环氧树脂/石墨双极板复合材料的性能分析

以固态环氧树脂(EP)粉与石墨(G)粉混合物为原料,通过低温热压烧结制得一种双极板材料.研究了EP/G复合材料的弯曲强度和电导率随环氧树脂含量、模压温度和保温时间的影响变化.结果表明:随着环氧树脂含量的增加,EP/G复合材料的弯曲强度呈先上升后下降趋势,在EP含量为10;(质量分数)时达到最大,而电导率呈下降趋势;随模压温度的升高,EP/G复合材料的弯曲强度逐渐变大,电导率则先增长后降低;随着保温时间的延长,EP/G复合材料的弯曲强度和电导率都呈现先增长后降低的变化趋势;环氧树脂含量为10;质量分数,模压温度为275 ℃,保温时间为100 min时,所得复合材料弯曲强度为53.11 Mpa,电导率达到209.25 S/cm.     

SiC/SiC复合材料高温力学性能研究

以聚碳硅烷为连续SiC陶瓷基体相的先驱体,三维四向SiC纤维预制体为增强相,采用聚合物先驱体浸渍裂解工艺制备了SiC纤维增强SiC陶瓷基(SiC/SiC)复合材料,分析表征了复合材料的组成、结构和力学性能.结果表明,SiC/SiC复合材料室温弯曲强度和断裂韧性分别为400 MPa和16.5 MPa·m1/2,优异的室温力学性能可以保持到1350℃.随着温度增加,弯曲强度基本不变,1350℃时因界面层受到破坏而断裂韧性稍有下降.     

热压烧结制备BN-MgAlON复合材料及其力学性能研究

以BN-MgAlON复合粉体为原料,Y2O3为烧结助剂,在N2气氛下热压烧结制备了BN-MgAlON复合材料,用X射线衍射和扫描电镜对材料的物相组成和显微结构进行了表征,研究了烧结温度对材料的物相组成、烧结性能和力学性能的影响.结果表明,在1650～1750℃可制备出致密的BN-MgAlON复合材料.材料主要成分为MgAlON、Sialon、BN和CaYAl3O7,随烧结温度的提高,MgAlON的衍射峰逐渐增强.1750℃下所得材料结构均匀致密,材料中Al、Mg、O、N分布比较均匀.材料的抗弯强度、断裂韧性和显微硬度均随着烧结温度的升高而提高.1750℃下的材料性能最好,其体积密度为2.79 g·cm-3,显气孔率为0.3;,抗弯强度为283 MPa,断裂韧性为3.85 MPa·m1/2,硬度为15.33 GPa.并且1750cc,恒温1h条件下烧结的得到的BN-MgAlON复合材料的抗冲刷性和耐磨性均远远优于耐磨钢B-hard-450.     

Si_3N_4粒度对逆反应烧结制备Si_3N_4/SiC复合材料性能的影响

研究了不同粒度的Si3N4粉体对制备的逆反应烧结Si3N4-SiC复合材料性能的影响。结果表明:同一升温制度下,Si3N4粒度从0.074 mm减小到0.045 mm,Si3N4-SiC复合材料体积密度增大,显气孔率变低,抗折强度降低。随着Si3N4粒度减小,材料中的Si3N4含量降低;中温保温从900℃升到1200℃,Si3N4含量升高;高温保温温度从1350℃到1500℃,材料内部氧化程度增高,Si3N4含量降低,SiO2含量升高;Si3N4-SiC复合材料玻璃相增多,玻璃相中有SiO2晶体析出,使得孔隙被生成的玻璃相和发育的SiO2晶粒填充,材料的气孔减少。     

原位生长莫来石增强磷酸铬铝复相陶瓷的制备及性能

以磷酸铬铝粘接剂、熔融石英、氢氧化铝为原料制备莫来石原位增强磷酸铬铝复相陶瓷,采用热分析、XRD、SEM、EDS、矢量网络分析测试等手段,研究不同温度对烧结体物相、显微结构、机械及介电性能的影响,并探讨莫来石原位生长和增强机理.结果表明:在1250 ～ 1500℃范围内,随温度升高,材料的致密度、抗弯强度、维氏硬度和介电常数均升高.1500℃煅烧可得致密的原位合成莫来石/磷酸铬铝复相陶瓷,材料晶粒发育比较完善,短棒状莫来石和球状磷酸铬铝晶粒清晰可见,基体致密程度受游离SiO2控制.复合材料介电常数、弯曲强度、维氏硬度分别达到3.7、117 MPa和5.3 GPa.当煅烧至1600℃时,晶粒快速长大,材料的强度降低.磷酸铬铝与莫来石颗粒间通过弥散强化、细晶强化、晶粒拔出等机制对复合材料起到增强的作用.     

TBA/H2O溶液冷冻干燥制备多孔Al2O3支架及其生物性能

以叔丁醇/蒸馏水(TBA/H2O)结晶体为模板,用冷冻干燥法制备出片层孔及圆形孔的两种孔型氧化铝支架材料,利用SEM观察支架形貌,测试了其生物性能,系统研究浆料溶剂组分含量、冷冻温度对支架材料形貌影响,探讨支架孔结构对成骨细胞附着的影响.结果表明:纯水浆料的多孔陶瓷支架形貌为片层状;加入叔丁醇后,片层间距减少;浆料中叔丁醇含量为90wt;时,孔道呈片层孔及圆形孔的双孔状;纯叔丁醇浆料的陶瓷支架形貌为圆形孔.双孔形貌支架的开孔孔隙率及总孔隙率最高,分别为78.5;和81.8;.孔径随冷冻温度的降低而减小.体外模拟实验表明:片层孔及圆形孔的双孔支架材料有利于细胞在其表面生长,材料表面细胞结构清晰,铺展形态良好.多孔支架材料对细胞的吸附率随孔径的增大而增大.冷冻温度为-10℃时,支架的压缩强度为90.6 MPa,符合骨组织工程中支架材料的强度值要求.     

反应热压烧结制备SiC/ZrB2复相陶瓷及其性能表征

以二硼化锆、硅和活性碳为原材料,在1850℃、20 MPa条件下,采用反应热压烧结工艺制备出了SiC/ZrB2陶瓷基复合材料.研究了添加剂(硅和活性碳)含量对ZrB2陶瓷烧结行为和力学性能的影响.借助X射线衍射和扫描电镜分析了复合材料的物相组成和微观结构.研究结果表明:添加剂可以显著提高复合材料的烧结致密度和力学性能.复合材料的XRD衍射图谱中只有ZrB2和SiC的衍射峰.当添加剂含量为12wt;时,复合材料的弯曲强度和断裂韧性分别达到584MPa和7.25MPa ·m1/2.显微结构分析表明,致密度的提高、晶粒粒径的减小以及断裂模式的转变是复合材料力学性能提高的主要原因.     

煅烧时间与温度对超导/铁磁复合材料性能的影响

采用传统的固相反应法在较低的烧结温度与较短的煅烧时间下制备了(La1.85Sr0.15CuO4)1-x(La2/3 Sr1/3MnO3)x(简写为LSCO/LSMO)超导/铁磁复合材料.结果显示:复合后LSMO中的结构没有发生明显改变,随着温度的降低,所有的复合材料在38 K左右均会出现电阻急剧下降,最终呈现超导现象.甚至当LSMO铁磁性材料掺入达到O.20mol时,复合材料仍旧呈现超导态.同时所有复合样品的超导转变温度TC随着x的增加呈现线性下降的趋势.因此,通过低温与短时的烧结方法可以避免处于晶界处的LSCO的CuO面被破坏,进而提高超导/铁磁复合材料中在晶界处的铁磁的共存含量.     

Ti3AlC2/Fe复合材料的制备及力学特性

以Ti3AlC2粉和还原铁粉为原料,在1300℃、30 MPa、保温30 min的热压条件下制得Ti3 AlC2/Fe复合材料,并研究了其组成及相关力学特性.结果表明:Ti3AlC2/Fe复合材料具有致密度高、组织均匀、增强相颗粒尺寸细小且分布较均匀等优点.经过热压烧结,Ti3AlC2会分解生成TiCxo.由于TiCx的增强作用,使得Fe基复合材料具有高的抗弯强度,在20vol; Ti3AlC2含量时达到最高的1091 MPa,并保持了良好的延展性.复合材料在800℃热震之后,除30vol; Ti3AlC2/Fe之外其他试样强度基本不变或略有升高,并且热震前后材料的断裂方式基本不变,表现出良好的抗热震特性.     

冰模板法制备反应结合多孔Si3N4/SiC复相陶瓷

以微米级SiC和Si粉为原料,采用冰模板法和氮化反应烧结法制备了孔道中修饰α-Si3N4、Si2N2O纳米线的β-Si3N4结合多孔SiC复相陶瓷.研究了反应烧结温度、SiC/Si比和固相含量对多孔陶瓷的物相结构、形貌、孔分布和压缩强度的影响.结果表明:多孔陶瓷具有层状定向通孔结构,孔隙率介于50; ～ 70;之间,孔径分布呈现双峰分布特点;当烧结温度达到1350℃以上时,在层状孔道中交织形成α-Si3N4和Si2N2O纳米线的网络结构.反应温度超过1450℃时,通过液态Si的氮化反应原位形成β-Si3N4结合相将SiC颗粒粘结起来;当浆料中Si含量由16wt;增加至33wt;时,多孔陶瓷的开气孔率从69.78;降至62.64;,而压缩强度由2.2 MPa提高到8.73 MPa;随着浆料固相体积含量从25;增加到45;,多孔陶瓷的气孔率从71.81;降至54.85;,同时压缩强度从4.99 MPa提高到24.16 MPa.     

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。     

Triethyl ammonium salt of O,O′-bis(p-tolyl)dithiophosphate, [Et3NH]+[(4-MeC6H4O)2PS2]−

Triethyl ammonium Salt of O,O′-bis(p-tolyl)dithiophosphate and O,O′-bis(m-tolyl)dithiophosphate have been obtained by reaction of p- and m-cresol, respectively with P₂S₅ in toluene and have been characterized by elemental analysis, IR, ¹H and ³¹P NMR spectroscopy. The molecular structure of O,O′-bis(p-tolyl)dithiophosphate has been determined. Crystal data: [Et₃NH]⁺[(4-MeC₆H₄O)₂PS₂]⁻: Monoclinic, P2₁/c, a=15.2441(9) ?, b=10.415(2) ?, c=3.9726(9) ?, β=91.709(7)°, V=2217.5(1) ?⁻³, Z=4.Supplementary materials Additional material available from the Cambridge Crystallographic Data Centre (CCDC no. 600927 for [Et₃NH]⁺[(4-MeC₆H₄O)₂PS₂]⁻ comprises the final atomic coordinates for all atoms, thermal parameters, and a complete listing of bond distances and angles. Copies of this information may be obtained free of charge on application to The Director, 12 Union Road, Cambridge CB2 2EZ, UK (fax: +44-1223-336033; email: deposit@ccdc.cam.ac.uk or www:http://www.ccdc.cam.ac.uk).     

Crystal structure of Zn4Na(OH)6SO4Cl·6H2O

The structure of Zn₄Na(OH)₆SO₄Cl·6H₂O, a secondary mineral from Hettstedt, Germany, was determined by single-crystal X-ray diffraction. The crystals are hexagonal,a=8.413(8),c=13.095(24) Å, space group $P\bar 3$ , Z=2. The structure was refined to R=0.0554 and R_w=0.0903 for 970 reflections with I≥3σ(I). The structure can be described as zinc hydroxide layers perpendicular toc, from which sulfates and chlorides extend. The layers are held together by a system of hydrogen bonds involving hexaaquo Na⁺ ions which occupy the interlayer space.     

Synthesis and Crystal Structure of 5-[2-(6-bromonaphthalenyloxymethyl)]-3-(4-morpholinomethyl)-1,3,4-oxadiazole-2(3<Emphasis Type="Italic">H</Emphasis>)-thione

Abstract  The title compound, C₁₈H₁₈BrN₃O₃S, a derivative of 1,3,4-oxadiazole, crystallizes in the triclinic space group P-1 with unit cell parameters a = 6.8731(3), b = 8.9994(4), c = 15.7099(6) ?, α = 92.779(3)°, β = 130.575(3)°, γ = 107.868(4)°, Z = 2. The dihedral angle between the mean planes of the planar naphthyl and morpholine (chair) rings with the planar oxadiazol ring is 50.1(8) and 76.8(6)°, respectively. The planar naphthyl ring is twisted 52.2(5)° with the mean plane of the morpholine ring. A group of four intermolecular close contacts are observed between a bromine atom and hydrogen atoms from the closely packed naphthyl, morpholine and oxy–methyl groups in the unit cell. These molecular interactions in concert with an additional series of π–π stacking interactions that occur between the center of gravity of the two 6-membered rings of the naphthalene group influence the twist angles of each of these three groups. A MOPAC AM1 calculation of the conformation energy of the crystal structure [226.0128(9) kcal] compared to that of the minimum energy structure after geometry optimization [29.9744(1) kcal] reveals a significantly reduced value. The twist angles of the three groups above also change after the AM1 calculation giving support to the influence of both intermolecular C–H···Br short-range interactions and Cg π–π stacking interactions on these angles which therefore play a role in stabilizing crystal packing. Graphical Abstract  Crystal structure of 5-{[(6-bromonaphthalen-2-yl)oxy]methyl}-3-(morpholin-4-ylmethyl)-1,3,4-oxadiazole-2(3H)-thione, C₁₈H₁₈BrN₃O₃S, is reported and its geometric and packing parameters described and compared to a MOPAC computational calculation. Electronic supplementary material  The online version of this article (doi:) contains supplementary material, which is available to authorized users.     

Crystal structure of irisolidone from the flowers of Pueraia lobata

Irisolidone (5,7-dihydroxy-6,4′-dimethoxyisoflavone) was isolated from the flowers of Pueraia lobata and its crystal structure was examined by X-ray single crystal diffraction. The crystal structure of irisolidone is monoclinic, space group P2₁/c with a = 15.491(9) ?, b = 7.895(4) ?, c = 13.321(7) ?, β = 110.546(9)° and Z = 4. Hydrogen bonding and aromatic π–π stacking assemble the title compound into a three-dimensional networking structure.     

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.