自蔓延高温合成氮化铝晶须形态和生长机理研究(1)

采用自蔓延高温合成技术(SHS),在高压氮气中成功地合成了氮化铝晶须,并对它的显微结构进行了研究.研究结果表明,由于制备时的生长条件极不稳定,出现不同形态的晶须形貌,除了细长均匀的氮化铝晶须外,还出现了各种其它不规则形状的产物.过饱和度的不同,产生了枝蔓晶结构.按照VS生长方式,在均衡生长条件下,生长为本征结构的氮化铝晶须.晶须顶端的杂质小液滴,为VLS生长方式创造了条件.通过光学显微镜观察,合成出的氮化铝晶须是透明的.     

氮化铝晶体的生长惯习面和晶体形态

本文采用氧化铝碳热还原方法制备出了多种形态的氮化铝单晶(晶须).通过透射电子显微镜电子衍射和X射线单晶衍射分析,确定了氮化铝单晶常见的生长惯习面,并分析和讨论了氮化铝晶须形态与氮化铝晶体结构与生长惯习面的关系.具有规则六棱柱锥形的AlN晶须的生长取向为[0001]晶向,而叶片状和四方截面形状的AlN晶须则大多沿〈21-1-3-〉晶向进行生长,细小的薄片状AlN晶须则多以{101-0}面和{101-1}面为生长面.     

自蔓延高温合成氮化铝晶须形态和生长机理研究(2)

在对自蔓延高温合成方法制得的AIN晶须形态研究的基础上,采用高分辩电镜等技术,对AIN晶须进行了生长机理研究,结果表明,晶须头部的小液滴显示氮化铝晶须可由VLS机制生成.光滑晶须头部的出现、过饱和度与晶须直径的关系、侧面的二次生长、生长台阶的出现,这些都说明VS机制在起作用.虽然在AIN晶须中发现层错和位错,但经过分析认为,它们都不是氮化铝晶须的生长机制.     

氮化铝（AlN）晶须碳热还原法合成研究

本文以氧化铝和石墨为原料，在普通氮气气氛条件下成功地合成出了氮化铝晶须。对碳热还原法合成ＡｌＮ晶须的工艺条件，显微形貌，生长取向和生长机一进行初步分析和探讨。由于生长条件不同，ＡｌＮ晶须通常呈六棱柱状，片状或四方形截面状等多种形态。     

氮化铝纳米线直接氮化制备工艺优化及形成机理分析

采用金属铝粉与氮气在一定温度下直接反应的方法,利用金属镁粉与NH4 Cl双重辅助氮化的优越性,制备出性能较好的氮化铝粉体纳米材料,主要包括纳米颗粒及纳米晶须.通过优化反应物的添加剂配比、反应温度、保温时间等反应条件,得到了形貌较好的氮化铝纳米线材料.在此基础上分析了氮化铝纳米线的反应生成过程,并采用VS机制对纳米线的生长机理进行了解释.     

PVT法同质外延制备大尺寸Al极性氮化铝晶体生长工艺及其表征分析研究

本文基于自主设计的氮化铝生长炉,开展了四组不同工艺条件下Al极性面氮化铝籽晶同质外延生长氮化铝单晶的生长特征及其结晶质量表征研究。研究发现:不同工艺条件下生长的晶体的拉曼图谱E₂(high)特征峰峰位表明,晶体内部均存在较小的拉应力;在坩埚顶部在相对较高温度2 210 ℃、坩埚底部与顶部温差42 ℃的低过饱和度生长条件下,晶体表面光滑,呈现阶梯流生长形貌,并具有典型的氮化铝单晶生长习性面,晶体初始扩张角大于40°,高分辨率X射线衍射(HRXRD)测得0002、1012反射摇摆曲线及拉曼光谱检测结果表明,该条件下生长的氮化铝晶体结晶质量优异,并可实现快速扩径。基于该生长条件,通过外延生长后成功获得尺寸ϕ45~47 mm的氮化铝单晶锭,相关表征结果表明生长的氮化铝晶体具有优越的结晶性能。     

合成温度对碳热还原法合成碳化硅晶须形貌的影响

以SiO2微粉为硅源,炭黑为碳源,氧化硼为催化剂,采用碳热还原法分别在1500 ℃、1550 ℃、1600 ℃制备了SiC晶须.通过扫描电镜,电子探针和透射电镜等分析手段,研究了合成温度对SiC晶须形貌的影响,探讨了晶须的生长机理.结果表明:当合成温度为1500 ℃时,所合成的SiC晶须形貌呈竹节状,选区电子衍射分析发现孪晶等面缺陷在晶须的生长方向上周期性出现;当合成温度在1550 ℃以上时,哑铃状晶须的数量会急剧增多,分析表明晶须表面包裹的串珠小球为β-SiC.在晶须的顶端发现催化剂熔球,由此推测生长机理为VLS机理,但当合成温度超过1550 ℃时,SiC会以VS生长机理沿径向沉积生成哑铃状晶须.     

液相体系晶须生长机理:拓展的ACP机制

晶须生长机制一直备受关注,然而"晶须到底是怎样生长为条状的?"这一科学问题始终未能得到解决.传统晶须生长机制不适用于液相体系晶须生长.本文试图提出液相体系晶须生长机制应为拓展的ACP(Anion Coordination Polyhedron)机制.因为传统的晶须生长机制未能解释液相体系晶须的生长形态,也未能解释晶须的多样性以及指导人工可控晶须生长.拓展的ACP生长机制克服了这些问题,并有效地指导人工晶须生长.     

溶胶凝胶法制备的莫来石晶须的形貌和生长过程研究

本文通过溶胶凝胶工艺制备了莫来石晶须，采用ＸＲＤ、ＳＥＭ、ＴＥＭ、ＳＡＤＰ和ＥＤＡＸ等分析测试技术研究了莫来石晶须的形貌，晶相组成和晶须的成分，结果表明，莫来石晶须是通过气固相反应按位错机理生长的，气相成分的波动可能是部分晶须的轴向不稳定生长、两次生长和其表面出现缺陷的主要原因。     

β-SiAlON晶须的诱导合成和生长机制研究

以β-SiAION粉料为晶种,SiC为基体,加入Si粉、AI粉和Al2O3粉在1900 K氮气气氛下合成β-SiAlON晶须,研究了晶须的显微结构、相组成和晶须增韧SiC复合材料的力学性能,并结合热力学研究了晶须的生长机制.结果表明:(1)以β-SiAlON粉料为诱导晶种时可以合成β-SiMON晶须材料,其生长机制为VLS机制和VS机制;(2)当以VLS机制生长时,晶须合成z值为1.56,直径约为200 -300nm,呈柱状和纤维状,当以VS机制生长时,晶须合成z值为1.76,直径为0.5～1.5 μm,呈柱状和竹节状,发育较为规则;(3)晶须相可有效提高复合材料的力学性能,相同组成的复合材料中,当β-SiAlON晶须相的含量较高时,材料可以在气孔率较高(32.1;)条件下获得了较好的抗折强度(55.2 MPa).     

Ti-Al-Nb2O5系原位合成Al2O3晶须的形成机理分析

本文研究了以粉埋法原位合成的Al2O3晶须的形态和反应过程以及晶须的生长机理.通过物相测试表明产物由Al2O3、TiAl3、NbAl3和少量的AlN相组成,SEM结合EDS分析表明原位合成了直径小于100nm的Al2O3晶须,晶须呈棉絮状分布于基体交界处.基于铝的过剩,TiAl3相是Ti-Al界面的唯一产物.Ti与O2以反应时间短的动力学势优先形成的TinOm中间产物是Al2O3晶须生成的控制步骤.Nb2O5与铝液的双效复合催化作用,提高了晶须的生成速率;同时Al的用量因AlN的生成而减小,导致生成晶须的催化活性点减小,而扩散到每个活性点周围的TinOm及Nb2O5浓度增加,导致晶须分布密而均匀.Al2O3晶核在催化剂的作用下以螺旋位错生长形成长径比较为理想的Al2O3晶须.     

Possibility of AlN growth using Li–Al–N solvent

The possibility of AlN growth using Li–Al–N solvent was investigated. Based on theoretical prediction, we selected Li₃N as a suitable nitrogen source for AlN growth. First, vapor phase epitaxy using Li₃N and Al as source materials was performed to confirm the following reaction on the growth surface: Li₃N+Al=AlN+3Li. The results suggest that the reaction proceeds to form AlN on the substrate under appropriate conditions. Next, AlN growth using Li–Al–N solvent was carried out. The Li–Al–N solvent was prepared by annealing of mixtures composed of Li₃N and Al. The results imply that AlN was formed under an Al-rich condition. Moreover, it was found that Li was swept out from AlN grains during growth. The results suggest that AlN growth using Li–Al–N solvent might be a key technology to obtain an AlN crystal boule.     

Effect of the seed crystallographic orientation on AlN bulk crystal growth by PVT method

The growth of AlN crystals by PVT method was investigated using TaC crucible in the temperature range of 2250‐2350 °C. AlN boules with 30 mm in diameter were successfully grown on the crucible lid by self‐seeded growth. The AlN boules consist of the spontaneously nucleated AlN single crystal grains with the {1010} natural crystalline face. The fast growth rate of more than 1 mm/h was achieved. AlN crystals grown on (11 0)‐, (10 0)‐, and (0001)‐face AlN seeds were investigated. Different experimental phenomena have been observed under particular condition. The crystal grown on (11 0)‐face seed has different natural crystalline face from the seed. For the crystal grown on (10 0) or (0001) seed, the crystal natural crystalline face is same as the crystallographic orientation of the seed. (© 2011 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

VLS Growth of ITO Whiskers Prepared by the Electron Shower Method

Indium tin oxide (ITO) whiskers were grown by VLS (vapour-liquid-solid) mechanism, using the electron shower method. The whiskers were grown above 200 °C, and the deposition rate was above 0.6 nm/s. The electron shower controlled the size of the whiskers, and the size was 30 nm in diameter and 600 nm in length. The whiskers grew along the substrate at t < 300 s, but grew in a direction perpendicular to the substrate at t > 300 s. When the ITO whiskers grown along the substrate were used as NO₂ gas sensor, the sensitivity was 340, and about 300 times higher than those of the whiskers grown in a direction perpendicular to the substrate and plate-like ITO crystallites.     

Reduction of the defect density in GaN films using ultra-thin AlN buffer layers on 6H-SiC

A low dislocation density of 10^7–8 cm⁻² in GaN thin films on 6H-SiC(0001) substrates grown by metalorganic chemical vapor deposition was achieved. By considering possible origins of dislocations in the GaN/AlN/Sic structure, two major dislocation reduction routes are proposed; ultra-thin AlN buffer layers and smooth AlN surfaces in an atomic scale. Experimentally, the effects of the surface roughness and structural perfection of the AlN buffer layer on GaN film quality were extensively investigated as a function of AlN film thickness. The reduced dislocation density was realized by using ultra-thin AlN buffer layers having a thickness of 1.5 nm, which is below the critical value for misfit dislocation generation. The smoother surface morphology and enhanced structural quality of ultra-thin AlN buffer layers were found to be the main parameters in reducing the defect density in the GaN film.     

氢氧化镁晶须的制备及其生长机理探讨

以Mgcl2和NaOH为原料,采用直接沉淀法制备氢氧化镁晶须.研究了添加不同晶控剂对氢氧化镁晶须生成的影响,同时对添加硬脂酸锌制备氢氧化镁晶须的工艺进行研究.采用扫描电子显微镜和粒度分析仪对产品进行表征.结果表明,硬脂酸锌和氯化铁对氢氧化镁晶须的生成具有导晶作用;所得产品为长径比10.7的氢氧化镁晶须.采用负离子配位多面体生长基元理论可以有效地解释氢氧化镁晶须的生成.     

Preparation and characterisation of fluorapatite whiskers

Fluorapatite (FAp) whiskers were prepared by using Molten Salt Synthesis (MSS) technique. β‐tricalcium phosphate (TCP) and various fluorine salts, along with potassium sulphate as a flux salt were used as starting materials for preparing FAp whiskers. Effects of flux to powder weight ratio, temperature and soaking time on the morphology were studied. The optimum temperature to obtain FAp whiskers was found to be 1175°C. The phase purity of the prepared FAp whiskers were confirmed by powder X‐ray diffraction and FTIR spectra, and the whiskers were further characterized by laser Raman spectra, chemical analysis and DTA/TGA thermal analysis. The morphology of the FAp whiskers were investigated by scanning electron microscope (SEM) analysis. (© 2008 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

六钛酸钾晶须的制备及生长机理的研究

通过KDC方法成功制备了六钛酸钾(K2Ti6O13)晶须,并进行了热重分析和差热分析,研究烧结时间和烧结温度对K2Ti6O13晶须结晶过程的影响,通过X射线衍射分析了K2Ti6O13晶须的相组成和晶体指数.此外,通过扫描电子显微镜和透射电子显微镜研究晶须的微观结构,揭示了K2Ti6O13晶须的生长机理.     

Low-pressure HVPE growth of crack-free thick AlN on a trench-patterned AlN template

A thick AlN layer was grown on a trench-patterned AlN/sapphire template by low-presssure hydride vapor phase epitaxy (LP-HVPE). Compared with the AlN layer grown on a flat AlN/sapphire template, the AlN layer grown on the trench-patterned AlN/sapphire template had a crack-free and smooth surface. The typical full-widths at half-maximum (FWHMs) of X-ray rocking curves (XRC) for the (0 0 0 2), (1 0 1¯ 2), and (1 0 1¯ 0) diffractions of the AlN layer on the trench-patterned AlN/sapphire template were 132, 489, and 594 arcsec, respectively. In addition, atomic steps were observed on the AlN layer on the trench-patterned AlN/sapphire template, and the root-mean-square (RMS) roughness of the AlN layer was determined to be 0.602 nm by atomic force microscopy (AFM).