NaSn2(PO4)3的水热合成与结构性能研究

应用水热合成技术制备了具有NASICON型结构的NaSn₂(PO₄)₃离子导体.研究了其结构与电导性能.结果表明,水热合成制备NaSn₂(PO₄)₃离子导体化合物,是一条新的途径,它比传统的高温固相反应方法更加方便有效,尤其容易获得较纯的物相及单晶,并且水热晶化产物与固相反应产物具有相同的结构和性能.     

铌酸锂多晶粉体的水热合成及表征

铌酸锂(LiNbO₃)晶体由于本身具有的优良性能在许多领域中都获得了广泛的应用.以LiOH·H₂O和Nb₂O₅为原料采用水热合成法成功地合成了铌酸锂多晶粉体,并采用FTIR谱、XRD谱和SEM对产物进行了表征.结果表明,采用水热合成法能够得到结晶完整的四方柱形LiNbO₃多晶粉体.同时考察了反应温度、晶化时间和Li源对水热合成产物的影响.     

AlPO4-5分子筛的水热及微波辐射法合成与表征——推荐一个研究型综合实验

介绍一个研究型综合实验——传统水热及微波辐射法合成AlPO4-5型分子筛及其表征。实验分别通过传统水热加热晶化及微波辐射加热晶化制备了AlPO4-5型分子筛,采用X射线粉末衍射仪(XRD)及红外光谱(FT-IR)法对产物的结构进行表征,产物的晶体形貌由扫描电子显微镜(SEM)进行表征,并用吸附/脱附等温线对产物的氮气吸附/脱附性能进行表征。     

乙二胺导向合成的微孔晶体磷酸钴的转化现象

以乙二胺为模板剂(SDA)合成微孔晶体磷酸钴, 可以得到多种不同的结构. 本文在合成四种不同结构类型的微孔磷酸钴(命名为CoPO-en-1, CoPO-en-2, CoPO-en-3, CoPO-en-4, en 为乙二胺的英文缩写)过程中发现, 它们之间不仅可以在水热合成条件下相互转化, 在焙烧处理条件下也能实现转化. 研究发现, 在水热合成过程中, CoPO-en-2、CoPO-en-4 分别是CoPO-en-1、CoPO-en-3 的晶化中间物, 在较低晶化温度下或者较高温度的晶化初期, 可以发现它们的身影. 一旦晶化温度升高或者晶化时间延长, 它们就分别转化为CoPO-en-1和CoPO-en-3. 在合成产物的热处理过程中发现: CoPO-en-2、CoPO-en-3、CoPO-en-4 都能够通过焙烧转化为CoPO-en-1. 这种现象表明, 几种微孔磷酸钴结构间的稳定性存在递变关系.     

前处理时间对Co_3O_4形貌及光催化性能的影响

以Co Cl2、Na2CO3为原料,以油酸钠(SOA)为表面活性剂,采用水热-热分解法合成了纯相尖晶石结构的Co3O4粉体。利用TG-DTA、XRD和SEM等手段跟踪反应过程,研究了不同水热时间对产物形貌和结构的影响,并根据实验结果分析了可能的反应机理及结构对光催化性能的影响。实验结果表明:制备前驱体的水热时间是影响产物形貌的关键因素,并且终产物的结构形貌很大程度上决定了其光催化性能。     

低温和低压下水热合成Na4Zr2(SiO4)3

以ZrOCl_2·8H_2O,Na_2SiO_3·9H_2O和NaOH为原料,在250℃约100bar的条件下,水热晶化合成出Na_4Zr_2(SiO_4)_3,并生长相应的单晶。讨论了水热反应及其条件.产物借助于XRD,Raman,~(29)Si MAS NMR以及阻抗谱技术进行了研究.结果表明产物具有与其他方法制备的Na_4Zr_2(SiO_4)_3相同的性质.     

以四乙基氢氧化铵-四甲基氯化铵为模板剂水热法合成 UZM-5 沸石

 以四乙基氢氧化铵 (TEAOH)-四甲基氯化铵 (TMACl) 为复合模板剂, 采用静态水热法合成了 UZM-5 沸石. 较为系统地考察了合成条件对 UZM-5 沸石的生长和晶化的影响, 并采用 X 射线衍射、红外光谱和热重等手段对样品进行了表征. 结果表明, 在 SiO2:(0.16~0.5)Al2O3:(0.4~1.0)TEAOH:(0.06~0.13)TMACl:20H2O 的初始反应物摩尔比条件下, 均能获得结晶良好的 UZM-5 沸石. 适宜的晶化温度为 403~423 K, 过高的晶化温度将导致无定形产物的生成. 当以硅溶胶为硅源时, 晶化只需 2 d, 而以硅酸或硅胶为硅源时则分别需要 4 d 和 5 d, 过长的晶化时间导致杂晶方钠石的生成. Na+ 的存在容易导致 UZM-9 沸石的生成, 影响产物的相选择性.     

简单方法合成α-MnO2和β-MnO2单晶纳米棒

通过简单的水热方法分别在150 ℃和220 ℃选择控制合成了单晶α-MnO2和β-MnO2纳米棒. 并用扫描电镜(SEM)、透射电镜(TEM)、能谱元素分析(EDX)、粉末X射线衍射(XRD)对产物进行了表征. 结果表明, 在水热反应过程中, 温度在控制合成α-MnO2和β-MnO2纳米棒中起到重要作用     

一种新颖层状磷酸镓化合物[Ga3(PO4)4](H3NCH2CH2)2NH2的合成与结构表征

晶体结构;水热合成;一种新颖层状磷酸镓化合物[Ga3(PO4)4](H3NCH2CH2)2NH2的合成与结构表征     

L-脯氨酸协助合成β-氢氧化镍和氧化镍花球及纳米三角片(英文)

以NH3·H2O和NaOH作为沉淀剂,通过水热方法在180℃,L-脯氨酸作用下,分别合成出了β-Ni(OH)2花球和纳米三角片。XRD结果表明合成出的β-Ni(OH)2产物是六方相,透射电镜(TEM)和场发射电镜(FESEM)表明花球直径为1~2μm,它是由厚15nm,边长110nm的三角片自组装形成的。对相应的β-Ni(OH)2前驱物在350℃空气下退火2h,分别得到NiO花球和纳米三角片。     

Synthesis, structure, and magnetic properties of a novel pillared layered iron(III) arsenate, [4,4'-bpyH2]3[Fe9(H2O)6F3(HAsO4)12(AsO4)2].2H2O

A three-dimensional iron arsenate [4,4'-bpyH2]3[Fe9(H2O)6F3(HAsO4)12(AsO4)2].2H2O, 1, has been synthesized using 4,4'-bipyridine as the templating agent under hydrothermal conditions. The structure is formed by FeO6, FeO3F3 octahedral units connected with HAsO4 and AsO4 units, forming one- and two-dimensional units in which the one-dimensional units act as a pillar. The presence of face-shared Fe-dimer units in the one-dimensional unit is noteworthy. Detailed magnetic studies indicate two possible magnetic interactions: antiferromagnetic interactions within the layer and a weak ferromagnetic polarization between the layers at very low temperatures through the Fe-dimer units.     

Na_（1－x）Zr（2－x）Nb_xP_3O_（12）系列化合物的水热晶化研究

采用水热晶化反应，制备出传统需要高温固相反应合成的掺杂ＮＡＳＩＣＯＮ化合物Ｎａ（１－ｘ）Ｚｒ（２－ｘ）ＮｂｘＰ３Ｏ１２（０＜ｘ＜１），并应用ＸＲＤ、ＩＲ方法对产物的晶体结构进行了研究，表明水热晶化产物是纯的物相并具有与ＮａＺｒ２Ｐ３Ｏ１２相同的结构．固体３１ＰＮＭＲ研究证实Ｎｂ（５＋）部分取代了Ｚｒ（４＋）所在位置，参与骨架的组成，并统计分布于结构中．水热晶化产物与固相反应产物具有相同的离子电导性能．     

Synthesis of FER Zeolite Using 4-(Aminomethyl) pyridine as Structure-directing Agent

This paper describes the synthesis of FER zeolite using commercially available 4-(aminomethyl)pyridine as organic structure-directing agent(OSDA). FER zeolites were prepared in mixtures with SiO₂/Al₂O₃ molar ratios in a narrow range and the resultant products possessed a typical flake-shaped morphology. The crystallization of FER zeolite was tracked in order to better understand the formation mechanism and the products obtained at different crystallization time were systematically characterized using multiple techniques. It showed that a majority of Si atoms and nearly all the Al atoms transformed into the solid phase during the hydrothermal synthesis. The rearrangement of inorganic species gave rise to zeolitic 5-membered rings(5-MRs) and 6-membered rings(6-MRs). Consequently, FER zeolite crystals were formed by the consumption of amorphous bulky gel/solid matrix. Tracking the synthesis process of FER can help.     

A new inorganic-organic hybrid iron(III) arsenate: (C2H10N2)[Fe(HAsO4)2(H2AsO4)](H2O). Hydrothermal synthesis, crystal structure, and spectroscopic and magnetic properties

A new iron(III) arsenate templated by ethylenediamine, (C2H10N2) [Fe(HAsO4)2(H2AsO4)](H2O), has been prepared by hydrothermal synthesis. The unit-cell parameters are a = 8.705(3) A, b = 16.106(4) A, c = 4.763(1) A, beta = 90.63(3) degrees; monoclinic, P2(1) with Z = 2. The compound exhibits a chain structure along the c-axis with the ethylenediammonium cations as counterion. The chains show isolated FeO6 octahedra with two HAsO4 and one H2AsO4 tetrahedra per FeO6 octahedron. The ESR spectrum at 5.0 K is isotropic with a g-value of 2.0, which remains practically unchanged at room temperature. Magnetic measurements indicate the presence of antiferromagnetic interactions. A value of -0.835 K for the J-exchange parameter has been calculated by fitting the magnetic data to a model for antiferromagnetic chains of spin S = 5/2.     

ZSM-34分子筛的合成及其催化甲醇转化制烯烃反应性能

以氯化胆碱为模板剂,采用水热合成法在较短的晶化时间内合成了OFF/ERI共晶体ZSM-34,考察了各种合成条件对产物的影响.通过调变合成参数可以获得不同ERI含量的ZSM-34.用X射线衍射、扫描电子显微镜和X射线荧光分析等对合成产物进行了表征.吸附实验显示,所合成的分子筛具有较大的孔容,其对正己烷的吸附容量为11.4%.HZSM-34分子筛对甲醇转化制烯烃(MTO)反应具有良好的催化活性和高的乙烯选择性,低碳烯烃(乙烯 丙烯)选择性高达86.0%,并且在反应过程中始终维持在较高的水平,不受甲醇转化率降低的影响.高温水蒸气处理后的分子筛酸性降低,大大抑制了MTO初始反应中丙烷的选择性,而初始低碳烯烃的选择性则明显提高.     

中孔分子筛MCM-41的合成与表征

以白炭黑和正硅酸乙酯为硅源,十二、十六烷基三甲基铵为模板剂,用水热法和室温直接法合成出中孔分子筛MCM-41,考察了对合成的影响因素,用红外光谱、吸附、孔分布、热分析等手段对这两种产物进行了表征。结果表明:这种分子筛可以在很宽的配比范围内获得,但较高水硅比更有利于合成;在水硅比较低的体系中得到了一种类MCM-41中孔相(亦应属于MCM-41),其XRD衍射峰较宽,2θ角度偏低,具有类似于无定形硅铝酸盐的骨架结构。     

Zur Synthese von kristallinen Metallsilicathydraten mit Schichtstruktur

Synthesis of Crystalline Metal Silicate Hydrates of Layer Structure The purpose of this paper is the synthesis of m etal s ilicate h ydrates by means of hydrothermal crystallization from the ternary systems M_2/nO? SiO₂? H₂O (M = Li, Na, K, Ca, Mg). The prepared products, the sodium silicates ilerite, magadiite, and kenyaite and a potassium silicate hydrate, are species of crystallization sequences of a hydrothermal quartz formation process at low temperatures. The product sequences, obtained under different crystallization conditions are given and discussed.     

Static and Ultrasonic‐assisted Aging Effects on the Synthesis of Analcime Zeolite

The synthesis of zeolite ANA under static hydrothermal conditions was performed accompanied by an additional static and ultrasonic‐assisted aging of the reaction mixture prior to crystallization. The aging process was compared with stirring‐assisted aging, microwave‐assisted aging and syntheses without any aging. The influence of aging time on the crystallization time of zeolite ANA was investigated. The static and ultrasonic‐assisted aging can shorten the crystallization time of the ANA phase. Moreover, ultrasonic‐assisted aging leads to altered morphologies of the particles. The products were characterized by X‐ray diffraction (XRD) and scanning electron microscopy (SEM).