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Bondlength alternation of nanoparticles Fe2O3 coated with organic surfactants probed by EXAFS 用EXAFS探测有机表面活性剂包覆纳米Fe2O3的键长变化
Pub Date : 1999-11-01 DOI: 10.1016/S0965-9773(99)00425-0
T Liu , L Guo , Y Tao , T.D Hu , Y.N Xie , J Zhang

The nanoparticles γ-Fe2O3 coated with surfactants, DBS, ST and CTAB, repsectively, were synthesized by microemulsion method. The coated ferric oxides, which show enhanced nonlinear optical properties compared with their bulk counterpart, were probed by EXAFS in solution forms. The x-ray absorption spectra for Fe K edge were measured at room temperature by help of synchrotron radiation light source. Extended x-ray absorption fine structure analysis shows that the coating layers of organic molecules interact with surface atoms of nanoparticles, the Fe-O bond length was extended.

采用微乳液法制备了表面活性剂DBS、ST和CTAB包覆的纳米γ-Fe2O3。用EXAFS对包覆后的三氧化铁溶液进行了探测,结果表明包覆后的三氧化铁具有增强的非线性光学性质。在同步辐射光源的帮助下,测量了Fe - K边在室温下的x射线吸收光谱。扩展x射线吸收精细结构分析表明,有机分子涂层与纳米粒子表面原子相互作用,Fe-O键长度被延长。
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引用次数: 25
Grain growth in nanocrystalline SnO2 prepared by sol-gel route 溶胶-凝胶法制备SnO2纳米晶的晶粒生长
Pub Date : 1999-10-01 DOI: 10.1016/S0965-9773(99)00387-6
C.H Shek , J.K.L Lai , G.M Lin

The isothermal grain growth of nanocrystalline SnO2, prepared by the sol-gel route was investigated at various temperatures between 500°C and 800°C. Grain growth data were analyzed using two different models. A conventional grain growth model for polycrystalline materials yields an extremely low activation energy of 47 kJ/mol, but large grain growth exponent n from 5 to 11. These values exceed the rational region deduced from conventional theory. An alternative model is based on the assumption that the ordering of the interface regions in nanocrystalline SnO2 occurs simultaneously with grain growth by structural relaxation. This structural relaxation model describes the grain growth kinetics satisfactorily and also yields a low activation energy of 31 kJ/mol appropriate for the rearrangement of atoms.

研究了溶胶-凝胶法制备的SnO2纳米晶在500 ~ 800℃温度下的等温晶粒生长。采用两种不同的模型对谷物生长数据进行分析。传统的多晶材料晶粒生长模型的活化能极低,只有47 kJ/mol,但晶粒生长指数n在5 ~ 11之间。这些值超出了从常规理论推导出的合理范围。另一种模型是基于这样的假设,即纳米晶体SnO2中界面区域的有序与晶粒生长同时发生,即结构弛豫。该结构松弛模型令人满意地描述了晶粒生长动力学,并产生了适合原子重排的31 kJ/mol的低活化能。
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引用次数: 72
Preparation of self-assembled cobalt nanocrystal arrays 自组装钴纳米晶阵列的制备
Pub Date : 1999-10-01 DOI: 10.1016/S0965-9773(99)00375-X
J.S Yin , Z.L Wang

Processing of self-assembled magnetic nanocrystals has vitally scientific and technological interests. In this paper, three different kinds of self-assemblies of cobalt nanocrystals were processed using particles processed by thermal decomposition of cobalt carbonyl in toluene. In case 1, two-dimensional self-assembly of cobalt nanocrystals with an average particle size of 9.2 nm and polydispersity of 9% has been formed. In case 2, macroscopic whisker structures composed of self assembled cobalt nanocrystals (with an average size of 8 nm) were formed during the thermal decomposition under an externally applied magnetic field. The whiskers can be aligned in the longitudinal axis direction during drying using an external magnetic field. In case 3, one-dimensionally ordered, densely packed self-assemblies have also been prepared using cobalt nanocrystals with irregular shape and larger particle sizes (10–20 nm). The formation of these different structures is attributed to the magnetic properties of cobalt particles with different sizes.

自组装磁性纳米晶体的制备具有重要的科学和技术意义。本文利用羰基钴在甲苯中热分解后的颗粒,制备了三种不同的钴纳米晶自组装体。在case 1中,形成了平均粒径为9.2 nm、多分散度为9%的钴纳米晶体的二维自组装。在案例2中,在外加磁场的作用下,在热分解过程中形成了由自组装钴纳米晶体组成的宏观晶须结构(平均尺寸为8 nm)。在干燥过程中,利用外部磁场可使晶须沿纵轴方向排列。在案例3中,使用形状不规则、粒径较大(10 - 20nm)的钴纳米晶体也制备了一维有序、密集排列的自组装体。这些不同结构的形成归因于不同尺寸钴颗粒的磁性。
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引用次数: 28
Effects of helium ion implantation on the structure of nanophase and coarse-grain titanium films 氦离子注入对纳米相和粗晶钛膜结构的影响
Pub Date : 1999-10-01 DOI: 10.1016/S0965-9773(99)00382-7
Zheng Gao , Yuzun Gao , Yonghong Li , Taisong Zhang , Yi Li

Nanophase and coarse-grain titanium films were prepared on Mo substrates by Ion Beam Assisted Deposition. Ion implantation of helium was used to simulate the behavior of helium in titanium films. Helium ions (100 keV) were implanted into the titanium films with a dose of 5 × 1017/cm2. The retained helium in the titanium films after implantation was detected by Enhanced Proton Back Scattering (EPBS). The microstructure of titanium films and the distribution of helium bubbles were studied by Transmission Electron Microscopy (TEM). It was found that helium bubbles were formed in the coarse-grain titanium films with a size distribution of 1 to 10 nm and a numerical density of 5 to 25 × 1022/m3. No helium bubble was observed in the nanophase titanium films. A discussion is presented for helium bubble formation.

采用离子束辅助沉积的方法在Mo衬底上制备了纳米钛膜和粗晶钛膜。采用氦离子注入法模拟了氦在钛膜中的行为。将氦离子(100 keV)以5 × 1017/cm2的剂量注入钛膜。利用增强质子反向散射(EPBS)技术检测钛膜注入后的氦残留。利用透射电子显微镜(TEM)研究了钛膜的微观结构和氦气泡的分布。结果表明,在粗晶钛膜中形成了氦泡,其尺寸分布为1 ~ 10 nm,数值密度为5 ~ 25 × 1022/m3。纳米钛膜中未观察到氦泡。对氦泡的形成进行了讨论。
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引用次数: 6
Structure, strength and toughness of nanocrystalline FeAl 纳米晶FeAl的结构、强度和韧性
Pub Date : 1999-10-01 DOI: 10.1016/S0965-9773(99)00385-2
M.A Morris-Muñoz , A Dodge , D.G Morris

Refining grain size to the nanocrystalline level has been suggested as a way of improving strength while enhancing ductility and toughness. In the present study, nanocrystalline bulk FeAl has been prepared by mechanical alloying and hot forging. Powders quickly reach a state of partial order during milling, and low temperature annealing is sufficient to chemically homogenise and give full order. Contamination during milling leads to the formation of carbide and oxide particles, which stabilise fine grains during heating. Bulk materials show grain sizes of 20nm to 100nm depending on the consolidation temperature. Hardness and compression strength show little change over this grain size range. Fracture toughness stays high down to moderately small grain sizes, falling only for consolidation at the lowest temperatures. There appears to be a reasonable range of fine grain sizes (40–100nm) where good interparticle bonding and high densities can be achieved leading to good strength and toughness.

将晶粒细化到纳米晶水平被认为是一种提高强度同时增强延展性和韧性的方法。本研究采用机械合金化和热锻法制备了纳米晶块状FeAl。粉末在碾磨过程中迅速达到部分有序状态,低温退火足以使化学均匀化并使其完全有序。铣削过程中的污染导致碳化物和氧化物颗粒的形成,在加热过程中使细晶粒稳定。根据固结温度的不同,块状材料的晶粒尺寸为20nm ~ 100nm。硬度和抗压强度在此晶粒尺寸范围内变化不大。断裂韧性在中等小晶粒尺寸下保持较高,仅在最低温度下凝固。在一个合理的细晶粒尺寸范围内(40-100nm),可以实现良好的颗粒间结合和高密度,从而获得良好的强度和韧性。
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引用次数: 85
Effect of oxygen deficiency on the Raman spectra and hyperfine interactions of nanometer SnO2 氧缺乏对纳米SnO2拉曼光谱和超精细相互作用的影响
Pub Date : 1999-10-01 DOI: 10.1016/S0965-9773(99)00373-6
C.H Shek , G.M Lin , J.K.L Lai

The Raman and Mössbauer spectra of nano-SnO2 specimens with crystallite size 3–16 nm were measured at room temperature. Specimens were annealed at different temperatures in oxygen atmosphere and vacuum respectively. Both the Raman and Mössbauer spectra of the specimens consist of crystalline and interface (or surface) components. The effects of oxygen deficiency on the Raman spectra are presented and correlated with the changes of the Sn-O bond properties, which were obtained from the corresponding Mössbauer spectra.

在室温下测量了晶粒尺寸为3 ~ 16 nm的纳米sno2样品的拉曼光谱和Mössbauer光谱。试样分别在氧气气氛和真空中进行不同温度的退火。样品的拉曼光谱和Mössbauer光谱均由晶体和界面(或表面)组分组成。研究了缺氧对拉曼光谱的影响,并将其与Sn-O键性质的变化联系起来。
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引用次数: 87
Characterization of barium titanate ceramic/ceramic nanocomposite films prepared by a sol-gel process 溶胶-凝胶法制备钛酸钡陶瓷/陶瓷纳米复合膜的表征
Pub Date : 1999-10-01 DOI: 10.1016/S0965-9773(99)00374-8
M.C Cheung , H.L.W Chan , Q.F Zhou , C.L Choy

Barium titanate (BaTiO3) ceramic/ceramic nanocomposite thick films (∼16μm) for ultrasonic transducer applications were prepared by a modified sol-gel process. Nano-sized BaTiO3 powder was dispersed in a sol-gel matrix of BaTiO3 to form a composite solution. Films were prepared by spin coating and then annealed at various temperatures. The crystallization of the composite film was studied by X-ray diffraction. The dielectric permittivity and the ferroelectric properties of the film were also measured.

采用溶胶-凝胶法制备了用于超声换能器的钛酸钡(BaTiO3)陶瓷/陶瓷纳米复合厚膜(~ 16μm)。将纳米BaTiO3粉末分散在BaTiO3溶胶-凝胶基质中形成复合溶液。采用旋涂法制备薄膜,并在不同温度下退火。用x射线衍射研究了复合薄膜的结晶过程。测定了薄膜的介电常数和铁电性能。
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引用次数: 40
A two step SPD processing of ultrafine-grained titanium 超细晶钛的两步SPD加工
Pub Date : 1999-10-01 DOI: 10.1016/S0965-9773(99)00384-0
V.V Stolyarov , Y.T Zhu , T.C Lowe , R.K Islamgaliev , R.Z Valiev

Equal channel angular pressing (ECAP) and high pressure torsion (HPT) are two severe plastic deformation (SPD) processes that have been used to process ultrafine-grained (UFG) materials. In this investigation, we have attempted to combine these two processes to refine the grain size of coarse-grained pure titanium. ECAP processing was first carried out at 500–450 °C to refine the grain size to about 300 nm. Further processing by HPT resulted in finer grain size and higher dislocation density. The second step, HPT processing, also increased the microhardness, ultimate strength, yielding strength and ductility of the UFG pure titanium.

等通道角挤压(ECAP)和高压扭转(HPT)是两种用于加工超细晶(UFG)材料的严重塑性变形(SPD)工艺。在本研究中,我们试图结合这两种工艺来细化粗晶纯钛的晶粒尺寸。首先在500-450℃下进行ECAP处理,将晶粒尺寸细化到约300 nm。HPT进一步加工后,晶粒尺寸更细,位错密度更高。第二步HPT处理也提高了UFG纯钛的显微硬度、极限强度、屈服强度和延展性。
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引用次数: 212
Correlation between microstructure and electrical properties of tungsten-silica nanocomposites 钨-二氧化硅纳米复合材料微观结构与电性能的关系
Pub Date : 1999-10-01 DOI: 10.1016/S0965-9773(99)00388-8
Tamar Tepper , Shlomo Berger

The electrical properties and the microstructure of nanocomposite materials composed of nano-sized amorphous silica powder and micron-sized tungsten powder were studied as a function of composition and heat treatment temperature. The dielectric constant and the electrical conductivity of the nanocomposites are higher than those of pure silica powder at all compositions. The percolation threshold of this system is about 20% vol. W. Above this composition a sharp increase in the dielectric constant and in the electrical conductivity occurs. This increase becomes even sharper after the nanocomposites are heat treated at 950°C for 1 hour. No changes in the microstructure are observed up to this temperature. It is suggested that the electrical properties of the nanocomposites are dominated mainly by dangling bonds at the W/SiO2 interfaces. Further research should be undertaken to investigate the factors controlling the dielectric constant and the electrical conductivity in order to obtain high capacitance materials with high dielectric constant and low electrical conductivity.

研究了由纳米非晶硅粉和微米级钨粉组成的纳米复合材料的电学性能和微观结构与材料成分和热处理温度的关系。纳米复合材料的介电常数和电导率均高于纯硅粉。该体系的渗透阈值约为20% vol. w,在此组合物之上,介电常数和电导率急剧增加。纳米复合材料在950°C下热处理1小时后,这种增加变得更加明显。在此温度以下,显微结构没有变化。结果表明,纳米复合材料的电学性能主要受W/SiO2界面悬垂键的影响。为了获得高介电常数、低电导率的高电容材料,需要进一步研究控制介电常数和电导率的因素。
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引用次数: 9
Demonstration of gas-phase combustion synthesis of nanosized particles using a hybrid burner 混合燃烧器气相燃烧合成纳米颗粒的实验研究
Pub Date : 1999-10-01 DOI: 10.1016/S0965-9773(99)00376-1
Margaret S Wooldridge , Stephen A Danczyk , Jianfan Wu

A new approach for gas-phase combustion synthesis of nanosized particles using a novel hybrid burner facility is demonstrated. The basis of the synthesis technique is to use both a premixed flame and a diffusion flame to control the synthesis environment. Specific experimental results for silica (SiO2) production from silane/hydrogen/oxygen/argon (SiH4/H2/O2/Ar) flames are presented. A parametric study of several burner conditions was conducted, and the subsequent effects on the particles produced were determined. Particle morphology was examined using transmission electron microscopy (TEM). The results indicated a broad variation in particle size and structure as a function of the burner operating conditions (in particular, reactant stoichiometry and flame geometry). Particle structures were aggregated with primary particles varying from 6–8 nm in size (high oxygen concentration conditions) to larger more continuous structures with primary particles 18–20 nm in size (low oxygen concentration conditions). Bulk material properties were examined using Fourier transform infrared spectroscopy (FTIR), thermal gravimetric analysis (TGA), nitrogen adsorption (BET) and x-ray diffraction (XRD).

介绍了一种新型混合燃烧装置用于气相燃烧合成纳米颗粒的新方法。该合成技术的基础是同时使用预混火焰和扩散火焰来控制合成环境。介绍了硅烷/氢/氧/氩(SiH4/H2/O2/Ar)火焰制备二氧化硅(SiO2)的具体实验结果。对几种燃烧条件进行了参数化研究,确定了后续对颗粒产生的影响。用透射电子显微镜(TEM)观察颗粒形态。结果表明,颗粒大小和结构的变化很大,这是燃烧器操作条件(特别是反应物化学计量和火焰几何形状)的函数。颗粒结构由6-8 nm大小(高氧浓度条件)到18-20 nm大小(低氧浓度条件)的更大的连续结构组成。采用傅里叶变换红外光谱(FTIR)、热重分析(TGA)、氮吸附(BET)和x射线衍射(XRD)对大块材料的性能进行了表征。
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引用次数: 14
期刊
Nanostructured Materials
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