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以高锰酸钾(KMnO4)和硫酸铵((NH4)2SO4)为主要原料,在150℃反应16h,水热法生长了棒状MnOOH晶体,然后以合成的棒状MnOOH晶体为前驱物,在硫酸溶液中,130℃水热反应12h,生长了棒状MnO2晶体.探索了KMnO4和(NH4)2SO4的用量以及反应温度对合成棒状MnOOH晶体的影响.利用X射线粉末衍射(XRD)、透射电子显微镜(TEM)和选区电子衍射等(SAED)等手段对产物进行了表征.结果表明,产物MnOOH为单斜结构的纯相,呈现棒状形貌,其平均直径约为72nm, 长度近9.2μm,显示单晶特性;产物MnO2为四方结构的纯相,呈现棒状形貌,其平均直径约为83nm, 长度达11μm,显示单晶特性. 相似文献
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利用水热法,以Zr(SO4)2·4H2O为原料,添加Na2SO4后合成出花状和棒状形貌可控的纳米ZrO2纳米粉体.随着SO42-浓度升高,t-ZrO2含量逐渐减少,颗粒微观形貌由三维花状变为二维棒状.利用XRD和SEM研究了Na2SO4对ZrO2粉体相结构、微观形貌和粒径的影响规律.确定了SO42-对结构和形貌调控的关键性作用,并提出了可能的成型机理.花状ZrO2对罗丹明B有良好的吸附性能,吸附容量达到20 mg/g,而棒状ZrO2的吸附性能一般,仅为4 mg/g. 相似文献
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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. 相似文献
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采用改进的垂直布里奇曼(Bridgman)法自发成核生长AgGaS2晶体,在生长初期对生长安瓿籽晶袋进行上提回熔,生长出外观完整、无裂纹的大尺寸AgCaS2单晶体.采用XRD对晶体进行分析,获得了(112)、(001)和(101)面的高强度尖锐衍射峰.采用不同配比的腐蚀剂对晶体(101)、(112)及(001)晶面进行化学腐蚀,然后采用金相显微镜和扫描电镜观察,结果显示,(101)晶面蚀坑为清晰的近似三角形的四边形蚀坑,(112)晶面蚀坑为清晰的近似三角锥形,(001)晶面则呈现互相垂直的腐蚀线.初步分析了不同蚀坑的形成原因,计算出(101)和(112)面蚀坑密度约为105/cm2数量级.结果表明,改进方法生长出的大尺寸AgGaS2单晶体结构完整、位错密度低,质量较好. 相似文献
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水热法合成Mnx Zn1-xO微晶体 总被引:1,自引:1,他引:0
本文采用水热法合成了MnxZn1-xO晶体,水热反应条件为3mol·L-1KOH作为矿化剂,填充度为35;,温度为430℃,在Zn(OH)2中添加一定量的MnO2为前驱物,反应时间为24h.通过X射线能谱仪测量了晶体中的Mn含量,随着前驱物中MnO2含量的增加,晶体中Mn的原子百分比随着增加,Mn最大原子百分比含量超过了2;,晶体的形貌具有纯ZnO晶体的六角柱形特征.显露柱面m{1010}、锥面p{1011}、负极面O面{0001}和正极面{0001}.晶体直径为50~200μm,高度为20~100μm. 相似文献
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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。 相似文献
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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。 相似文献
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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. 相似文献
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A. L. Bingham J. E. Drake C. Gurnani M. B. Hursthouse M. E. Light M. Nirwan R. Ratnani 《Journal of chemical crystallography》2006,36(10):627-630
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). 相似文献
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Tosha Barclay Wallace Cordes Fu-May Yang Shaw-Tao Lin 《Journal of chemical crystallography》1997,27(6):359-362
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. 相似文献
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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. 相似文献
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Lin Zhu Karl Seff Thomas Witzke Lutz Nasdala 《Journal of chemical crystallography》1997,27(5):325-329
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 Rw=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. 相似文献
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Jerry P. Jasinski Ray J. Butcher Anil N. Mayekar H. S. Yathirajan B. Narayana B. K. Sarojini 《Journal of chemical crystallography》2009,39(10):761-765
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. 相似文献
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Zun-Ting Zhang Xue-Ling Zhang Bo-Lun Yang Yao-Dong Zhang 《Journal of chemical crystallography》2006,36(7):407-411
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. 相似文献