用于纳米粒子合成的微乳液

微乳液作为纳米反应器的最大优点是可以实现纳米粒子尺寸控制。体系中水的含量、表面活性剂、助表面活性剂等都是控制粒子尺寸的可调因素,研究这些因素对所合成的纳米粒子尺寸以及产量的影响对于实际应用有重要的意义。本文评述了近年来相关的研究进展,对微乳液法在合成纳米粒子中的应用前景作了展望。     

溶剂热法合成ZnSe纳米球

以乙酸锌和Se粉为原料,环己酮为溶剂,于180 ℃反应24 h制得黄色纳米球ZnSe,其结构和性能经XRD,SEM及TEM表征.     

溶剂热法合成碳纳米材料

本文综述了溶剂热法合成多种碳纳米管、纳米电缆、纳米棒、纳米球和纳米空心锥的研究现状。350 ℃下用金属钾还原六氯代苯,在用不同催化剂时,可分别得到碳纳米管和碳球,碳球的形成可以解释为石墨层的微条卷曲而成。600 ℃下金属镁还原乙醇得到了竹节状和Y-型碳纳米管。500 ℃下还原四氯化碳和碳酸钠可得到平均直径为100 nm的碳纳米管。700 ℃下金属锌还原乙醚制成了左右螺旋型交织的碳纳米管。在硫的存在下,200 ℃以下二茂铁热解成非晶碳纳米管和Fe/非晶碳纳米同轴电缆。     

碳化硅纳米材料的溶剂热合成

本文综述了溶剂热法制备一系列碳化硅纳米材料的研究,包括一维纳米线、纳米带、纳米棒、二维纳米片及空心球等;同时,碳源过量时可形成碳包覆碳化硅的复合材料。使用废塑料作为碳源合成了碳化硅纳米材料,为废塑料的回收再利用提供了新途径。通过使用碘、硫等添加剂,有效降低了合成温度,显示出溶剂热技术在制备碳化硅方面的独特优势。     

碳化硅纳米材料的溶剂热合成

本文综述了溶剂热法制备一系列碳化硅纳米材料的研究,包括一维纳米线、纳米带、纳米棒、二维纳米片及空心球等;同时,碳源过量时可形成碳包覆碳化硅的复合材料。使用废塑料作为碳源合成了碳化硅纳米材料,为废塑料的回收再利用提供了新途径。通过使用碘、硫等添加剂,有效降低了合成温度,显示出溶剂热技术在制备碳化硅方面的独特优势。     

Co3O4 纳米棒的溶剂热合成及形成机理分析

Co3O4 nanorods have been synthesized at 160℃ for 10 h in the solution of oleic and n-cetane by an emulsion-solvothermal method using Co（NO3）2·6H2O as starting materials. The as-prepared product was characterized by X-ray powder diffraction（XRD）,transmission electron microscope（TEM）,and vibrating sample magnetometer（VSM）. The formation mechanism of the prepared product was analyzed based on formation of rod-like micelles of oleic acid. Cobalt ions can migrate into the micelle core for the nucleation and growth of Co3O4 . The results show that the as-prepared Co3O4 nanorods are with the average size 25×100 nm and in the cubic phase. The magnetic susceptibility meets about linearly with the applied magnetic field at room temperature,and the coercivity （Hc）and remanent magnetization（Ms）values of the product at room temperature are 353 Oe and 0.4 emu/g,respectively. This simple route is also expanded to synthesize other materials with the rod-like morphology.     

微乳辅助的溶剂热法合成磷酸钐纳米棒

自1991年碳纳米管被发现以来,一维纳米材料以其独特的电、磁、光学和机械性质以及在纳米器件和功能材料上的巨大应用潜力而引起全世界的广泛关注,人们通过模板法、溶胶-凝胶法、水热法及微乳液法等多种方法合成了一系列一维纳米材料,其中微乳液法是近几年来兴起的较有发展前景的纳米材料的合成方法,微乳液是由油相、水相、表面活性剂和助表面活性剂组成的均匀稳定的体系,水相在表面活性剂和助表面活性剂的作用下均匀地分散在油相中,     

反相微乳液法合成钛酸钡纳米棒

本文在W/O型反相微乳液(Reverse Microemulsion)体系中制得了BaTiO3纳米棒, 考察了ωo值、反应物浓度等因素对BaTiO3纳米棒尺寸及形貌的影响. 用TEM、XRD和电子衍射对材料进行了表征,并用ICP测试了产品中钡与钛的摩尔比.     

混合溶剂热合成BaFBr∶Eu~(2+)微纳米晶及其性能表征

通过水和乙醇的混合溶剂热方法制备了不同形貌和粒径的BaFBr∶Eu2+微纳米晶.研究了不同反应条件对产物的影响,初步提出了产物的形成机制.用场发射扫描电镜(FE-SEM)、高分辨透射电子显微镜(HRTEM)、X射线粉末衍射(XRD),荧光光谱(PL)对BaFBr∶Eu2+进行了表征.结果表明:反应温度、时间及十六烷基三甲基溴化铵(CTAB)用量对产物物相、形貌及粒径有显著影响;制备的BaFBr∶Eu2+经退火后有优越的发光性能:用280nm光激发,在390nm处有对应于Eu2+4f65d12(t2g)→4f78(S7/2)跃迁的强发射峰,是计算机辐射成像板(Imaging Plate)中X射线存储荧光粉潜在可应用材料,本文为优质高效X射线存储荧光材料的可控制备提供了简洁的路径.     

溶剂热合成制备纳米In1-xAlxP固溶体

在160℃下,以1,2-二甲氧乙烷为溶剂和配合剂用溶剂热合成法成功地制得10～12 nm的In_1-xAl_xP固溶体,固溶度x在0～0.55之间。XRD和TEM用以鉴定产物的结构和形貌,XPS给出产物的固溶度和纯度。     

Phenol Solvothermal Synthesis of JBW-Type Zeolites

Phenol was used as an aromatic and acidic solvent in solvothermal synthesis.JBW-type zeolites were successfully synthesized in a phenolic system.The as-synthesized microporous crystals were characterized by powder X-ray diffraction analysis and scanning electron microscopy techniques.The results indicate that phenol is a good organic solvent and has a huge potential of application in studying crystallization mechanism and synthesizing novel microporous materials.     

溶剂热法直接合成酞菁铜晶体

以喹啉为溶剂, 在反应釜中将1,3-二异吲哚、钼酸铵和二水乙酸铜在喹啉中反应, 降至室温后得到长10.5 mm针状的酞菁铜单晶, 最佳的反应条件: 以10 mL喹啉为溶剂, 于270 ℃反应8 h, 产率为51.3%.     

Solvothermal reduction of graphene oxide in dimethylformamide

The reduction of graphene oxide (G-O) is one of the most promising methods for the large scale production of graphene-based materials. In this paper, we report a simple and non-toxic method to produce reduced graphene oxide (rG-O) by refluxing G-O in N, N-dimethylformamide without the aid of a reducing agent. The rG-O materials with high degrees of reduction are prepared and the levels of reduction are controlled using reflux time. Successful reduction is confirmed by combustion-based elemental analysis and X-ray photoelectron and Fourier transform infrared spectroscopy.     

链式钴微米六方片的溶剂热合成及磁性

以十二硫醇和聚乙烯吡咯烷酮（PVP）为结构导向剂、乙二醇和乙二胺为混合溶剂,利用溶剂热技术成功地制备了Co粒子,并用XRD、SEM、TEM、HRTEM及SQUID对材料的晶体结构、形貌及磁性进行研究. 结果表明：Co粒子属hcp相,呈六方片状,直径约为2 μm,厚度约为80 nm,大量的六方片相互交叉连接成链式结构,并且六方薄片由更为细小的丝带状的纳米片（厚度约为10 nm）构成;室温下样品表现出良好的铁磁性特征,其饱和磁化强度Ms、剩余磁化强度Mr及矫顽力分别为126.6 emu/g、13.7 emu/g和163.4 Oe.     

Synthesis of the Complex Fluoride LiBaF_3 through a Solvothermal Process

The complex fluoride LiBaF3 is solvothermally synthesized at 180℃ and characterized by means of X-ray powder diffraction, scanning electron microscopy, thermogravimetric analysis and infrared spectroscopy. In the solvothermal process, the solvents, mole ratios of initial mixtures and reaction temperature play important roles in the growth of the single crystal.     

Solvothermal Synthesis of a New Amine-Templated Vanadium Sulfate

A new organic-templated vanadium sulfate with formula [C₄H₁₂N₂][V^III (OH)(SO₄)₂] · H₂O 1 has been prepared under solvothermal conditions by using a mixture of glycol and water as solvent. The structure of this compound was characterized by IR, element analysis, TG and single crystal X-ray diffraction. The title compound crystallizes in the space group monoclinic, P2₁/c, a = 9.290(4) Å, b = 18.264(7) Å, c = 7.132(3) Å, β = 98.149(8)°,V = 1197.88 Å³, Z = 4. Structural analysis indicates that the title compound 1 possesses a 1D chain structure formed by VO₆ octahedra and SO₄ tetrahedra.     

一维链状硫酸铟的溶剂热合成与表征

在溶剂热条件下, 以三乙烯四胺(TETA)作为模板剂, 合成出具有一维链状结构的硫酸铟化合物(C6H22N4)0.5[In(OH)](SO4)2(1). 采用红外光谱、热重分析、ICP、元素分析、粉末X射线衍射及单晶X射线衍射等手段对其进行了表征. 结果表明, 化合物1属于单斜晶系, P2(1)/c空间群, a=1.05240(3) nm, b=1.36802(4) nm, c=0.75295(2) nm, β=101.558(2)°, V=1.06204(5) nm3, Z=4, R1=0.0368, wR2=0.0897, GOF=1.068. 其结构是由InO4(OH)2八面体和SO4四面体通过共顶点连接形成的一维阴离子Tancoite-type 链. 质子化的TETA阳离子通过与阴离子链中的O原子之间的氢键作用将一维链连接成为三维超分子结构.     

Preparation of Copper Phthalocyanine Crystals Using Solvothermal Synthesis

A novel solvothermal synthesis method for the direct growth of B-form crystals of copper phthalocyanine（CuPc） is presented in this article. With quinoline as solvent, crystals were grown after cooling the reaction mixture of 1,3-diiminoisoindoline and copper oxide, heated for 9 h at 270 ℃, to room temperature in an autoclave. These high quality crystals were suitable for characterization measurements. The single-crystal diffraction data show a monoclinic system unit cell： a=1.4668（3） nm, b=0.48109（10） nm, c=1.9515（7） nm, a=90°, B=121.04（2）°, r=90°, where the corresponding cell volume is 1.17991 nm^3. Needle-like single crystals of CuPc up to 10.5 mm in length were obtained. The influences of different temperatures, reaction time and solvent volume on the crystal yields were also discussed. Optimum reaction conditions were 10 mL of quinoline, at 270 ℃ for 8 h.     

溶剂热合成具有海绵状结构的介孔SnO2

采用溶剂热方法, 以SnCl4·5H2O/尿素/乙醇三元体系合成了具有特定结构的前驱体, 该前驱体经焙烧后得到了具有海绵状结构的介孔SnO2. 利用X射线粉末衍射(XRD)、傅立叶红外吸收光谱(FT-IR)、透射电镜(TEM)、热分析(TG-DTA)和氮气等温吸附鄄脱附等方法对产物的结构、形貌和热稳定性进行表征. 结果表明, 300 ℃焙烧处理后的样品由粒径约为5 nm的纳米粒子堆积而形成海绵状结构, 其中孔的尺寸范围在2-8 nm, 样品比表面积达到了134 m2·g-1.     

FeSb2纳米棒的溶剂热合成与电化学脱嵌锂性能

用溶剂热法合成了作为一种新型锂离子电池负极材料的FeSb2纳米棒. 高分辨透射电镜(HRTEM)观察表明, FeSb2纳米棒的直径为20～40 nm, 长度为0.2～1.0 μm. 恒流充放电测试和循环伏安测试显示, FeSb2纳米棒首次可逆容量达到543 mAh•g−1, 经过10次循环后, 可逆容量保持在353 mAh•g−1. 虽然首次库仑效率仅为64%, 但仍明显优于FeSb2纳米颗粒, 并在10次循环后基本稳定在90%. FeSb2纳米棒在循环过程中仍可能发生粉化和破裂, 导致电极逐渐失效.