掺杂Ni/Al对热障涂层抗高温氧化性和结合强度的影响

YSZ(Ni,Al)粉末颗粒通过电泳沉积技术在高温镍基合金600上沉积一层厚度均匀的YSZ(Ni,Al)复合热障涂层,并在室温下干燥24 h后,进行真空烧结致密化处理.真空致密化处理后的YSZ(Ni,Al)复合热障涂层在1100℃下氧化不同小时并测量涂层的结合强度.由于掺杂了镍铝氧化初期在涂层表面形成一层致密的氧化薄膜,有效地阻止了空气中的氧气进一步进入涂层内部从而提高了涂层的抗高温氧化性能,另外在陶瓷涂层YSZ中掺杂了金属元素,降低了陶瓷涂层与高温镍基合金的热膨胀系数的不匹配,使涂层表面更加平整致密,同时也提高了涂层与基体的结合强度.     

SDC/YSZ双层电解质薄膜的制备与特性

利用脉冲激光沉积技术(PLD)在MgO单晶片基底上制备Ce0.8Sm0.2O2-δ/ZrO2∶Y2O3 (SDC/YSZ)双层电解质薄膜.X射线衍射仪(XRD)和扫描电子显微镜(SEM)的结果显示SDC/YSZ双层电解质薄膜沿(111)方向择优生长,随着退火温度的升高,薄膜变得均匀致密,结晶度得到改善,(111)衍射峰强度变大,择优生长取向明显;电化学测量表明,SDC/YSZ双层电解质薄膜的离子电导率比单层YSZ薄膜的离子电导率高.     

低温超晶格YSZ/STO/YSZ电解质薄膜的制备及表征

采用脉冲激光沉积法(PLD),在Al2O3 (ALO)衬底上,将Y2O3∶ZrO2(YSZ)和SrTiO3 (STO)按照YSZ/STO/YSZ的顺序依次沉积,形成超晶格YSZ/STO/YSZ电解质薄膜,利用SEM、XRD和交流阻抗对其形貌、相结构和电学性能进行了表征.结果表明,衬底温度为700℃形成的超晶格YSZ/STO/YSZ电解质薄膜颗粒大且均匀,排列紧密且呈规律圆柱状;YSZ、STO均沿(111)方向择优生长;低温时电导率比单层YSZ电解质薄膜高出4个数量级,是较为理想的低温固体燃料电池电解质.     

染料敏化太阳能电池中SrCO3包覆TiO2电极的界面特性研究

用水热法制备TiO2纳米材料,并对TiO2表面进行修饰.通过场发射扫描电子显微镜(SEM)和光电子能谱(XPS)对材料表面结构和成分进行分析.结果表明TiO2薄膜表面包覆了一层粒径较大的SrCO3颗粒,整个电极表面呈现均匀的多孔结构.使用电化学工作站对电池进行光电性能分析和EIS测试,由Ⅰ-Ⅴ曲线的结果可得,修饰后的电极性能更优越,短路电流提高了39.9;,光电转化效率提高了38.3;.由电化学阻抗谱(EIS)测试结果可以看出,修饰后TiO2/dye/电解质的界面阻抗大于修饰前,说明包覆层在一定程度上起到了阻碍电荷复合的作用,从而减小了暗电流.     

Ce0.8Sm0.2O1.9-BaCe0.8Sm0.2O2.9复合电解质的成分对其电化学性能的影响

采用一步溶胶凝胶法制备摩尔比分别为9∶1、7∶3、5∶5和3∶7的复合电解质Ce0.8Sm0.2O1.9(SDC)-BaCe0.8Sm0.2O2.9(BCS)粉末,研究复合电解质SDC-BCS的相成分对电导率及其电化学性能的影响.结果表明:随着SDC含量的增加,复合电解质SDC-BCS的晶粒尺寸增大、电导率提高;复合电解质的晶界电导率均高于单相SDC的晶界电导率.不同成分的复合电解质制备的NiO-SDC-BCS|SDC-BCS|LSCF-SDC-BCS单电池的功率密度随着SDC含量的增加而提高.当SDC∶BCS的摩尔比为9∶1时,其单电池700 ℃的最大功率密度为550 mW/cm2,是单电池NiO-SDC|SDC|LSCF-SDC最大功率密度的3倍.     

固体氧化物燃料电池NiO@GDC复合阳极制备及性能研究

采用溶胶凝胶法制备NiO@GDC复合阳极材料.以NiO、GDC作为阳极、YSZ为电解质、GDC为阻挡层、LSCF为阴极制备单电池,并研究不同NiO/GDC质量比对粉体形貌及单电池电性能的影响.通过XRD、SEM以及电化学工作站等测试手段分别对粉体、物相及电池的电性能进行了测试与表征.结果表明,750℃下,3; H2O+H2还原气氛下测试,阳极中NiO/GDC质量比为5∶5时单电池具有最好的电池输出性能,最高开路电压为1.08 V,功率密度是0.4 W/cm2,极化电阻是1.0 Ω·cm2.     

SnO2/TiO2共掺杂氧化钽基固体电解质的制备和性能研究

采用草酸盐共沉淀法制备出具有三斜结构的共掺杂固体电解质Ta1-x-yTixSnyO2.5-δ(x=0.077,y=0～0.053)材料.利用X射线衍射分析、扫描电子显微镜、差热分析、阻抗分析等方法对该固体电解质进行了热性能和电性能分析,研究发现经Sn4+和Ti4+共掺杂之后,将氧化钽基电解质的高温三斜相稳定到了室温,在其结构中因掺杂产生更多氧空位从而提高了氧化钽基电解质的电导率.在973 K条件下,固体电解质Ta0.89Ti0.077Sn0.033O2.5-δ的离子电导率为0.76×10-1S/cm,活化能为0.696 eV,同时该共掺杂固体电解质具有较低的热膨胀系数3.78×10-6 K-1,属于低膨胀材料,具有良好的热稳定性和热循环性能.     

核壳结构的LSCF-GDC复合阴极的合成研究

采用静电纺丝技术制备结构均一的LSCF纤维,再利用溶胶法在纤维表面包裹一层GDC纳米粉体,构建核壳结构的LSCF-GDC复合阴极.运用DTA-TG、XRD、SEM、EDS和电化学工作站等测试手段分别对静电纺丝纤维的热性能、物相组成、粉体及单电池的形貌、阴极成分和单电池的电性能等进行了表征.研究结果表明,通过静电纺丝法可以制备纳米级LSCF纤维.该纤维经过800℃烧结后,形成直径在150～200 nm长度超过100μm的LSCF纤维.以Ce(NO3)3·6H2O、Gd(NO3)3·6H2O溶胶作为原料,与LSCF混合可以制备具有核壳结构的LSCF-GDC复合材料.该材料与通过涂刷烧结的方式可以在GDC//GDC+NiO半电池表面制备具有纤维结构的多孔阴极.制备后的电池为LSCF-GDC//GDC//GDC+NiO结构,该单电池在700℃下,以H2为燃料,空气为氧化气的最大功率密度为0.64 W/cm2,极化阻抗为0.04Ω·cm2.     

固相反应后复合电解质BaCe0.8Y0.2O2.9-Ce0.8Gd0.2O1.9的化学稳定性研究

采用溶胶-凝胶燃烧法和机械混合法制备摩尔比为1∶1的BaCe0.8Y0.2O2.9(BCY)-Ce0.8Gd0.2O1.9(GDC)复合粉末,并在1550℃烧结保温5h获得复合电解质片.对BCY-GDC复合电解质的化学稳定性以及电化学性能稳定性进行研究.结果表明:BCY-GDC复合电解质在1550℃烧结时会发生固相反应,形成以BaCe1-x-yGdxYyO3-α相为主的显微组织.固相反应后的BCY-GDC复合电解质在700℃3;CO2和沸水中的稳定性高于单相BCY;基于固相反应后BCY-GDC复合电解质的单电池在700℃下20h测试时间内的开路电压以及最大功率密度的稳定性均高于相同条件下BCY电解质的单电池.     

高锰酸钾对石墨烯及石墨烯-CaTi2O4(OH)2复合材料电化学性能的影响

由于CaTi2O4(OH)2导电性较差,为进一步提升CaTi2O4(OH)2电化学性能,将具有优异导电性的石墨烯材料与之复合.采用C为原料,H2 SO4为插层剂,KMnO4为氧化剂还原制得石墨烯,将两者复合制备石墨烯-CaTi2 O4(OH)2复合材料.研究高锰酸钾用量对石墨烯-CaTi2O4(OH)2复合材料电化学性能的影响.利用X射线衍射(XRD)和扫描电子显微镜(SEM)对样品的显微结构、形貌进行检测分析,采用恒电流充放电(CP)和循环伏安(CV)等技术测试其电化学性能.实验结果表明:当高锰酸钾用量5 g时,可以制备出氧化、还原程度良好,电化学性能优异的石墨烯,与CaTi2O4(OH)2复合制得样品电极,其电化学性能最优,在5 A/g的工作电流密度下,样品比电容高达394.2 F·g-1是纯CaTi2O4(OH)2电容值(162 F·g-1)的2.43倍.     

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.     

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 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.