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.     

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.     

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.     

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.     

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).     

First-principles coexistence simulations of supercooled liquid silicon

We perform first-principles coexistence simulations of the low-density and the high-density phases of supercooled liquid silicon and find a negative slope for the coexisting line in the temperature-pressure plane. Electron density maps and electron-localization function plots of the two phases of silicon show marked differences. The calculated differences suggest more localized electrons in the low-density liquid compared to the high-density liquid, coming from an increased population of covalent bonds, which further explain the calculated negative slope in the two phase coexistence regime. This is consistent with the presence of a pseudo-gap in low-density liquid silicon, absent in the high-density liquid which shows a metallic behavior.     

Crystal structures of thecis andtrans isomers of dithiahexahydro[3.3]metacyclophane

Structures of both thecis andtrans isomers of dithiahexahydro[3.3]metacyclophane, ?C₆H₄?CH₂SCH₂?C₆H₁₀?CH₂SCH₂?, have been determined, wherecis andtrans refer to the attachments to the cyclohexane ring. Thecis form crystallizes in the monoclinic space groupP2₁/c witha=8.4299(11)Å,b=21.772(2)Å,c=8.9724(13)Å, β=116.574(11)^o, andZ=4. Thetrans isomer packs into the monoclinic space groupP2₁ witha=8.159(16)Å,b=10.185(5)Å,c=9.558(2)Å, β=112.435(18)^o, andZ=2. The cyclohexane ring of thecis isomer is in the chair conformation, while the cyclohexane of thetrans isomer is found in a twisted boat conformation.     

CTAB与SDBS对碳酸锶粒子生长形态调控及机理研究

以表面活性剂CTAB和SDBS为化学添加剂,采用化学共沉淀法对碳酸锶晶体的生长形态进行调控,成功地制备出了实心的树枝状和花瓣为空心的花状碳酸锶粉体,并用X射线衍射(XRD)、扫描电子显微镜(SEM)和傅里叶变换红外光谱(FT-IR)等分析手段对样品进行了表征;最后重点对化学添加剂可能产生的影响机理进行了初步的探讨.结果表明,CTAB和SDBS在晶体生长的过程中能起到显著的影响作用,两者对粒子分散性能的作用效果相反,而且后者对晶体(013)和(213)晶面表面能降低的贡献明显大于前者.     

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.     

Synthesis of spinacine and spinacine derivatives: crystal and molecular structures of Nπ-hydroxymethyl spinacine and Nα-methyl spinaceamine

The natural amino acid L-Spinacine (4,5,6,7-tetrahydro-1H-imidazo[4,5-c]pyridine-6-carboxylic acid) has been synthesized following a new pathway which gives a chemically and optically pure product with an excellent yield. The crystal structures of a synthetic intermediate, N^π-hydroxymethyl-spinacine, and a spinacine derivative, N^α-methyl-spinaceamine, have been investigated through X-ray diffraction: Spi(πMeOH)·H₂O, monoclinicP2 _i,a=8.571(1),b=6.682(1),c=8.588(1) Å, and β=94.67(1)^o. Spm(αMe)·2HCl·H₂O, triclinicP l,a=7.492(4),b=10.799(3),c=7.040(2) Å, α=91.88(2), β=98.36(3) and γ=73.34(3)^o. Spi(πMeOH) crystallizes with a water molecule and displays a zwitterionic character. The carboxylate group is in equatorial position and forms a short electrostatic interaction of 2.618(2) Å between one of its oxygens and the protonated nitrogen of the tetrahydropyridine ring. The crystal packing is assured by strong O?H???O, O?H???N, N?H???N intermolecular hydrogen bonds and C?H???O close contacts. The biprotonated compounds Spm(αMe) crystallizes with two Cl^? anions and a water molecule. The positive charge on the imidazole ring is delocalized on the conjugated moiety N=C?N. The crystal is built up by clusters formed by two biprotonated Spm(αMe) molecules, four Cl^? anions and two water molecules linked together by hydrogen bonds.