一步水热法制备无水硫酸钙晶须

以生石膏为原料,六水氯化镁为形貌控制剂,采用水热法一步合成了无水硫酸钙晶须.借助SEM、TEM、XRD和XPS等测试手段考察了水热条件对无水硫酸钙晶须的影响,研究了无水硫酸钙晶须的生长过程.结果表明:镁/钙摩尔比n(MgCl2·6H2O)/n(CaSO4· 2H2O)=2.5,反应温度180℃,反应时间2h,可生长出长度为20 ～ 40 μm,直径0.5～2 μm的无水硫酸钙晶须.无水硫酸钙晶须生长过程为:片状CaSO4·2H2O-纤维状CaSO4·0.5H2O-纤维状CaSO4.     

NH4+-NH3缓冲体系制备碱式硫酸镁晶须及生长机理

碱式硫酸镁晶须的分子式为xMgSO4·yMg(OH)2·zH2O,是一种人工合成具有一定长径比的无机功能材料.作为填充剂,可提高材料的抗拉强度等机械性能,也可以起到阻燃的作用.在NH4+-NH3缓冲体系,用常压一步法制备长度为10～30μm,直径为0.05～0.3μm,长径比为30～150的MgSO4·5Mg(OH)2·3H2 O晶须.采用XRD、SEM、TG、TEM对产品进行表征,结合表征结果对反应浓度、反应温度、反应时间和陈化时间等影响因素进行研究.对碱式硫酸镁的生成机理进行第一性原理分析,碱式硫酸镁晶须生长习性符合位错螺旋生长机制.采用缓冲体系稳定溶液酸碱性,降低反应溶液的非理想性,可以使晶体在非受迫情况下定向生长,为进一步工业应用,实现低能耗生产碱式硫酸镁晶须提供了重要参考.     

硫酸镁与氨水水热反应合成碱式硫酸镁晶须

以MgSO4·7H2O和氨水为原料进行MgSO4·5Mg(OH)2·3H2O晶须(MOS)制备的实验.研究了水热反应温度、时间、镁离子浓度及原料配比对水热反应后液相及固相组成和MOS形貌结构的影响.结果表明,合成MOS的最优条件为反应温度190℃,反应时间5h,镁离子浓度3 mol/L,n(七水硫酸镁)∶n(氨水)比例为0.6∶1.合成MOS的母液能够实现循环利用,所得产品为形貌结构完整的MOS晶须.     

含钛电炉熔分渣浸出废液合成莫来石晶须及热稳定性研究

通过共沉淀-熔盐法成功地用含钛电炉熔分渣浸出废液制备出了高附加值的莫来石晶须.通过对反应原料Al/Si(摩尔比)、煅烧温度、保温时间等因素的系统研究,确定了合成莫来石晶须的最佳条件,即在Al/Si为3,煅烧温度为950℃,保温时间为5h条件下,制备出了结晶性好、尺寸均一及热稳定性能较好的莫来石晶须,其直径在20～150 nm,长度在0.5～1.5 μm,长径比大于10,莫来石晶体的生长方向平行于[001]方向,沿c轴方向生长.在最优条件下制备出的晶须能在较宽的范围内(室温～ 1000℃)下保持较好的热稳定性.     

常压化学水解反应生长氧化锌晶体

采用ZnCl2·2H2O在常压下高温水解反应生长ZnO晶体,反应温度为500℃.当以SiC为衬底时,可以获得六棱柱形氧化锌晶体,直径约为10μm,长为30～100 μm.当衬底为蓝宝石时,氧化锌沿[0001]呈定向柱状生长,柱的直径为5～10 μm,柱之间具有较多的内部缺陷.当以ZnO为衬底时,在{0001}面,形成连续膜,表面扫描电镜分析表明,晶体具有明显的极性生长特征,[0001]方向呈螺旋柱状生长.在{0001}面,晶体的平整性较好,呈现台阶性生长.     

人工可控氢氧化镁晶须生长

从负离子配位多面体生长基元模型出发,根据大维度生长基元的结构特性,讨论了人工可控氢氧化镁晶须生长,主要介绍了多元醇法及镁盐过饱和度法.多元醇法的实质是醇中的羟基在一定条件下与大维度生长基元中的羟基发生假联结(即吸附),使得与多元醇发生了假联结的晶面生长速率大大减小或甚至停止生长,而其他晶面仍然保持原有的速率生长以致形成晶须.镁盐过饱和度法就是使得生长基元[Mg-Ax](x-2)-(A≠OH-)的浓度很大,且要远比[Mg-(OH)x](x-2)-组分浓度大4倍以上,以先形成碱式镁盐晶须,碱式镁盐晶须再与适当的碱液反应,即可制备得氢氧化镁晶须.     

丁醇-变频微波-水热法制备优质碱式硫酸镁晶须及表征

以MgSO4·7H2O、NaOH为原料,采用丁醇-变频微波-水热法制备了优质碱式硫酸镁晶须.样品用XRD,SEM,TEM,TG-DTA进行了物相、粒度、晶体形貌结构和热分析.考察了传统的水热法、变频微波-水热法、丁醇-水热法、丁醇-变频微波-水热法四种工艺对碱式硫酸镁晶须晶形、结构、分散性的影响.实验发现,在水热反应体系中加入体积分数为25;的丁醇,并采用变频微波加热,调节微波炉反应温度T=130 ℃,反应时间t=9 h时可获得粒度分布均匀、晶形好、分散性好、表面光滑、缺陷少的优质碱式硫酸镁晶须.透射电镜下估算晶须直径约为0.8～1.1 μm,长度约为60～100 μm.初步分析了微波、丁醇对碱式硫酸镁晶须生长的作用.     

拓扑化学法制备棒状(KxNa1-x)NbO3粉体

以Na2CO3、K2CO3、Nb2O5和KCl为原料,采用拓扑化学反应法合成出一维方向生长钙钛矿结构的棒状KxNa1-x NbO3 (KNN)粉体.首先采用熔盐法合成出棒状的前驱体K2Nb8O21晶体,系统研究了Nb2O5与KCl的起始质量比、合成温度对kNb8O21晶体显微结构和形貌的影响,研究发现当Nb2O5与KCl的质量比为3/8,850℃下保温3h可以获得长度为80～100 μm,直径为3～8 μm的棒状K2Nb8O21晶体,且晶体沿[100]方向生长;然后以棒状的前驱体K2Nb8O21为模板晶粒,采用拓扑化学反应法制备出棒状KNN晶体,研究了Na2 CO3的添加量、烧成温度和保温时间对棒状KNN晶体显微结构和形貌的影响.结果表明:添加过量10wt;的Na2CO3,在900℃下保温3h可以获得沿[001]方向生长的棒状KNN晶体,其中K/Na =47.31/52.69,接近1/1,其长度和宽度分别为30 ～ 50 μm和2～6 μm.     

烧结助剂对硼酸镁晶须晶体结构与抗压强度的影响

本研究以硼酸和碱式碳酸镁为原料,采用原位合成法制备了硼酸镁晶须,通过热分析(TG)、X射线衍射(XRD)和扫描电子显微镜(SEM)对样品进行表征,考察不同烧结助剂对硼酸镁晶须晶体结构、表面形貌、孔隙率及抗压强度的影响.实验结果表明,当未添加烧结助剂时,孔隙率为62.57;,抗压强度为10.32 MPa,晶须直径为0.2～0.6 μm,长度为3～5 μm.添加烧结助剂会降低硼酸镁晶须的孔隙率并提高其抗压强度.当烧结助剂为MgF2时,孔隙率为51.77;,抗压强度为14.51 MPa;当烧结助剂为Na4P2O7时,孔隙率为43.79;,抗压强度为21.09 MPa.     

硫酸钾熔盐法微硅粉制备莫来石晶须研究

以微硅粉和Al2(SO4)3为反应物料,硫酸钾为熔盐介质,分别在800℃、900℃、1000℃和1100℃下煅烧并保温1h,溶解、过滤、烘干后得到白色疏松状莫来石粉体.利用XRD和SEM对合成粉体进行物相分析和显微形貌观察.结果表明:1000℃为合成莫来石最佳温度,合成的莫来石晶须直径为0.1 ～0.8 μm,长度为4～5 μm.同时对莫来石晶须的形成机理进行了探讨.     

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.