陶瓷纤维/莫来石晶须原位增强堇青石-莫来石轻质隔热材料

以蓝晶石、粘土、氧化镁粉为原料,以淀粉为造孔剂和固化剂,引入适量的硅酸铝陶瓷纤维或多晶莫来石纤维和AlF3,通过莫来石晶须在陶瓷纤维表面的原位形成,制备了具有陶瓷纤维/莫来石晶须互锁结构的堇青石-莫来石轻质隔热材料.研究了陶瓷纤维在AlF3的作用下对材料显微结构观察、常温力学性能和导热系数的影响.研究表明:在AlF3的作用下,莫来石晶须在硅酸铝纤维表面垂直生长,部分穿插在发育良好的堇青石晶粒中;这种具有陶瓷纤维/莫来石晶须互锁结构的的陶瓷材料,其力学性能得以提高并降低了材料的导热系数.     

造孔剂及烧结温度对堇青石支撑体性能的影响

以人工合成堇青石粉为原料,使用碳粉、淀粉、聚苯乙烯微球为造孔剂,采用挤压成型和固态粒子烧结法制备多孔堇青石陶瓷支撑体.研究了造孔剂种类、用量及烧结温度对支撑体开孔率、抗压强度、空气渗透速率等性能的影响,并用XRD和SEM分析了不同造孔剂对样品的物相组成及断面形貌的影响.研究结果表明:添加造孔剂不会改变试样的物相组成,但对试样的基本性能影响显著,其中添加聚苯乙烯微球的试样开孔率最大,微孔间连通性最好,造孔效果最好;烧结温度能使材料致密化,可以有效提高抗压强度,当温度为1300℃、添加10;的聚苯乙烯微球时制备出的支撑体性能最优.此时开孔率为53.81;,抗压强度为8.36 MPa,空气渗透速率为5.99 m3·h-1·Pa-1·m-2,耐碱腐蚀率为99.97;.     

原位反应烧结制备莫来石-锌铝尖晶石多孔陶瓷研究

以天然高岭土以及活性氧化铝、氧化锌为原料,通过添加天然长石,以石墨为造孔剂,原位反应烧结制备了莫来石-锌铝尖晶石多孔陶瓷.采用XRD、SEM、EDS能谱分析分别确定了试样的物相组成、显微结构与微区化学组成.采用阿基米德排水法与抗压强度测定法测定了试样的孔隙率与抗压强度.结果表明:当原位合成温度为1450～1500℃范围时,试样的物相组成为莫来石与锌铝尖晶石,莫来石呈针状晶须,锌铝尖晶石晶形发育良好,材料的抗压强度增加迅速,为最合适的原位合成温度.长石的加入促进了针状莫来石的形成,促进了材料的烧结,提高了多孔陶瓷的强度.     

高岭土成型体水热转化无粘结剂4A分子筛研究

以煤系高岭土与碳质造孔剂、凹凸棒石增强剂加水混匀成型,经高温焙烧活化,水热反应转化4A分子筛,重点探讨了成型体的活化制度及造孔剂的作用机制.结果表明,造孔剂过量会使成型体的强度降低,欠量则不能形成丰富的前驱孔通道,无法保证晶化液进入体内充分反应;成型体的煅烧温度过低和/或时间过短,高岭石及造孔剂得不到充分分解,而温度过高和/或时间过长,会使偏高岭土的活性降低,且使前驱孔通道塌陷,皆影响分子筛的转化.高岭土与11;造孔剂和3;增强剂加水混匀并滚制成φ3mm的小球,在750℃锻烧3h,形成多孔活化体,再经水热转化可形成结晶良好、晶体互联交织生长的4A分子筛聚集体,宏观上保持原有的球形未变,其抗压碎力达115 N/颗,静态水吸附率达23.75;.     

高温烟气过滤陶瓷的制备与性能研究

本论文以堇青石为过滤陶瓷骨料,以高岭土、钾长石、锂辉石为结合剂,以木炭粉为造孔剂,通过半干压成型工艺成型,研制了高温烟气过滤陶瓷.详细研究了结合剂、造孔剂添加量以及成型压力、烧成温度对高温烟气过滤陶瓷的体积密度、显气孔率、抗压强度等性能的影响,并对原料配方进行了优化,优化配方为:堇青石75wt;、结合剂25wt;、炭粉造孔剂50wt;、三聚磷酸钠0.5wt;.研究结果表明:试样的显气孔率随造孔剂添加量的增加而升高、随结合剂添加量的增加而减小;抗压强度和烧结密度随造孔剂添加量的增加而减小、随结合剂添加量的增加而升高;随成型压力的增大,过滤陶瓷的显气孔率呈逐渐减小的趋势,抗压强度则不断增大.随烧成温度的升高,过滤陶瓷的显气孔率呈先升高后减小的趋势,而抗压强度则逐渐增大.     

莫来石纤维增强堇青石质陶瓷材料性能研究

以堇青石粉为原料,碳粉为造孔剂,甲基纤维素(MC)为粘结剂,甘油、乙醇为润滑剂,通过挤压成型和固态粒子烧成法制备具有高开孔率,高强度的陶瓷.通过烧结温度和保温时间的正交实验确定堇青石基体材料的烧结制度.通过考察烧结温度和莫来石纤维(PMF)添加量对纤维陶瓷性能的影响,确定使纤维与基体材料结合程度最佳的烧结制度和莫来石添加量.采用SEM、XRD表征样品的断面形貌和晶相种类,以分析基体材料和莫来石纤维的相互作用对陶瓷性能的影响.结果表明:1300℃下保温2 h的堇青石陶瓷综合性能较佳;含纤维陶瓷的烧结温度越高,莫来石纤维与堇青石基体的结合越紧密,莫来石纤维的增强作用越明显,但高于1300℃时,复合陶瓷的抗压强度会由于堇青石基体材料强度下降而下降;莫来石纤维添加量为20;时,陶瓷开孔率为49.25;,抗压强度为15.69 MPa,比无纤维的陶瓷增加了153;.     

大尺寸系列孔隙度高强人造岩芯的研制

采用矾土、氧化铝与硬质碎瓷粒为骨料, 选用硅溶胶、高岭土、煅烧滑石和方解石组成的MgO-CaO-Al2O3-SiO2低共熔混合物作为晶界结合剂,以木屑和煤粉为造孔剂,利用浇注成型技术制备出大尺寸系列孔隙度高强人造岩芯.其主要技术指标为:尺寸:65mm×150mm,孔隙度:26.6～45.4%,抗压强度:37.5～51.1 MPa.同时,SEM测试发现岩芯中的气孔呈三维连通状分布,且直径在100μm以下的微孔居多.     

高强度莫来石陶瓷微晶薄板的研究

为了降低莫来石微晶陶瓷的合成成本,用粉煤灰、铝矾土与叶腊石等为原料,以氟化铝(AlF3)为矿化剂,在相对较低的温度下合成了莫来石质的陶瓷微晶薄板。采用综合热分析仪(TG-DSC)、X射线衍射仪(XRD)和扫描电子显微镜(SEM)对样品进行表征。结果表明:随煅烧温度的升高,试样的气孔率和吸水率逐渐降低,试样中莫来石晶相含量、弯曲强度、密度逐渐增加。当煅烧温度为1200℃时,试样得弯曲强度达到96MPa。AlF3矿化剂的加入有利于促进莫来石的析晶和微晶板材的烧结,随AlF3矿化剂加入量的逐渐增加,试样的弯曲强度呈现先增加后降低的趋势,其适合的加入量为4.0wt%。     

莫来石轻质球形料结构与性能

对以铝矾土为主要原料制备获得的莫来石轻质球形料进行了系统的结构与性能研究,研究结果表明:轻质莫来石球形料的主要化学成分为Al2O3和SiO2,物相为莫来石相,球形颗粒表面莫来石柱状结晶交织排布,内部含有大量气孔,堆积密度为1.60 g/cm3,颗粒体积密度为1.75 g/cm3,显气孔率为38;,耐火度大于1790℃,800℃下导热系数为0.245 W/(m· K),热震5次后球形保持率大于95;.     

多孔PZT 95/5铁电陶瓷的孔隙率与电性能

以不均匀粒度的聚甲基丙烯酸甲酯(PMMA)微球为造孔剂,用造孔剂燃烧工艺(BURPS)制备了多孔PZT95/5铁电陶瓷.研究PMMA的添加量对多孔PZT95/5铁电陶瓷的物相组成、孔隙率和电性能的影响.X射线衍射分析显示PMMA的添加对陶瓷的物相组成没有影响,SEM结果显示PMMA微球在PZT 95/5铁电陶瓷中引入了与其大小相近的气孔;孔隙率结果表明多孔PZT 95/5铁电陶瓷的孔隙率随着坯体中PMMA的体积分数增加而增加;电性能方面,电滞回线测试和介电温谱测试结果分别表明样品的剩余极化强度和介电常数随着孔隙率的增加而减小.     

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。