羟基磷灰石粉体的低温无压烧结行为

用热膨胀仪、X射线衍射仪和扫描电镜对沉淀法所制的羟基磷灰石(HA)粉体和其陶瓷坯体的烧结行为进行了研究。结果表明,球磨处理和粉体煅烧温度对HA坯体的烧结行为均有明显影响。球磨处理能减少粉体团聚,经球磨处理后,不同煅烧温度下的粉体粒径均小于100 nm,坯体在1050℃时收缩达到最大值,比未球磨处理时约低100℃。在相同烧结条件下,700℃、750℃和800℃煅烧粉体所得坯体最大收缩率分别为18%、21%和16.8%,最大收缩率对应温度分别为990℃、950℃和1000℃。750℃煅烧后的粉体的烧结性能最好,其坯体在1050℃无压烧结可得到相对密度98%的HA材料。     

溶胶-凝胶法制备Al2O3粉体及其陶瓷的性能研究

以硝酸铝、柠檬酸为原料,采用溶胶-凝胶法制备Al2O3粉体.利用X射线衍射仪、扫描电子显微镜对Al2O3粉体的晶体结构、形貌及粒径进行表征,并研究以MgO-CuO-TiO2作为添加剂时,Al2O3陶瓷的烧结特性及介电性能.结果表明:干凝胶经1000℃煅烧2h后得到了分散性良好的Al2O3粉体,粒径大约为50～ 80 nm.随着MgO掺杂量的增加,Al2O3陶瓷的相对密度、介电常数以及Q·f值都呈先增大后减小的趋势;随着温度的升高,烧结体的相对密度不断增大.当烧结温度为1500℃,MgO含量为0.5wt;时,Al2O3陶瓷的综合性能较好:相对密度为91.52;,介电常数和Q·f值达到最大值分别为9.46,19862 GHz.     

Ce、Fe共置换锰酸钇陶瓷的结构和磁性能研究

采用低温固相法制备Y0.85Ce0.15Mn0.8Fe0.2O3粉体,经高温烧结制得陶瓷,研究了Ce、Fe共置换对锰酸钇陶瓷的微结构和磁学性能的影响.采用XRD对Y0.85Ce0.15Mn0.8Fe0.2O3粉体和陶瓷进行物相分析,利用TEM和FESEM对样品进行显微形貌分析;同时研究了Y0.85Ce0.15Mn0.8Fe0.2O3陶瓷的磁学性能,并利用XPS分析了其中磁性离子的价态分布.结果表明,前驱体经800℃煅烧后可制得单相Y0.85Ce0.15Mn0.8Fe02O3纳米粉体;该粉体经1450℃烧结制得致密的Y0.85Ce0.15Mn0.8Fe0.2O3陶瓷,其反铁磁转变温度为29K,在低温下存在反铁磁有序;与YMn0.8Fe0.2O3相比,Y0.85Ce0.15Mn08Fe0.2O3中Fe2+含量降低,Mn离子的混价结构由Mn2 +/Mn3+转变为Mn3 +/Mn4+,陶瓷的磁性转变温度降低.     

MgO掺杂LKNN无铅压电陶瓷的致密化烧结

本文采用传统烧结法成功制备了MgO掺杂的Li0.06(K0.5Na0.5)0.94NbO3+xMgO(LKNNMx)陶瓷,研究了烧结温度和MgO掺杂量对LKNNMx陶瓷结构与性能的影响。结果表明:MgO掺杂有效地促进了陶瓷的烧结,随MgO掺杂量的增加,LKNNMx陶瓷的致密化烧结温度大幅度降低。当MgO掺杂量为0.1%时,在1060℃烧结制备的陶瓷样品,其相对密度达到90%;当MgO掺杂量增加到1.5%时,在1000℃烧结制备的陶瓷样品,其相对密度高于92%,并保持了较好的压电性能。     

pH值及烧结温度对制备β-TCP粉体的影响

为了研究反应体系的pH值、烧结温度对磷酸钙粉体物相和形貌的影响,采用氢氧化钙和磷酸为原料,氨水为pH调节剂,通过化学共沉淀法制备磷酸钙前驱体.并通过在不同温度下进行烧结,制得β-TCP粉体.用X射线衍射(XRD)、红外光谱(FT-IR)、扫描电镜(SEM),对制备的磷酸钙进行表征和分析.结果表明:pH值为7、烧结温度1100 ℃情况下可得到较纯的β-TCP粉体.     

改进的共沉淀法制备YAG纳米粉体及透明陶瓷

采用改进的共沉淀法制备YAG透明陶瓷,研究了沉淀剂与金属盐溶液的摩尔比对粉体合成的影响以及成型压力对陶瓷烧结的影响.利用X射线衍射仪和场发射电子显微镜对实验样品进行表征.结果表明:当沉淀剂与金属盐溶液的摩尔比为NH4 HCO3/([Al3+]+[Y3+])=8,使用改进的共沉淀法在1000℃煅烧2h制备出平均粒径约为65 nm的YAG纳米粉体.以此YAG粉体为原料,TEOS为烧结助剂,经100 MPa成型后,在1750℃下真空烧结15 h获得透明陶瓷.     

自增韧和增强的镁铝尖晶石透明陶瓷

用化学配比n为1.0,1.3,1.5和1.8的MgO·nAl2O3粉体分别制备出了镁铝尖晶石透明陶瓷MA1.0,MA1.3,MA1.5和MA1.8.这些陶瓷是通过真空烧结和热等静压两步烧结方法制得的.由于第二相物质氧化铝晶粒的析出,陶瓷相对密度随着化学配比的增高而降低.然而,与化学配比陶瓷相比,这些非化学配比陶瓷表现出了较高的机械性能,陶瓷断面的扫描电镜照片显示非化学配比陶瓷多为穿晶断裂模式,这种断裂模式对陶瓷的强韧化作出了主要贡献.     

钛酸钡陶瓷制备及介电性能研究

采用钛酸四丁酯和硝酸钡为主要原料的微波辅助草酸盐沉淀法,在最佳的工艺参数下合成晶粒尺寸约为30～ 50 nm的钛酸钡粉末.再通过对纳米粉体造粒、成型、排胶和烧结等工艺处理制备钛酸钡陶瓷.研究陶瓷的最佳烧结温度与烧结时间,并且讨论其对介电性能的影响规律.利用透射电子显微镜分析粉体的形貌,XRD和扫描电子显微镜分别分析陶瓷的物相和断面形貌.结果表明,利用微波辅助草酸盐沉淀法合成的粉体制备陶瓷的烧结温度为1270℃,烧结时间为3h.并且其介电常数在室温下可达到2397.6.     

水热法生长立方MgO微晶研究

以尿素与Mg(NO3)2·6H2O在不同的反应温度和不同物质的量配比条件下,制备出前驱体Mg5(OH)2(CO3)4·4H2O/MgCO3,经煅烧得到立方MgO微晶粉末.利用X射线衍射仪(XRD)和扫描电子显微镜(SEM)对所制得产物的晶相和形貌进行了表征.结果表明:当尿素和Mg(NO3)2·6H2O物质的量的比为2∶1时,在160℃的水热反应条件下,制备出立方MgO前驱体微晶,在1000℃煅烧2h后能够获得晶型完整、形貌规则、粒径约为5μm的MgO立方微晶.     

粉体粒径及烧结工艺对ZrB2陶瓷致密化行为与晶粒长大的影响

利用热压烧结(HP)和放电等离子烧结(SPS)制备了ZrB2陶瓷,研究了粉体粒径和烧结工艺对ZrB2陶瓷致密化行为和晶粒长大的影响.结果表明,相同工艺下以平均粒径为200 nm的ZrB2粉体为原料替代平均粒径为2μm的ZrB2粉体可以明显促进粉体的致密化烧结,采用SPS替代HP工艺可以显著降低粉体的致密化温度,采用平均粒径为200 nm的ZrB2粉体在1900℃进行SPS工艺烧结即可实现ZrB2陶瓷的致密化烧结.     

CsI-LiCl共晶材料的坩埚下降法生长与闪烁性能研究

本文采用坩埚下降法,在真空密封的石英坩埚中成功生长出CsI-LiCl与CsI-LiCl:Na共晶闪烁体。通过扫描电子显微镜(SEM)观察晶体微结构表明该共晶中LiCl相与CsI相存在周期性的层状排列,CsI相的厚度在5 μm左右。共晶样品的X射线激发发射谱显示在CsI-LiCl和CsI-LiCl:Na共晶样品存在缺陷发光,在CsI-LiCl样品中还观察到了纯CsI的自陷激子(STE)发光。CsI-LiCl样品在α粒子激发下的多道能谱中观察到明显的全能峰,这一结果证明CsI-LiCl共晶可用于热中子探测的潜力。     

静电纺丝法制备CeO2微纳米纤维及其除氟性能

以聚丙烯腈(PAN)为载体,六水合硝酸铈[Ce(NO₃)₃·6H₂O]为原料,采用静电纺丝法制备了Ce(NO₃)₃/PAN纤维,在空气中热处理得到CeO₂微纳米纤维,通过XRD、BET和SEM对CeO₂微纳米纤维进行表征。采用静态吸附实验探讨了CeO₂微纳米纤维去除水溶液中氟离子的性能,考察了溶液pH值、初始氟离子浓度及共存阴离子等对吸附性能的影响。结果表明,pH=3时,CeO₂微纳米纤维对F^-的吸附性能最佳,CeO₂吸附量随着F^-浓度的增大呈上升趋势。CeO₂微纳米纤维对F^-的吸附等温线遵循Langmuir模型,二级动力学模型能很好地描述CeO₂微纳米纤维对F^-的吸附过程。CeO₂微纳米纤维的除氟性能优良,可为其实际应用提供理论参考。     

X-ray analysis of sideroxol from <Emphasis Type="Italic">Sideritis leptoclada</Emphasis>

Sideroxol (1), a kaurane diterpene which has the ent-7α,18-dihydroxy-15β,16β-epoxykaurane structure (MW = 320.47, C₂₀H₃₂O₃) was obtained from the acetone extract of Sideritis leptoclada plant as well as from some other Sideritis species. It crystallizes in the orthorhombic space group P2₁, 2₁, 2₁ with a = 10.967(3), b = 24.555(5), c = 6.372(4) Å, Dc = 1.240 g cm⁻³, Z = 4, and refines to R = 0.065 for 721 independent reflections. The skeleton consists of three fused six-membered rings and a five-membered ring with fused epoxide. The six membered rings exhibited slightly distorted chair conformation. In addition to sideroxol, two kaurane and five kaurene diterpenes were isolated from the hexane and acetone extracts of the studied plant.     

New zeotype borophosphates with chiral tetrahedral topology: (H)0.5M1.25(H2O)1.5[BP2O8]·H2O (M = Co(II) and Mn(II))

Two new isostructural open‐framework zeotype transition metal borophosphate compounds, (H)_0.5M_1.25(H₂O)_1.5[BP₂O₈]·H₂O (M = Co(II) and Mn(II)) were synthesized by mild hydrothermal method. The structure of compounds were characterized by single‐crystal X‐ray diffraction which have ordered, alternating, vertex‐sharing BO₄, PO₄, and (MO₄)OM(H₂O)₂ groups with hexagonal, P 6₁ 2 2 (No 178) space group and unit cell parameters for Co a = 9.4960(6) Å, c = 15.6230(13) Å, for Mn a = 9.6547(12) Å, c = 15.791(3) Å, Z = 1 for both of them. TGA/DTA analysis, IR spectroscopy were used for characterization. Magnetic susceptibility measurements for both of the compound indicate strong antiferromagnetic interaction between metal centers. (© 2005 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Photoluminescence characteristics of Mg- and Si-doped GaN thin films grown by MOCVD technique

We have studied the optical, structural and surface morphology of doped and undoped GaN thin films. The p- and n-type thin films have been successfully prepared by low-pressure MOCVD technique by doping with Mg and Si, respectively. The different carrier concentrations were obtained in the GaN thin films by varying dopant concentrations. Photoluminescence (PL) studies were carried to find the defect levels in the doped and undoped GaN thin films at low temperature. In the undoped GaN thin films, a low intensity and broad yellow band peak was observed. The donor–acceptor pair (DAP) emission and its phonon replicas were observed in both the Si or Mg lightly doped GaN thin films. The dominance of the blue and the yellow emissions increased in the PL spectra, as the carrier concentration was increased. The XRD and SEM analyses were employed to study the structural and surface morphology of the films, respectively. Both the doped and the undoped films exhibited hexagonal structure and polycrystalline nature. Mg-doped GaN thin films showed columnar structure whereas Si-doped films exhibited spherical shape grains.     

Solubility of Ag2O into the Na2O–B2O3–Al2O3 system

The solubility of Ag₂O was measured for the Na₂O–B₂O₃ and Na₂O–B₂O₃–Al₂O₃ system with the rotating crucible method and static method, respectively, under air atmosphere at temperatures ranging from 1273 to 1423 K. The contamination of melts from crucibles could be avoided by the rotating crucible method, with which it became possible to measure the solubility of Ag₂O for the Na₂O–B₂O₃ system above the melting point of Ag for the first time. It was found that the addition of Na₂O decreases the solubility of Ag₂O while the addition of Al₂O₃ had little effect on the solubility. The effect of Na₂O and Al₂O₃ on the solubility of Ag₂O is expressed by interaction coefficients and is analyzed in terms of the basicity of melts. The solubility of Ag₂O in Na₂O–B₂O₃–Al₂O₃ melts increased with increased temperature. This phenomena was explained by a small enthalpy change in oxidation of silver.     

Considerations on the structure and physical properties of B2O3-SiO2 and GeO2-SiO2 glasses

Data of density, refractive index and thermal expansion coefficient for B₂O₃-SiO₂ and GeO_2-SiO₂ glasses have been analyzed. The volumes of the structural units are the same found for the vitreous B₂O₃, GeO₂ and SiO₂. The volume of any structural unit is constant over the entire composition region of the glass system. The same has been found for the differential refraction and unit refraction of the structural units in these glasses. Different features are observed for the differential expansion of the structural units. There is a considerable change with composition in the differential expansion of BO₃, GeO₄ and SiO₄ units. The effect is attributed to a change in the asymmetry of vibrations with the number of Si-O-B or Si-O-Ge linkages in the matrix. The thermal expansion coefficient is mainly determined by the contribution of B₂O₃ or GeO₂ in the concerned glasses.     

Molecular structure and crystal packing of uncomplexed 1,6-bis(N-cyano-p-methoxy-anilino)-2,4-hexadiyne, C22H18N4O2

The X-ray crystal structure of 1,6-bis(N-cyano-p-methoxy-anilino)-2,4-hexadiyne, C₂₂H₁₈N₄O₂, is determined. The crystal packing is dominated by phenyl stacking interactions. Weak C–H···N hydrogen bonds help align the molecules. C–H··· hydrogen bonding is not apparent.     

Structural and electrical properties of vapour phase grown Cd1 − xFexTe single crystals

Cd_1 − xFe_xTe single crystals were prepared by vapour phase growth method in the composition range of 0 ≤ x ≤ 0.03. Chemical analysis, surface morphology, structural investigations and electrical properties were carried out by EDAX, SEM, XRD, TEM and transport technique, respectively. Microscopic variations between the target and actual compositions were noticed. Morphology studies revealed that dislocation aided growth is active in the present crystals. TEM and XRD studies confirmed that the samples of all compositions crystallized in zinc blende structure, and the lattice parameters varied almost linearly decreases with Fe content. At room temperature, the resistivity of the Cd_1 − xFe_xTe crystals of all compositions (x = 0.01, 0.015, 0.02, 0.025 and 0.03) lies in the range of 3.5-6.5 M Ω, the activation energies lie in the range of 63-133 meV, and the samples were show the ‘p’ type conductivity.     

空位浓度对纤锌矿CdS电子结构和光学性质影响的第一性原理研究

本文基于密度泛函理论的平面波超软赝势方法,采用第一性原理研究了含Cd空位缺陷CdS和含S空位缺陷纤锌矿CdS的几何结构、能带结构、电子态密度及光学性质。通过计算分析可知,含Cd空位缺陷的CdS体系均为p型半导体,含S空位缺陷的CdS体系跃迁方式均由直接跃迁变为间接跃迁。Cd、S空位缺陷的CdS体系的态密度总能量降低。空位CdS体系相较于本征CdS体系的静介电常数均有提高,并随着空位浓度的增大而增大,Cd空位缺陷体系更为明显,极化能力得到显著提升。空位Cd的CdS体系相较于本征CdS体系在红外波段存在明显的吸收,空位S的CdS体系相较于本征CdS体系在可见光波段存在明显的吸收。