添加碳对ZrB2-SiC陶瓷的低温致密化和力学性能影响

以纳米ZrB2粉体为原材料,采用热压烧结的方法制备了ZrB2-SiC超高温陶瓷,研究了碳含量对ZrB2-SiC陶瓷致密度、微结构和力学性能的影响.结果表明:纳米粉体显著降低了ZrB2-SiC陶瓷的烧结温度,在1500℃即可获得95.1;的致密度,在1800℃实现了超高温陶瓷的致密化烧结;添加碳能够进一步促进ZrB2-SiC陶瓷的低温致密化,同时抑制晶粒长大.当碳的含量为1.0wt;时,材料表现出最佳的烧结性能,在1700℃热压烧结的ZrB2-SiC陶瓷致密度达到99;以上,而且烧结后的材料表现出优异的力学性能.     

Al2O3陶瓷非等温烧结研究

以高纯α-Al2O3粉体为原料,采用非等温烧结法制备了纯Al2O3陶瓷(AL)及掺杂MgO-Y2O3复合助剂的AJ2O3陶瓷(ALMY).研究了AL和ALMY在不同烧结温度下的相对密度、显微结构及硬度.结果表明,在非等温烧结中,纯Al2O3致密化的烧结温度范围较窄,烧结温度为1500℃时,其相对密度及硬度分别为98.1;和18.1GPa,当烧结温度为1600℃时,AL由于晶粒显著粗化,且产生了晶内气孔,相对密度及硬度分别显著下降到94.6;和12.5 GPa.MgO-Y2O3复合助剂的引入拓宽了Al2O3致密化的烧结温度范围,细化了显微结构,烧结温度在1500℃和1600℃时,ALMY的相对密度均在98;以上,硬度分别为19.2 GPa和17.6 GPa.     

MgO-CeO2烧结助剂对高SiC含量SiC基复相陶瓷致密性与导热性能的影响

以MgO-CeO2为烧结助剂,采用热压烧结工艺在1850C制备了SiC含量为80wt;的SiC-AlN复相陶瓷.研究了不同助剂含量对复相陶瓷致密性与导热性能的影响.结果表明:适量的烧结助剂能够对SiC-AlN复相陶瓷起到促进烧结作用.烧结助剂含量为6wt;时,样品显气孔率偏大;当助剂含量提高至8wt;～14wt;时,样品显气孔率显著降低,能够完全烧结致密化.复相陶瓷在烧结助剂含量为1Owt;时获得最佳的致密性,其显气孔率仅为0.14;.在烧结助剂含量为8wt;时,样品具有最高的热导率51.72 W·m-1·K-1.复相陶瓷的热导率主要受样品致密性和晶界相的影响,不足或过量的烧结助剂都会使样品的热导率降低.     

AlN含量对SiC基复相陶瓷性能的影响

以MgO-CeO2为烧结助剂,采用热压烧结工艺在1850℃下制备了SiC基复相陶瓷.研究了不同AlN含量对复相陶瓷致密性与导热性能的影响.结果表明:不添加AlN时,试样致密性最差,气孔率和体积密度分别为4.71;和2.43 g/cm3.AlN含量升高至5wt;时,试样致密性有所提高.AlN含量进一步升高至10wt;～20wt;,试样完全致密,气孔率和体积密度分别保持在0.20;和3.31 g/cm3.在AlN含量为10wt;时,样品具有最高的热导率51.62 W·m-1·K-1,同时弯曲强度和断裂韧性达到顶点,分别为731.3 MPa和7.3 MPa·m1/2.     

掺CeO2的MgO-CaO材料缺陷形成及扩散动力学研究

以分析纯Mg(OH)2和Ca(OH)2为起始原料,CeO2为掺杂剂,经行星球磨机混合后压制成圆柱形试样,在1650℃温度条件下保温3h烧成,制备了MgO-CaO材料.采用X-射线衍射仪、场发射扫描电子显微镜和高温电导率测试仪对试样进行了分析表征.研究结果表明:少量CeO2的掺入(0.5wt; ～0.75wt;)即可有效促进材料的烧结致密化.在烧结致密化过程中,随着晶界的迁移及气孔排除,方镁石与方钙石晶粒不断长大,且方镁石晶粒长大更为明显,形成以方镁石为基体,方钙石晶粒被方镁石包裹的空间结构,但MgO由于本征缺陷产生的O2-空位在晶界迁移过程中的聚集和融合,在方镁石晶粒内形成了难以排除的气孔.CeO2促进材料烧结的本质在于CeO2可与CaO发生有限置换固溶反应,降低Ca2空位的扩散激活能,有利于Ca2空位的扩散.     

TiO2烧结助剂对纳米η-Al2 O3制备氧化铝陶瓷的影响

为降低氧化铝陶瓷制备成本,改善其性能,以价格低廉的纳米η-Al2 O3为原料,TiO2为烧结助剂,制备氧化铝陶瓷.研究了TiO2加入量对纳米η-Al2 O3氧化铝陶瓷的体积密度、显气孔率、物相组成和微观结构的影响.结果表明:TiO2通过增加氧化铝中铝离子点缺陷数量而提高其扩散系数,促进氧化铝陶瓷的致密化及晶粒的生长.η-Al2 O3到α-Al2 O3的相变首先在氧化铝颗粒表面进行,然后迅速扩散至内部完成.通过计算晶胞参数大小,定量证明刚玉晶体发育良好,引入适量TiO2对氧化铝陶瓷高温性能和化学稳定性影响较小.当TiO2加入量为2wt;,烧结温度为1600℃时,氧化铝陶瓷的性能优良,体积密度为3.70 g/cm3、显气孔率为1.2;,存在一定数量的晶间气孔和晶内气孔,晶体间结合紧密,晶粒尺寸10～30μm.     

Y2O3-Al2O3含量对Si3N4陶瓷相组成、致密化、显微结构和力学性能的影响

以α-Si3N4粉为原料,通过添加不同含量的Y2O3-Al2O3烧结助剂(6wt;、8wt;和10wt;),在1800℃下采用热压烧结制备了Si3 N4陶瓷,研究了Y2 O3-Al2 O3含量对Si3 N4陶瓷的物相、致密度、显微结构与力学性能的影响,结果表明:添加6wt;的Y2 O3-Al2 O3助剂即可获得高致密的Si3 N4陶瓷,继续增加助剂含量对Si3 N4陶瓷的致密度影响不大,但是显著影响 α-Si3 N4相和β-Si3 N4相的含量,较高的Y2 O3-Al2 O3助剂含量有利于α-Si3 N4转化为β-Si3 N4.不依赖于Y2 O3-Al2 O3助剂含量,Si3 N4陶瓷均包含细小的等轴晶粒和大尺寸的棒状晶粒,呈现双峰结构,但是Y2 O3-Al2 O3助剂含量增加到10wt;时,可以显著增加棒状晶粒的数量,形成更显著的双峰结构.基于当前研究,发现加入低含量的Y2O3-Al2O3助剂(6wt;),可以获得高硬度高强度的Si3N4陶瓷,而引入高含量的Y2O3-Al2O3助剂(10wt;),则可以获得高韧性高强度的Si3N4陶瓷.     

MnO添加对40（50 Cu-Ni）-（NiFe2 O4-10 NiO）金属陶瓷惰性阳极的影响

采用粉末冶金法对40(50Cu-Ni)-(NiFe2O4-10NiO)金属陶瓷进行MnO掺杂实验,并对不同添加量试样进行烧结致密化与电解腐蚀性能研究。结果表明：在烧结过程中Mn2+会取代部分基体尖晶石中Ni2+发生晶格畸变,提高烧结活性,当添加量为3wt;时,试样收缩率为18.5;,致密度达97.7;;24 h杂质含量最低,电解24 h后铝液中的Cu、Fe、Ni、Mn的杂质含量最低,分别为0.069wt;、0.121wt;、0.115wt;、0.028wt;。     

SiC微粉添加量对SiC耐磨材料结构和性能的影响

以紧密堆积的三级配SiC颗粒(粒径为325 μm、212 μm、80 μm,质量比为17∶7∶1)为基础配方,将Owt;、1wt;、2wt;、3wt;和4wt;且粒径为5μm的SiC微粉添加到SiC耐磨材料中,经1600℃保温3h烧制,研究了SiC微粉添加量对SiC耐磨材料结构和性能的影响.结果表明:SiC微粉可促进SiC耐磨材料的烧结致密化,并改善其力学性能,当其添加量为3wt;时,试样的综合性能较优,其体积密度和显气孔率分别为2.63 g/cm3和7.62;,硬度、抗折强度和磨损量分别为2458 HV、183 Mpa和0.26 g/min.SiC耐磨材料烧结性能和力学性能的提高可归因子SiC微粉充填在SiC颗粒间,缩短了扩散传质路径,且较小粒径的SiC微粉具有较大的表面能,烧结时易于晶粒重排,保证了烧结网络的连续性,增大了颗粒间的结合程度.     

AlN/Mo/TiB2微波衰减材料的制备及介电性能研究

采用放电等离子烧结制备了AlN/Mo/TiB2微波衰减材料.研究了TiB2的含量对复合材料的相组成、致密度、电阻率及介电性能的影响.利用XRD、SEM、网络分析仪对样品的相组成、微观结构、介电性能进行测试分析.结果表明:随着TiB2的含量的增加,复合陶瓷的致密度先增大后减小,当加入15wt; TiB2时,致密度达到最大,为98.71;.加入TiB2有利于复合陶瓷介电常数和介电损耗的增加.从电导率测试结果可知,复合陶瓷的渗流阈值在TiB2含量为15wt;.     

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.     

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.     

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)     

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.     

Selinidin: Crystal structure generated by C–H···O, C–H···π and π-π interactions

The title compound, 9,10-dihydro-8,8-dimethyl-2-oxo-2H,8H-benzo[1,2-b:3,4-b']dipyran-9-yl-2-methyl-2-butenoate, C₁₉H₂₀O₅, was isolated from the roots of Selinum vaginatum. The compound crystallizes into monoclinic space group P2 ₁ with unit cell parameters: a = 12.830(2) Å, b = 9.041(1) Å, c = 14.983(1) Å, β = 95.09(1)°, Z = 4. The crystal structure has been determined using direct methods and refined by full-matrix least-squares to a final R value of 0.0529 for 3142 observed reflections. There are two independent molecules, A and B, per asymmetric unit. In both the molecules, the coumarin nucleus is planar. However pronounced differences are observed in the conformation of dihydropyran ring which has a half-chair conformation with an 8β-9α orientation in molecule A and is intermediate between half-chair and sofa in molecule B. Differences also occur in the conformation of the 2-methylbutenoyloxy side chain at C9 due to the different geometry of C–H···π interactions in molecules A and B. Molecules A and B are connected by π–π interactions between their coumarin fragments forming dimers. The dimers interact through C–H···O and C–H···πhydrogen bonds.     

Chromene and Imidazole Based D-π-A Chemosensor Preparation and Its Anion Responsive Effects

We have designed and synthesized the colorimetric chemosensor through the reactions of 2-(4H-chromen-4-yildene)malonitrile and 4-imidazolecarboxaldehyde. Due to its well conjugated D-π-A system and the existence of NH- fragment in structure, we expected that the chemosensor can detect anion using NH- fragment in the imidazole moiety of the structure. In this regard, UV-Vis absorption spectra were measured to investigate sensing properties of the probe toward different anions in DMSO. This chemosensor can detect both fluoride and cyanide ion with absorption change in intensity. In addition, pH sensing property was also investigated upon the addition of hydroxide ion. These properties are related to the deprotonation effect. The ICT system in this molecule was also observed by the computational approach using Material Studio 4.3 package.     

电子显微分析在表征纳米晶体化学组分中的应用

纳米材料的化学组分及含量影响其光、电、声、热、磁等物理性能,电子显微分析是表征纳米晶体化学组分的重要方法之一.本文综述了X-射线能谱(EDS)、X-射线波谱(WDS)、电子能量损失谱(EELS)和选区电子衍射(SAED)等现代电子显微分析技术在表征纳米晶体化学组分、形貌、尺寸和结构等方面的应用及其研究进展,并比较了这些分析方法存在的差异,提出了其应用中存在的不足及今后的研发方向.     

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.