CdS籽晶扩大技术北大核心

采用物理气相传输(PVT)法制备大尺寸硫化镉(CdS)籽晶,通过调整源区与生长区温差进行了籽晶扩大实验,并进行了X射线衍射(XRD)、红外透过率和腐蚀坑密度等测试。研究表明,在15,10,5和2℃等不同温差条件下,均可实现CdS籽晶的扩展,扩展的晶体区域具有和初始籽晶相同的晶向,而且低温差利于获得更大的单晶扩展面积。当温差为5℃时,扩展出的CdS单晶的X射线衍射半高宽(FWHM)较小、红外透过率较高且腐蚀位错密度较低,表明此时晶体的质量较好;当温差增大为10℃和15℃时,蒸气过饱和度高、晶体生长速率大,导致晶体质量变差;当温差减小为2℃时,晶体生长驱动力不足,这容易形成不稳定的生长界面并导致晶体质量下降。     

基于PVT法自发形核生长AlN晶体的研究

根据物理气相传输法(PVT) AlN晶体生长特点及工艺要求,自主设计了AlN晶体生长炉及其配套热场.FEMAG软件热场模拟结果表明,自主设计的晶体生长炉及其配套热场可以达到AlN晶体生长所需坩埚内部温度梯度要求.基于设计的PVT生长炉,开展了在2 250℃生长温度、40 h长晶时间条件下的自发形核生长实验.实验研究结果表明,在该工艺条件下,通过自发形核可生长得到典型长度为3～Smm、直径为2 mm的高质量AlN单晶;AlN晶体的c-plane(0001)生长速率最快,易形成尖锥形晶体结构,不利于晶体的扩径;Raman表征图谱中AlN晶体的E2 (high)半峰宽仅为5.65 cm-1,表明AlN晶体质量非常高;SEM、EDS分析得出晶体内部质量较为均匀,c-plane和m-plane腐蚀形貌特征明显.     

高温形核层对蓝宝石衬底AlN薄膜质量的影响

采用两步生长模式的金属有机化学气相沉积方法在蓝宝石衬底上外延生长AlN薄膜,通过高分辨X射线衍射和原子力显微镜分析方法,研究发现蓝宝石衬底上外延生长的AlN薄膜晶体质量与高温AlN形核层的形核密度及晶粒大小密切相关,而形核密度决定于高温AlN形核层的初始铝体积流量,晶粒的大小取决于其厚度。优化了高温AlN形核层的初始铝体积流量和厚度等工艺参数。当高温AlN形核层的初始铝体积流量为30 cm3/min、生长时间为9 min时,高温AlN形核层的形核密度和晶粒大小最优,外延生长的AlN薄膜位错密度最低,表面最平整,晶体质量最好。     

坩埚位置对PVT生长AlN晶体过程中物质传输的影响

使用FEMAG晶体生长模拟仿真软件以及自主开发的PVT法有限元传质模块对全自动、双电阻加热物理气相沉积炉开展了AlN晶体生长工艺过程中不同坩埚埚位对温度场、过饱和度场及烧结体升华速率等影响的模拟仿真分析研究。模拟仿真结果表明:在给定工艺条件下,坩埚埚位较低时烧结体温度较高且内部温差较小,烧结体升华表面存在较大的Al蒸气分压梯度,各表面升华速率较快且均匀,籽晶衬底生长前沿温度场呈微凸分布,有利于晶体扩径及生长高质量晶体。随着坩埚埚位的上升,低温区向坩埚壁扩展,预烧结体内轴向及径向温度梯度增加,籽晶衬底附近径向温度梯度逐步降低,过饱和度区域扩大且增强。在坩埚埚位较高情况下,坩埚内原料升华变得不均匀,坩埚侧壁存在高过饱和区域,极易在坩埚壁上发生大量的AlN多晶沉积。模拟分析结果与大量实际晶体生长实验后的坩埚壁处沉积现象及剩余烧结体原料形态相符,较好地验证了模拟仿真分析结果的准确性。     

物理气相法制备AlN晶体

研究了物理气相法制备AlN晶体的过程中生长条件的改变对晶体生长的影响.实验中,采用带石墨环的坩埚组件可以避免高温下钨坩埚体和盖的粘结问题.随着生长温度的升高,AlN晶体的形态从晶须过渡到棱形晶粒.温度高于1950℃时,才能制备出颗粒状.AlN晶体.同时,研究了过饱和压对晶体生长的影响.目前,已经制备出直径为1mm的高质量的六棱柱形的.AlN单晶,最大的单晶体的直径达2mm.     

物理气相法制备AlN晶体

研究了物理气相法制备AlN晶体的过程中生长条件的改变对晶体生长的影响.实验中,采用带石墨环的坩埚组件可以避免高温下钨坩埚体和盖的粘结问题.随着生长温度的升高,AlN晶体的形态从晶须过渡到棱形晶粒.温度高于1950℃时,才能制备出颗粒状.AlN晶体.同时,研究了过饱和压对晶体生长的影响.目前,已经制备出直径为1mm的高质量的六棱柱形的.AlN单晶,最大的单晶体的直径达2mm.     

SiC籽晶上生长AlN单晶的断裂特性研究

通过扫描电镜(SEM)观察了SiC籽晶上生长AlN单晶的断裂面形貌。模拟了SiC籽晶与AlN晶体之间的应力分布。通过计算不同晶面的面间距,确定了六方晶系的AlN晶体中m面为解理面。拉曼光谱仪对不同晶面的特性进行了表征。结果表明,断裂面为m面,即裂纹扩展并沿m面解理形成断裂面。切割面为c面,AlN沿垂直于c方向生长。拉曼光谱中波数为656.2 cm-1的（E2(high)声子模为AlN单晶中的特征拉曼峰） 声子模式的半高宽为6.5 cm-1,晶体质量高。残余的张应力是裂纹产生的主要原因。     

无籽晶Pb_(1-x)Sn_xTe大单晶生长的研究

用升华法在密封安瓿的石英表面长成了Pb_(1-x)Sn_xTe(x～0.20)大单晶。利用初始次临界过冷,使单晶籽晶在原位置上接近平衡的条件下成核,从而可以快速长成优质单晶。未经处理装料中的游离成分对缺陷浓度,即:。夹裹物、孔洞、位错和低角晶界影响很大。退火装料中的过量Te(δ～0.01克分子％)对由汽-固机理成核是必要的,在适当的热条件下就能生成优质单晶。这种晶体的表观生长速率在所研究的整个过冷范围内(O≤△T≤25℃)与△T呈线性关系,且装料偏离化学配比对它影响很大。发现生长取向对总的生长速率影响不明显。本文还对晶体特性和晶体生长中可能存在的驱动力作了定性讨论。     

液封Czochralski技术生长的InP单晶中位错产生和传播的X射线形貌观察

用x射线衍射形貌研究了液封直拉(LEC)技术在[111]方向生长的InP单晶中位错的产生和传播。首先,确定了由籽晶向生长晶体传播的位错的类型,并描述了采用缩颈过程的影响。柏格斯矢量的确定表明,位错是固着型的,柏格斯矢量平行于<(?)>方向,沿<(?)>方向传播。其次描述了晶体生长期间集结于晶体表面的位错传播。观察了位错的滑动传播,滑动是在三个向下倾斜的{111}滑移面上,它与[(?)]生长方向倾斜。对LEC生长晶体中高位错密度的有关机理进行了讨论。     

大尺寸锑化铟晶体生长等径技术研究

为了获得高质量的晶体,需要解决大尺寸锑化铟晶体生长过程中的精确等径控制问题.阐述了采用提拉法生长晶体时的直径控制原理及方法,分析了影响等径控制的温度与时滞因素,并采用计算机辅助控制方法解决了大尺寸锑化铟晶体生长过程中的精确等径控制问题.生长出的3in锑化铟晶体的生长条纹不明显,位错密度小于10个/cm2.     

HVPE法生长AlN薄膜材料

利用自制立式HVPE设备,在蓝宝石衬底上进行了不同载气情况下AlN的生长试验,生长温度1 000℃。在采用H2作载气情况下,由于预反应严重,没能生长出AlN薄膜,只得到一些白色AlN粉末;而在分别采用Ar和N2作载气的情况下,则成功生长出AlN薄膜,但由于生长温度低,AlN生长均为岛状生长模式。在生长速率较快时,AlN薄膜是以〈0001〉AlN为主的AlN多晶;而在较低生长速率下,得到的AlN薄膜由为〈0001〉取向的AlN岛组成。试验还发现:用Ar作载气更有利于AlN晶核的横向生长,用N2作载气则有相对高得多的AlN成核密度。     

溅射AlN技术对GaN基LED性能的影响

研究了在图形蓝宝石衬底(PSS)上利用磁控溅射制备AlN薄膜的相关技术,随后通过采用金属有机化学气相沉积(MOCVD)在相关AlN薄膜上生了长GaN基LED.通过一系列对比实验,分析了AlN薄膜的制备条件对GaN外延层晶体质量的影响,研究了AlN薄膜溅射前N2预处理功率和溅射后热处理温度对GaN基LED性能的作用机制.实验结果表明:AlN薄膜厚度的增加,导致GaN缓冲层成核密度逐渐升高和GaN外延膜螺位错密度降低刃位错密度升高;N2处理功率的提升会加剧衬底表面晶格损伤,在GaN外延膜引入更多的螺位错;AlN热处理温度的升高粗化了表面并提高了GaN成核密度,使得GaN外延膜螺位错密度降低刃位错密度升高;而这些GaN外延膜位错密度的变化又进一步影响到LED的光电特性.     

Faster Growth of 6H-SiC Single Crystals by a Physical Vapor Transport Technique with Two Crucibles

For fast growth of 6H-SiC single crystals, a physical vapor transport (PVT) technique with two crucibles is proposed herein. By providing the growth chamber with a small continuous flux of Si vapor, the growth rate is enhanced by three times over the conventional PVT technique. The utilization ratio of the raw material is also improved. Energy dispersive analysis of X-rays (EDAX) shows that the Si content of the grown crystal is the same as that of the seed crystal. Scanning electron microscopy (SEM) indicates that, compared with conventional techniques, fewer micropipes are created in crystals grown by the technique using two crucibles.     

The Effect of AlN Nucleation Temperature on the Growth of AlN Films via Metalorganic Chemical Vapor Deposition

AlN epilayers were grown directly on sapphire (0001) substrates using a combined growth scheme, consisting of a low-temperature nucleation layer and a second layer grown by high-temperature pulsed atomic layer epitaxy via metalorganic chemical vapor deposition. With an emphasis on the nucleation layer, its growth temperature was varied from 470°C to 870°C, and obvious differences in the surface morphology, crystal quality, and strain states of the overall AlN epilayers were observed. Based on atomic force microscopy, x-ray diffraction, and Raman spectroscopy results, these differences are ascribed to the nucleation sites and the subsequent grain size. Due to the enhanced mobility of Al adatoms with increasing temperature, the nucleation sites decrease and the subsequent grain size increases, leading to the achievement of atomically flat AlN epilayers with good crystal quality for the nucleation layer grown at 570°C. However, at higher nucleation layer growth temperature, the properties of the AlN epilayers deteriorate due to the possible appearance of misaligned AlN grains. A model is also developed according to all observations.     

用VGF法生长6英寸锗单晶中籽晶熔接工艺研究

采用垂直梯度凝固(VGF)法生长单晶时,其温度梯度较低,生长速率较小,目前已成为生长大直径、低位错密度晶体的主流技术之一.在VGF法生长单晶的过程中,籽晶的熔接工艺直接影响着单晶生长的成败.研究了拉速器速度、保温时间及石英棉用量对6英寸(1英寸=2.54 cm)锗单晶VGF生长中籽晶熔接的影响,并确定了最佳的籽晶熔接工艺.研究结果发现,当拉速器速度为3～4 mm/h、保温时间为75～100 min、石英棉用量为15～20 9时,实现了对籽晶熔接工艺的精准控制,熔接长度为12～22 mm,位错密度小于500 cm-2,有效地降低了生产成本,提高了生产效率和单晶率.     

Fast vapor growth of cadmium telluride single crystals

Cadmium telluride single crystals were grown at growth rates of 35 mm per day by the physical vapor transport (PVT) method under high temperature gradient conditions. This is believed to be the highest PVT growth rate of CdTe reported to date. Lamellar twins are the only ones present in the CdTe crystals grown under optimal conditions in this work. At growth rates up to 15 mm per day, the crystals have a dislocation density of ∼10⁴ cm⁻². The etch pit density increases to ∼10⁵ cm⁻² with an increase of the growth rate up to 35 mm per day. Based on a uniform thermal field and high interface stability, which are established by large temperature gradients up to 40°C/cm at the growth interface, spurious nucleation and lateral twins were effectively eliminated, and the density of the lamellar twins remained low at crystal growth rates up to 35 mm per day. The major contributions of the high temperature gradients to the single crystalline growth and the apparent origin of polycrystalline grains are also discussed in this paper.     

Seeded growth of AlN crystals on nonpolar seeds via physical vapor transport

Seeded growth of AlN single crystals was demonstrated in an induction-heated, high-temperature reactor via a physical vapor transport (PVT) process. AlN seeds were prepared from a self-seeded boule containing large single-crystalline grains. Seeded growth was interrupted several times in order to refill the AlN powder source, and a dedicated process scheme was used to ensure epitaxial growth on the seed surface, after prior exposure to air. The growth temperatures were in the range of 2200–2300°C, and the reactor pressure was in the range of 500–900 torr of UHP-grade nitrogen during each growth run. Under these growth conditions, a seed (10 mm diameter) expanded at an angle of 45°, and a larger single crystal up to 18 mm in diameter was obtained. The as-grown surface had three facets, of which facet (1120) was smooth and featureless while the other two, (4150) and (2570), showed serrated morphologies. The double-crystal x-ray rocking curve and glow discharge mass spectroscopy analysis confirmed that the grown crystal was of high crystalline quality with low impurity incorporation.     

Morphology and crystalline property of an AIN single crystal grown on AIN seed

AIN single crystal grown by physical vapor transport (PVT) using homogeneous seed is considered as the most promising approach to obtain high-quality AIN boule.In this work,the morphology of AIN single crystals grown under different modes (3D islands and single spiral center) were investigated.It is proved that,within an optimized thermal distribution chamber system,the surface temperature of AIN seed plays an important role in crystal growth,revealing a direct relationship between growth mode and growth condition.Notably,a high-quality AIN crystal,with (002) and (102) reflection peaks of 65 and 36 arcsec at full width at half maximum (FWHM),was obtained grown under a single spiral center mode.And on which,a high-quality AlxGa1-xN epitaxial layer with high Al content (x =0.54) was also obtained.The FWHMs of (002) and (102) reflection of AlxGa1-xN were 202 and 496 arcsec,respectively,which shows superiority over their counterpart grown on SiC or a sapphire substrate.     

Growth and crystal quality of inp crystals by the liquid encapsulated czochralski technique

The growth of InP single crystals by the liquid encapsulated Czochralski (LEC) technique has been studied from the standpoint of improving crystal quality. Twin-free crystals have been grown reproducibly in the <lll>P direction under the following conditions; (1) using starting material which does not contain fine InP particles, (2) controlling the cone shape of the crystals such that the angle with the growth axis is less than 19.68°, (3) arranging the.hot zone to produce a temperature at the top surface of the B₂O₃ encapsulant layer below 550°C. It has been confirmed that electrical properties of nominally undoped crystals are dominated by the impurity, Si, and the concentration of Si in an LEC crystal corresponds to that of the starting material. The dislocation densities of undoped LEC InP crystals depend on thermal stresses during the growth process. This knowledge has led to the growth of dislocation-free crystals.     

基于AlN和GaN形核层的AlGaN/GaN HEMT外延材料和器件对比

使用金属有机物化学气相淀积(MOCVD)方法在蓝宝石衬底上分别采用AlN和GaN作为形核层生长了AlGaN/GaN高电子迁移率晶体管(HEMT)外延材料,并进行了器件制备和性能分析.通过原子力显微镜(AFM)、高分辨率X射线双晶衍射仪(HR-XRD)和二次离子质谱仪(SIMS)等仪器对两种样品进行了对比分析,结果表明采用AlN形核层的GaN外延材料具有更低的位错密度,且缓冲层中氧元素的拖尾现象得到有效地抑制.器件直流特性显示,与基于GaN形核层的器件相比,基于AlN形核层的器件泄漏电流低3个数量级.脉冲Ⅰ-Ⅴ测试发现基于GaN形核层的HEMT器件受缓冲层陷阱影响较大,而基于AlN形核层的HEMT器件缓冲层陷阱作用不明显.