室温氧化还原反应制备AgCuSe三元纳米棒

在室温下通过氧化还原反应制备了AgCuSe三元纳米棒.用X射线粉末衍射、透射电镜和X射线光电子能谱对产物进行了表征.X射线粉末衍射结果表明,产物是四方相AgCuSe;透射电镜结果表明,产物是纳米棒,其直径为5～20nm,长度为200～600nm;X射线光电子能谱结果表明,产物的纯度是很高的,没有单质Ag、Cu等杂质.应用化学热力学原理讨论了产物AgCuSe的生成机理.热力学计算表明,在这个反应体系中最终产物是纯AgCuSe.溶剂乙二胺不仅作为双齿配体与Ag+和Cu+形成稳定的配合物,而且还能溶解金属硒、增强硒的反应性,乙二胺在控制AgCuSe的成核和纳米棒的生长过程中起着重要的作用.     

溶剂热再结晶合成由纳米颗粒自组装成的一维CdS纳米棒

采用两种不同的溶剂热路径合成出了不同形貌和尺寸的CdS纳米晶, 一种是以无水乙二胺(en) 为溶剂, CdCl₂·2.5H₂O和硫脲(H₂NCSH₂N) 为镉源和硫源, 在不同反应温度(160 ℃-220 ℃ 下制备出了CdS纳米晶, 讨论温度对CdS纳米晶生长的影响; 另一种是以en为溶剂, 将在160 ℃下合成的产物在200 ℃下原位再结晶生长2-8 h, 分析原位生长时间对CdS纳米晶生长的影响. 通过X射线衍射(XRD)、 扫描电子电镜(SEM) 和透射电子电镜(TEM) 等表征产物的物相、 形貌和微结构, 分析可知: 两种路线合成的产物均为六方相CdS; 当温度为160 ℃时, 产物形貌为纳米颗粒状, 当温度高于160 ℃时, 产物为CdS纳米棒状; 同时, 在200 ℃下原位再结晶生长不同时间后发现产物形貌由纳米颗粒转变为纳米棒, 通过场发射扫描电镜(HRTEM) 分析可知: 纳米棒是由零维纳米颗粒自组装而成. 最后, 讨论了影响产物CdS纳米晶形貌转变的因素和纳米棒的生长机理.     

单晶Si表面离子束溅射沉积Co纳米薄膜的研究

采用离子束溅射沉积法，在单晶Si基片上制备了不同厚度(1—100nm)的Co纳米薄膜.利用原子力显微镜、X射线光电子能谱(XPS)仪和X射线衍射仪对不同厚度的Co纳米薄膜进行了分析和研究.结果表明：当薄膜厚度为1—10nm时，沉积颗粒形态随薄膜厚度增加将由二维生长的细长胞状过渡到多个颗粒聚集成的球状.当膜厚大于10nm时，小颗粒球聚集成大颗粒球，颗粒球呈现三维生长状态.表面粗糙度随膜厚的增加呈现先增加后减小的趋势，在膜厚为3nm时出现极值.XPS全程宽扫描和窄扫描显示：薄膜表面的元素成分为Co，化学态分别 关键词： 离子束沉积 纳米薄膜 X射线光电子能谱 X射线衍射     

低温条件下单晶氮化铝纳米线生长机理的研究

在25mL的不锈钢反应釜中，利用无水三氯化铝与叠氮化钠在无溶剂的条件下直接反应，成功地合成出了单晶氮化铝纳米线，反应温度为450℃，有效反应时间为24h.高分辨率透射电子显微镜测试结果显示，纳米线多为长直线状外貌特征，直径在40—60nm范围内，最大长度可达几个微米.高分辨率电子衍射和X射线衍射结果都表明，多数纳米线为六方结构，也有少量呈现面心立方结构.同时，提出了长直线状六方和面心立方单晶氮化铝纳米线的生长机理的假设，并对六方单晶氮化铝纳米线生长方向的人工控制也进行了讨论. 关键词： 六方单晶氮化铝 纳米线 X射线衍射 透射电子显微镜     

简单溶液法制备氧化锌纳米棒及光学性质

以水合醋酸锌(ZnAc₂·2H₂O)和水合肼(N₂H₄·H₂O)为反应物,在未使用任何表面活性剂的简单反应体系中制得了ZnO纳米棒。采用X射线衍射(XRD)、扫描电子显微镜(SEM)、高分辨透射电镜(HRTEM)和室温荧光光谱对产物的晶体结构、形貌和发光性质进行了表征和分析。测试结果表明,所得产物为六方纤锌矿结构ZnO纳米棒,平均直径为120 nm,产物结晶完整,尺寸均匀。这种简单溶液法制备的ZnO纳米棒在386 nm处具有一个尖锐的紫外发光峰,发射光谱的半峰全宽仅为18 nm,在可见光区有一个较弱的宽频发光带。在该反应体系中通过调控混合溶剂的配比,不使用任何表面活性剂的条件下,为ZnO一维纳米棒的形核和生长提供了微型反应空间。     

Cu/C核/壳纳米结构的气相合成、形成机理及其光学性能研究

采用乙酰丙酮铜为原料, 通过化学气相沉积大批量制备出Cu/C核/壳纳米颗粒和纳米线. 研究结果表明, 通过控制沉积温度可对Cu/C核/壳纳米材料的形貌和结构进行很好的控制. 比如, 沉积温度为400 ℃时可获得直径约200 nm的Cu/C核/壳纳米线, 沉积温度为450 ℃ 时可获得直径约200 nm的Cu/C核/壳纳米颗粒和纳米棒的混合产物, 沉积温度为600 ℃时可获得直径约22 nm的Cu/C核/壳纳米颗粒. 获得的Cu/C核/壳纳米结构是由一个新颖的凝聚机理形成的, 而这种机理不同于著名的溶解-析出机理. 紫外-可见光谱和荧光光谱分析结果表明: Cu/C核/壳纳米线和纳米颗粒均在225 nm处出现Cu的吸收峰, 同时在620 和616 nm处分别出现了纳米线和纳米颗粒的表面等离子共振吸收峰. Cu/C核/壳纳米线在312 和348 nm处、 Cu/C核/壳纳米颗粒在304 和345 nm处出现荧光发射谱峰. 关键词： Cu/C核/壳结构 纳米线 纳米颗粒 光学性能     

炸药爆轰法制备纳米石墨粉及其在高压合成金刚石中的应用

介绍了一种制备纳米石墨粉的新方法——负氧平衡炸药爆轰法. 对合成的黑粉产物进行x射线衍射分析，确认其为石墨结构，平均晶粒度为2.58 nm. 透射电子显微分析的结果表明，炸药爆轰法制备的黑粉为六方结构的纳米石墨粉，颗粒呈球形或椭球形. 用小角x射线散射法测定纳米石墨粉的粒度分布在1—50 nm，有92.6wt%的粉末粒度小于16 nm. 平均粒径为8.9 nm. 纳米石墨粉的比表面积约为500—650 m²/g. 在六面顶压机中用纳米石墨粉在Fe粉触媒的作用下进行金刚石的高压合成实验 关键词： 纳米石墨粉 爆轰 金刚石 合成     

用SAXS和XRD方法研究TiO2纳米颗粒微观结构

用溶胶-凝胶方法制备了TiO₂纳米样品,并对该样品在300℃到800℃温度区域进行了退火处理.应用同步辐射X射线粉末衍射(XRD)方法研究了经不同热处理温度的TiO₂纳米颗粒的结构相变.应用同步辐射小角X射线散射(SAXS)方法研究了TiO₂纳米颗粒的表面分形与界面特性.得到纳米颗粒粒度与退火温度的变化规律,讨论了表面界面特征与相变的关系. 关键词： X射线小角散射 X射线衍射 2纳米颗粒')" href="#">TiO₂纳米颗粒     

水热法制备ZnS:Cu,Tm超细X射线发光粉

研究了水热法合成的ZnS: Cu,Tm超细X射线发光粉及其光致发光(PL)和X射线激发发光(X-ray excited luminescence,XEL)光谱特性.200 ℃水热处理12 h直接合成样品的纳米晶粒径约15 nm,尺寸分布窄,分散性好,具有纯立方相的类球形结构.氩气保护下900 ℃退火1 h后的样品存在一定的团聚,但团聚后尺寸为200—600 nm,为超细X射线发光粉,此时样品为纯六方相的类球形为主的结构.所有样品的PL和XEL光谱均为宽带谱.水热法直接合成样品的XEL强度最强时,样品的Cu/Zn,Tm/Cu比值分别为3×10^-4和2.在此比值条件下,900 ℃退火1 h样品的XEL发光最强,此时其两个峰值分别位于453,525 nm.发光强度增强的同时粒径很小,对提高成像系统分辨率非常有意义.通过比较PL光谱与XEL光谱特性,讨论了PL和XEL光谱的发光机理和其不同的激发机理. 关键词： ZnS:Cu Tm 水热法 X射线激发发光     

Co3O4纳米花的合成及其磁性

通过水热和热处理的方法，制备了产物Co3O4纳米花. 用X射线粉末衍射、场发射扫锚电镜、透射电镜和红外光谱等手段对产物进行了表征. 结果表明，产物纳米花是由大量的Co3O4纳米须组成，纳 米须的直径为20?40 nm，长度为100?500 nm，具有纳米孔结构，比表面积约为34.61 m2/g. 磁性测量表明，在零场冷却条件下，产物主要表现为反铁磁性；在加场冷却条件下，闭锁温度约为34K时，产物主要表现为铁磁性．     

Synthesis of ZnS nanorods by annealing precursor ZnS nanoparticles in NaCl flux

ZnS nanorods were fabricated by annealing precursor ZnS nanoparticles, which were prepared by one-step, solid-state reaction of ZnCl₂ and Na₂S through grinding by hand at ambient temperature, in NaCl flux. The as-prepared ZnS nanorods have diameters of 40-80 nm, and lengths up to several micrometers. The structural features and chemical composition of the nanorods were investigated by X-ray diffraction (XRD), transmission electron microscopy (TEM), selected area electron diffraction (SAED), high-resolution transmission electron microscopy (HRTEM), and Raman spectra.     

Low temperature thermoelectric properties of Cu intercalated TiSe2: a charge density wave material

Y₂O₃ nanoparticles and nanorods have been firstly synthesized in bulk Ti-Y films prepared by magnetron sputtering on Si (100) substrates at different temperatures. X-ray photoelectron spectroscopy (XPS), X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), and energy dispersive X-ray spectroscopy (EDS) are used to characterize the structure, morphology, and composition of the as-synthesized nanoparticles and nanorods. The mechanical properties of the sputtered films are investigated using nanoindentation techniques. The results indicate that both the nanoparticles and nanorods have a pure cubic Y₂O₃ structure resulting from the reaction of Y atoms with the residual O₂ in the vacuum chamber, and are free from defects and dislocations with uniform diameters of about 30 nm. The Y₂O₃ nanoparticles mainly distribute at the grain boundaries of the Ti matrix and the nanorods have lengths ranging from 250 nm to more than 1 μm with the growth direction parallel to the (002) plane. As the growth temperature elevates, the nanoparticles turn to be coarsening while more and longer nanorods are inclined to form. Compared with the Ti film, the TiY films have a remarkable increase in hardness, but do not exhibit expected increase in elastic modulus. Finally, the growth mechanism is also briefly discussed.     

Sodium dodecyl sulfate-assisted synthesis of CoWO4 nanorods

CoWO₄ nanorods were synthesized at 453 K for 12 h by a hydrothermal technology from Na₂WO₄ · 2H₂O and CoCl₂ · 6H₂O in the presence of sodium dodecyl sulfate (SDS). The as-synthesized CoWO₄ nanorods were characterized by various techniques of X-ray diffraction, transmission electron microscopy, scanning electron microscopy, and X-ray detector. Luminescent properties of the samples were measured at room temperature. The results showed that CoWO₄ products are nanorods with diameters of about 20 nm, and lengths ranging between 100 and 200 nm. CoWO₄ nanorods display a very strong PL peak at 453 nm with the excitation wavelength 300 nm. The possible formation mechanism of CoWO₄ nanorods was suggested.     

Synthesis of nanorods FePO4 via a facile route

Iron phosphate nanorods were synthesized via a novel facile route. The structure, composition, and morphology of the prepared material were characterized by X-ray diffraction (XRD) and transmission electron microscope (TEM), respectively. The diffraction lines were indexed to the hexagonal structure. The diameter of these nanorods is about in the range of 20–30 nm and the length 50–100 nm. The preferential growth direction of the prepared material was the [100]. The reaction mechanism for the synthesis of FePO₄ nanorods was also primarily discussed. Compared to the bulky and the irregular nanoparticles, the nanometer ones will be more fascinating for application in many areas.     

Hydrothermal synthesis and magnetic properties of CuSb<Subscript>2</Subscript>O<Subscript>6</Subscript> nanoparticles and nanorods

Nanoparticles and nanorods of CuSb₂O₆ are prepared by hydrothermal method and its high temperature α-phase is stabilized at room temperature. The average size of the nanoparticles is ca. 13.7 nm. The nanorods, with a width of ca. 20 nm and an aspect ratio of ca. 5, are the agglomerates composing of smaller nanoparticles with an average size of ca. 8.3 nm. Compared with the high temperature α-phase of bulk sample at 400 K, the lattice of nanophases elongated in ab plane and compressed along c direction. The CuSb₂O₆ nanoparticles exhibit predominant paramagnetic phenomenon. The difference in magnetic properties of the nanoparticles and nanorods indicates the interfacial interaction of agglomerated nanoparticles.     

Synthesis and characterization of nanophased silver tungstate

Silver tungstate (Ag₂WO₄) nanoparticles in two different morphologies are prepared by controlling the reaction kinetics of aqueous precipitation. X-ray diffraction studies reveal that the silver tungstate nanoparticles are in the α-phase. SEM images show the rod-like and fiber-like morphologies of the nanoparticles with high aspect ratios. The TGA and DTA studies show the high thermal stability of the nanorods. The average crystallite sizes (20–30 nm) of the rod-like silver tungstate estimated from TEM is consistent with the XRD results     

Annealing of gold nanoparticles on GaP(111)B: initial stage of GaP nanowire growth

GaP(111)B substrate was strewn with 30 nm colloidal Au nanoparticles. Organic residues were removed by: A) boiling in acetone and isopropylalcohol followed by a DI water rinse, B) treatment A + HF:H₂O, C) treatment A + O₂ plasma for 10 min, 20 min, and 40 min, and D) treatment A combined with O₂ plasma (10 min) and HF:H₂O. The substrate thus had original ‘epi‐ready' oxides (A), or fresh native oxides (B and D), or new added oxides (C). The samples were annealed at T_a = 650 °C for 10 min under PH₃ and H₂ in an MOVPE chamber. This resulted in the growth of GaP stumps along [111]B on each sample. Their length was <3 nm (B and D), ～20 nm (A), and ～220 nm (C 40 min). Elemental Ga is left as P₂O₅/Ga₂O₃ oxides form on etched GaP(111)B at room temperature. We believe that as the oxides disintegrated during annealing, they released the elemental Ga that combined with phosphorus from PH₃, and this led to the growth of the GaP stumps. (© 2014 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Fabrication and characterization of GaP/polymer nanocomposites for advanced light emissive device structures

GaP nanoparticles have been prepared using white P and a mild aqueous synthesis at decreased temperature followed by ultrasonication and stored as the suspension in water–ethanol mixture. They were characterized by standard methods of X-ray diffraction, transmission electron microscopy, Raman light scattering, and photoluminescence. Properties of GaP nanoparticles were compared with industrial and specially grown perfect GaP single crystals. It was shown that the GaP nanoparticles in suspension are the most suitable for high quality GaP/polymers nanocomposites because only they are uniform with dimensions of about 10 nm which is optimal for appearance of the pronounced quantum confinement effect. Polyglycidyl methacrylate (PGMA), polyglycidyl methacrylate-co-polyoligoethyleneglycol methacrylate (PGMA-co-POEGMA), and biphenyl vinyl ether (BPVE) polymers were used to prepare GaP polymer nanocomposites. The thickness of the polymer nanocomposite film was about 250–300 nm defined from AFM scratch experiment. The resulting nanocomposites yielded a bright luminescence at room temperature in a broad band with the maximum ranging from 2.5 to 3.2 eV and showed pronounced quantum confinement effects and other interesting and important for application phenomena leading to dramatic 1 eV expansion of GaP luminescence to the UV spectral region.     

Effect of reaction condition on microstructure and properties of (NiCuZn)Fe2O4 nanoparticles synthesized via co-precipitation with ultrasonic irradiation

Nano-spinel ferrites synthesized via chemical co-precipitation method are small in size and have serious agglomeration phenomenon, which makes separation difficult in the subsequent process. Ni_0.4Cu_0.2Zn_0.4Fe₂O₄ ferrites nanoparticles were synthesized via co-precipitation assisted with ultrasonic irradiation produced by ultrasonic cleaner with 20 kHz frequency using chlorinated salts and KOH as initial materials. The effects of ultrasonic power (0, 40 W, 60 W, 80 W) and reaction temperature on the microstructure and magnetic properties of ferrite nanoparticles were investigated. The structure analyses via XRD revealed the successful formation of pure (NiCuZn)Fe₂O₄ ferrites nanospinel without any impurity. The crystallites sizes were less than 40 nm and the lattice constant was near 8.39 Å. The TEM showed ferrite particle polygonal. M−H analyses performed the saturation magnetization and coercivity of ferrite nanoparticles obtained at the reaction temperature of 25℃ were higher than at 50℃ with same power. The samples exhibited the highest values of Ms 55.67 emu/g at 25℃ and 47.77 emu/g at 50℃ for 60 W and the lowest values of Hc 71.23 Oe at 25℃ for 40 W and 52.85 Oe at 50℃ for 60 W. The squareness ratio (SQR) were found to be lower than 0.5, which revealed the single magnetic domain nature (NiCuZn)Fe₂O₄ nanoparticles. All the outcomes show the ultrasonic irradiation has positive effects on improving the microstructure and increasing magnetic properties.     

Large-scale synthesis of GaN nanorods and their photoluminescence

Large quantities of gallium nitride (GaN) nanorods have been synthesized via direct reaction of metallic gallium vapor with flowing ammonia at 970 °C in a quartz tube. The nanorods have been confirmed as crystalline wurzite GaN by powder X-ray diffraction, selected-area electron diffraction and X-ray photoelectron spectrometry. Transmission electron microscopy and scanning electron microscopy reveal that the nanorods are straight and uniform, with diameters ranging from 40 nm to 150 nm and lengths up to hundreds of micrometers. The growth mechanism is discussed briefly. Photoluminescence measurements on bulk GaN nanorods at room temperature show two strong peaks at 377 nm (3.28 eV) and 360 nm (3.44 eV) attributed to the zero-phonon donor-acceptor pair transition and the donor-bound exciton, respectively. Received: 19 April 2001 / Accepted: 10 May 2001 / Published online: 20 June 2001