ZnO纳米块体材料的制备及其性能的研究

采用连续成型方式压制了纳米ZnO素坯，考察了素坯密度、烧结时间、致密化温度等参数与 成型方式的关系.用场发射扫描电镜表征了烧结体微观组织特征.测定了ZnO纳米块体材料中 硬度随烧结温度的变化规律.结果表明，采用连续成型方式可使素坯密度提高56％、烧结时 间缩短了3h、致密化温度降低200℃.场发射扫描电镜显示烧结体内部密度及颗粒尺寸分布 均匀.硬度测定结果显示ZnO纳米块体材料中显微硬度随烧结温度的变化不是单调的，而是随 烧结温度的升高显微硬度先升高后降低，拐点对应的晶粒尺寸为50—60nm. 关键词： ZnO纳米块体 连续成型 硬度     

放电等离子烧结制备纳米Ni块体材料

 采用自悬浮定向流法制备纳米Ni粉体,利用放电等离子烧结技术制备出了直径10 mm、厚2 mm,致密度为96.8 %,显微硬度为4.17 GPa的纳米块体材料。用X射线衍射仪、扫描电子显微镜和显微硬度计分析了烧结块体样品的相组成、晶粒尺寸、微观形貌和显微硬度。研究表明：随烧结温度的升高,块体样品的致密度和晶粒尺寸增大,当烧结温度为650 ℃时,致密度最高,晶粒尺寸为44.8 nm;显微硬度随烧结温度的增高先增大后减小,当烧结温度为550 ℃时,显微硬度最大为4.33 GPa;较高烧结温度下,断口微观形貌的纳米级韧窝出现,显示了韧性断裂的特征。     

纳米ZrO2(4Y)的快速高压烧结研究

纳米Y2O3稳定的ZrO2粉在4GPa高压下、1000－1200℃烧结2min致密成型。完整块体致密度为99．3％。在高压烧结过程中,由于外加压力对扩散的促进作用,活化能比用其它方法烧结时降低,约为48kJ/mol,晶粒长至40－70nm。四方度及晶胞体积略小于常压烧结样品的数值。高压快速烧结ZrO2(4Y)陶瓷为棕色、深灰色或黑色。快速高压烧结所得样品结构存在某种非均匀性。     

纳米ZrO_2(4Y)的快速高压烧结研究

纳米Y2 O3 稳定的ZrO2 粉在 4GPa高压下、10 0 0～ 12 0 0℃烧结 2min致密成型。完整块体致密度为 99.3%。在高压烧结过程中 ,由于外加压力对扩散的促进作用 ,活化能比用其它方法烧结时降低 ,约为 4 8kJ/mol,晶粒长至 4 0～ 70nm。四方度及晶胞体积略小于常压烧结样品的数值。高压快速烧结ZrO2 (4Y)陶瓷为棕色、深灰色或黑色。快速高压烧结所得样品结构存在某种非均匀性。     

高温高压烧结高硬度高致密度块体金属钨及钨基合金W-TiC

采用高温高压烧结方法,烧结纯钨和TiC颗粒弥散增强W-TiC合金材料,对钨及W-TiC合金的烧结致密化行为和力学性能进行了研究。结果表明:在压力为5.0GPa、温度为1 500℃的条件下烧结15min可获得良好的烧结样品,块体钨的致密度达到99.3%,硬度达到6.43GPa;在相同的高温高压烧结条件下,添加质量分数为1.5%的TiC,获得的W-TiC合金致密度达到99.0%,硬度达到7.58GPa。极端高压环境不但能抑制钨及钨合金在烧结过程中的晶粒长大,还能降低烧结温度,提高烧结效率,增加烧结体的致密性。在此基础上进一步探索了钨及钨基合金W-TiC的高压烧结动力学、微观结构、机械性能与烧结压力和烧结温度的关系。     

压力及高压增氧对La2-xSmxCuO4结构及输运性质的影响

 对常压、高压、高压增氧条件下合成的La_2-xSm_xCuO₄（0≤x≤2.0）结构进行了研究。常压合成样品清晰地反应出样品由T→T+T′→T′相的变化，其中，T相：0相似文献   

高性能ZnO纳米块体材料的制备及其拉曼光谱学特征

利用六面顶高压设备制备了高密度、低脆性、纳米级的ZnO块体材料，用MDI/JADE5 X射线衍射仪(Cu靶)和XL30S-FEG场发射扫描电子显微镜对高压样品的相组成、晶粒尺寸及微观形貌进行了表征.利用E55+FRA106/5傅里叶变换激光拉曼光谱仪通过ZnO块体样品位于50—500cm^-1之内的拉曼光谱, 研究了极性半导体纳米材料的拉曼光谱学特征.发现在极性半导体ZnO纳米块体材料中，没有出现明显的尺寸限制效应. 关键词： ZnO纳米块体 拉曼光谱 尺寸限制效应     

粗晶和纳米晶Sm_3Co合金的制备及其性能研究

本文针对Sm3Co粗晶和纳米晶合金材料的制备和基础性能进行了研究.采用磁悬浮熔炼技术多次精炼制备出Sm3Co粗晶合金.以此为母材,利用高能球磨非晶化和放电等离子烧结致密化并同步晶化的技术路线,制备出平均晶粒尺寸为8 nm的超细纳米晶Sm3Co合金块体材料.构建了Sm3Co纳米晶合金的晶体结构模型,并结合其显微组织的表征,分析了Sm3Co纳米晶合金的磁性能和力学性能,并与粗晶合金进行了比较粗晶Sm3Co合金不具有硬磁特性,而同种成分的纳米晶合金则表现出一定的硬磁特性.纳米晶Sm3Co合金的显微硬度和弹性模量分别达到4.87 GPa和63.7 GPa,比粗晶合金增大约8.7%和13.3%.本文研究结果为Sm-Co体系合金的基础性能及其纳米尺度效应提供了系统的参考依据.     

高压对纳米ZnO和ZnO/SnO2复合材料的结构和发光性能的影响

 利用溶胶-凝胶法制备出了纳米晶ZnO与含有3%摩尔分数SnO₂的ZnO/SnO₂复合材料,在六面顶压机上对制备出的两种样品进行了室温下、6GPa的高压处理。采用X射线衍射（XRD）、透射电子显微镜（TEM）和光致荧光谱（PL）等方法,对高压处理前后样品的结构和发光性质进行了表征。结果表明：高压处理后回收到的纳米晶ZnO和ZnO/SnO₂复合材料的平均粒径分别减小5.9%和26.3%;高压处理后ZnO和ZnO/SnO₂复合材料光致发光谱的发光带强度都有所降低,但ZnO/SnO₂复合材料发光带强度降低幅度比纯ZnO小,对产生这些现象的原因进行了讨论。     

高压导致纳米TiO2形变的电子显微研究

α-PbO₂相TiO₂高压相具有适宜的带隙能和可见光范围的光催化能力,是一种适用于可见光、高效且环保的光催化材料.本文使用金刚石对顶压砧对锐钛矿纳米球进行加压-卸压处理得到了α-PbO₂相TiO₂高压相.利用透射电子显微镜对比初始样品和卸压样品,观察结果表明晶粒发生了明显形变,高分辨图显示其晶粒中存在大量[100]方向层错和形变孪晶,其中亚微米级晶粒中形成了透镜形片层结构的形变孪晶带;纳米级晶粒中形成了扇形多重形变孪晶.研究表明高压下锐钛矿TiO₂可以发生明显的形变,其形变的微观机制与金属类似,主要为形变孪晶和层错滑移,形变孪晶的形成存在明显的尺寸效应.这些结果为TiO₂高压相变的尺寸效应研究提供了一个新的切入点,同时还为制备孪晶α-PbO₂相TiO₂高压相提供了方法.     

Grain evolution of nano-crystals ZnO under HP and HT

Grain evolution of nano-crystals ZnO under high temperature and pressure is studied using a cubic high pressure apparatus. The structure, grain sizes and morphology of the samples are characterized by X-ray diffraction and field emission scanning electron microscopy. The results show that the grain sizes of ZnO grow rapidly at temperature 200°C under pressure. At temperature lower than 300°C (including 300°C), the grain sizes of the samples first increase with the pressure increasing from 1 to 3 GPa and later decrease from 4 to 6 GPa. The activation volume from 1 to 3 GPa and from 4 to 6 GPa is calculated respectively using the phenomenological kinetic grain growth equation at temperature 300°C. At temperature higher than 400°C (including 400°C), the grain sizes of the samples increase with the pressure increasing from 1 to 6 GPa. ZnO nano-bulks with good quality can be obtained under the specific conditions.     

In-situ observations and acoustic measurements upon fragmentation of free-floating intermetallics under ultrasonic cavitation in water

Grain refinement in alloys is a well-known effect of ultrasonic melt processing. Fragmentation of primary crystals by cavitation-induced action in liquid metals is considered as one of the main driving mechanisms for producing finer and equiaxed grain structures. However, in-situ observations of the fragmentation process are generally complex and difficult to follow in opaque liquid metals, especially for the free-floating crystals. In the present study, we develop a transparent test rig to observe in real time the fragmentation potential of free-floating primary Al₃Zr particles under ultrasonic excitation in water (an established analogue medium to liquid aluminium for cavitation studies). An effective treatment domain was identified and fragmentation time determined using acoustic pressure field mapping. For the first time, real-time high-speed imaging captured the dynamic interaction of shock waves from the collapsing bubbles with floating intermetallic particles that led to their fragmentation. The breakage sequence as well as the cavitation erosion pattern were studied by means of post-treatment microscopic characterisation of the fragments. Fragment size distribution and crack patterns on the fractured surface were then analysed and quantified. Application of ultrasound is shown to rapidly (<10 s) reduce intermetallic size (from 5 mm down to 10 μm), thereby increasing the number of potential nucleation sites for the grain refinement of aluminium alloys during melt treatment.     

Grain fragmentation in ultrasonic-assisted TIG weld of pure aluminum

Under the action of acoustic waves during an ultrasonic-assisted tungsten inert gas (TIG) welding process, a grain of a TIG weld of aluminum alloy is refined by nucleation and grain fragmentation. Herein, effects of ultrasound on grain fragmentation in the TIG weld of aluminum alloy are investigated via systematic welding experiments of pure aluminum. First, experiments involving continuous and fixed-position welding are performed, which demonstrate that ultrasound can break the grain of the TIG weld of pure aluminum. The microstructural characteristics of an ultrasonic-assisted TIG weld fabricated by fixed-position welding are analyzed. The microstructure is found to transform from plane crystal, columnar crystal, and uniform equiaxed crystal into plane crystal, deformed columnar crystal, and nonuniform equiaxed crystal after application of ultrasound. Second, factors influencing ultrasonic grain fragmentation are investigated. The ultrasonic amplitude and welding current are found to have a considerable effect on grain fragmentation. The degree of fragmentation first increases and then decreases with an increase in ultrasonic amplitude, and it increases with an increase in welding current. Measurement results of the vibration of the weld pool show that the degree of grain fragmentation is related to the intensity of acoustic nonlinearity in the weld pool. The greater the intensity of acoustic nonlinearity, the greater is the degree of grain fragmentation. Finally, the mechanism of ultrasonic grain fragmentation in the TIG weld of pure aluminum is discussed. A finite element simulation is used to simulate the acoustic pressure and flow in the weld pool. The acoustic pressure in the weld pool exceeds the cavitation threshold, and cavitation bubbles are generated. The flow velocity in the weld pool does not change noticeably after application of ultrasound. It is concluded that the high-pressure conditions induced during the occurrence of cavitation, lead to grain fragmentation in a pure aluminum TIG weld during an ultrasonic-assisted TIG welding process.     

Char characteristics and particulate matter formation during Chinese bituminous coal combustion

The characteristics of char particles and their effects on the emission of particulate matter (PM) from the combustion of a Chinese bituminous coal were studied in a laboratory-scale drop tube furnace. The raw coal was pulverized and divided into three sizes, <63, 63–100, and 100–200 μm. These coal samples were subjected to pyrolysis in N₂ and combusted in 20 and 50% O₂ at 1373, 1523, and 1673 K, respectively. Char samples were obtained by glass fiber filters with a pore size of 0.3 μm, and combustion-derived PM was size-segregated by a low pressure impactor (LPI) into different sizes ranging from 10.0 to 0.3 μm. The characteristics of char particles, including particle size distribution, surface area, pore size distribution, swelling behavior and morphology property, were studied. The results show that, coal particle size and pyrolysis temperature have significant influence on the char characteristics. The swelling ratios of char samples increase with temperature increasing from 1373 to 1523 K, then decrease when the temperature further increases to 1623 K. At the same temperature, the swelling ratios of the three size fractions are markedly different. The finer the particle size, the higher the swelling ratio. The decrease of swelling ratio at high temperature is mainly attributed to the high heating rate, but char fragmentation at high temperature may also account for the decrease of swelling ratio. The supermicron particles (1–10 μm) are primarily spherical, and most of them have smooth surfaces. Decreasing coal particle size and increasing the oxygen concentration lead to more supermicron-sized PM formation. The influence of combustion temperature on supermicron-sized PM emission greatly depends on the oxygen concentration.     

Grain refinement in coarse-grained 7475 Al alloy during severe hot forging

Grain refinement taking place in a coarse-grained 7475 Al alloy was studied in multidirectional compression at 490°C and at a strain rate of 3?×?10^?4?s^?1. The integrated flow curve displays significant work softening just after yielding and an apparent steady-state plastic flow at high strains. The structural changes are characterized by the development of deformation or microshear bands in coarse-grain interiors, followed by homogeneous evolution of new grains at high strains. The new grains are considered to be developed by a kind of continuous reaction through grain fragmentation that is similar to continuous dynamic recrystallization (cDRX). The mechanism of fine grain production and the factors controlling grain refinement during hot multidirectional deformation are discussed in detail.     

Ceramic synthesis of 0.08BiGaO_3–0.90BaTiO_3–0.02LiNbO_3 under high pressure and high temperature

In this paper, the preparation of 0.08BiGaO_3–0.90BaTiO_3–0.02LiNbO_3 is investigated at pressure 3.8 GPa and temperature 1100–1200?C. Experimental results indicate that not only is the sintered rate more effective, but also the sintered temperature is lower under high pressure and high temperature than those of under normal pressure. It is thought that the adscititious pressure plays the key role in this process, which is discussed in detail. The composition and the structure of the as-prepared samples are recorded by XRD patterns. The result shows that the phases of Ba TiO_3, BaBiO_(2.77), and Ba_2Bi_4Ti_5O_(18) with piezoelectric ceramic performance generate in the sintered samples. Furthermore, the surface morphology characteristics of the typical samples are also investigated using a scanning electron microscope. It indicates that the grain size and surface structure of the samples are closely related to the sintering temperature and sintering time. It is hoped that this study can provide a new train of thought for the preparation of lead-free piezoelectric ceramics with excellent performance.     

Grain orientation and magnetic evaluation of the hot forged Bi-Sr-Ca-Cu-O system

The Bi-Sr-Ca-Cu-O superconductor (BSCC) shows strong anisotropy in its physical and mechanical properties. Therefore, superconducting properties may be changed with the degree of grain orientation. In this paper, we describe the process of hot forging in the Bi-Sr-Ca-Cu-O system. In the hot forging temperature range of 770 ～ 820°C, highly dense samples have been obtained under the applied pressure of 200 ～ 300 kg/cm². Critical current density J_c is increasing with increase of grain orientation. Grain orientation is usually checked by X-ray analysis. However, it is found that the BSCC compound has a different value of grain orientation in the surface and inside the samples. Magnetic evaluation is effective for checking grain orientation in bulk samples.     

X射线荧光光谱高压制样方法和技术研究

使用自行设计研制的高压制样模具和高压制样技术(专利号: 201310125772.5),对岩石、土壤,水系沉积物等地质样品进行高压制样研究,这是国内首次的高压制样尝试,并取得了显著的成果。不加粘结剂,用1600 kN高压能使各种类型地质粉末样品压制成型。而且,经高压制备的试样片表面致密、平整、光滑、光亮,不龟裂,不分层,不掉粉末,消除了对X射线荧光光谱仪分析室的污染,为X射线荧光光谱分析粉末制样开辟了一条新途径。通过对元素分析线、背景强度、校准曲线斜率、方法的精密度和制样的重现性的对比研究表明：高压(1 600 kN)制备的试样片较常规压力(400 kN)元素的峰背比值、灵敏度显著地提高,检出限明显降低、分析结果更接近标准值、精密度和样品制备的重现性均有较大提高。还利用电子显微镜和X射线衍射对这些高压试样片(1600 kN)和常规压力的试样片(400 kN)作了表面形态和结构的对照研究,研究表明：高压试样片(1 600 K)较常规压力的试样片(400 kN)二氧化硅谱峰的半高宽均变宽。表明峰形发生了变异,变化的原因可能是在高压下SiO₂晶格被破坏,粒度减小,因而使高压制备的试样片表面更加坚实、致密、平滑、不掉粉末,减少了颗粒度和矿物效应,提高了分析结果的精密度和准确度。     

不同物理形态复合肥的激光诱导击穿光谱特性分析

为深入了解激光诱导击穿光谱技术应用于复合肥成分的检测机制,选用不同物理形态(粉状和颗粒状)的复合肥样品,在不同压力下制得片状样品进行实验,以分析不同物理形态复合肥样品的激光诱导击穿光谱特性。实验分别对比了0,0.5,2,4,6MPa下粉末和颗粒的N,P,K的等离子体光谱特性。研究结果表明,在压力较小时,两种形态样品的光谱特性存在较大差别,且颗粒状样品的谱线强度明显高于粉末状样品。而随着压力的增加,两者的光谱特性的差别逐渐减小。对于同一形态样品,随着压力的增加,各主要元素的特征谱线强度均呈现先增加后减小的变化趋势。