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以锗、二氧化锗为原料,铜片为沉积衬底,通过水热沉积过程制备出了锗纳米针状结构.采用扫描电子显微镜(SEM)、能量色散光谱(EDS)、透射电子显微镜(TEM)及高分辨透射电子显微镜(HRTEM)等检测手段对样品进行了分析与表征.结果表明,样品具有典型的针状特征,其长度大于10 μm,由单晶锗和无定形锗氧化物外层所组成.运用金属催化气-液-固和氧化物辅助生长机理,解释了锗纳米针状结构的形成与生长. 相似文献
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采用水热法在高压反应釜内的高温、高压超临界水热环境下,以去离子水为反应介质,使活性高且难溶于水的一氧化硅粉末(SiO)通过硅原子的重结晶成核生长出本征硅纳米线。通过温度控制仪控制高压反应釜内温度和压力的变化,探索制备硅纳米线的最佳水热条件。通过多次实验探索,得知水热法制备硅纳米线的最佳条件是温度大于等于450℃、压力在9~10 MPa。然后通过扫描电子显微镜(SEM)、能量色散X射线光谱仪(EDX)、高分辨透射电镜(HRTEM)观察SiNWs的形貌和结构,分析其组成成分。通过SEM可观察到硅纳米线表面光滑、最小直径达50 nm及长度为3~5μm,由EDX图像可知SiNWs中只有硅和氧两种元素,而且Si∶O原子数比为3.5∶1.0。在HRTEM下可知硅纳米线是由芯部的晶体硅结构和外部无定形的二氧化硅包覆层组成,且包覆层小于5 nm。研究了本征SiNWs的拉曼光谱,发现拉曼主峰蓝移且在低频发生不对称宽化,分析认为是硅纳米线中存在的压应力和缺陷导致的。同时,在实验的基础上解释水热法制备SiNWs的机制,SiO在水热环境下歧化反应生成硅和二氧化硅,然后Si和SiO2开始堆叠生成SixO,即大量的纳米团簇,在一定温度下硅原子重结晶,同时在SixO的引导下沿一维方向生长。 相似文献
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硅(Si)因拥有高的比容量,资源丰富等优势有望成为下一代高性能锂离子电池负极材料,但其导电性差和循环过程中体积膨胀严重等缺陷限制了其进一步应用。采用喷雾干燥法,以玉米淀粉、纳米硅和NH4VO3作为原料,经碳化与氮化后获得氮化钒/纳米硅/碳复合微球(Si@VN/C)。氮化钒的引入提供了电子/离子快速传输通道,提高了纳米硅的导电率,并使纳米硅保持了良好的结构稳定性。碳层将作为纳米硅颗粒的保护层,避免纳米硅与电解液直接接触,有效缓解纳米硅充放电后的体积膨胀。Si@VN/C展现出良好的循环性能,在0.2 A·g-1电流密度下循环130圈后容量为818 mAh·g-1,在0.5 A·g-1高电流密度下循环300圈后可逆容量仍保持580.5 mAh·g-1。 相似文献
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以正硅酸乙酯为硅源,Ce(NO_3)_3·6H_2O为铈源,通过溶胶-凝胶一步法合成CeO_2/SiO_2纳米复合氧化物。通过N2-吸脱附、X射线衍射仪、扫描电子显微镜、透射电子显微镜、X射线光电子能谱仪、化学吸附仪等技术对复合氧化物的物相结构、形貌、尺寸、化学价态、氧化还原特性进行分析。结果表明,通过该合成方法可获得高分散、球状、孔隙发达的CeO_2/SiO_2复合氧化物;复合氧化物粒径在40 nm~70 nm,CeO_2粒径尺寸在4 nm~6 nm之间;孔结构以中孔为主,优化了纯CeO_2和纯SiO_2的大孔结构;CeO_2与SiO_2间发生了显著的相互作用形成了化学键,有效提高了CeO_2的氧化还原特性。 相似文献
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融盐电解法直接制备太阳能级硅新工艺的探讨 总被引:3,自引:1,他引:2
验证了熔融盐电解法制备高纯硅是可行的,拉曼光谱检测结果表明了二氧化硅在以氯化物为电解质的熔融盐中电解还原生成了硅。在此基础上,提出了一个以废弃的石英光纤废料为原料的太阳能级硅制备新工艺。 相似文献
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利用扫描电镜(SEM)和能谱仪(EDS)观测了经高频感应炉燃烧后高硅样品熔体中硅的存在形态和组成,从不同角度考察了样品中硅对熔融效果产生的影响,以及对高频感燃烧红外吸收法测定碳和硫结果的影响。结果显示:仅使用纯钨做助熔剂时,含硅样品熔体中的硅主要以球状的二氧化硅颗粒镶嵌于氧化钨和氧化铁等基体中,硅的存在使得高频燃烧红外吸收法测定碳和硫的准确度变差,且随着样品中硅含量的增加,这种影响的程度逐步增大。通过对影响机理进行分析认为:生成的二氧化硅使得熔体的流动性变差,且接受电磁感应形成感应电流的能力也同时减弱,从而对测定结果的精密度和正确度造成影响。实验在使用钨助熔剂的基础上,进行了添加纯锡或纯铁助熔剂的试验,结果表明:添加一定量纯锡或纯铁助熔剂,可以降低样品熔点,提高熔池温度,大大改善熔融效果,从而提高碳和硫测定的精密度和正确度。 相似文献
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以硅酸钠溶液和硝酸铜溶液为原料,采用水热合成法合成硅孔雀石,考察了制备前驱体时反应物滴加顺序、反应温度、水热结晶温度、反应时间和矿化剂等因素对硅孔雀石合成的影响,采用红外、XRD、化学分析等手段对产物进行表征。结果表明,在硅酸钠溶液中滴入硝酸铜溶液,反应温度为35℃,时间4h,加入40mL质量浓度为0.1mol/L的Na2SiO3和20mL质量浓度为0.1mol/L的NaOH混合液为矿化剂,水热反应温度120℃,时间6h的条件下,得到了纯度较高的天蓝色硅孔雀石。 相似文献
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采用熔盐电解法通过直接电解SiO2、TiO2混合物料来制备硅钛合金。热力学计算结果表明,在700℃下,SiO2和TiO2的理论分解电压分别为1.28V和1.37V,生成的单质硅和钛在高温下能够自发进行合金化反应,生成硅钛系列合金,且容易倾向于生成稳定合金相TiSi2合金。研究表明,以摩尔比50∶1的SiO2/TiO2混合物料为原料,在等摩尔比的CaCl2-NaCl混合熔盐中,在700℃、2.4V槽电压下,经过5h电解后,制备得到TiSi2/Si合金,微观形貌为粒径0.2~2.5μm的多孔颗粒堆积,单质硅颗粒覆盖在TiSi2合金颗粒表面。 相似文献
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采用熔盐电解法,以质量比为1:1的CuO、SiO2混合氧化物为反应原料,制备得到Cu3Si/Si多孔颗粒,粒径为0.05~2.8μm。结合XRD、SEM和EDS等手段,分析了CuO/SiO2的电脱氧反应路径。结果表明,CuO优先被电解还原生成单质Cu,SiO2则与熔盐中的Ca^2+和O2^-结合生成中间产物CaSiO3。CaSiO3进一步脱氧得到单质Si。硅铜合金化反应生成中间产物Cu9Si、Cu15 Si4和Cu3Si。将Cu3Si/Si复合物组装成锂离子电池负极,在200、500、800、1000、2000和200 mA/g放电电流密度下,可逆比容量分别为1346.22、754.3、661.4、564.8、192.1和1030.6 mAh/g,材料的倍率性能显著提升。 相似文献
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S. A. Golovin N. B. Fomicheva N. V. Rogov A. A. Morozyuk 《Powder Metallurgy and Metal Ceramics》1993,32(5):414-416
Features of structure formation and the phase composition of facing alloys based on Fe-Cr-Ni with different silicon contents during plasma deposition in order to improve the wear resistance of low-carbon steels are studied. With a silicon content exceeding 4% a network of silicon oxide SiO2 forms along grain boundaries preventing dendrite development. The materials are strengthened due to formation during facing of silicide inclusions CrSi2 and MoSi0.65.Tula Polytechnic Institute. Translated from Poroshkovaya Metallurgiya, No. 5, pp. 44–47, May, 1993. 相似文献
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Li Shuxin Ma Shuzhen Xu Mingyuan Shang Yanli Li Junran Zhang Shaohua ZHANG Yuanjing Gao Song 《中国稀土学报(英文版)》2004,22(Z3)
The electrorheological(ER) materials of pure SiO2 ( Sample 1 ), Ce-doping SiO2 ( Ce-SiO2, Sample 2) and Ce-SiO2 adsorbed chitosan (Ce-SiO2-chitosan, Sample 3 ) were prepared using Na2SiO3, Ce( NO3 )3 and chitosan as starting materials. Their ER properties were studied. The results show that Ce-doping can enhance the ER activity of SiO2, and the ER activity of SiO2 can be further improved by adsorbing chitosan on the surfaces of Ce-SiO2 particles.The ER activity of a particle material is correlated with the average grain size, surface area, pore volume and average pore size of the material. 相似文献
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E. Dal Martello G. Tranell S. Gaal O. S. Raaness K. Tang L. Arnberg 《Metallurgical and Materials Transactions B》2011,42(5):939-950
The use of high-purity carbon and quartz raw materials reduces the need for comprehensive refining steps after the silicon
has been produced carbothermically in the electric reduction furnace. The current work aims at comparing the reaction mechanisms
and kinetics occurring in the inner part of the reduction furnace when pellets or lumpy charge is used, as well as the effect
of the raw material mix. Laboratory-scale carbothermic reduction experiments have been carried out in an induction furnace.
High-purity silicon carbide and two different high-purity hydrothermal quartzes were charged as raw materials at different
molar ratios. The charge was in the form of lumps (size, 2–5 mm) or as powder (size, 10–20 μm), mixed and agglomerated as pellets (size, 1–3 mm) and reacted at 2273 K (2000 °C). The thermal properties of the quartzes
were measured also by heating a small piece of quartz in CO atmosphere. The investigated quartzes have different reactivity
in reducing atmosphere. The carbothermal reduction experiments show differences in the reacted charge between pellets and
lumps as charge material. Solid–gas reactions take place from the inside of the pellets porosity, whereas reactions in lumps
occur topochemically. Silicon in pellets is produced mainly in the rim zone. Larger volumes of silicon have been found when
using lumpy charge. More SiO is produced when using pellets than for lumpy SiO2 for the same molar ratio and heating conditions. The two SiC polytypes used in the carbothermal reduction experiments as
carbon reductants presented different reactivity. 相似文献
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以紫钨为原料制备超细WC-Co硬质合金 总被引:1,自引:1,他引:1
超细硬质合金具有高硬度、高耐磨性等优异性能,保证超细硬质合金的晶粒度小而且均匀的一个关键因素就是以粒度细小、分布均匀的超细WC粉末为原料。超细WC粉末的制备过程中,常用的氧化物原料为蓝钨,以紫钨为原料的制备工艺报道较少。采用相同的工艺,分别以蓝钨和紫钨为原料制备出超细WC粉末,并采用相同工艺制备出超细硬质合金,对两种产品性能进行对比,发现以紫钨为原料制备出的超细硬质合金晶粒度小,强度和硬度高,具有较好综合性能。 相似文献
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《粉末冶金学》2013,56(36):339-348
AbstractThe reaction-bonding process to prepare silicon nitride by nitriding silicon compacts was studied, and an examination made of the influence of raw material and process variables on the properties of the resulting silicon nitride. The silicon powder grain size and the impurities content were considered as powder variables, and the green density and thermal cycles as process parameters. The examination of green-density effects indicates that, under the experimental conditions, the gas permeation of nitrogen through the silicon compacts was the rate-determining step of the reaction-bonding process. Regarding the effect of nitriding temperature, the final conversion, Si to Si3N4, is an increasing function of the temperature in the range 1300–1400°C. As to the composition of silicon nitride obtained, α-phase formation is favoured when oxygen is present as an impurity in silicon powder. Finally, physical, chemical, and thermomechanical tests showed that reaction-bonded silicon nitride has good bending strength (21 kgf/mm2) and can be used in very severe conditions up to 1200°C. 相似文献