Mg2+掺杂Li4Ti5O12陶瓷靶材的制备及其性能研究

本实验以Mg(OH)2作为镁源,将1wt;、2wt;、3wt;、4wt;、5wt;的Mg(OH)2粉末与纯Li4Ti5O12粉末球磨混合,使用粉末冶金的方法烧结制备出了Mg2+掺杂的Li4Ti5O12陶瓷靶材,分别研究了烧结温度为880 ℃、900 ℃、930 ℃、950 ℃、980 ℃时Mg2+掺杂Li4Ti5O12陶瓷靶材的收缩率、致密度和力学性能的变化情况;通过对Mg2+掺杂Li4Ti5O12陶瓷靶材进行XRD衍射分析和断面的SEM分析可以得出,Mg(OH)2的最佳掺杂量为4wt;,陶瓷靶材的最佳烧结温度为950 ℃.可以得到抗弯强度为83.189 MPa、相对密度为96.041;、维氏硬度为的364.26HV500、物相单一的Mg2+掺杂的Li4Ti5O12陶瓷靶材.     

表面活性剂辅助合成Y2O2S:Eu3+,Mg2+,Ti4+红色长余辉材料

以表面活性剂十二烷基硫酸钠为均匀分散剂,通过液相与固相相结合的方法制备了Y2O2S∶Eu3+,Mg2,Ti4+红色长余辉材料.采用X射线衍射(XRD)、扫描电镜(SEM)、激发与发射光谱、热释光谱等手段对材料进行了表征.研究结果表明,与高温固相法相比,样品的最低合成温度与最佳合成温度均降低了200～300℃,其发光特性没有改变,表面活性剂的添加影响了样品的形貌.同时,对表面活性剂引入后,Y2O2S∶Eu3+,Mg2+,Ti4+的生长机制和发光机理进行了讨论.     

SrTiO3/Mg6Ti5O16复合陶瓷的微波介电性能研究

通过传统固相烧结法制备了xSrTiO3-(1-x)Mg6Ti5O16微波介质陶瓷,并研究其晶体结构、显微结构及微波介电性能.xSrTiO3-(1-x)Mg6Ti5O16复合陶瓷主要含有MgTiO3、SrTiO3和Mg6Ti5O16三相;复合陶瓷晶粒分布紧密,尺寸大小不均匀;适当增加SrTiO3含量可以有效提高介电常数和品质因数,并使谐振频率温度系数趋于正值.1420 ℃烧结的3.8;SrTiO3-96.2;Mg6Ti5O16复合微波陶瓷可获得最佳微波介电性能:εr=17, Q×f =42729 GHz和τf=5 ppm/℃.     

Ti3C2 MXene复合材料改善PMMA-LiBH4的储氢性能

通过浸渍-还原的方法合成Ti3C2/rGO/MF(三聚氰胺泡沫)复合材料(TGMF),然后将TGMF与PMMA-LiBH4结合,形成PMMA-LiBH4/TGMF(PL/TGMF)复合材料.系统地研究了PL/TGMF的储氢性能.实验表明,与PL/GMF相比,PL/TGMF具有更低的初始放氢温度,且在300～400℃具有较快的放氢速率,虽然PL/TGMF的接触角略有减小,但仍具有较好的疏水性.机理研究表明:低温下LiBH4与PMMA反应生成Li3BO3和LiB5O8,高温下(300～400℃)LiBH4与PMMA、Ti3C2相互作用生成Li2B8O13和TiB12、TiB.     

铈掺杂二氧化钛的化学态分析

采用溶胶-凝胶法制备纯TiO2粉末和5mol; Ce掺杂TiO2粉末,利用X射线衍射仪(XRD)、X射线光电子能谱仪(XPS)和紫外-可见分光光度计(UV-Vis)表征样品的相变过程和化学态变化,主要探讨了Ce掺杂对TiO2相变温度、物相组成、化学态及吸收光谱范围的影响.结果表明:掺杂Ce抑制了TiO2的相转变和晶粒长大.随着热处理温度升高,Ce掺杂TiO2的晶格氧峰增强而吸附氧峰降低,而且Ti2p3/2结合能减小,Ce3+逐渐被氧化为Ce4+.掺杂Ce拓宽了TiO2的可见光谱吸收范围.     

La掺杂TiO2薄膜的制备及其光电流研究

采用溶胶凝胶-浸渍提拉法在ITO导电玻璃表面制备了纯TiO2薄膜和La掺杂TiO2薄膜,对其进行350℃、450℃、550℃保温2h热处理.利用XRD、SEM、EDS、XPS对样品结构、形貌、成分进行表征,利用电化学工作站对薄膜进行光电流测试,研究了La掺杂以及不同热处理温度对TiO2薄膜结构及光电流的影响.结果表明:La掺杂有细化TiO2晶粒和抑制锐钛矿相向金红石相转变的作用.随热处理温度提高,纯TiO2薄膜与La掺杂TiO2薄膜光电流密度均先增大后减小,450℃热处理后纯Ti02薄膜光电流密度为180 μA·cm-2,此温度下La掺杂TiO2薄膜光电流密度为650 μA·cm-2,是纯TiO2薄膜的3.6倍.     

放电等离子烧结制备LaTiO3的反应过程研究

采用放电等离子烧结方法制备LaTiO3材料.基于不同温度烧结样品的物相组成变化,对SPS烧结制备LaTiO3的反应过程进行研究.研究结果表明:SPS烧结制备LaTiO3的反应过程可以分为低温、中温和高温三个阶段.随着烧结温度升高,由于系统环境变化和高温氧缺位的形成,Ti的价态经历了Ti3+ →Ti4+→Ti3+/Ti4 +→Ti3+的转变.由于相变阻力的存在,LaTiO3并不能由原料直接生成,在低温和中温阶段要经历La2Ti2O7,La2/3TiO3,La5Ti5O17等中间相.LaTiO3相的生成主要发生在1400～ 1550℃,并在1550℃生成单相LaTiO3.     

溶胶-凝胶法制备高Mg含量Zn1-x MgxO薄膜

采用溶胶-凝胶法在石英玻璃基板上制备了ZB1-xMgxO薄膜,研究退火温度对高Mg含量Zn0.5Mg0.5O薄膜的相组成、相偏析及紫外-可见透过光谱中吸收边移动的影响,当退火温度≤500℃时,Zn0.5Mg0.5O薄膜未发生相偏析现象,且400℃退火处理制备的Zn0.5Mg0.5O薄膜的紫外-可见透过光谱中吸收边蓝移最大.因此,对于高Mg含量Zn0.5Mg0.5O薄膜,退火温度是影响Mg2+在ZnO中固溶度的关键因素,且400℃是其理想的退火温度.在此条件下研究了不同Mg含量对Zn1-xMgO(x=0～0.8)薄膜带隙调节的影响,随着Mg含量的增加,其紫外-可见透过光谱中紫外光区吸收边呈现规律性蓝移,光学带隙值Eg从纯ZnO的3.3 eV调节至4.2 eV.     

Mg-Si-Sn-Bi材料退火过程中微结构演变与热电性能

利用单质粉末冷压成型及高真空500℃-2h烧结制备了Mg-Si-Sn-Bi材料,随后对制备材料在真空下600℃退火处理,并对制备材料的组成和热电性能进行研究.结果表明,500℃烧结材料仅仅由Mg2Sn和Mg2Si两相混合物构成.材料600℃退火,部分化合物分解,Sn和Si首先以单质形式存在;随后Si融入剩余的Mg2Sn结构中,形成Mg2(Sn,Si)固溶体;Sn以金属纳米尺寸状态存在;分解的Mg与真空石英玻璃管内残留的氧反应生成MgO相.而且,退火时间延长,Mg2(Sn,Si)固溶体和纳米尺寸的金属Sn含量增多.材料中Mg2(Sn,Si)固溶体含量越多,Seebeck系数绝对值越大;材料中纳米尺寸的金属Sn含量越多,电阻率越小.含有纳米尺寸金属Sn的Mg-Si-Sn-Bi材料因Seebeck系数绝对值大和电阻率小,具有较大的功率因子.     

纳米分散颗粒Li1.2Ni0.2Mn0.6O2材料的制备及性能

以乙酸盐和一水合柠檬酸为原料,采用溶胶-凝胶法合成锂离子电池纳米级富锂锰基正极材料Li1.2 Ni0.2 Mn0.6 O2.X射线衍射(XRD)结果显示所得产物为结晶度良好、离子混排程度低的纯相结构材料;扫描电镜(SEM)结果显示所得材料为纳米颗粒(颗粒直径均在300 nm以内),且具有圆形或者正六边形形状结构,表面光滑,粒度分布均匀.研究了高温焙烧温度对Li1.2 Ni0.2 Mn0.6 O2材料结构形貌及电化学性能的影响,重点探讨了结构形貌对电化学性能的影响规律.实验结果表明:当焙烧温度为850℃和900℃时,材料的形貌结构更好,电化学性能更为理想.     

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。     

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.     

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。     

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.     

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.