温和条件下混合碱辅助水热合成硅酸镁纳米管

在混和碱的辅助下, 以普通氢氧化镁和二氧化硅粉末为原料在温和条件下高效合成硅酸镁纳米管。采用XRD, TEM, FTIR, 氮气吸附等多种手段对产物进行了表征, 并对其合成过程进行了研究。结果表明氢氧化钠和氢氧化钾的共融液能提高反应物间的溶解性, 促进反应可以在温和条件下加快进行。250℃下合成硅酸镁纳米管, 传统水热法至少需要7 d, 混合辅助水热合成只需36 h。与传统的水热法相比, 混和碱辅助的水热法是一种温和且高效的过程。     

高分子辅助水热制备单晶碲纳米管

Te single-crystal nanotubes were synthesized using Na₂TeO₃ and (NH₂)₂CS as starting materials and pol-yacrymide (PAM) as morphology-director under hydrothermal conditions. The obtained products were characteri-zed by XRD, FESEM, SEM and TEM techniques. The results show that Te nanotubes grow along c axial with the inner diameters of 100～500 nm, wall thickness of 80～160 nm and lengths of 5～10 μm. A possible mechanism for the growth of Te nanotubes was discussed.     

水热法合成掺杂铁离子纤蛇纹石纳米管

本工作研究了在水热条件下纤蛇纹石纳米管的人工合成，通过掺杂Fe³⁺离子替代了纤蛇纹石晶格中的Mg²⁺离子。采用X-射线衍射、扫描电镜、透射电镜、红外光谱和电子自旋共振谱等手段研究了掺杂离子对纤蛇纹石晶体生长和晶体结构的影响。X-射线衍射分析表明随着掺杂Fe³⁺离子量的增加所得到的纤蛇纹石样品其晶胞参数b值逐渐减小。电子自旋共振谱、红外光谱分析表明Fe³⁺离子部分替代了Mg²⁺离子和Si⁴⁺离子进入纤蛇纹石的八面体和四面体结构单元。透射电镜研究表明掺杂前后所得到的纤蛇纹石内径分别为6～8 nm和8～15 nm。     

锐钛矿型TiO_2纳米管的离子液体辅助水热合成及紫外光催化活性

在离子液体[Bmim]OH辅助的水热条件下合成了结晶度较好的偏钛酸纳米管,经470℃煅烧2 h,可转变为锐钛矿型TiO2纳米管.对产物的物相、形貌和比表面积等进行了表征.结果表明,锐钛矿型TiO2纳米管的比表面积约为355 m2/g,主孔径约为25 nm.锐钛矿型TiO2纳米管和偏钛酸纳米管均呈现出明显的紫外光催化降解对氯苯酚的活性,锐钛矿型TiO2纳米管的降解效率约为44%(1 h).离子液体的加入不仅可扩大水热合成的温度范围,且有助于提高偏钛酸纳米管的结晶度.     

勃姆石AlOOH纳米管的合成与表征

一维无机纳米管材料的合成是目前材料化学的研究热点。鉴于氧化铝在催化及吸附等方面的广泛应用,对氧化铝纳米管的制备有很多报道。如有文献报道采用无模板方法,从无机铝源或氢氧化铝溶     

水热法合成Bi2S3纳米管及其生长机理

以硝酸铋[Bi(NO)3]和硫化钠(Na2S)为反应原料, 采用水热法在120 ℃下反应12 h, 制备出Bi2S3纳米管. 利用X射线粉末衍射(XRD)、扫描电子显微镜(SEM)、透射电子显微镜(TEM)、选区电子衍射(SAED)和高分辨透射电镜(HRTEM)对其结构和形貌进行了表征. 结果表明, 所制备的产物是结晶良好的正交相Bi2S3纳米管, 其外径为100~500 nm, 内径为50~200 nm, 长为1~5 μm. 根据实验结果讨论了Bi2S3纳米管的生长机理. 初步研究了反应温度和矿化剂种类对产物形貌和结构的影响.     

由黄连混合生物碱合成黄连碱

以中药黄连提取物黄连混合生物碱为起始原料,经脱甲氧基或亚甲二氧基、还原加氢、环合和氧化脱氢四步反应合成了黄连碱,总收率16%,其结构经1H NMR和ESI-MS表征.     

2种不同体系下镁碱沸石的水热合成及表征

介绍了研究型综合性实验--2种不同体系下镁碱沸石的水热合成及表征。该实验以传统水热晶化方法为基础,通过使用乙二胺和吡咯烷2种有机胺,在2种合成体系下分别制备了镁碱沸石FER,采用X射线粉末衍射仪(XRD)及固体核磁(MAS NMR)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,并使用氮气吸附/脱附测试对产物的性质进行表征。本文从实验教学的角度出发,整个实验步骤安排合理,内容丰富,可操作性强,充分体现了"制备合成-表征分析"的综合性科研思维模式,在让学生熟悉无机化学与材料化学科研中所使用的合成方法与表征手段的同时,也有助于学生了解科学研究工作的基本过程。     

甘氨酸存在条件下水热合成可层离双氢氧化物

Exfoliative Mg/Al layered double hydroxide (Mg/Al-LDHGly) was obtained via hydrothermal synthesis in the presence of glycine. The product prepared by hydrothermal reaction for 10 h at 120 ℃ possesses high thermal stability and maximal crystallite size in a, c directions. TEM and SEM analyses show that Mg/AlLDHGly was of well-crystallized hexagonal product with stacks of slightly curved layers. Benefiting from mechanism investigation on its gradual delamination in formamide, rapid delamination of Mg/Al-LDHGly at room temperature was realized, which provided fundamental for preparation of (Mg/Al-LDHGly)/polymer nanocomposites by using exfoliation-adsorption method.     

在温和条件下巨磁阻材料La0.5Ba0.5MnO3的水热合成与表征

报道了在温和条件下巨磁阻材料La_0.5Ba_0.5MnO₃的水热合成.系统地研究了原料配比、碱度、时间和温度对产物合成的影响,在最佳合成条件下得到了结晶度较高的纯相,并通过XRD、DTA-TG、化学分析及碘量法对产物进行了表征.该化合物属立方晶系,晶胞参数为α=0.3913nm,V=0.05990nm₃,Mn的平均价态为3.5,在1T的外磁场下,磁阻比(MR)的极大值为29%.     

水热条件下碳纳米管/硫氧镁化合物纳米复合材料的制备和表征

碳纳米管(CNT)因其完美的结构,优良的力学性能以及低的密度[1~3]而将会成为一种新型的结构复合材料增强剂。可是,研究发现,碳纳米管几乎不溶于所有的溶剂,而且,在结构复合材料中,碳纳米管与基体没有很好的连接性[4]。这些都很大的阻碍了碳纳米管在结构复合材料中的应用。为了解     

Hydrothermal Synthesis of Metal Silicates

Organically templated metal phosphates have been extensively studied because of interesting structural chemistry and potential applications in catalysis. However, in most cases the organic templates cannot be removed without collapse of the frameworks. This is in contrast to the high thermal stability and extensive applications of zeolites in refinery and petrochemical processes.Therefore, studies have been directed to the synthesis of transition metal silicates to produce more stable frameworks. Our synthetic methods are twofold, namely mild hydrothermal reactions in Teflon-lined autoclaves at 100-200 ℃ using organic amines as templates and high-temperature,high-pressure hydrothermal reactions in gold ampoules contained in a high-pressure reaction vessel at ca. 550 ℃ and 150 Mpa using alkali metal cations as templates. In this presentation I will report the high-temperature, high-pressure hydrothermal synthesis, crystal structures, and solid-state NMR spectroscopy of a number of new silicates of indium, uranium, and transition metals.     

碱式硫酸镁晶须水热过程结晶动力学研究

采用水热法合成了碱式硫酸镁晶须,利用扫描电镜、透射电镜、X射线能谱仪和X射线衍射仪等对产物的形貌和组成进行表征。通过考察不同温度下SO42-浓度随时间的变化,对碱式硫酸镁晶须的结晶动力学进行了研究。利用MATLAB软件和Runge-Kutta数值解法对实验数据进行处理,得出不同温度下晶须的结晶动力学方程。对晶须的几种生长机理模型进行分析发现,低温和高温的动力学模型不同,反应温度为170℃、180℃、190℃时的动力学模型分别为MB-1、MB-2和MB-3,结晶机理为多核控制表面生长,结晶速率由表面反应控制;反应温度为200℃和210℃时,结晶机理发生了变化,为单核控制表面生长,结晶动力学模型分别为MC-2和MC-3。     

Differential Scanning Calorimetry at Hydrothermal Conditions of Amorphous Materials Prepared by Drying Sodium Silicate Solutions

Concentrated sodium silicate solutions with a molar SiO₂:Na₂O ratio of 3.3 and a SiO₂ content of 27 mass% were dried up to 63 d at temperatures between 40 and 100°C to residual water contents between 12 and 38 mass%. The dried solid materials were investigated by differential scanning calorimetry (DSC). Pressure tight autoclave crucibles were applied to suppress evaporation and boiling of the samples during heating. Two thermal events are discussed with respect to glass transition. This revised version was published online in August 2006 with corrections to the Cover Date.     

钙镁硅酸盐溶度积常数的测定

借助高频等离子体发射光谱分别测定了一定温度下钙镁硅酸盐(CaO.mSiO2、MgO.mSiO2,其中m为模数)饱和溶液中Ca2 、Mg2 的平衡浓度,从而计算该温度下钙镁硅酸盐的溶度积常数,并研究了温度及水玻璃模数对钙镁硅酸盐溶度积常数的影响。结果表明,在同一温度下钙硅酸盐溶度积常数比镁硅酸盐溶度积常数小,在30℃下,水玻璃模数m为3.29时,钙硅酸盐的溶度积常数为1.14×10-8,而镁硅酸盐的溶度积常数为2.29×10-5;随着温度升高钙镁硅酸盐溶度积常数减小,当温度升高至90℃时,钙硅酸盐的溶度积常数减小至0.92×10-8,而镁硅酸盐的溶度积常数减小至1.68×10-5;在同一温度下随着水玻璃模数的增加,与其对应钙镁硅酸盐溶度积常数减小,由于模数的增加使沉淀中硅酸根离子直径变大,与钙镁离子反应生成钙镁硅酸盐晶体更易于沉淀,且更不易溶解,从而使钙镁硅酸盐的溶度积常数减小。     

MgSO4·5Mg(OH)2·3H2O的水热合成及反应时间对其形貌的影响

Both whisker and nanometer MgSO₄·5Mg(OH)₂·3H₂O(MOS) were prepared by hydrothermal method at 140℃ for different times， using NaOH and MgSO₄·7H₂O as raw materials. The MgSO₄·5Mg(OH)₂·3H₂O part- icles were characterized by powder X-ray diffraction(XRD)，thermal analysis(TGA-DSC)， infrared spectroscopy(FT-IR)，transmission electron microscopy(SEM) and scanning electron microscopy(TEM). The size distribution in whisker-like and nanocrystalline materials are in the range of 10～50μm and 10～20nm respectively. The whisker MOS is metastable phase in MgSO₄-NaOH-H₂O system at 140℃，whereas nanometer MOS is stable phase.     

MgSO_4·5Mg(OH)_2·3H_2O的水热合成及反应时间对其形貌的影响(英文)

０IntroductionWhiskerswithhighaspectratiohavebeenexten－sivelyusedascompositematerialsinalloys，ceramics，cementandplastic犤１～５犦，sincetheyhavespecificdesirepropertiessuchashighmeltingpoint，lowdensityandhighmodulus犤６犦．Magnesiumoxysulfate（MOS）com－poundshowsthehighcrystallinityandaspectratiotomakeitapotentialreinforcingmaterialforplastics，resinandrubber犤７，８犦．Inpastyears，MgSO４·５Mg（OH）２·３H２Ohasbeensynthesizedbyhydrothermalreactionusingmagnesiumhydroxideandmagnesium…     

Hydrothermal Synthesis of Magnesium Silicate Montmorillonite for Polymer-Clay Nanocomposites

Conditions of hydrothermal synthesis of magnesium silicate montmorillonite Mg₃Si₄O₁₀(OH)₂·nH₂O with a particle size of 50–100 nm are optimized, including the temperature, initial chemicals, reaction medium, and run duration.__________Translated from Zhurnal Prikladnoi Khimii, Vol. 78, No. 1, 2005, pp. 28–35Original Russian Text Copyright © 2005 by Golubeva, Korytkova, Gusarov.