泡生法蓝宝石单晶不同生长阶段的数值模拟研究

针对泡生法蓝宝石单晶生长的不同生长阶段的温场、流场和固液界面形状进行数值模拟研究.并分析了加热器相对坩埚的轴向位置和不同生长速率对蓝宝石单晶生长的影响.结果表明:在蓝宝石单晶生长中,在靠近坩埚壁面和固液界面的熔体内,等温线密,温度梯度较大;在靠近坩埚底部的熔体内,等温线稀疏,温度梯度较小.随着晶体高度的增加,熔体对流由放肩阶段的两个涡胞变成等径阶段的一个涡胞,熔体平均温度有小幅度下降;加热器相对坩埚的轴向位置对晶体生长炉内温场和固液界面形状影响很大,随着加热器位置上移,晶体内平均温度升高,温度梯度减小;熔体内平均温度降低,温度梯度增大.同时固液界面凸度增大.随着晶体生长速率增大,固液界面凸度增大,界面更加凸向熔体.     

PVT法生长大直径6H-SiC晶体感应加热对系统的影响

采用有限元分析法系统地研究了大尺寸6H-SiC晶体PVT法生长装置中感应加热线圈的不同高度和匝间距对生长腔、粉源以及晶体生长温度场的影响;分析比较了线圈不同高度和匝间距时晶体生长面径向温度梯度的变化.结果表明:在中频电源的输出功率和频率固定,盲孔内径不变的情况下,通过调整线圈匝间距和高度可以减小晶体生长面径向温度梯度,改善晶体的质量,同时又有较高的生长速率.     

半导体单晶生长过程中的位错研究

阐述了现有的半导体单晶位错模型,即临界切应力模型和粘塑性模型的基本理论及应用状况.分析了熔体法单晶生长过程中影响位错产生、增殖的各种因素,以及抑制位错增殖的措施.与熔体不润湿、与晶体热膨胀系数相近的坩埚材料,低位错密度的籽晶可有效地抑制生长晶体的位错密度;固液界面的形状及晶体内的温度梯度是降低位错密度的关键控制因素,而两因素又受到炉膛温度梯度、长晶速率、气体和熔体对流等晶体生长工艺参数的影响.最后,对熔体单晶生长过程的位错研究进行了展望.     

碲锌镉垂直布里奇曼法晶体生长过程固液界面的演化

计算模拟了半导体材料碲锌镉垂直布里奇曼法单晶体生长过程,以等温线图展示了固液界面形状的演化,分析了温度梯度和坩埚移动速率对固液界面形状以及晶体内组分偏析的影响.计算结果表明在凝固的初始段,固液界面的凹陷深度较大,随后有较大幅度的减小.整个凝固过程中固液界面的凹陷深度值有一定的波动性.提高温度梯度、降低坩埚移动速率均能有效地减小固液界面的凹陷,改善晶体的径向组分偏析.     

CaF2晶体的生长与光学性能

采用导向温度梯度法(TGT)生长CaF2晶体,建立了生长炉内的垂直温度梯度场.研究表明影响晶体质量及光学性能的主要因素包括坩埚材料、温度场、生长程序及原料纯度等.从大量的实验中总结出TGT法生长高质量CaF2晶体的生长条件如下:石墨坩埚;轴向梯度≤2℃/mm;生长降温速率1.5～2.5℃/h;冷却速率≤40℃/h.     

蓝宝石单晶生长坩埚热应力分析

针对蓝宝石单晶生长过程中因热应力集中坩埚使用寿命短问题,基于ANSYS有限元分析,对晶体熔化过程中的坩埚进行瞬态传热分析,在此基础上进行不同情况下热-结构耦合分析,计算得出晶体完全熔化后坩埚的热应力分布情况.分析显示:最大热应力存在于坩埚与托盘结合处;在满足晶体生长条件下,减缓升温速度,减小温度梯度,增大托杆中间空隙,改变托盘托杆材料等方法可以减小热应力.     

PVT法SiC单晶生长传热分析

研究了PVT法生长SiC过程中的传热行为,以优化生长条件、获得高质量单晶.该研究是针对坩埚盖(籽晶粘附于坩埚盖上)和炉盖之间的传热行为进行的.研究认为,坩埚盖上部石墨毡开孔形状和大小对坩埚盖的径向温度场有很大影响.采用本文简化的模型可以估算坩埚在不同位置下、不同的石墨毡开孔形状和大小时坩埚盖和炉盖之间总的辐射热阻和传热量.对影响坩埚盖和炉盖之间传热的因素进行了讨论.另外,讨论了在生长过程中动态调整坩埚盖散热条件的可行性.     

高质量半绝缘Φ150mm 4H-SiC单晶生长研究

采用数值模拟研究PVT法Φ150 mm 4H-SiC单晶生长的功率、频率选择、坩埚位置及保温厚度等关键生长参数.研究表明Φ150 mm 4H-SiC单晶生长功率是2inch 4H-SiC生长功率的2倍,优化的加热频率在5 kHz以下,系统分析不同生长参数下生长腔内径向及轴向温度梯度的变化规律.在此基础上初步的进行了Φ150 mm 4H-SiC单晶的生长工作,获得了无裂纹、直径完整的高质量SiC衬底材料.拉曼光谱Mapping测量显示Φ150 mm SiC衬底全片无多型,均为4H-SiC晶型.X光摇摆曲线显示半宽小于30 arcsec.采用掺杂过渡金属V杂质,获得了电阻率超过5×109 Ω·cm的150mmSiC衬底.     

SiC晶体的PVT生长系统及测温盲孔对热场的影响

实验中研究了不同结构参数的测温盲孔对晶体生长面热场的影响,结果分析表明:径向温度梯度和轴向温度梯度与测温盲孔的深度和半径近似成正比关系,但测温盲孔尺寸变化对径向温度梯度和轴向温度梯度的影响效果不同;改变测温盲孔尺寸适于调节径向温度梯度;测温盲孔半径和深度的增加均可导致坩埚盖上SiC多晶生长速率提高.     

高品质6英寸N型4 H-SiC单晶生长研究

PVT法生长SiC单晶生长腔的温场分布是影响晶体质量的重要因素.采用数值模拟研究了保温层和坩埚结构以及线圈位置对6英寸SiC晶体生长温场的影响,优化出了适合高品质6英寸SiC晶体生长温场分布,在此条件下生长无裂纹的6英寸N型4H-SiC晶体.用高分辨率X射线衍射、拉曼光谱和缺陷检测系统对所加工的SiC衬底片的质量进行了表征.测试结果表明,晶型为单一的4H-SiC,微管密度小于1 cm-2,电阻率范围为0.02～0.022Ω·cm,X射线摇摆曲线半高宽为21.6″.     

高温下锂离子在低掺镁铌酸锂晶体中的扩散

研究了高温富锂气氛下锂离子在低掺镁铌酸锂晶体中的扩散.采用气相输运平衡法制备了掺杂1mol; MgO的不同锂含量的铌酸锂(Mg1LN)晶体,采用热分析仪测试了晶体的居里温度.制备了一系列不同锂含量的Mg1LN多晶料,拟合了晶体锂含量与居里温度的关系.采用Boltzmann-Matano法求解了扩散方程.结果表明,扩散温度为1100 ℃时,Mg1LN晶体中锂离子扩散系数为3.2×10-9~13.0×10-9 cm2/s,当扩散温度为1145 ℃时锂离子扩散系数约是1100 ℃时扩散系数的三倍.因此,适当提高扩散温度是提高气相输运平衡法制备近化学计量比低掺镁铌酸锂晶体效率的有效办法.     

Controlling the axial temperature gradient in inductively heated Czochralski systems

A heating system is described that allows to increase the temperature gradients in rf‐heated Czochralski setups during the growth. This system applies an active afterheater, operated by a separate induction coil parallel to that heating the crucible. By changing the inductivity of an additional coil located outside the growth chamber, the ratio of the rf currents flowing through the crucible and afterheater and, consequently, the geometry of the heat input to the setup can be altered. The efficiency of the heating systems has been demonstrated in various experiments.     

预烧温度对La0.67Ca0.33MnO3陶瓷结构及电学性能的影响

采用溶胶-凝胶法成功制备了La0.67Ca0.33MnO3粉末,并通过改变预烧温度获取电学性能优异的陶瓷.利用X射线衍射(XRD)、扫描电子显微镜(SEM)、四探针法对不同预烧温度处理后的La0.67Ca0.33MnO3陶瓷的物相、结构、微观形貌和电学性能进行测试,分析预烧温度对材料的晶粒尺寸和电学性能的影响,从而摸索出最佳预烧温度.实验结果表明:样品的结晶性能好物相纯,随着预烧温度的增加,晶粒尺寸、致密度、收缩率和电阻温度系数(TCR)在不断减小,电阻率先减小后增加.在300℃预烧,1450℃烧结得到的样品具有较高的TCR值达到了40.8;·K-1.     

催化剂焙烧温度和乙炔焰温度对火焰法催化裂解乙烯制备碳纳米管的影响

研究了600℃/700℃/800 ℃/900℃/1000℃五组催化剂焙烧温度和980℃/1050℃/1100℃三组乙炔火焰温度变化对火焰法催化裂解乙烯制备碳纳米管的影响.发现不同的催化剂焙烧温度和乙炔焰温度对合成产物影响突出,两者均存在致使产量最大的温度工况,但在产物准直度和管径均匀度等方面有些工况的表现较佳.     

金刚石微粉低温化学镀镍品质影响因素

研究络合剂、镀液pH值、温度对金刚石微粉低温化学镀镍品质的影响。在温度为35 ℃、pH值为5时,通过改变络合剂配比,对镀液稳定性,镀层沉积速率、形貌和磷(P)含量进行测试分析。结果表明,20 g/L的柠檬酸+5 g/L的琥珀酸为本文最优的络合剂配比,其化学镀液稳定性好、沉积速率较快(0.391 5 g/h),镀层致密无漏镀,P含量为11.73%(质量分数)。用最优络合剂,通过改变镀液pH值、温度,对化学镀样品的镀层沉积速率、形貌、P含量进行测试分析。结果表明,镀液温度为35 ℃,pH值为3～13时,随着pH值增大,沉积速率逐渐增大,P含量逐渐减小。但pH值高于11时,反应速率过快,不易稳定镀液pH值,且镀液易分解,因此pH值在5～11较为合适。在镀液pH值为5,温度为30～50 ℃时,随着温度升高,沉积速率和P含量都随之增高,镀层致密无漏镀。但温度高于45 ℃时,反应速率过快,不易稳定镀液pH值,因此温度在35～45 ℃较为合适。     

Synthesis and crystal structure of 1-vinyl-cis-2,3-diphenylaziridine

1-Vinyl-cis-2,3-diphenylaziridine, C₁₆H₁₅N, has been synthesized and characterized by spectroscopic methods and single crystal X-ray analysis. The structure was studied at room temperature (2a) (18°C) and at low temperature (2b) (–70°C). The title compound crystallizes in the space group Cm with Z=2 showing no phase transformation between the two temperatures. The cell parameters area=8.258(3),b=15.880(3),c=5.827(2)Å, =122.32(2)° for (2a) anda=8.188(2),b=15.762(3),c=5.724(1)Å, =121.57(2)° for (2b). Both the studies show nearly the same conformation. With the exception of the vinyl group, the molecule hasm symmetry, so, the asymmetric unit is half a molecule. The mirror plane of the space group cuts the aziridine ring through the N atom. The vinyl group is distributed on two symmetrical positions by means of the same mirror plane. In this way, the crystal is built with the two diastereoisomers of the title compound.     

X-ray structures of fifty year old crystals of cholesterol iodide forms I and II

  The molecular framework of steroids was firmly established from the successful X-ray analysis of cholesteryl iodide crystals over fifty years ago. At the time, this was a triumph for the rapidly developing technique of X-ray crystallography. We describe here new analyses of cholesteryl iodide using crystals of forms I and II^(A) which are at least 50 years old. Comparison of these two structures reveals subtle differences in the geometry of the steroid skeleton, the attached side chain and the covalently bound iodine. The crystals of both forms occur in the same monoclinic space group, P2₁, with similar but nevertheless different unit cells, particularly in the b-axis length. As a consequence, there are subtle differences in the packing mechanisms of the two polymorphs. The two forms were originally classified by Bernal and Crowfoot, on the basis of their studies of more than 60 crystals of sterols and sterol derivatives, as “normal, type A - the common form” (corresponding to form II) and “reverse or type B” (corresponding to form I), respectively. Those crystals of form I which have survived for almost 55 years are poor X-ray diffractors at room temperature and have been analysed at liquid N temperature, diffracting well under these conditions. Form II crystals diffract well at room temperature and for this reason the crystals were not cooled. The main differences in geometry occur in the side-chain which is disordered in the room temperature form II crystals, whilst the individual ring conformations in the steroid skeleton are similar, ring A being a strained chair, ring B a 7α/8β half-chair, ring C a symmetrical chair and D a 13β/14α half-chair. (A) Originally denoted Forms B and A respectively. See Additional Note (A) for explanation.

MgAl2O4:Cr3+单晶光纤生长与荧光温度特性研究

采用激光加热基座法制备了0.5at;Cr3+掺杂镁铝尖晶石单晶光纤.通过XRD、荧光光谱、荧光寿命测试对所制备的单晶光纤的晶相、荧光温度特性进行了实验研究,结果表明所制备的MgAl2O4:Cr3+单晶光纤的主晶相为MgAl2O4晶相,镁铝尖晶石晶相结构并没有因Cr3+掺入而发生改变,在405nmLED激发下,随着温度升高MgAl2O4:Cr3+单晶光纤荧光强度下降,尤其是2E→4A2能级跃迁产生的荧光强度下降明显,同时随着温度的升高,MgAl2O4:Cr3+单晶光纤的荧光寿命随温度单调下降,系统荧光寿命从室温293K的7.74ms下降到723K的0.5ms左右.由于其相对较长的荧光寿命,MgAl2O4:Cr3+单晶光纤非常适合作为荧光温度敏感材料应用于荧光寿命型光纤温度传感器.     

High-temperature X-ray analysis of phase evolution in Sr-doped zinc-silicate glasses

Bone grafts are required in many clinical situations. Autografts are the traditional gold standard for treating conditions requiring bone grafts. However autografts have inherent drawbacks such as donor site morbidity, pain and increased operative time. An alternative for autografts are synthetic grafts. A series of strontium doped zinc silicate glasses were developed which were investigated using high temperature X-ray diffraction (HT-XRD) in order to establish phase transformations, which occur up to the first crystallization temperature, (T_p1), thus identifying the composition-structure relationships which arise during this thermal processing. In analysing BT110 it was observed that all glass material crystallised into 4 phases including strontium zinc silicate, sodium calcium silicate, calcium silicate and strontium silicate, leaving no residual glass phase. BT111 and BT112 were shown to contain a residual glassy phase alongside for BT111, sodium zinc silicate, larnite and silicon oxide and for BT112 strontium silicate, calcium silicate, sodium silicate and silicon oxide. In the case of BT111 the residual glass phase appears to be rich in strontium. The residual glass phase being Sr enriched with respect to the glass-ceramic may offer increased release of Sr²⁺ from the material; important for the regulation of osteoblastic and osteoclastic activity. BT113 crystallized to form strontium silicate, sodium silicate, and strontium zinc silicate. BT114 crystallized to form strontium silicate and sodium silicate. The biocompatibility of phases formed in BT113 and BT114 is as yet unknown. Further knowledge will be generated by later work examining the biocompatibility of these phases identified in this research. However, on the basis of these results, the materials (BT110-BT112) exhibit potential as a bone graft substitutes, whilst BT113-BT114 give rise to phases with unknown biocompatibility and so warrant further investigation.