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Synthesis and TEM study of nanoparticles and nanocrystalline thin films of silver by high pressure sputtering 高压溅射法制备银纳米粒子和银纳米晶薄膜及其透射电镜研究
Pub Date : 1999-11-01 DOI: 10.1016/S0965-9773(99)00408-0
R. Chandra, P. Taneja, J. John, P. Ayyub, G. K. Dey, S. K. Kulshreshtha
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引用次数: 33
Nucleation and growth of hemispherical-grained Si by rapid thermal CVD 半晶硅的快速热气相沉积成核和生长
Pub Date : 1999-11-01 DOI: 10.1016/S0965-9773(99)00389-X
S. Berger, O. Raslin, H. Gilboa, E. Iskevitch, H. Spielberg, S. Levy
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引用次数: 0
Compositional partition in Ag-Nb alloy clusters produced by a plasma-gas-condensation cluster source 等离子体-气体凝聚团簇源产生的Ag-Nb合金团簇中的成分分配
Pub Date : 1999-11-01 DOI: 10.1016/S0965-9773(99)00415-8
K. Wakoh , T. Hihata , D.L. Peng , K. Sumiyama

We have produced Ag-Nb clusters by a facing-target type plasma-gas-condensation cluster source as our first step toward alloy cluster formation. The Ag-Nb clusters have been deposited on substrates and examined by a transmission electron microscope with a nano-beam energy dispersive X-ray analysis. We have obtained Ag-Nb alloy clusters with the sizes range between 5 and 10 nm in diameter. Their chemical compositions are broadly dispersed and partitioned into Ag-rich and Nb-rich ones, being consistent with the immiscible type equilibrium phase diagram. This result suggests that alloy cluster formation is driven by the alloy phase stability.

作为我们迈向合金团簇形成的第一步,我们已经通过面向目标型等离子体-气体冷凝团簇源生产了Ag-Nb团簇。在衬底上沉积了Ag-Nb簇,并用透射电子显微镜对其进行了纳米束能量色散x射线分析。我们获得了直径在5 ~ 10nm之间的Ag-Nb合金团簇。它们的化学成分分布广泛,分为富银和富铌两种,符合非混相型平衡相图。结果表明,合金团簇的形成是由合金相稳定性驱动的。
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引用次数: 17
The effect of Ni on the cryogenic attritor milling of Metglas Fe78B13Si9 Ni对meglas Fe78B13Si9低温磨耗器铣削的影响
Pub Date : 1999-11-01 DOI: 10.1016/S0965-9773(00)00428-1
B Huang , H.G Jiang , R.J Perez , S.R Nutt , E.J Lavernia

The addition of 17 at.% of elemental Ni powders to the cryogenic attritor milling of Metglas Fe78B13Si9 slowed the mechanical crystallization of the α-Fe and Fe2B phases. Transmission electron microscopy (TEM) observation and energy dispersive spectroscopy (EDS) analysis indicated that no more than 3.60 at.% of Ni dissolved into the Metglas, which was well within the equilibrium solubility limit of Ni in α-Fe. It is proposed that the addition of Ni impede mechanical crystallization during attritor milling by inhibiting bending and wear-like processes which could otherwise cause crystallization.

加上17个at。元素Ni粉末对Metglas Fe78B13Si9的低温磨耗器磨铣减缓了α-Fe和Fe2B相的机械结晶。透射电镜(TEM)观察和能谱(EDS)分析表明其不大于3.60 at。%的Ni溶解在metglass中,完全在Ni在α-Fe中的平衡溶解度范围内。提出Ni的加入通过抑制可能导致结晶的弯曲和类磨损过程来阻碍磨耗器铣削过程中的机械结晶。
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引用次数: 4
Structure transition comparison between the amorphous nanosize particles and coarse-grained polycrystalline of cobalt 钴纳米非晶颗粒与粗晶多晶的结构转变比较
Pub Date : 1999-11-01 DOI: 10.1016/S0965-9773(99)00394-3
Changsheng Xie , Junhui Hu , Run Wu , Hui Xia

Amorphous cobalt nanoparticles were synthesized by laser-inductive vaporization condensation technique. The nanoparticles are in fine size dispersion and the average particle size is 20 nm. When heating the amorphous cobalt nanoparticles in O2 ambient condition there is a sharp exothermic reaction in temperature range from 2072°C to 2972°C with a peak temperature of 260°C and exothermic enthalpy of 100.08 kJ/mol. When heating in Ar ambient condition, the amorphous cobalt nanoparticles may begin to transform from the amorphous solid to a supercooled liquid state at about 167°C and keep the supercooled liquid state in a wide temperature span from 167°C to 277°C, followed by crystallization at 277°C. The crystallization takes place in the temperature span from 277°C to 477°C. The corresponding exothermic heat is equal to 23.2 kJ/mol, which is larger than the heat of fusion of bulk cobalt (14.4 kJ/mol).

采用激光感应汽化缩合技术合成了非晶态钴纳米颗粒。纳米颗粒呈细粒度分散,平均粒径为20 nm。在O2环境条件下加热非晶态钴纳米颗粒,在2072 ~ 2972℃范围内发生剧烈放热反应,放热焓为100.08 kJ/mol,峰值温度为260℃。在Ar环境条件下加热时,非晶态钴纳米颗粒在167℃左右开始由非晶态固体转变为过冷液态,并在167 ~ 277℃的较宽温度范围内保持过冷液态,随后在277℃下结晶。结晶发生在277 ~ 477℃的温度范围内。相应的放热为23.2 kJ/mol,大于大块钴的熔合热(14.4 kJ/mol)。
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引用次数: 50
Nucleation and growth of hemispherical-grained Si by rapid thermal CVD 半晶硅的快速热气相沉积成核和生长
Pub Date : 1999-11-01 DOI: 10.1016/S0965-9773(99)00389-X
S Berger , O Raslin , H Gilboa , E Iskevitch , H Spielberg , S Levy

Hemispherical-grained Si (HSG) coating was deposited on an amorphous Si layer by using a rapid thermal chemical vapor deposition (RTCVD) process. The formation of the HSG coating consists of “seeding” and subsequent isothermal annealing stages. The microstructure and surface morphology of the HSG coating was studied after various stages of its formation by TEM and HRSEM techniques. The “seeding” process results in formation of nanometer size Si crystals on the substrate. Each Si crystal is covered with a thin amorphous Si film which forms a hemisphere shape. The annealing process results in growth and crystallization of polycrystaline Si hemispheres. The RTCVD process enables high control of the size and crystallinity of the Si hemispheres. The mechanism of formation and growth of the HSG coating is discussed and compared with other fabrication methods.

采用快速热化学气相沉积(RTCVD)工艺在非晶硅层上沉积了半晶硅(HSG)涂层。HSG涂层的形成包括“播种”和随后的等温退火阶段。利用透射电镜(TEM)和热扫描电镜(HRSEM)研究了HSG涂层在不同形成阶段的微观组织和表面形貌。“播种”过程导致在衬底上形成纳米尺寸的Si晶体。每个硅晶体都覆盖着一层薄薄的非晶硅膜,形成一个半球形状。退火过程导致了多晶Si半球的生长和结晶。RTCVD工艺可以高度控制Si半球的尺寸和结晶度。讨论了HSG涂层的形成和生长机理,并与其他制备方法进行了比较。
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引用次数: 0
FIM and 3D atom probe analysis of Cu/Nb nanocomposite wires Cu/Nb纳米复合线的FIM和三维原子探针分析
Pub Date : 1999-11-01 DOI: 10.1016/S0965-9773(99)00386-4
X Sauvage , L Thilly , F Lecouturier , A Guillet , D Blavette

Two kinds of Cu/Nb nanocomposite wires were investigated using field ion microscopy (FIM) and 3D atom probe. These two techniques revealed for the first time the nanoscale microstructure of nanocomposite wire cross sections. FIM investigations confirmed the Cu and Nb texture and the disorientation between (111) Cu and (110) Nb planes. Low angle Nb/Nb grain boudaries were also observed. Thanks to 3D atom probe, parts of niobium fibres and copper channels a few nanometer width were mapped out in 3D. Smooth Cu/Nb interfaces were attributed to stress-induced diffusion. Shear bands, observed perpendicular to the wire axis, were attributed to tracks of moving dislocations in a copper channel.

采用场离子显微镜(FIM)和三维原子探针对两种Cu/Nb纳米复合线进行了研究。这两种技术首次揭示了纳米复合线材截面的纳米级微观结构。FIM研究证实了Cu和Nb织构以及(111)Cu和(110)Nb平面之间的失向。还观察到低角度Nb/Nb晶界。得益于三维原子探针,部分铌纤维和几纳米宽的铜通道被三维绘制出来。Cu/Nb界面光滑归因于应力诱导扩散。观察到的垂直于导线轴线的剪切带归因于铜通道中移动位错的轨迹。
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引用次数: 21
Threshold behavior in the formation of nanoscale silicon particles prepared by sputtering 溅射制备纳米级硅颗粒形成的阈值行为
Pub Date : 1999-11-01 DOI: 10.1016/S0965-9773(99)00401-8
D.H Pearson , A.S Edelstein

DC magnetron sputtering of silicon was carried out at 175 watts in argon gas at pressures from 100 mtorr to 900 mtorr. Sputter deposits were collected on an array of transmission electron microscopy (TEM) grids placed between the sputter source and a cold-finger located 10.5 cm above the sputter source. The resulting deposits were analyzed by TEM, and the morphologies were found to include granular films, well-defined particles 5–13 nm in diameter, and transition morphologies between that of particles and granular films. The resulting morphology map, as a function of sputtering pressure and TEM-grid location, indicated that particles were more likely to form at higher pressures and locations farther from the source. In addition, results obtained by varying the cold-finger temperature and the sputter-source/cold-finger distance indicated that the temperature of the cold-finger can play a significant role in particle formation at small sputter-source/cold-finger separations. Deposits with granular-film morphologies were amorphous under most conditions. However, deposits containing particles exhibited the diamond-cubic crystalline phase under some conditions as well as the amorphous phase.

在175瓦的氩气中进行了硅的直流磁控溅射,压力从100毫微米到900毫微米。在放置在溅射源和位于溅射源上方10.5 cm的冷指之间的一系列透射电子显微镜(TEM)网格上收集溅射沉积物。通过透射电镜对沉积物进行了分析,发现沉积物的形貌为颗粒状膜、直径为5 ~ 13 nm的颗粒状膜、颗粒状膜和颗粒状膜之间的过渡形貌。作为溅射压力和tem网格位置函数的形貌图表明,在高压力和远离源的位置更容易形成颗粒。此外,通过改变冷指温度和溅射源/冷指距离得到的结果表明,在小溅射源/冷指分离时,冷指温度对颗粒形成有重要影响。在大多数条件下,具有颗粒膜形态的沉积物是无定形的。然而,含有颗粒的沉积物在某些条件下表现为金刚石立方晶相以及非晶相。
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引用次数: 7
Novel synthesis of Al13-cluster based alumina materials al13簇基氧化铝材料的新合成
Pub Date : 1999-11-01 DOI: 10.1016/S0965-9773(99)00412-2
M. Wang , M. Muhammed

The polyoxocation Al13O4(OH)24(H2O)127+, known as an Al13 cluster, has been synthesized by controlled hydrolysis of aluminum(III) aqueous solution at 70 oC, and pH between 5.0 and 6.0. The formation of the polyoxocation Al13O4(OH)24(H2O)127+ in solution was experimentally confirmed by 27Al NMR. The Al13 cluster-containing powder was obtained by precipitating the polyoxoaluminate ion from the solution by the addition of a suitable salt, e.g. sodium sulphate or ammonia oxalate. The obtained powder was characterized by TGA, XRD, and SEM. It was found that the sulfate-precipitated powder had three different crystal structures, i.e. monoclinic fiber, monoclinic rectangle shaped crystal and tetrahedral shaped crystal, while the oxalate powder obtained from the oxalate precipitation was a spherical-particles powder with particle size around 200 nm. XRD of the Al13-sulfate showed that the powder consisted of a cubic phase with a unit cell size of 17.9Å. After calcination of the Al13-sulfate and Al13-oxalate salts at 1000 °C, the powder was converted to α-alumina. The α-alumina powder obtained from the oxalate route was about 100 to 200 nm in diameter.

在70℃、pH 5.0 ~ 6.0的条件下,对铝(III)水溶液进行控制水解,合成了多氧化Al13O4(OH)24(H2O)127+,称为Al13簇。用27Al核磁共振实验证实了溶液中多氧化Al13O4(OH)24(H2O)127+的形成。通过加入适当的盐,如硫酸钠或草酸氨,从溶液中沉淀出多氧铝酸盐离子,得到含Al13簇的粉末。用TGA、XRD、SEM对所得粉体进行了表征。结果表明,硫酸盐沉淀粉末具有单斜纤维、单斜矩形晶体和四面体晶体三种不同的晶体结构,而草酸盐沉淀得到的草酸盐粉末为粒径在200 nm左右的球形颗粒粉末。硫酸铝13的XRD分析表明,该粉体为立方相,晶胞尺寸为17.9Å。al13 -硫酸盐和al13 -草酸盐在1000℃下煅烧后,粉末转化为α-氧化铝。草酸法制备的α-氧化铝粉体直径约为100 ~ 200 nm。
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引用次数: 52
Structure transition comparison between the amorphous nanosize particles and coarse-grained polycrystalline of cobalt 钴纳米非晶颗粒与粗晶多晶的结构转变比较
Pub Date : 1999-11-01 DOI: 10.1016/S0965-9773(99)00394-3
C. Xie, Junhui Hu, R. Wu, H. Xia
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引用次数: 50
期刊
Nanostructured Materials
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