纯稀土纳米晶Gd块体材料的结构与磁性

采用放电等离子烧结技术（简称SPS技术）及热处理制备了全致密纯稀土纳米晶Gd块体材料，研究了材料的微结构和磁性。X衍射结果表明材料在烧结过程中形成了一定程度的c轴织构。TEM观察显示，烧结态纳米晶Gd的平均晶粒尺度在10nm左右；热处理后，平均晶粒尺寸达到100nm。PPMS测试发现与粗晶Gd相比，纳米晶Gd的居里温度以及饱和磁化强度均有所下降。说明Gd的纳米化对其磁性具有重要影响。     

块体纳米晶Ni-Fe合金的制备及表征

采用直流电沉积方法制备块体纳米晶镍铁合金材料,经过工艺参数和成分的优化,提出可连续施镀,并有很高镀厚能力及晶粒尺寸、晶粒结构和合金成分可控的电沉积工艺配方及工艺方法,利用扫描电子显微镜（SEM）、透射电子显微镜（TEM）、X射线衍射分析（XRD）等检测设备进行分析和表征,结果表明,获得的块体纳米晶镍铁合金材料表面光滑致密、结构均匀,材料平均晶粒尺寸在25nm左右。最佳工艺参数为：电流密度Dk=5～dm2,pH值3．5,温度60℃。     

放电等离子烧结制备块状纳米晶SmCo5烧结磁体

采用放电等离子烧结（SPS）技术制备了致密纳米晶SmCo5烧结磁体，研究了磁体的结构和磁性能。X衍射结果表明，烧结磁体具有CaCu5结构，说明SPS过程可以获得稳定的1：5相。TEM观察显示，磁体由平均晶粒尺寸约为30nm的1：5相构成。室温时磁体的矫顽力高达2208kA/m，而剩磁比高达0，7，说明在纳米晶之间存在强烈的晶间交换耦合作用。烧结磁体具有良好的高温性能，773K时的矫顽力为456kA/m，矫顽力温度系数β为-0．212％/K。     

金属铝纳米晶块体材料的制备与性能表征

在惰性气体保护的全封闭系统内,采用直流氢电弧蒸发-冷凝与放电等离子烧结相结合的技术制备出高致密度、晶粒尺寸细小且分布均匀的纯铝纳米晶块体材料.对制备材料的结构分析表明,铝纳米晶块体具有很高的纯度,纳米晶界面洁净无杂相.对制备的铝纳米晶块体的力学性能测试表明,其显微硬度为2.12GPa,比铝粗晶材料提高了约6倍;而弹性模量与粗晶块体相比变化不大.     

SPS烧结工艺对填充方钴矿热电性能的影响

采用熔融淬火和高温退火法合成填充方钴矿Yb_(0. 3)Co_4Sb_(12)块体,用高能球磨的方法将已经填充的方钴矿研磨为微纳米级粉末,然后采用等离子体快速烧结(SPS)技术将其烧结成块体材料。通过XRD分析材料的物相结构,使用SEM和TEM观察粉体和块体材料的微观形貌,发现高能球磨后的晶粒尺寸为50～500 nm,分布较宽。重点研究讨论了烧结温度和烧结压力等烧结工艺对热电传输性能的影响:发现随着烧结温度的提高,材料的热电性能先升高后降低,这是由于烧结温度的升高使得样品致密度有效提高,引起材料热电性能提升,而过高的烧结温度造成材料晶粒异常长大导致材料的热导率提升,热电性能劣化;提高烧结压力可以略微提高样品的致密度与热电性能。研究发现,当烧结温度约为875 K、烧结压力约为90 MPa时,材料的热电性能最佳,热电优值(ZT值)在750 K时达到1.19。     

高纯多晶LaB6纳米块体阴极材料的制备及表征

采用放电等离子烧结技术, 以氢直流电弧法制备的La-LaH₂纳米粉末为原料, 制备了高纯LaB₆多晶纳米块体热阴极材料. 系统研究了LaH₂的脱氢反应、SPS合成LaB₆的烧结反应式, 并用XRD、SEM、TEM和AFM对LaB₆烧结块体的相与结构进行了表征. 实验结果表明, LaH2在796.4℃时发生脱氢反应; SPS制备得到了单相LaB₆纳米多晶块体, 纯度达到99.867%, 相对密度达到99.2%, 和其他烧结方法相比, 样品显微硬度及抗弯强度等性能显著提高. 晶体为大小均匀, 形态规则完整的等轴晶, 50MPa, 烧结温度1250～1350℃范围内平均晶粒尺寸为120nm, 随烧结温度的升高, 晶粒尺寸逐渐增大.     

合金元素对块体纳米晶Fe3Al材料磁学性能的影响

为了研究合金元素对块体纳米晶Fe3Al材料磁学性能的影响,通过铝热反应熔化法制备了纳米晶Fe3Al以及分别含Ni质量分数10%、Cr质量分数10%、Mn质量分数10%和含Ni质量分数10%-Cu质量分数2%的块体纳米晶Fe3Al.在振动样品磁强计(VSM)上测得合金的磁滞回线,分析其磁性能,采用X射线衍射仪进行结构分析和平均晶粒尺寸计算.结果表明:各样品的磁滞回线呈倾斜状且狭长,磁滞损耗很小;含Ni质量分数10%的样品饱和磁化强度Ms较大,剩余磁化强度Mr和矫顽力Hc较其他样品最小,具有较好的软磁性能;添加合金元素后几种材料的晶粒尺寸变小,磁性能有较大变化,合金元素对纳米晶Fe3Al块体材料的磁性能影响明显.     

纳米γ-Ni-Fe合金的磁电阻

用机械球磨Fe2O2—NiO氧化物和氢气还原原位合金化法，制备出纳米γ—Ni—xFe(x=20％-39％，质量分数)合金，并通过XRD、TEM、SEM、BET等方法研究了材料的微观结构与制备条件的关系．结果表明：当氢气还原原位合金化的温度为600-700℃时，合金化完全，Ni—Fe合金的晶粒尺寸为15-55nm，平均颗粒尺寸小于100nm；在30K至室温范围内，块体纳米Ni—Fe合金的各向异性磁电阻率（MR)随温度的降低线性地增加．室温MR＝0．98％，在50K，MR值达8．7％，高磁电阻的原因可能是纳米Ni—Fe合金强烈的磁相关界面散射．     

激光烧结快速制备自由形状纳米块体材料的试验研究

基于选区激光烧结快速成形技术，以纳米Al2O3粉体材料为研究对象，进行了自由形状纳米块体材料制备的研究。研究结果表明，在适当的工艺参数下，可制备出任意形状的Al2O3块体材料，材料内部组织结构致密，晶粒尺寸保持在40nm以内。与其他烧结方法相比，激光烧结制备的纳米材料晶粒尺寸更为细小，组织结构更为致密。     

SmCo7块状纳米晶烧结磁体的制备和性能

采用放电等离子烧结技术制备了致密纳米晶SmCo6.6Nb0.4烧结磁体,研究了磁体的结构和磁性能.结果表明,烧结磁体具有TbCu7结构,说明通过SPS过程可以获得稳定的1:7相;磁体由平均晶粒尺寸约为30 nm的1:7相构成,磁体的室温矫顽力高达2.8 T,而剩磁比高达0.74,说明在纳米晶之间存在强烈的晶间交换耦合作用.烧结磁体具有良好的高温性能,773K时的矫顽力为0.48 T,矫顽力温度系数β为-0.169%/K.     

Thermal properties and microstructure of bulk nanocrystalline Gd material

Bulk nanocrystalline gadolinium (Gd) material has been consolidated from Gd nanoparticles using spark plasma sintering (SPS). High density (>99.5%) bulk nanocrystalline material was achieved after sintering at a temperature of 280 °C with a pressure of 500 MPa. Microstructure analysis shows that the consolidated bulk material exhibits a single phase with hexagonal close packed structure and a fine grain microstructure with a mean grain size of about 15 nm. The structural transformation from hexagonal condensed packed to face centered cubic was not observed, and the second-order magnetic transition remained in the nanocrystalline Gd sample. The Curie temperature of the nanocrystalline Gd decreased by more than 10.7 K below that of the coarse-grained. The activation energies for the coarse-grained and the as-consolidated Gd materials are 2.7702 and 1.0130 eV, respectively.     

纳米晶Ba_（1－x）Pb_xTiO_3的合成与表征

以醋酸铅、硬脂酸钡和钛酸丁酯为原料，用硬脂酸凝胶法（ＳＡＧ）合成了粒度均匀、粒径１０－２０ｎｍ的Ｂａ（１－ｘ）ＰｂｘＴｉＯ３纳米晶粉末．利用红外光谱（ＩＲ）、热重（ＴＧ）和差热分析（ＤＴＡ）研究了纳米晶粉末的合成过程．用ＴＥＭ、ＸＲＤ观察和研究纳米晶的形貌及晶体结构，并用发射光谱测定样品的纯度．     

Deformation twinning in nanocrystalline materials

Nanocrystalline (nc) materials can be defined as solids with grain sizes in the range of 1-100 nm. Contrary to coarse-grained metals, which become more difficult to twin with decreasing grain size, nanocrystalline face-centered-cubic (fcc) metals become easier to twin with decreasing grain size, reaching a maximum twinning probability, and then become more difficult to twin when the grain size decreases further, i.e. exhibiting an inverse grain-size effect on twinning. Molecular dynamics simulations and experimental observations have revealed that the mechanisms of deformation twinning in nanocrystalline metals are different from those in their coarse-grained counterparts. Consequently, there are several types of deformation twins that are observed in nanocrystalline materials, but not in coarse-grained metals. It has also been reported that deformation twinning can be utilized to enhance the strength and ductility of nanocrystalline materials. This paper reviews all aspects of deformation twinning in nanocrystalline metals, including deformation twins observed by molecular dynamics simulations and experiments, twinning mechanisms, factors affecting the twinning, analytical models on the nucleation and growth of deformation twins, interactions between twins and dislocations, and the effects of twins on mechanical and other properties. It is the authors’ intention for this review paper to serve not only as a valuable reference for researchers in the field of nanocrystalline metals and alloys, but also as a textbook for the education of graduate students.     

Thermal expansion behavior and microstructure in bulk nanocrystalline selenium by thermomechanical analysis

Thermal expansion behavior of bulk nanocrystalline (NC) Se samples with a grain size range of 16–46 nm was studied by thermomechanical analysis (TMA) in the temperature range 290–373 K. Bulk NC Se samples were prepared by isothermally crystallizing the as-quenched bulk amorphous solid at 373–478 K. The glass transition and crystallization of the remaining amorphous Se in the partially crystallized samples were studied by TMA, and compared with the results of differential scanning calorimetry (DSC). The glass transition temperature, as determined from the thermal expansion behavior, was 308 K, 11 K lower than the value by DSC analysis. A structural densification phenomenon was observed in a grain growth process of an as-crystallized NC Se sample by TMA. It was found that the linear thermal expansion coefficient of the bulk NC Se sample increased with a reduction of grain size, from which the deduced thermal expansion coefficient of the interface decreased with the refinement of the grain size.     

Structure and properties of nanocrystalline materials

The present article reviews the current status of research and development on the structure and properties of nanocrystalline materials. Nanocrystalline materials are polycrystalline materials with grain sizes of up to about 100 nm. Because of the extremely small dimensions, a large fraction of the atoms in these materials is located at the grain boundaries, and this confers special attributes. Nanocrystalline materials can be prepared by inert gas-condensation, mechanical alloying, plasma deposition, spray conversion processing, and many other methods. These have been briefly reviewed. A clear picture of the structure of nanocrystalline materials is emerging only now. Whereas the earlier studies reasoned out that the structure of grain boundaries in nanocrystalline materials was quite different from that in coarse-grained materials, recent studies using spectroscopy, high-resolution electron microscopy, and computer simulation techniques showed unambiguously that the structure of the grain boundaries is the same in both nanocrystalline and coarse-grained materials. A critical analysis of this aspect and grain growth is presented. The properties of nanocrystalline materials are very often superior to those of conventional polycrystalline coarse-grained materials. Nanocrystalline materials exhibit increased strength/hardness, enhanced diffusivity, improved ductility/toughness, reduced density, reduced elastic modulus, higher electrical resistivity, increased specific heat, higher thermal expansion coefficient, lower thermal conductivity, and superior soft magnetic properties in comparison to conventional coarse-grained materials. Recent results on these properties, with special emphasis on mechanical properties, have been discussed. New concepts of nanocomposites and nanoglasses are also being investigated with special emphasis on ceramic composites to increase their strength and toughness. Even though no components made of nanocrystalline materials are in use in any application now, there appears to be a great potential for applications in the near future. The extensive investigations in recent years on structure-property correlations in nanocrystalline materials have begun to unravel the complexities of these materials, and paved the way for successful exploitation of the alloy design principles to synthesize better materials than hitherto available.     

Stress-dependent deformation behaviour in bulk nanocrystalline titanium–nickel alloys

In this study, the deformation mechanisms operating with stress in bulk nanocrystalline (NC) titanium–nickel with an average grain size below a critical size of 10–20?nm have been investigated. We demonstrate a sequential variation of the deformation mechanism from grain boundary (GB) sliding and grain rotation to grain growth and dislocation activity with the increase of the deformation stress. These deformation mechanisms are different from the previous understanding that below a critical grain size of 10–20?nm, GB sliding and grain rotation govern plastic deformation of NC materials.     

Localized strain and heat generation during plastic deformation in nanocrystalline Ni and Ni–Fe

Room temperature tensile testing was performed on a coarse-grained polycrystalline Ni (32 μm), a nanocrystalline Ni (23 nm) and two nanocrystalline Ni–Fe (16 nm) electrodeposits at two strain rates of 10^?1 and 10^?2/s. Strain localizations and local temperature increases were simultaneously recorded during tensile testing. For all materials, higher loads or higher strain rate generally resulted in higher peak temperature with the highest temperatures recorded in the fracture regions. The maximum temperature for the nanocrystalline materials was just over 80 °C, which is significantly below the reported temperatures for the onset of thermally activated grain growth. Therefore, the previously reported grain growth observed on similar materials after tensile deformation is likely not thermally activated but a stress-induced phenomenon. Despite the wide grain range from 16 nm to 32 μm, all samples exhibited similar strain localization behavior. Local strain variations initiated in the early stage of macroscopic uniform deformation, subsequent necking and fracture took place in the region of initial strain localization. While the coarse-grained polycrystalline Ni exhibited little strain rate sensitivity, gradually increased strain rate sensitivity was observed for the 23 nm Ni and the two 16 nm Ni–Fe samples, suggesting that both dislocation-mediated and grain-boundary-controlled mechanisms were operative in the deformation of the nanocrystalline Ni and Ni–Fe samples.     

NiAl-B composites with nanocrystalline intermetallic matrix produced by mechanical alloying and consolidation

Powder mixtures with equiatomic Ni–Al stoichiometry and with the addition of 5, 10, 20 and 30 vol% of boron were mechanically alloyed in a high-energy SPEX mill. Differential scanning calorimetry (DSC) was used for examination of the thermal behaviour of the milled powders. The mechanically alloyed powders and powders after DSC examinations were investigated by X-ray diffraction (XRD). For all the powder mixtures, a nanocrystalline NiAl intermetallic phase was formed during milling. With the increase of boron concentration in the mixtures, more intense refinement of the NiAl grain size during mechanical alloying was observed. Scanning electron microscopy (SEM) and energy dispersive X-ray spectroscopy (EDS) examinations showed that the produced powders have composite structure, with boron particles uniformly distributed in the nanocrystalline NiAl intermetallic matrix. The density of the composite powders decreases with the increase of boron content, following the rule of mixture.The produced powders were subjected to consolidation by hot-pressing at 800 °C under the pressure of 7.7 GPa for 180 s. The produced bulk materials were investigated by XRD, SEM and EDS as well as characterised by hardness, density and open porosity measurements. It was found that during applied consolidation process the nanocrystalline structure of the NiAl matrix was maintained. The average hardness of the bulk composite samples is in the range of 10.58–12.6 GPa, depending on boron content, increases with the increase of boron content, and is higher than that of the NiAl intermetallic reference sample (9.53 GPa). The density of the bulk composite samples is the same as that of the corresponding powders after milling, decreases with the increase of boron content and is lower than that of the NiAl reference sample. To the best of our knowledge, the NiAl-B composites with nanocrystalline intermetallic matrix have been produced for the first time.     

Interfacial Characteristics of Nanocrystalline FeMoSiB Alloys

By using X-ray diffraction (XRD), transmission electronic microscopy (TEM) and transmissionMssbauer spectroseopy (TMES), the formation, structure and properties including microhardnessand electrical resistivity of nanocrystalline FeMoSiB alloys have been investigated. By annealing theas-quenched FeMoSiB sample at 833-1023K for 1 h, nanocrystalline materials with grain sizes of15 to 200 nm were obtained. Mssbauer spectroscopy results reveal a quasi-continuous distributionfeature of P(H)-H curves for 15 nm-and 20 nm-grained samples. Also, it was found that resistivityand microhardness of nanocrystalline Fe-Mo-Si-B alloys exhibit strong grain size effect.     

Thermal conductivity of nanocrystalline silicon: importance of grain size and frequency-dependent mean free paths

The thermal conductivity reduction due to grain boundary scattering is widely interpreted using a scattering length assumed equal to the grain size and independent of the phonon frequency (gray). To assess these assumptions and decouple the contributions of porosity and grain size, five samples of undoped nanocrystalline silicon have been measured with average grain sizes ranging from 550 to 64 nm and porosities from 17% to less than 1%, at temperatures from 310 to 16 K. The samples were prepared using current activated, pressure assisted densification (CAPAD). At low temperature the thermal conductivities of all samples show a T(2) dependence which cannot be explained by any traditional gray model. The measurements are explained over the entire temperature range by a new frequency-dependent model in which the mean free path for grain boundary scattering is inversely proportional to the phonon frequency, which is shown to be consistent with asymptotic analysis of atomistic simulations from the literature. In all cases the recommended boundary scattering length is smaller than the average grain size. These results should prove useful for the integration of nanocrystalline materials in devices such as advanced thermoelectrics.