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Processing, microstructure and mechanical properties of 25 vol% YAG-Al2O3 nanocomposites 25 vol% YAG-Al2O3纳米复合材料的制备、显微组织和力学性能
Pub Date : 1999-11-01 DOI: 10.1016/S0965-9773(99)00396-7
W.Q Li , L Gao

A co-precipitation method was investigated to manufacture 25 vol% YAG-Al2O3 nanocomposites with excellent strength characteristics at room temperature. The as-prepared powders were sintered by hot-pressing in N2 to nearly full density with heating rate of 10°Cmin−1 to 1400°C for 1h and at 30MPa pressure. The microstructure was characterised using X-ray diffraction (XRD), scanning electron microscopy (SEM), energy-dispersive spectroscopy (EDS) and transmission electron microscope (TEM). Microstructural results of hot-pressed composites reveal that the intergranular YAG grains of micrometer size (≈800nm) were dispersed at the grain boundaries of a dense Al2O3 matrix, and most fine grain YAG grains of nanometric size (≈100nm) were entrapped within the Al2O3 grains in the composite. The room temperature fracture strength and fracture toughness of the hot-pressed composites were 611MPa and 4.53MPa·m−1/2, respectively. These strength and fracture toughness values are higher than those reported in other studies for YAG-Al2O3 system. It is proposed that the improvement of mechanical property of hot-pressed nanocomposites is due to the reduction of the grain size of the matrix and the improved strength of the grain boundaries in 25 vol% YAG-Al2O3 nanocomposite.

采用共沉淀法制备了具有优异室温强度特性的25 vol% YAG-Al2O3纳米复合材料。在30MPa压力下,以10°Cmin - 1 ~ 1400°C的升温速率,在N2中热压烧结至近满密度。采用x射线衍射(XRD)、扫描电子显微镜(SEM)、能谱(EDS)和透射电子显微镜(TEM)对其微观结构进行了表征。热压复合材料的显微组织结果表明,微米尺寸(≈800nm)的YAG晶粒分散在致密Al2O3基体的晶界处,而大多数纳米尺寸(≈100nm)的YAG晶粒被包裹在复合材料的Al2O3晶粒中。热压复合材料的室温断裂强度和断裂韧性分别为611MPa和4.53MPa·m−1/2。这些强度和断裂韧性值高于YAG-Al2O3体系的其他研究报告。结果表明:25vol % YAG-Al2O3纳米复合材料的力学性能的提高是由于基体晶粒尺寸的减小和晶界强度的提高。
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引用次数: 58
Synthesis of monodisperse Au, Pt, Pd, Ru and Ir nanoparticles in ethylene glycol 单分散Au, Pt, Pd, Ru和Ir纳米颗粒在乙二醇中的合成
Pub Date : 1999-11-01 DOI: 10.1016/S0965-9773(99)00419-5
F Bonet , V Delmas , S Grugeon , R Herrera Urbina , P-Y Silvert , K Tekaia-Elhsissen

Au, Pt, Pd, Ru and Ir nanoparticles with a narrow size distribution have been synthesized by chemical reduction of their corresponding metal species in ethylene glycol. In all cases, the average particle size was found to be smaller than 10 nm. Particle size was mainly controlled by varying the initial total metal concentration, the reaction temperature, and the concentration of PVP. With the exception of Ir, metal particle agglomeration and sintering was prevented by the addition of PVP, a well known protective agent that also aids particle dispersion.

在乙二醇中对Au、Pt、Pd、Ru、Ir等金属进行化学还原,合成了尺寸分布较窄的纳米颗粒。在所有情况下,发现平均粒径小于10纳米。粒径主要通过改变初始总金属浓度、反应温度和PVP浓度来控制。除Ir外,金属颗粒的团聚和烧结可以通过添加PVP来防止,PVP是一种众所周知的保护剂,也有助于颗粒分散。
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引用次数: 315
Structural stability of titania thin films 二氧化钛薄膜的结构稳定性
Pub Date : 1999-11-01 DOI: 10.1016/S0965-9773(99)00413-4
P.I Gouma , P.K Dutta , M.J Mills

This paper studies the stability of thin films of nanostructured titania at elevated temperatures. Thin films of titania are intended for use in many applications, including high-temperature gas sensing devices. The initial structure of the films consists of nanocrystalline anatase (∼8nm). Exposure of the films to temperatures > 400°C results in the nucleation and subsequent rapid growth of rutile grains (final grain size > 300nm). In-situ, hot-stage experiments in the TEM were carried out, which revealed details about the nucleation and abnormal grain growth processes in this system. It is argued that coarsening of the nano-structure following the transformation is a characteristic of polymorphic reactions from metastable to stable phases. The nucleation process is a critical rate-controlling process for maintaining nanosize grains in the transformed material.

本文研究了纳米二氧化钛薄膜在高温下的稳定性。二氧化钛薄膜可用于许多应用,包括高温气体传感装置。薄膜的初始结构由纳米晶锐钛矿(~ 8nm)组成。薄膜在温度>下的曝光;400°C导致金红石晶粒形核并随后迅速长大(最终晶粒尺寸>300海里)。通过原位热阶段TEM实验,揭示了该体系的成核和异常晶粒生长过程。本文认为,纳米结构的粗化是多晶反应从亚稳态到稳定相的一个特征。成核过程是相变材料中保持纳米级晶粒的关键速率控制过程。
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引用次数: 61
Comparison of grain size distributions obtained by XRD and TEM in milled FCC powders 用XRD和TEM比较了FCC粉的粒度分布
Pub Date : 1999-11-01 DOI: 10.1016/S0965-9773(99)00410-9
J. Guerrero-Paz , D. Jaramillo-Vigueras

Measurements of grain size in powders of the Cu-15at%Al, Cu-20at%Ni, Cu and Ni systems, milled for different times were conducted. X-ray diffraction (XRD) (Warren-Averbach method) and transmission electron microscopy were used for that purpose. From both techniques, distributions of grain diameter (length) were obtained, which permitted to compare both results. Such results were interpreted by considering previous studies of particle size evolution and microstructural evolution. A better comprehension of phenomena that occur in the mechanical alloying, as the grain refinement and the solid solution formation, is attained.

The grain size results obtained by the two techniques were coincident for the Cu-15at%Al system. This system did not present adherence of the powders to the milling media. In the case of the Cu-20at%Ni, Cu and Ni systems, that presented adherence, the results were coincident solely in the powder milled for 864 ks. This is explained due to the microstructural homogenization, reached until that time.

The grain size as a function of the milling time of the two classes of FCC systems, being referred to the adherence phenomenon, presented opposed trends. For example, for the Cu-at15at%Al system, the 70% of the population of grains had a grain size smaller than 7.5, 12 and 20 nm for the milling times of 180, 360 and 864 ks respectively. In the case of the Cu-20at%Ni, Cu and Ni systems, the 70% of the population of grains had a grain size smaller than 35, 22 and 16 nm for the milling times of 180, 360 and 864 ks respectively. These contrary trends reflect different mechanisms of grain size refinement.

A maximum value of grain size of 20 nm required to form the solid solution in the Cu-at15%Al and Cu-20%atNi systems was found.

对Cu-15at%Al、Cu-20at%Ni、Cu和Ni体系不同磨矿时间的粉末粒度进行了测量。x射线衍射(XRD) (Warren-Averbach方法)和透射电子显微镜用于该目的。通过这两种技术,获得了晶粒直径(长度)的分布,从而可以比较两种结果。这些结果是通过考虑先前的粒度演化和微观结构演化的研究来解释的。对机械合金化过程中出现的晶粒细化和固溶体形成等现象有了更好的理解。两种方法得到的Cu-15at%Al体系的晶粒尺寸结果是一致的。该系统不存在粉末对研磨介质的粘附性。在Cu-20at%Ni的情况下,Cu和Ni体系呈现粘附性,结果仅在研磨864 k的粉末中一致。这是由于微观结构的均匀化,直到那个时候才达到。两类催化裂化体系的晶粒度随磨矿时间的变化趋势相反,称为黏附现象。例如,对于Cu-at15at%Al体系,在铣削180、360和864 ks时,70%的晶粒尺寸分别小于7.5、12和20 nm。在Cu-20at%Ni、Cu和Ni体系中,研磨时间分别为180、360和864 ks时,70%的晶粒尺寸分别小于35、22和16 nm。这些相反的趋势反映了不同的晶粒细化机制。在Cu-at15%Al和Cu-20%atNi体系中,形成固溶体所需的晶粒尺寸最大值为20 nm。
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引用次数: 19
Manufacturing and structure investigation of TiN-Al2O3-multilayers tin - al2o3多层膜的制备及结构研究
Pub Date : 1999-11-01 DOI: 10.1016/S0965-9773(99)00400-6
H. Bauer, B. Arnold, K. Bartsch, R. Rennekamp, A. Leonhardt
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引用次数: 5
Surfaces of doped nanophase cerium oxide catalysts 掺杂纳米相氧化铈催化剂的表面
Pub Date : 1999-11-01 DOI: 10.1016/S0965-9773(00)00431-1
A.E.C Palmqvist , M Wirde , U Gelius , M Muhammed

Solid solutions of nanophase cerium oxides have been prepared and the relationship between their bulk crystal structure and surface characteristics has been studied at room temperature with X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS). Dopants with a valence lower than +4, such as Ca2+, Nd3+, and Pb2+, introduce structural defects (oxygen vacancies) in the cerium oxide lattice, which has been found to affect the redox catalytic activity of the materials. The introduction of oxygen vacancies leads to the appearance of an O1s core level peak with a shift of 2.0–2.5 eV to higher binding energies as compared to the core level peak of the lattice oxygen in CeO2. The intensity of this high binding energy O1s peak varies with the expected concentration of oxygen vacancies in the surface, the type of dopant cation and its concentration in the solid solution. It was found that carbonate and hydroxide species are responsible for the appearance of this O1s peak, presumably as a result of capping of oxygen vacancies at the surface. The implications of these surface groups on the catalytic activity of the materials are discussed.

制备了纳米氧化铈固溶体,利用x射线衍射仪(XRD)和x射线光电子能谱仪(XPS)在室温下研究了其体晶结构与表面特性的关系。Ca2+、Nd3+和Pb2+等价态低于+4的掺杂剂会在氧化铈晶格中引入结构缺陷(氧空位),从而影响材料的氧化还原催化活性。氧空位的引入导致O1s核能级峰的出现,与CeO2中晶格氧的核能级峰相比,O1s核能级峰向更高结合能偏移了2.0 ~ 2.5 eV。这种高结合能O1s峰的强度随表面氧空位的预期浓度、掺杂阳离子的类型及其在固溶体中的浓度而变化。发现碳酸盐和氢氧化物是O1s峰出现的原因,可能是由于表面氧空位的封顶。讨论了这些表面基团对材料催化活性的影响。
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引用次数: 86
Preparation of nanoscale α-Al2O3 powder by the polyacrylamide gel method 聚丙烯酰胺凝胶法制备纳米级α-Al2O3粉体
Pub Date : 1999-11-01 DOI: 10.1016/S0965-9773(99)00417-1
H Wang , L Gao , Weiqun li , Qiang li

Nanoscale α-Al2O3 powder has been prepared by the polyacrylamide gel method. Because polymer-network inhibit the aggregate of Al2O3, nanoscale α-Al2O3 powder with about 10 nm size can be obtained. Its calcination temperature is 1100°C, which is 100°C lower than general calcination temperature in other methods.

采用聚丙烯酰胺凝胶法制备了纳米级α-Al2O3粉体。由于聚合物网络抑制了Al2O3的聚集,可以得到粒径约为10 nm的纳米级α-Al2O3粉末。其煅烧温度为1100℃,比其他方法的一般煅烧温度低100℃。
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引用次数: 40
Nanometric grain formation in ductile powders by low-energy ball milling 低能球磨在韧性粉末中的纳米晶粒形成
Pub Date : 1999-11-01 DOI: 10.1016/S0965-9773(99)00403-1
J Guerrero-Paz , D Jaramillo-Vigueras

Based on microstructural observations by TEM and in particle size distribution done by sedimentation-photometry, a new grain size refinement mechanism for ductile powders in mechanical alloying is proposed. A 90–95% of the particle population was of submicrometric fragmented particles. These were detected from the beginning of the milling process up to 90 ks. It seems that the fragmentation of the original particles occurred under dynamic conditions to generate those submicrometric ones. Under these conditions the original grain size (100 nm to 350 nm) was preserved and a low level of dislocations was observed at these submicrometric particles. Once these submicrometric particles were deformed, grains smaller than 20 nm were observed. It seems from TEM results that the submicrometric fragmented particles were also deformed under dynamic conditions. This could be a new grain size refinement mechanism present in ductile metallic powder systems where the fragmentation is the dominant stage from the beginning of the milling up to some intermediate milling time.

In the Cu-20at%Ni, Cu and Ni systems where the particle coalescence process was the dominant stage during all the milling process, a derivation of the mechanism proposed by Hellstern [3] was identified. In our case, powders were mainly deformed by slip and not by shear.

It recognizes that the way to refine the grain size in milled powders is influenced at least by the metallic system used as well as by the equipment and the process conditions employed.

基于透射电镜的显微组织观察和沉积光度法的粒度分布,提出了一种新的机械合金化韧性粉末粒度细化机理。90-95%的粒子群是亚微米级的碎片粒子。这些都是从铣削过程开始到90k检测到的。原始颗粒的破碎似乎是在动态条件下发生的,从而产生了亚微米颗粒。在这些条件下,原始晶粒尺寸(100 nm至350 nm)被保留,并且在这些亚微米颗粒上观察到低水平的位错。一旦这些亚微米颗粒变形,就会观察到小于20纳米的颗粒。从TEM结果来看,亚微米颗粒在动态条件下也发生了变形。这可能是一种新的晶粒细化机制,存在于韧性金属粉末体系中,其中破碎是从铣削开始到铣削中间时间的主要阶段。在Cu-20at%Ni、Cu和Ni体系中,在整个铣削过程中,颗粒聚结过程是主导阶段,对Hellstern[3]提出的机制进行了推导。在我们的情况下,粉末主要是由于滑移而不是剪切而变形的。它承认在磨粉中细化粒度的方法至少受到所使用的金属体系以及所采用的设备和工艺条件的影响。
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引用次数: 12
Synthesis of powders and films using a new laser ablation technique 用激光烧蚀新技术合成粉末和薄膜
Pub Date : 1999-11-01 DOI: 10.1016/S0965-9773(99)00406-7
R. Houriet, R. Vacassy, H. Hofmann
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引用次数: 17
Cluster size effect observed for gold nanoparticles synthesized by sol-gel technique as studied by X-ray photoelectron spectroscopy 用x射线光电子能谱研究溶胶-凝胶法制备金纳米颗粒的团簇尺寸效应
Pub Date : 1999-11-01 DOI: 10.1016/S0965-9773(99)00409-2
S Shukla , S Seal

Gold nanoparticles have been synthesized by sol-gel technique. AFM analysis shows the presence of ≤ 12–14 nm and 40–60 nm sized particles for H2S/not heated and H2S/heated samples respectively. XPS analysis of H2S/not heated sample reveals that the core-level Au 4f7/2 B.E. is shifted by +0.3 eV with increase in the FWHM by 0.2 eV relative to the respective bulk values of 84.0 eV and 1.1 eV. The results are interpreted in terms of the changes in the electronic structure due to finite cluster size and creation of +ve charge over the surface of cluster during the photoemission process itself. The electronic structure of Au nanoparticles (or clusters) produced by present sol-gel technique is compared with that of Au clusters deposited by evaporation method described in the literature.

采用溶胶-凝胶法制备了金纳米颗粒。AFM分析表明,H2S/未加热和H2S/加热样品分别存在≤12-14 nm和40-60 nm大小的颗粒。H2S/未加热样品的XPS分析表明,相对于体积值84.0 eV和1.1 eV, FWHM增加0.2 eV,核心能级Au 4f7/2 B.E.位移+0.3 eV。这些结果可以解释为由于团簇大小有限而导致的电子结构的变化,以及在光发射过程中团簇表面产生的+ve电荷。将溶胶-凝胶法制备的金纳米粒子(或团簇)的电子结构与文献中描述的蒸发法制备的金团簇进行了比较。
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引用次数: 80
期刊
Nanostructured Materials
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