废旧电池溶胶-凝胶法制备Mn-Zn铁氧体的研究

以硝酸溶解废旧碱性锌锰电池所得的溶液为原料,用溶胶-凝胶法制备出了具有尖晶石结构的Mn-Zn铁氧体.借助于XRD、IR和SEM技术,对制备过程进行跟踪检测并对纳米晶铁氧体的晶体形貌进行表征.研究表明:制备Mn-Zn铁氧体的适宜条件为:金属离子和柠檬酸的比例为1:1(mol),pH=5.0,干凝胶煅烧时间为2h,煅烧温度为650℃;所得产物基本为球形,具有粒径小,分散均匀的特点.     

溶胶-凝胶/燃烧法制备锰锌铁氧体及其吸波性能研究

采用溶胶-凝胶法制备了锰锌铁氧体Mn0.3Zn0.7Fe2O4,确定了适用于锰锌铁氧体制备的工艺条件,并利用XRD、SEM、TG-DSC和网络分析仪等对样品进行了表征.结果表明:溶液pH值约为7.0,柠檬酸与金属离子的摩尔比为1∶1,煅烧温度为1050℃,煅烧时间为3h时,所制得的Mn0.3Zn0.7Fe2O4铁氧体呈现单一的锰锌铁氧体相,颗粒尺寸约为160 nm,并且分布均匀.制得的Mn0.3Zn0.7Fe2O4铁氧体兼具介电损耗能力和磁损耗能力,并且在12.5～ 15 GHz频率范围内反射损耗均达到了-10 dB,表现出良好的微波吸收性能.     

溶胶-凝胶法制备V2O5微晶及其合成活化能研究

以NH4VO3和CO( NH2)2等为起始原料,采用溶胶-凝胶法制备了V2O5微晶.研究了煅烧温度对产物物相和显微结构的影响,以及反应的合成活化能.采用X射线衍射、扫描电镜等手段对产物进行了表征.结果表明,后处理温度为500℃可得到V2O5微晶,当反应温度超过600℃时,V2O5微晶表现出(001)晶面的取向生长特征.通过差热分析,计算得到其合成活化能为95.81 kJ/mol.     

AACH热分解法制备α-Al2O3超细粉末

以NH4Al(SO4)2与NH4HCO3为原料,采用共沉淀法制备出前驱物碳酸铝铵(AACH),并煅烧得到超细α-Al2O3粉末. 研究了pH值、滴加速度及醇水混合溶剂等因素对反应产物的影响,并对前驱物AACH的高温相变过程和α-Al2O3籽晶对θ-Al2O3→α-Al2O3相变的影响进行了分析.利用XRD、TEM和BET等对粉体的性能进行表征.结果表明:在醇水混合溶剂中控制反应体系的pH值为9～10,将硫酸铝铵溶液以＜18 mL/min的速度滴入碳酸氢铵溶液,可合成颗粒细小、粒度分布均匀且分散性优异的AACH前驱物.不含籽晶的AACH煅烧时α相完全转化温度为1150 ℃,获得α-Al2O3粒径约为100 nm,而α-Al2O3籽晶的加入可将完全转变温度降至1050 ℃,获得的α-Al2O3粒径约为70 nm.     

NH4F含量及煅烧工艺对氧化铝相变及α-Al2O3微观形貌的影响

为研究NH4F含量及煅烧工艺对氧化铝相变及α-Al2O3微观形貌的影响,向Al(OH)3粉体中引入不同质量分数的NH4F,经不同条件煅烧后获得Al2 O3粉体样品.采用X射线衍射仪和扫描电子显微镜进行物相分析和晶相形貌观察.结果表明,NH4F的引入可以显著降低Al2 O3的相变温度,含量5.0; NH4F的Al(OH)3在900℃保温2.5h全部转变为α-Al2O3,这比传统的转变温度低200～ 250℃.同时,随着NH4F含量的增加,α-Al2O3晶粒形貌由颗粒状变为平面六角片状.但是平面六角片状α-Al2 O3在1200℃是不稳定的,长时间煅烧时,α-Al2O3晶体又"熔解"为小颗粒晶粒.     

溶液燃烧法制备Mg2B2O5亚微米棒

以六水硝酸镁、硼酸、甘氨酸、尿素为原料,运用溶液燃烧法合成了Mg2B2O5亚微米棒.利用XRD,SEM,TPG-DTA表征手段对产物及产物前驱体进行表征.讨论了不同温度、燃烧剂、Mg∶B比例和煅烧时间对产物的物相、形貌的影响.确定合成Mg2B2O5亚微米棒的最佳工艺条件为甘氨酸做燃烧剂、Mg∶B=1:1、在900℃煅烧4h,得到的产物呈棒状,直径分布在200 ～400 nm之间,长径比分布在3～6之间.     

溶液燃烧法合成La和Ce共同改性的γ-Al2O3

采用溶液燃烧法,以硝酸铝,硝酸镧,硝酸铈为氧化剂,氨基乙酸为还原剂,制备La和Ce共同改性的γ-Al2O3。利用XRD、TG-DTA、TEM、XPS等分析手段对产物以及前驱体进行表征,系统考察煅烧时间、煅烧温度、反应物的摩尔配比等工艺参数对最终产物的组成和粒径的影响,并确定了最佳工艺条件。溶液燃烧法制备La/Ce/γ-Al2O3最佳反应条件为:硝酸镧和硝酸铈的物质的量比为2∶1,煅烧时间为4 h,煅烧温度为950℃。     

共沉淀法制备Al2O3-ZrO2复合纳米粉体

以ZrOCl2·8H2O、Al(NO3)3·9H2O、Y(NO3)3为原料,NH4HCO3 (AHC)为络合剂,采用共沉淀法制备Al2 O3-ZrO2复合纳米粉体.利用X射线衍射分析(XRD)、扫描电镜(SEM)、透射电子显微镜(TEM)、激光粒度分析仪等对Al2 O3-ZrO2复合粉体进行测试表征,详细研究了pH和AHC/Zr摩尔比对复合粉体的影响.结果表明,当前驱体的煅烧温度低于1200℃时,只形成t-ZrO2相,当煅烧温度达到1300℃时,α-Al2O3相开始形成;沉淀反应的pH和AHC/Zr摩尔比对Al2O3-ZrO2复合粉体的产率有很大的影响.在pH7、AHC/Zr =4.5:1的条件下制备前驱体,经过1300℃煅烧2h得到两相纯度高,分散性能好,粒度分布窄,平均粒径为0.75 μm的Al2O3-ZrO2复合粉体.     

煅烧温度对络合溶胶-凝胶法制备ZnGa2O4微晶形貌及光催化性能的影响

采用EDTA络合溶胶-凝胶法制备了尖晶石结构的ZnGa2O4微晶.通过XRD、SEM等分析方法对ZnGa2O4微晶进行了测试和表征.研究了不同煅烧温度对其物相组成、显微结构及光催化性能的影响.结果表明,以乙酸锌和氧化镓为反应原料,以乙二胺四乙酸为络合剂,在650～800℃能合成单一物相的ZnGa2O4微晶.在700℃时可以成功制备八面体形的ZnGa2O4微晶,在800℃时可以合成棒状的ZnGa2O4微晶;随着温度从650～800℃逐渐升高,其对罗丹明B的光催化降解性能逐渐提高.     

碳酸盐沉淀法合成Nd3+:Y2O3激光陶瓷纳米粉体

以Y2O3粗粉、Nd2O3、硝酸和NH4HCO3为原料,通过共沉淀法制备了Nd3+:Y2O3透明激光陶瓷纳米粉体,并采用TG/DTA、XRD、FTIR、TEM以及EDS等测试方法对粉体性能进行了表征.结果表明,在先驱物中添加适量SO42-离子能减轻煅烧得到的Nd3+:Y2O3粉体的团聚,使粉体粒度均匀并呈球形分布.在1100 ℃煅烧4 h所得粉体粒度均匀,粒径在50～70 nm之间,具有较好的分散性,适合作为制备透明激光陶瓷的粉体材料.     

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.     

Crystal structures of the cis and trans isomers of a tetrathia[3.3.3.3]cyclophane

Both the cis and trans isomers of 3,11,18,26-tetrathiatricyclo[26.2.2.1^5,9.2^13,16.1^20,24] hexatriaconta-5,7,9,20,22,24-hexene have been prepared and structurally characterized. Each of these centrosymmetric tetrathia dimers includes two cyclohexane rings in chair conformations with either 1,4-cis or 1,4-trans bonding and two meta-substituted benzene rings. The cis isomer packs into the monoclinic space group P2₁/a with a = 10.485(3)Å, b = 10.3956(18)Å, c = 14.1343(10)Å, = 105.200(13)°, Z = 2 and refined to an R factor of 0.046. The trans isomer crystallizes in the monoclinic space group P2₁/c with a = 10.7217(12)Å, b = 5.6797(7)Å, c = 25.415(5)Å, = 96.001(12)°, Z = 2 and refined to an R factor of 0.043. In the cis structure each benzene ring faces a cyclohexane ring while in the trans structure the cyclohexane rings face one another.     

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.     

电沉积法制备ZnO纳米棒阵列及其发光特性

本文以掺F的SnO2导电玻璃为基板,以硝酸锌水溶液为电解液,采用三电极恒电位体系电沉积制备ZnO纳米棒阵列,系统考察了硝酸锌浓度和沉积电位等工艺参数对ZnO纳米棒阵列的微观形貌及其发光性能的影响规律.结果表明,硝酸锌浓度和沉积电位对纳米棒阵列的形貌有显著影响,控制适宜的工艺条件可以制备出直径分布均匀、结晶性好且纯度高的六方纤锌矿ZnO纳米棒阵列.荧光光谱分析表明,电沉积制备出的ZnO纳米棒阵列在385 nm附近有一个强荧光发射峰,且发光性能稳定、对纳米棒阵列微观形貌的细微变化不敏感,使其在发光二极管和激光器等领域具有广阔的应用前景.