衍射仪(XRD)、扫描电子显微镜(SEM)、透射电子显微镜(TEM)和电化学工作站等对V2O5粉体的微观结构与电化学性能进行了测试。结果表明,所得粉体为纯V2O5相,前驱体溶液的pH值和酸化所用酸的酸根阴离子影响了最终粉体的晶体发育和微观结构。其中,利用HNO3酸化NH4VO3溶液至pH值=3制得的粉体为直径约100nm的纳米棒,在0.5和1C的放电速率下循环30次后,放电比容量仍有150mAh/g左右,且大电流放电性能更好。     

陈化时间对Nd:YAG纳米粉体制备及性能的影响

以NH4Al(SO4)2·12H2O,Y(NO3)3·5H2O,Nd(NO3)3·5H2O为原料,碳酸氢铵为沉淀剂,研究了共沉淀法制备Nd:YAG纳米粉体过程中陈化时间对粉体性能的影响.采用pH计,FT-IR,XRD和TEM测试手段对其进行表征.陈化过程中PH值先减小后增大,XRD曲线显示共沉淀法中不同陈化时间都能得到纯相粉体,而24h所得粉体最好,粉体TEM图谱表明陈化24h所得到的粉体粒径更小,分散性较其他粉体更好.结果表明:共沉淀法制备Nd:YAG纳米粉体过程中陈化时间不影响纯相粉体的制得,但对粉体粒径大小及分布和团聚程度有直接的影响.陈化24h的粉体颗粒最小并且均匀,团聚很少.     

均相沉淀法制备掺钕钇铝石榴石(Nd∶YAG)纳米粉末

采用均相沉淀法,以Al(NO3)3.9H2O、Y2O3、Nd2O3、(NH4)2SO4和NH4HCO3为原料,正硅酸乙酯为添加剂,制备Nd∶YAG纳米粉末;并探讨了均相沉淀法制备Nd∶YAG纳米粉末的反应机理。研究结果表明,粉体在800℃时为无定型态,当温度达到900℃时析出大量YAlO3(YAP)和少量Y3Al5O12(YAG)晶体,当温度达到1000℃时就全部转化为YAG立方晶相;混合溶液生成沉淀物是由Al 3+的沉淀所决定的;Al 3+首先均相成核,随后Y3+和Nd3+以Al沉淀物为异相核发生异相成核,形成的沉淀物覆着于Al沉淀物表面,推测沉淀物结构可能为钇包覆铝的核壳结构。     

直接沉淀法合成Sc2O3纳米粉

研究了直接沉淀法合成Sc2O3纳米粉的工艺。以硝酸钪[Sc(NO3)3]为母盐,氨水(NH3.H2O)作沉淀剂,采用直接沉淀法合成出网状的前躯沉淀物,同时分析了前驱体的热分解过程。通过X射线衍射和红外光谱对前躯体的物相组成进行了定性分析,结果表明,该前躯沉淀物为γ-ScOOH.nH2O与NH4Sc3(SO4)2(OH)6.nH2O的两相混合物。前躯体经过微化处理后,在1 000℃的温度下煅烧,生成的Sc2O3纳米粉具有纯度较高、颗粒粒度小(40 nm)、粒度分布窄、近似球形Sc2O3的性能,但是粉体产生了轻微团聚的现象。     

微波烧结Al2O3/SiC纳米复合陶瓷的研究

以分析纯Al(NO3)3.9H2O·NH3.H2O和50 nm的SiC粉体为原料,采用溶胶-凝胶法制备干凝胶,经热处理合成Al2O3/SiC纳米复合粉体。利用微波烧结制备Al2O3/SiC纳米复合陶瓷,并与常规烧结比较,分析了两种烧结方法对制备试样的力学性能影响。结果表明,与常规烧结相比,微波烧结可以提高Al2O3/SiC纳米复合陶瓷的强度和韧性,改善材料的显微结构,促进致密化和晶粒生长。     

不添加烧结助剂制备透明的Y2O3陶瓷

以Y2O3粗粉、碳酸氢铵、硝酸和氨水为原料,通过沉淀法制备了Y2O3纳米粉体.发现沉淀工艺和煅烧温度显著影响Y2O3纳米粉的颗粒大小和尺寸分布,从而影响烧结体的密度和透光性.用X射线衍射分析仪、透射电镜、图像分析仪等研究发现,pH=8时制得的沉淀先驱物经1000℃煅烧,可得到粒度为33 nm,近球形,分散性好,尺寸分布窄的Y2O3粉体.该粉体不加任何添加剂,在1700℃真空烧结4 h可得到透明Y2O3陶瓷.     

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.     

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.     

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.     

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.     

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.     

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.     

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.     

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。     

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.