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。     

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。     

碳化硅单晶材料的溶剂热合成与表征

SiC single crystals have been prepared by the method of solvothermal synthesis with a system of SiCl4, CCl4 and metal K in an auto clave. X-ray diffraction (XRD), Raman spectra and transmission electron microscopy(TEM) were used to characterize the products. XRD reveals that the products are SiC crystals and TEM exhibits that SiC single crystal sofwires and platelets are obtained under different usages of metal K. The SiC wires have diameters of 10～20 nm and length up to 1.5μm; the platelets have lateral dimensions of 0.1～3 μm, exhibiting regular polygonal shapes and step-bunched side surface. Furthermore, the growth mechanism of the SiC single crystals is discussed and the effect of super saturation on the crystal growth and morphology is also investigated.     

微乳液体系中溶剂热合成Co纳米纤维

纳米材料的小尺寸及大的表面积使其在光学、电学、磁学以及化学性质上与体相材料具有显著的差异 ,从而在催化、电子、光学、磁性存储和超导等多方面具有很大的应用前景 [1] .目前 ,已经开发出许多制备纳米颗粒的技术 ,如溅射法、共沉淀法、溶胶 -凝胶法、水热法和微乳液法等 .其中利用微乳液等两亲分子有序组合体进行化学反应制备纳米材料是近十几年发展起来的新方法 ,该方法由于具有实验装置简单、易于操作和粒度可控等优点而引起人们的重视 [2 ] .微乳液是一种高度分散的间隔化液体 ,水 (或油 )相在表面活性剂 (助表面活性剂 )的作用下以…     

溶剂热合成碳纳米管

自1991年Iijima发现碳纳米管以来,碳纳米管因其独特的结构和物理化学性质而成为人们的研究热点。     

溶剂交换法制备一维有机纳米材料

利用溶剂交换法制备了几种有机小分子化合物的一维纳米材料,并分别用SEM、TEM、XRD等对其结构进行了表征.分析了纳米材料的生长过程,讨论了有关的机理,并研究了其吸收光谱和荧光光谱等光物理行为.结果显示,有机纳米结构的形貌和尺寸对分子聚集体的光谱性质具有调制作用,使得它们展示出不同于溶液和体材料的优良纳米特性.     

溶剂热法合成花朵状钴磁性粉体及表征

采用一种简单的溶剂热法成功的合成了花朵状的钴磁性粉体。通过X射线粉末衍射(XRD),扫描电子显微镜(SEM)等对样品进行物相与形貌的表征。结果表明样品为六排堆积(hcp)和面心立方结构(fcc)混合结构的钴单质,形貌为由很多个厚度约为50～150 nm的菱形花瓣构成的花朵状结构,每个花朵的尺寸约为2μm左右。采用振动样品磁强计(VSM)测试了样品的磁性能,测试表明样品在室温下表现出铁磁性,饱和磁化强度(Ms)为140 emu.g-1,剩磁(Mr)为9.4 emu.g-1,矫顽力(Hc)为280 Oe。     

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CdSxSe1-x棒状纳米材料

以乙二胺为溶剂，制备了直径为10～20 nm、长度100～150 nm的棒状CdS_xSe_1-x纳米晶体，并对其形成过程及机理进行了探讨。研究发现CdS_xSe_1-x纳米晶体在120 ℃下就可形成且纳米棒的形貌不受温度及反应物配比的影响。紫外-可见光谱表明得到的CdS_xSe_1-x纳米晶体的光学性质可通过简单改变反应物中S与Se的配比进行调控。     

铟锡氧化物纳米粉体的低温溶剂热法制备

以氯化铟和氯化锡为原料,氨水为沉淀剂,先用化学沉淀法制备了前驱体,然后将该前驱体以乙二醇为溶剂在聚四氟乙烯内衬的反应釜中于低至190 ℃下反应,获得了铟锡氧化物(ITO)纳米粉体。采用扫描电子显微镜(SEM)、X射线衍射(XRD)及纳米粒度仪Zetasizer Nano-ZS对在不同温度、不同时间下反应的所得的ITO纳米粉体进行了表面形貌、结构和粒度分布等分析。结果表明,制备的ITO纳米粉体为立方晶相,粉体的平均颗粒小于100 nm;与已有的ITO纳米粉体制备方法相比,本溶剂热法制备过程无需高温烧结、流程简单,反应过程所需的温度可低至190 ℃,是迄今为止文献报导制备ITO的最低温度,同时所得产物纯度高、粒度均匀、分散性很好。     

Synthesis of Metastable Ternary Pd-W and Pd-Mo Transition Metal Carbide Nanomaterials

Research and catalytic testing of platinum group transition metal carbides have been extremely limited due to a lack of reliable, simple synthetic approaches. Powder samples have been reported to phase separately above 1%, and only thin-film samples have been reported to have appreciable amounts of precious metal doping. Herein, we demonstrated, through the simple co-precipitation of Pd and W or Mo precursors and their subsequent annealing, the possibility to readily form ternary carbide powders. During the investigation of the Pd-W ternary system, we discovered a new hexagonal phase, (PdW)₂C, which represents the first non-cubic Pd ternary carbide. Additionally, the solubility of Pd in the Pd-W-C and Pd-Mo-C systems was increased to 24 and 32%, respectively. As a potential application, these new materials show an enhanced activity for the methanol oxidation reaction (MOR) compared to industrial Pd/C.     

碳化硅纳米管的制备及表征

Silicon carbide nanotubes (SiCNTs) were prepared by chemical vapor deposition (CVD). Methyltrichlorosilane (MTS) was selected as the SiC gaseous source and, ferrocence and thiophene as the catalyst and the cocatalyst, respectively. The influences of pyrolysis temperature, the content of catalyst and the cocatalyst, and the mole ratio between H₂ and MTS, on the shape of the pyrolysis products were investigated, respectively. The products were characterized by SEM, EDX, XRD and HRTEM, respectively. Novel type of multi-walled SiCNTs, with 30～80 nm and 15～20 nm outer and inner diameters, respectively, were observed.     

Synthesis of Silicon Carbide Fibers by Sol-Gel Processing

Silica-phenolic resin hybrid fibers with carbon-to-silicon atomic ratios of 2.6 to 5.4 have been prepared from ethanol solutions of tetraethoxysilane, phenolic resins, water, and hydrochloric acid with a tetraethoxysilane-H₂O−HCl molar ratio of 1:2:0.01 by sol-gel processing. The hybrid fibers have been heated at 1500°C in Ar for carbothermal reduction to convert them into silicon carbide fibers. The effects of the holding time at 1500°C and the carbon-to-silicon atomic ratio of the hybrid fibers on the free carbon content in the silicon carbide fibers have been investigated. It has been found that the conversion is complete by the heat-treatment for more than 2 h. The silicon carbide fibers with a free carbon content of ca. 2 wt% have been obtained from the hybrid fibers with the ratios of 2.6 to 4.3.     

Synthesis of Silicon Carbide Whiskers from Substituted Silicon Alkoxides and Rayon Fibres

Silicon carbide whiskers (SiC_W) were synthesized through sol-gel process by impregnating the rayon fibres with sols of methyltriethoxysilane (MTEOS), phenyltriethoxysilane (PTEOS) and dimethyldiethoxysilane (DMDEOS) and pyrolyzing the impregnated rayon fibres at 1400°C in argon atmosphere. The SiC_W synthesized through this method were needle like, straight and their aspect ratio was found to be greater than 100 except in the case where DMDEOS was used as silica source.     

Hollow Silicon Carbide Nanostructures

Hollow silicon carbide nanostructures with length up to 1 m have been produced for the first time along with threadlike structures. The preparation of SiC nanostructures from silicon and carbon at 1000-1100 °C was carried out without prior gasification of these elements. The growth of SiC nanostructures involves a step featuring atomization of silicon and carbon at such low temperatures. The growth of SiC nanotubes upon the reduction of carbon by SiO₂ in the initial period of the preparation proceeds with their predominant formation as bundles. Silicon carbide may correspond to the highly textured -modification.     

Synthesis of Poly(silyne-co-hydridocarbyne) for Silicon Carbide Production

Pre-ceramic polymers have previously been shown to be polymeric precursors to silicon carbide, diamond and diamond-like carbon. Here, we report the synthesis of a pre-ceramic polymer, poly(silyne-co-hydridocarbyne), which was electrochemically synthesized from one monomer containing both silicon and carbon in its structure. The polymer is soluble in common solvents such as CHCl₃, CH₂Cl₂ and THF. Since the polymer contains both silyne and carbyne on its backbone, it can be easily converted to silicon carbide upon heating under an ambient inert atmosphere, or to SiO₂ under ambient air atmosphere. Poly(silyne-co-hydridocarbyne) was characterized with UV/Vis spectroscopy, FTIR, ¹H-NMR, GPC and Raman spectroscopy. Conversion of the polymer to SiC ceramic was accomplished by heating at 1000 and 750°C under an argon atmosphere and characterized with optical microscopy, SEM, X-Ray and Raman spectroscopies.     

碳化硅和碳化硼在电催化中的应用

燃料电池是具有广泛应用前景的新能源技术。碳载铂基催化剂(Pt/C)是最常用的燃料电池电极催化剂,不过Pt/C稳定性较差、且成本高昂,严重限制了燃料电池的规模化应用。共价型碳化物碳化硅和碳化硼,由于具有极强的共价键,其物化稳定性优异,成为制备高稳定性、低成本的燃料电池催化剂的重要基础材料。本文总结了相关研究成果,介绍了碳化硅和碳化硼的独特优势,讨论了相关研究的发展方向。     

碳化硅和碳化硼在电催化中的应用

燃料电池是具有广泛应用前景的新能源技术。碳载铂基催化剂（Pt/C）是最常用的燃料电池电极催化剂,不过Pt/C稳定性较差、且成本高昂,严重限制了燃料电池的规模化应用。共价型碳化物碳化硅和碳化硼,由于具有极强的共价键,其物化稳定性优异,成为制备高稳定性、低成本的燃料电池催化剂的重要基础材料。本文总结了相关研究成果,介绍了碳化硅和碳化硼的独特优势,讨论了相关研究的发展方向。