黄金电铸层硬度的影响因素探讨

利用X射线光谱仪、扫描电子显微镜以及显微维氏硬度计对电沉积黄金样品进行了分析测试,发现不同电沉积样品其维氏硬度值不同.将不同电沉积样品的晶粒大小、织构系数以及显微维氏硬度值进行了对比,发现当电沉积黄金晶粒小到纳米级时,会出现反常Hall-Petch效应;显微维氏硬度值高的样品(111)晶面具有强的择优取向,硬度最高的电沉积黄金样品可以达到117.0HV0.2,其(111)晶面的织构系数可以达到70.59;.且织构系数高的样品在扫描显微镜下观察到表面平整度更高.因此,电沉积工艺中可以通过添加剂的使用,来控制晶粒的择优取向,从而得到硬度更高、表面平整度更好的样品.     

不同能量密度下脉冲激光烧蚀制备纳米Si晶粒成核生长动力学研究

在室温、10 Pa氩气环境下,采用脉冲激光烧蚀(PLA)技术,通过改变激光能量密度,在烧蚀点正下方、与烧蚀羽辉轴线平行放置的衬底上沉积制备了一系列纳米Si晶薄膜.采用SEM、Raman散射谱和XRD对纳米Si晶薄膜进行了表征.结果表明:沉积在衬底上的纳米Si晶粒分布在距靶一定的范围内,晶粒尺寸随与靶面距离的增加先增大后减小;随着激光能量密度的增加,晶粒在衬底上的沉积范围双向展宽,但沉积所得最大晶粒尺寸基本保持不变,只是沉积位置随激光能量密度的增加相应后移.结合流体力学模型、成核分区模型和热动力学方程,通过模拟激光烧蚀靶材的动力学过程,对纳米Si晶粒的成核生长动力学过程进行了研究.     

微波熔盐沉积制备AlN纳米晶及光致发光特性研究

以高纯AlCl3和Li3N为反应原料,NaCl和KCl为混合熔盐,使用微波熔盐沉积法在700℃制备出A1N纳米晶.利用XRD、SEM、EDS等对纳米晶的物相、形貌进行了定性和定量表征,并使用PL测试了材料的光学性质,分析了主要缺陷类型.XRD测试结果表明,实验获得产物为六方纤锌矿结构的AlN.使用Scherrer公式估算了AlN 产物的晶粒平均粒度大小约为35.6 nm,表明所得确为AlN纳米晶.SEM观测到的纳米晶形貌为方形,分布均匀且晶粒形状几近,平均粒度约为35 nm.EDS测试结果显示AlN纳米晶中Al和N的原子相对百分含量为50.521;和49.479;,其化学配比几近于1∶1物质的量比.室温PL测试发现发光中心在435 nm,缺陷主要是杂质缺陷类型.以上结果充分表明微波熔盐沉积法是一种制备AlN纳米晶的有效方式.     

水热反应温度对碱性条件下TiO2纳米晶生长动力学及其光电性能的影响

以钛酸丁酯为原料,在碱性条件下水热合成了锐钛矿相TiO2纳米晶.采用X射线衍射仪、比表面积测试仪、扫描电子显微镜等方法对纳米晶粒的晶体结构、比表面积以及光阳极的表面形貌分别进行表征,研究水热反应温度对TiO2纳米晶生长动力学过程的影响规律.结果表明:随着温度的升高,锐钛矿相纳米晶的平均晶粒尺寸先增大后减小.光电转换性能测试表明,电池的光电转换性能随着水热反应温度的升高而增大,在220℃时获得最大光电转换效率4.05;( 1sun,100 mW/cm2).并分析了水热反应温度对碱性条件下TiO2纳米晶粒的生长动力学过程和电池光电转换性能的影响机制.     

纳米结构TiN薄膜的制备与性能研究

利用自行研制的磁过滤等离子体设备,在室温条件下的不锈钢基底上成功地制备了性能良好的纳米结构TiN薄膜.运用原子力显微镜和X射线衍射仪对其结构和形貌进行了表征.利用纳米硬度仪测量了TiN薄膜的硬度和弹性模量.结果显示:沉积的TiN薄膜表面非常平整光滑,致密而无缺陷;硬度远高于粗晶TiN的硬度;TiN晶粒尺寸在30～50nm;沉积过程中在基底上施加的负偏压会影响纳米结构TiN薄膜的结构和性能.     

微纳米复合金刚石自支撑膜的制备及微观结构的研究

在30 kW级直流电弧等离子喷射化学气相沉积装置下,采用Ar-H2-CH4混合气体,通过控制工艺参数,在多晶钼衬底上制备了微纳米复合多层金刚石自支撑膜.采用拉曼光谱对其进行成份分析、SEM观察膜体表面形貌,采用聚焦离子束(FIB)技术对其进行原位刻蚀,用高分辨电镜观察对其进行微观表征.结果显示,同普通微米膜相比,多层膜体是由微米晶金刚石层和纳米晶金刚石层组成,表面光滑,微米层与纳米层间具有相互嵌套式的界面,微/纳米复合多层金刚石自支撑膜中包含有纳米级金刚石晶粒、微米级金刚石晶粒和无定形碳.     

电沉积法制备ZnO纳米棒阵列及其发光特性

本文以掺F的SnO2导电玻璃为基板,以硝酸锌水溶液为电解液,采用三电极恒电位体系电沉积制备ZnO纳米棒阵列,系统考察了硝酸锌浓度和沉积电位等工艺参数对ZnO纳米棒阵列的微观形貌及其发光性能的影响规律.结果表明,硝酸锌浓度和沉积电位对纳米棒阵列的形貌有显著影响,控制适宜的工艺条件可以制备出直径分布均匀、结晶性好且纯度高的六方纤锌矿ZnO纳米棒阵列.荧光光谱分析表明,电沉积制备出的ZnO纳米棒阵列在385 nm附近有一个强荧光发射峰,且发光性能稳定、对纳米棒阵列微观形貌的细微变化不敏感,使其在发光二极管和激光器等领域具有广阔的应用前景.     

MPCVD法纳米金刚石膜的制备及分析

利用MPCVD方法在玻璃基片上成功的制备了非常光滑、致密均匀的纳米金刚石膜.沉积工艺分为两步:成核,CH4/H2=3;;生长,O2/CH4/H2=0.3:3:100;沉积过程中保持工作压力为4.0kPa,衬底温度500℃.拉曼、透射电镜、红外光谱、表面轮廓仪等的测试表明:膜层由纳米级金刚石晶粒组成,最大晶粒尺寸小于100nm,成核密度大于1011/cm2.成核面晶粒的点阵常数较大,表明存在较多缺陷,表面粗糙度小于2nm,在可见光区完全透明,红外光学性能接近金刚石单晶理论值.     

无电镀沉积于硅衬底上铜纳米晶的场发射性能

采用无电镀沉积技术在经过机械抛光的单晶硅衬底上沉积了铜纳米晶.利用X射线衍射数据,估算出所沉积铜纳米晶的平均粒径大约为40nm.对120s无电镀沉积样品的场发射测试表明,该样品的开启场强为～5.5V/μm,在场强达到9.26V/μm时的场发射电流密度可达到62.5μA/cm2.对相应的沉积过程和场发射机理进行了分析.结果表明,无电镀沉积技术有可能成为制备具有较好场发射性能的金属/硅冷阴极的一种可供选择的方法.     

LICVD法纳米硅制备过程中的成核及生长

自行设计制备了激光诱导化学气相沉积法(LICVD)纳米制粉装置,利用该装置制备的纳米硅粉其粒度波动在30～60nm之间.通过对不同反应气体流量条件下的激光能量阈值研究表明,随反应气体流量的增加,所需激光能量阈值大致成线性增加.利用透射电镜和高分辨电镜对其形貌进行了表征,并对其成核与生长进行了分析,在成核长大初期,晶核周围的Si原子浓度较高,纳米硅晶应以层状长大方式为主.当纳米晶中有螺型位错等晶体缺陷形成时,会为Si原子的"落座"提供生长所需的台阶源,晶粒将以螺旋状生长方式长大.在长大过程中,纳米晶会发生跳跃式长大现象.以跳跃方式长大的晶粒通常在两晶粒的结合面处伴有晶体缺陷发生或亚晶界产生.较低的反应气体流速条件下,纳米硅的择优生长方向为<112>晶向;而在较高的反应气体流速条件下其择优生长方向变为<111>晶向.     

Molecular dynamics simulations of grain growth in nanocrystalline Ag

Isothermal grain growth behaviors, including the effect of temperature and mean grain size, of nanocrystalline Ag are investigated using the molecular dynamics simulations with an analytical embedded atom potential. The atomistic simulations provide a level of atomic details on microscopic mechanism and process of grain growth that still remains inaccessible to experiments. The small grain size and high temperature accelerate the grain growth, it is the same as the conventional polycrystalline materials. The grain growth processes of nanocrystalline Ag are well characterized by a power-law growth curve, followed by a linear relaxation stage. Beside grain boundary migration and grain rotation mechanisms, the dislocations (or stacking faults) serve as the intermediate role in the grain growth process.     

二氧化钛纳米晶囊泡微乳液在聚氨酯涂饰体系中的应用

以钛酸丁酯为原料,十六烷基三甲基溴化铵与十二烷基苯磺酸钠自组装形成的囊泡为微反应器,制备了二氧化钛纳米晶囊泡微乳液.将二氧化钛纳米晶囊泡微乳液与水性阳离子聚氨酯复配,得到聚氨酯/TiO2囊泡微乳液(UPC/TVM)复合皮革涂饰剂,采用TEM、马尔文粒径分析和紫外漫反射等方法,研究了TiO2囊泡微乳液和聚氨酯配比对涂饰剂分散、成膜、涂饰性能的影响.研究结果表明,TiO2囊泡微乳液与聚氨酯形成均一的微乳液,粒径尺寸在80 nm左右.TiO2囊泡微乳液的加入,使得UPC/TVM3膜与UPC膜相比,抗张强度、断裂伸长率和吸水性都有所提高并出现明显的抗紫外效果.UPC/TVM复合皮革涂饰剂应用实验结果表明涂层的抗水性提高,耐折性能没有改变.     

The structure and properties of nanocrystalline Fe78B13Si9 alloy

A new method has been employed to prepare a nanocrystalline alloy from amorphous ribbons and some of the structure-dependent properties of this alloy have been studied and compared with those of coarse-grained crystalline and amorphous FeBSi alloys. The new method of preparing nanocrystalline alloys involves annealing isothermally an amorphous ribbon of the same composition. By comparing the structure-dependent properties, it can be concluded that the novel properties of the nanocrystalline alloy reflect the unusual nature of its grain boundaries.     

Formation and properties of Fe-based amorphous/nanocrystalline alloy coating prepared by wire arc spraying process

Wire arc spraying process was used to deposit FeBSiCrNbMnY amorphous/nanocrystalline alloy coating onto stainless steel substrate. The microstructure of the coating was characterized by using X-ray diffraction (XRD), scanning election microscopy (SEM) equipped with energy dispersive X-ray analysis (EDXA) and transmission electron microscopy (TEM). The coating is about 500 μm in thickness with fully dense and low porosity. The microstructure of the coating is classified into two regions, namely, a full amorphous phase region and homogeneous dispersion of α Fe, Cr nanoscale particles with a scale of 30–60 nm in a residual amorphous matrix region. The formation mechanism of the amorphous and nanocrystalline alloy was discussed. Mechanical properties, such as microhardness and wear resistance of the coating were also analyzed. The Vickers hardness of the coating is around Hv = 900–1050. The relatively wear resistance of the amorphous/nanocrystalline alloy coating is about 3× than that of crystalline structure 3Cr13 martensite stainless steel coating under the same wear testing condition. The FeBSiCrNbMnY amorphous/nanocrystalline alloy coating has high microhardness and excellent wear resistance.     

Novel solution routes of synthesis of metal oxide and hybrid metal oxide nanocrystals

Novel solution routes covering a wide range of processes like hydrothermal, solvothermal and supercritical techniques have been described in detail with reference to the processing of a wide range of advanced inorganic nanocrystalline materials and organic-inorganic hybrid nanocrystalline materials. The significance of the thermochemical calculations, in situ surface modification and the experimental parameters has been discussed. One step in situ fabrication of advanced functional nanocrystalline materials by soft solution processing has also been discussed briefly. Synthesis of nanocrystals of metal oxides and hybrid nanocrystals and also processing several nanocomposites like carbon nanotubes: metal oxide, activated carbon: metal oxide, etc. has been reviewed in relation to various process parameters. The effect of doping, size, shape and quality on the properties of nanocrystalline materials has been discussed in relation to the photoluminescence and photocatalytic characteristics.     

TiO2颗粒原位合成TiB2对B4C陶瓷材料组织与力学性能的影响

碳化硼是一种应用广泛且极具潜力的结构陶瓷,具有低密度、高强度、高硬度、耐磨损、耐腐蚀等优良性能,但是韧性差、烧结温度高的特性限制了其更为广泛的应用.本文采用原位合成和硅溶渗反应烧结相结合的方式制备TiB2增强B4C陶瓷材料,再分别对所制备的复合陶瓷材料的力学性能和显微组织进行研究,研究结果表明:原位合成的TiB2颗粒分布更加均匀,晶粒更加细小且原位合成的TiB2颗粒主要分布在B4C边界,对B4C陶瓷材料起到增韧补强的作用;当添加量达到8wt;时,弯曲强度出现最大值为269 MPa,断裂韧性最大值为7.73 MPa·m1/2,是TiO2添加量为0wt;的B4C陶瓷材料的2.46倍.     

Preferential coalescence of nanocrystalline silicon on different film substrates

The characteristics of nanocrystalline silicon deposited on different film substrates were studied. Through atomic force microscopy, field emission scanning electron microscopy, Raman scattering and Hall effect measurements, we investigated and compared the morphology, columnar grain size, crystallinity and Hall mobility of nanocrystalline silicon on different film substrates. The mechanisms affecting the characteristics of nanocrystalline silicon deposited to different substrates were studied in detail.     

Formation of the nanocrystalline state by twinning crystals

The formation of the nanocrystalline state under the action of a concentrated load applied to crystals is studied. It is established that the relaxation of the enormous stresses (on the order of the shear modulus) arising under the indenter proceeds through twinning, which results in the fragmentation of the structure into nanoblocks. The properties of the nanocrystalline material thus obtained are explained based on the consideration of grain boundaries as twin boundaries that represent another phase of the material.     

乙酰丙酮对PMMA负载锐钛矿型TiO2薄膜及其光催化性能影响

以钛酸丁酯作为钛源,水为溶剂,乙酰丙酮(AcAcH)为表面修饰剂,采用微波水热辅助溶胶-凝胶法制备了纳米晶二氧化钛水溶液,利用提拉镀膜法在聚合物聚甲基丙烯酸甲酯(PMMA)基板上沉积得到了透明TiO2纳米晶薄膜.通过X射线衍射(XRD)、红外光谱(FTIR)、透射电子显微镜(TEM)、原子力显微镜(AFM)和紫外-可见光吸收光谱(UV-Vis)等对TiO2纳米颗粒和薄膜的晶相组成、表面形貌及光学性能进行表征.同时通过紫外光光催化降解罗丹明B研究了TiO2薄膜的光催化性能.结果表明:通过引入乙酰丙酮,可以得到高度分散、晶相为锐钛矿型的TiO2水溶胶,在PMMA基板上沉积得到的薄膜表面平整、致密,具有良好的透光率,经过180 min紫外光照射,对罗丹明B的降解率达到90;以上.