液固相水热法制备氧化硅纳米线

利用液固相水热反应方法, 以硅溶胶为硅源, 在三价铁辅助下与乙二胺的水溶液在180 ℃反应4 d后生成具有P21212空间群结构的单晶氧化硅纳米线. 用扫描电子显微镜、透射电子显微镜和多晶X射线衍射对制备的样品进行了表征, 系统研究了有机胺、金属盐、反应时间及反应温度等条件对氧化硅纳米线生长的影响. 结果表明, 随着有机胺碳链的增长, 产物形貌逐渐由纳米线转变为纳米片; 金属阳离子的存在对纳米线形貌有较大的影响, 而阴离子的存在并不影响纳米线的生成; 过低的铁含量导致反应进行不完全, 而过多的铁盐加入则会导致反应中剩余铁氧化物吸附到氧化硅纳米线表面, 进而影响到产物纯度; 反应时间延长及反应温度的提高都有利于氧化硅纳米线的生长. 最佳反应条件为: 有机胺为乙二胺, 硝酸铁为铁源, 硅溶胶为硅源, 硅/铁摩尔比为1∶0.4, 乙二胺与水的体积比为8∶5, 温度为180 ℃.     

Hydrothermal Synthesis of Nanorods and Nanowires of Mg/Al Layered Double Hydroxides

Layered double hydroxides (LDHs) are a class of synthetic anion clays, characterized by the formula[MⅡ1-xMⅢx (OH)2]x (An- )x/n·yH2O (where M =metal and A = anion, usually carbonate)[1-3]. A large number of LDHs with a wide variety of M Ⅱ-M Ⅲ cation pairs including M Ⅰ-M Ⅲ ( e. g. , Li-Al ) and M Ⅱ-MⅣ( e. g. , Co-Ti) have been reported. Thus the identities of the cations(MⅠ , MⅡ , MⅢ and MⅣ) and the interlayer anion (An-) together with the value of the stoichiometric coefficient (x) may vary widely, giving rise to a large class of isostructural materials.     

Na6[Ti5O12(OH)2]: A New Titanate Containing $\rm{{_{\infty }^{1}}}$[Ti5O12(OH)2]6− Ribbons

Na₆[Ti₅O₁₂(OH)₂] is the first structurally characterized sodium oxohydroxotitanate. The compound can be prepared via hydrothermal treatment of TiO₂ (Anatas) in NaOH (10n ) for 96 h at 250° in an autoclave. The crystal structure of Na₆[Ti₅O₁₂(OH)₂] consists of infinite ribbons [Ti₅O₁₂(OH)₂]^6?. The orthorhombic arrangement has Pbcn (No. 60) symmetry with the lattice constants a=18.668(4) Å, b=6.5333(13) Å, and c=9.829(2) Å.     

Hydrothermal Synthesis and Characterization of Per ovskite PbTiOs3Powders from Different Precursors

Perovskite-type of PbTiO₃ fine powders which are homogeneous in physic-chemical properties has been hydrothermally synthesized from the different precursors. The borderline reaction conditions, such as temperature and time, for the formation of PbTiO₃ were established and the effect of the precursor on the particle properties was investigated. As a precursor, Pb-Tialko-carbonate xerogel dispersed in 2-methoxyethanol was found to be effective for the synthesis of the PbTiO₃ powders with a lower agglomeration and a simple mode of particle-size.     

Hydrothermal Synthesis and Characterization of Perovskite PbTiO_3 Powders from Different Precursors

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水热-热解法制备具有一维结构的Co3O4多晶

采用温和的水热-热解法, 在一定温度下, 通过调节Na2CO3溶液和可溶性钴盐的摩尔比控制产物的形貌, 得到具有一维结构的水热产物. 以该产物为前驱体制备了具有一维结构的Co3O4多晶. 以六次甲基四胺、尿素等代替Na2CO3溶液作为沉淀剂, 均得到了一维纳米结构的Co3O4, 表明CO2-3在水镁石CoO2层间的嵌入是得到一维结构水热产物的关键.     

不同形貌TiO2的水热合成及对苯酚的降解研究

采用水热合成法, 通过对溶液的pH值、反应物配比、陈化温度及陈化时间等条件的控制, 合成出不同晶型及形貌的TiO2纳米粒子. 结果表明, 溶液的pH＝11, n(钛酸丁酯):n(三乙醇胺)＝1:2, 陈化温度为150 ℃, 陈化时间为48 h时, 能得到较规则的、长径比约为4:1的棒状TiO2. 当溶液pH<10时, 得到球形的TiO2纳米粒子; 陈化时间为24 h时, 得到纺锤形TiO2纳米晶. 以上合成的纳米粒子均为锐钛矿型, 但当溶液的pH>12时, 则得到板钛矿型TiO2粒子. 以苯酚为降解模型, 考察了不同形貌TiO2的光催化活性.     

中性介质中PbTiO3粉末的水热合成与表征

作为一种重要的铁电材料,钙钛矿(PE)结构的PbTiO3因具有较高的居里温度(475 ℃)和优异的铁电性质而得到广泛应用.如何获得高质量PbTiO3粉末以改进电子器件性能一直是研究的热点课题,有关PbTiO3的大量工作集中于其粉末的合成与性能的研究[1,2].与其它方法相比,水热法在合成粉体材料方面表现出许多优越性,如粉体颗粒较均匀,形状可控制等,因此,近年来对水热法合成PbTiO3粉末有较多研究报道[3,4].     

不同TiO2原料制备一维钛酸盐纳米材料

以不同二氧化钛为原料, 用水热法制备一维钛酸盐纳米材料. 原料一次粒径和晶体结构对一维纳米钛酸盐的形貌和结构的影响很大. 原料的一次粒径越小, 反应过程中产物的形貌和晶相转变越快; 纯锐钛矿相有利于钛酸盐纳米管的形成, 而少量金红石相则有利于纳米管向纳米线的进一步转变和晶相转变.     

稀土改性钛酸铅微粉的水热合成及其性能研究

用水热法合成了几种稀土（Ｌａ，Ｐｒ，Ｎｄ，Ｓｍ，Ｅｕ）和锰掺杂改性的钛酸铅（ＰｂＴｉＯ３，简称ＰＴ）陶瓷微粉，研究了掺Ｌａ和Ｍｎ的ＰＴ固溶体的四方（铁电）相与立方（顺电）相之间的相变，掺杂Ｌａ（ｘ（Ｌａ）＝０．０４）和Ｍｎ（ｙ（Ｍｎ）＝０．０１）的ＰＴ固溶体的居里温度大约为４００℃，测定了稀土掺杂量（ｘ＝０．０４～０．０８）与其压电性能之间的关系，随Ｌａ掺杂量的增加，ＰＴ固溶体的ｄ３３增大，ｇ３３     

原硅酸镉纳米线的合成与表征

硅酸盐因其基本结构单元[SiO4]四面体可通过共用顶点连接成各种结构形式,易形成具有大比表面积的多孔结构,且具有良好的热稳定性和化学稳定性,目前已广泛用于选择性催化、分子筛、气体的吸附与分离等领域．另外,硅酸盐还是一类优良的发光材料基质．如Mn^2 或其它稀土离子激活的Zn2SiO4、Mg2SiO4和CdSiO3等．由于原料来源广泛和价格低廉．硅酸盐的研究已引起人们的关注．     

Effect of Urea on the Morphology of Co3O4 Nanostructures and Their Application for Potentiometric Glucose Biosensor

In this study, an effect of different concentrations of urea on the morphology of cobalt oxide (Co₃O₄) nanostructures was investigated. The Co₃O₄ nanostructures are fabricated on gold coated glass substrate by the hydrothermal method. The morphological and structural characterization was performed by scanning electron microscopy, and X‐ray diffraction techniques. The Co₃O₄ nanostructures exhibit morphology of flowers‐like and have comprised on nanowires due to the increasing amount of urea. The nanostructures were highly dense on the substrate and possess a good crystalline quality. The Co₃O₄ nanostructures were successfully used for the development of a sensitive glucose biosensor. The presented glucose biosensor detected a wide range of glucose concentrations from 1×10^?6 M to 1×10^?2 M with sensitivity of a ?56.85 mV/decade and indicated a fast response time of less than 10 s. This performance could be attributed to the heterogeneous catalysis effect at glucose oxidase enzyme, nanoflowers, and nanowires interfaces, which have enhanced the electron transfer process on the electrode surface. Moreover, the reproducibility, repeatability, stability and selectivity were also investigated. All the obtained results indicate the potential use of the developed glucose sensor for monitoring of glucose concentrations at drugs, human serum and food industry related samples.     

Hydrothermal Synthesis and Phase‐, Morphology‐Evolution Mechanism of Lead Titanate Nanostructures Assisted with Tetramethylammonium Hydroxide

Lead titanate nanostructures with different phases and morphologies, layered hexagonal PbTiO₂(CO₃)_0.3‐ (NO₃)_0.35(OH) nanosheets, pyrochlore Pb₂Ti₂O₆ nanodendites, pre‐perovskite PbTiO₃ nanofibres and perovskite PbTiO₃ nanoplates, have been synthesized via a conventional hydrothermal route assisted with different concentrations of tetramethylammonium hydroxide (TMAH). X‐ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and high‐resolution TEM (HRTEM) were employed to characterize the phase, morphology and growth behavior of the synthesized samples. The results reveal that at low TMAH concentration the obtained samples are mainly of PbTiO₂(CO₃)_0.3(NO₃)_0.35(OH) nanosheets. With the TMAH concentration increasing, the obtained samples change to pyrochlore Pb₂Ti₂O₆ nanodendites, pre‐perovskite PbTiO₃ nanofibres and perovskite PbTiO₃ nanoplates in turn. With the basis of the experimental results, the phase‐ and morphology‐evolution mechanism of the lead titanate nanostructures is discussed by combining the analysis of the lattice structure feature and the properties of TMAH.     

水热法制备表面修饰的钛酸锶纳米微粉

以工业原料和常用试剂TiCl4、Sr(NO3)2和KOH为基础原料,通过添加表面活性剂十二烷基苯磺酸(DBS),采用水热法制备出表面包裹有DBS的钛酸锶纳米微粉,并应用红外光谱,X射线衍射谱,透射电子显微镜,热分析等一系列手段对其微结构进行了表征.结果表明:样品为表面包裹有DBS的钛酸锶纳米微粉,其形状较为规则,粒度分布较窄,单分散性较好.粒子的平均粒径为120nm,包裹膜的平均厚度为6nm左右.根据X光谱测量,表面修饰后的钛酸锶纳米微粉均以立方相存在.一般体相钛酸锶微粉为极性粉体.而表面修饰后的钛酸锶纳米微粉能够较为稳定地悬浮于非极性液体如正己烷中,说明SrTiO3粉体的极性表面被DBS包裹后,变为非极性.     

超细钛酸钡粉体的水热合成

以偏钛酸和氢氧化钡为原料,用水热反应制备了超细钛酸钡粉体,其结构经XRD和-IEM表征。粒径60nm-100nm。较佳的反应条件为：偏钛酸20mmol,n(Ba)：n(Ti)=1．2,于240℃反应8h,加入少量异丙醇可明显改善粉体的分散性能。     

水热-固相热解法制备不同形貌的四氧化三钴纳米微粉

以氨水和氢氧化钾水溶液为沉淀剂,利用沉淀-固相热解法和中压水热-固相热解法,制备了不同形貌的Co₃O₄纳米微粉.在水热条件下,得到了立方和六角片状的Co₃O₄微粉,采用XRD和TEM等手段跟踪反应过程并表征产物,在此水热反应体系中影响产物Co₃O₄形貌的主要因素是pH值和NO₃^-.     

Hydrothermal synthesis of nickel hydroxide nanostructures in mixed solvents of water and alcohol

Nickel hydroxide nanosheets and flowers have been hydrothermally synthesized using Ni(CH₃COO)₂·4H₂O in mixed solvents of ethylene glycol (EG) or ethanol and deionized water at 200 °C for different time. The phase and morphology of the obtained products can be controlled by adjusting the experimental parameters, including the hydrothermal time and the volume ratio of water to EG or ethanol. The possible reaction mechanism and growth of the nanosheets and nanoflowers are discussed based on the experimental results. Porous nickel oxide nanosheets are obtained by heating nickel hydroxide nanosheets in air at 400 °C. The products were characterized by using various methods including X-ray diffraction (XRD), fourier transform infrared (FTIR), transmission electron microscopy (TEM), selected-area electron diffraction (SAED), field emission scanning electron microscopy (FESEM). The electrochemical property of β-Ni(OH)₂ nanosheets was investigated through the cyclic voltammogram (CV) measurement.     

水热法制备三维网状TiO2纳米线薄膜及其光电化学性能

为了构建纳米二氧化钛(TiO2)的特殊结构以提高TiO2纳米材料的光催化性能, 利用水热法在钛箔表面制备了三维网络结构的TiO2纳米线薄膜(W-film). 通过场发射扫描电子显微镜(FESEM)及X射线衍射(XRD)仪对样品进行了表征. 结果表明, 三维网络TiO2纳米线薄膜是由大量非定向生长的锐钛矿型纳米线组成, 直径为10-30 nm, 长度大于5 μm. 利用紫外-可见分光光度计(UV-Vis)对W-film 进行光学性能研究, 结果表明在350-700 nm波长范围内W-film的吸光度均大于TiO2纳米粒子(P25)薄膜(P-film)的吸收度, 同时吸收带边发生红移, 且吸光度随水热时间增加而增加. 进一步在Na2SO4溶液中研究了W-film的光电化学性能, 结果表明其光电化学性能较P-film优异. 并以甲基橙为目标降解物考察了W-film的光催化性能. 在相同测试条件下, W-film光催化降解甲基橙的速率是P-film的2.3倍, 展示了良好的应用前景. 这种复合W-film电极兼有柔性和可外加电场的双重优点, 拓展了TiO2薄膜的应用领域.     

Direct Synthesis of Nanocrystalline Hydroxyapatite by Hydrothermal Hydrolysis of Alkylphosphates

Summary.  The influence of reaction conditions (temperature, type of catalyst, time) on the base-catalyzed reaction of mono-, di-, and trialkylphosphates (alkyl = methyl, ethyl, i-propyl, n-butyl) with Ca²⁺ ions and on the structure and composition of the reaction products was studied. The composition of the calcium phosphates depends mainly on the reaction temperature. At temperatures below 100°C, a nanocrystalline solid product transforming into dicalcium phosphate by heating (calcination) was found. Pure nanocrystalline hydroxyapatite was prepared by hydrothermal synthesis at 160°C from mono- and dialkylphosphates. The size of hydroxyapatite crystallites was about 1 nm, the particle size about 150 nm. Agglomerated particles of hydroxyapatite larger than 2 μm were prepared at 200°C. Hydrothermal reaction of trialkylphosphates with Ca²⁺ ions at 200°C produced CaHPO₄. The experimental results were used to propose a reaction mechanism for base-catalyzed hydrothermal reactions of alkylphosphates with Ca²⁺ ions. Received October 4, 2001. Accepted (revised) November 19, 2001