添质铝金红石(TiO2)单晶体焰熔法生长实验及机理

使用添加适量(原子分数为0 4%)Al2O3的金红石粉料,采用焰熔法成功地生长了尺寸为20mm×30mm的透明金红石单晶体,而采用相同工艺使用纯金红石粉料生长的晶体却是蓝黑色不透明的·添质铝在晶体生长过程中有如下作用:Al3 在晶体中取代Ti4 的位置,减少了氧的配位数,因而减少了晶体形成时对氧的需求,从而减少了由于Ti4 还原而形成的Ti3 和非本征氧空位的数量;由于Al3 半径小于Ti4 ,因此增加了正离子间距,使氧离子更易于迁移;形成添质后晶体的本征(固有)缺陷对Al′Ti V¨O,提供氧离子扩散通路·因此适量Al2O3的添加从宏观上增加了氧离子在晶体中的扩散速度,避免了大量色心的形成,从而在生长过程中可直接获得透明的金红石单晶体·     

金红石单晶体制备方法发展现状

金红石单晶体拥有较高的双折射率,在可见-红外波段透过性良好,因此,作为特殊介电材料、红外窗口材料、制作光隔离器的材料等,被广泛地应用于现代光学通讯领域。然而,高品质金红石单晶体的生长技术仍然是国际上的难题,相关基础研究理论匮乏。人们尝试过多种方法生长金红石单晶体,但目前比较成功的只有光浮区法和焰熔法。分析了光浮区法和焰熔法的优势和不足。由于焰熔法可制备较大尺寸的晶体,且焰熔法生长设备的技术进步,使其晶体质量得到提高,因此,作为商品应用的金红石晶体主要还是焰熔法制备。指出了使用数字精密控制技术、基于传热学和流体力学设计的焰熔法晶体生长技术是金红石单晶体制备的重要发展方向。     

碲锌镉晶体的In、Cd双源气氛退火研究

采用改进的垂直Bridgman法生长出尺寸为Φ20 mm×40 mm、外观完整无裂纹的Cd0.9Zn0.1Te(CZT)单晶体.沿晶体解理面切割晶片,在In、Cd气氛下进行退火热处理,经973K退火140 h后,采用能量色散谱仪(EDS)、ZC36型高阻仪和傅里叶红外分光光度计等研究了退火对晶片的成分、电学、光学性能的...     

高注量中子辐照金红石单晶电学特性的研究

金红石单晶体经中子辐照后，不仅由无色透明变为深兰色，而且导电特性发生很大变化，且由高绝缘材料变为n型半导体，作者分别在低温、室温及高温下，研究了样品电阻随温度的变化关系，并在空气和真空气氛下，对比研究了气氛对辐照后样品导电特性的影响。结果表明，金红石晶体经中子辐照后，在低温下具有典型的半导体导电特性；在高温下于空气中退火，样品会被逐渐氧化，最后变为无色的绝缘体；在10^-4Pa高真空气氛中退火，样品表现出点缺陷导电行为，且缺陷离子具有两个不同的激发能级（0.06eV和0.12eV)，分别对应子H^ 和Ti^3 ，且在整个过程中没有发现样品被氧化。     

直拉法LiNbO_3单晶体的小面生长

用直拉法生长了不同取向的LiNbO_3单晶体,通过对这些晶体的外部形态和不同截面的浸蚀图象的观测,获得不同方向提拉晶体的小面形貌。采用三种方法确定了LiNbO_3晶体小面面指数,它们是(10·2)、(11·2)和(01·2)及它们的反演面(10·2)、(11·2)和(01·2)。并测定了小面尺寸与界面曲率半径的关系和出现小面的临界曲率半径,其结果与理论预期相符。     

注入电压对Ti6A14V合金离子注氧层结构的影响

采用等离子体基氧离子注入技术对Ti6A14V合金进行表面处理。注入电压选取-30和-50kV。注入层的结构用X射线光电子能谱、小掠射角X射线衍射、Raman光谱进行表征。注入样品在注氧层中均形成了以TiO_2为主的键结构,-30kV低电压注入样品的注氧层中TiO_2为非晶态,经过500℃真空退火后,TiO_2结晶形成金红石。而-50kV高注入电压则可在注氧层中直接形成粒径为nm的金红石。     

微纳米三水碳酸镁晶须的制备及性能

以菱镁矿为原料,无水乙醇为添加剂,采用低温水溶液法,制备平均直径为500 nm、部分直径为55 nm、最大长径比为40、均匀棒状的MgCO3·3H2O晶须。采用SEM,XRD,TGA和FTIR对其形貌、物相和质量进行表征。探讨热解温度、添加剂种类对晶体形貌和质量的影响,系统分析MgCO3·3H2O晶体的形成机理。结果表明:最佳热解温度为50℃、有效添加剂为无水乙醇。MgCO3·3H2O晶体在结晶过程中,镁-氧八面体以共顶点的形式连接沿[010]晶向快速生长,形成一维棒状单晶体。MgCO3·3H2O晶体的生长符合液-固机理。MgCO3·3H2O晶体中存在结晶水和结构水,比例为2:1,其结构式为Mg(HCO3)(OH)·2H2O。     

铸造多晶硅生长过程中氧的传递过程研究

定向凝固法生长铸造多晶硅系统中,氧的平衡涉及到三个界面,它们是坩埚与熔体界面、熔体与气相界面以及晶体与熔体界面。因此氧的传递包含可能的三个过程:(1)氧从坩埚中向硅熔体中进行扩散;(2)氧的分凝导致氧从熔体中进入凝固的晶体中;(3)氧在熔体表面以SiO的形式挥发。     

水热法培育刚玉单晶体

焰融存积法(Verneuil法)合成刚玉的技术已经相当成熟;然而用此法生长的晶体往往具有内应力大和镶嵌度高等缺点。与焰融法相比,在水热条件下,晶体是处于较低的温度和很小的温度梯度的情况下缓慢地生长的,因此在高温高压的水溶液中有可能培育出完整度较高的刚玉单晶体。近年来国外一些实验室相继开展了水热法合成刚玉晶体的研究。但一般来说,这方面的工作目前尚属初始阶段。     

热处理参数对异步轧制硅钢极薄带三次再结晶的影响

采用常规和异步轧制分别将0 3mm厚的成品取向硅钢板冷轧到0 10mm以下,然后在不同气氛的热处理炉中进行三次再结晶高温退火,研究同步、异步轧制条件下,热处理工艺参数(退火温度、保温时间、退火气氛、升温速度)对取向硅钢极薄带的磁性能和三次再结晶行为的影响·结果表明,相同的工艺参数下,真空退火的硅钢极薄带的磁性能优于氢气处理的;退火温度越高,保温时间越长,升温速度越快,磁性能越好,三次再结晶发展得越完善·     

Role of β(FeAl) nanoparticles in abnormal grain growth in the annealing of cast Cu-Al-Mn-Fe shape memory alloys

In this study, the low-cost production of Cu-Al-Mn-Fe shape memory alloy single crystals exceeding 46 mm by abnormal grain growth was realized only through annealing their cast alloys. The results show that the misorientation formed during annealing may be responsible for such abnormal grain growth process. It was confirmed that this misorientation resulted from the dissolution of bcc β(FeAl) nanoparticles during heat treatment at a sufficiently temperature of approximately 1173 K. The rate of migration of the abnormal grain boundary was experimentally measured to be approximately 9.3 × 10^-5 m s^-1 within 2 min of the commencement of abnormal grain growth. Additionally, the range of composition of the alloys that can lead to abnormal grain growth was determined. When the Cu-13.0Al-6.5Mn-3.2Fe single crystal close to the [100] direction was deformed to a pre-strain of 12%, full shape recovery happened without any residual strain. At that time, the superelastic strain was approximately 9%. Such a superelastic characteristic remained nearly constant over 50 cycles, showing excellent fatigue resistance. The superelastic properties of the present Cu-13.0Al-6.5Mn-3.2Fe single crystal are compared to those of commercial Ni-Ti-based shape memory alloys. Therefore, it can be considered as a new kind of superelastic material having practical applications. The obtained results should be of great significance in the development of Cu-based shape memory alloys. Furthermore, it is expected that a similar microstructure can be designed for the production of more metallic single crystals.     

重掺Sb硅单晶中氧沉淀的研究

本文用化学腐蚀和透射电镜及其能谱分析研究了重掺Sb硅单晶中的氧沉淀。化学腐蚀结果表明,Sb的掺入有促进形核的作用,但其最大成核速率仍在750℃左右。随着退火时间的延长,沉淀密度首先增加,而后又下降。透射电镜观察到氧沉淀呈平行四边形平板状,并发现有氧沉淀群及与沉淀相连的位错缠结,但未发现层错。对氧沉淀大小的测量结果表明,它的生长满足t~(3′4)规律。能谱分析指出,Sb元素不参与氧沉淀。为解释Sb的掺入促进形核,本文提出了空位和间隙硅原子影响氧沉淀形成的模型。按此模型,单位体积晶坯的自由能变化应为ΔG_v=-ΔH_v(O)(T_e(O)-T)/T_e(O)-ΔH_v(Si)(T-T_e(Si))/T_e(Si)假设Sb的掺入增加空位浓度,减小间隙硅原子浓度。为此,间隙硅原子的饱和温度将降低。由上式,ΔG_v将随Sb浓度的增加而为更大的负值。因此,氧沉淀形核速率将随掺Sb浓度的增加而加速。     

一种简便方法制备ZnO薄膜及其特性研究

该文介绍了一种制备ZnO薄膜的简便方法:先在真空中蒸发沉淀Zn薄膜,再在空气中进行加热退火处理,使薄膜结晶变成ZnO薄膜。薄膜的X射线衍射谱(XRD)表明使用上述方法得到的是结晶良好的ZnO薄膜,对薄膜的发光特性研究表明,薄膜的光致发光谱(PL)与薄膜的制备条件密切相关。同时还系统研究了薄膜的PL谱与退火温度、退火时间和通气与否的关系,对实验结果给出了初步的解释。     

施主态氧沉淀的微观分布

本文利用扩展电阻研究了低温退火及低-高温二步退火后P-CZ硅中新施主的微观分布。指出在新施主的氧沉淀界面模型下,通过扩展电阻法测量新施主的分布提供了确定氧的微小沉淀的一个灵敏的方法,其灵敏度取决于原始电阻率,新施主的分布可以通过讨论氧沉淀的分布,氧沉淀动力学过程以及晶体生长的液流模型得到解释。     

SnO2纳米线的制备及结构表征

以SnO₂粉末和碳粉的混合物为源,高纯氮气为载气,利用化学气相沉积法在1 000 ℃下,在溅有Au的单晶Si衬底上制备了SnO₂纳米线。用SEM、XRD测试技术对样品进行了结构、形貌的表征,利用PL技术分析了样品的发光特性。由分析可知,样品均为四方金红石结构,退火时间对样品形貌具有一定的影响,但不影响其结构。所制备的SnO₂纳米线结晶质量较高,其生长遵循VLS机制。     

Undercooling evolution of pure Sn droplets in various atmospheres based on fast scanning calorimetry

Undercooling of Sn droplets in different atmospheres was studied by fast scanning calorimetry （FSC） at cooling rate of 1,000 K/s. It is found that the undercooling decreased with increasing partial pressure of oxygen. Randomly distributed SnO2 islands were observed to form on the droplet surface, which likely has promoted the heterogeneous surface nucleation. As the partial pressure of oxygen changes, the nucleation rate and growth of SnO2 led to different oxide islands, which resulted in various potential catalytic sites for the nucleation of the molten Sn droplet. The results showed that the nucleation process of the Sn droplets was sensitive to the solidification environment, and therefore the atmosphere should be taken into account in the study of the nucleation behavior of the single Sn droplets.     

用于空间半导体区熔生长仿真系统的数学模型

本文提出一个晶体区熔生长的数学模型,可以根据炉管上十个热电偶的温度值计算出试样中的温场,再进一步计算出熔区位置、熔区宽度、生长界面的形状、生长速率和生长界面处的温度梯度等.材料科学家根据上述参数,可实时监控晶体的生长.     

Ni51Mn25．5Ga23．5单晶大的自发相变应变和磁感生应变

通过交流磁化率、电阻、有无磁场下的马氏体相变应变测量,研究了Ni51Mn25．5Ga23．5单晶的马氏体相变和磁感生应变特性。伴随马氏体相变,该单晶展现出一个应变量高达-1．62％的自发双向形状记忆效应。采用磁场下冷却的方法,在材料的马氏体相获得了一个量值高达-1．5％且可逆的磁感生应变,该值近似为零场下冷却测量得到的磁感生应变的2倍。根据单晶生长机制和NiMnGa合金形状记忆特性,对上述结果进行了讨论。     

Crystals of haemoglobin with the T quaternary structure bind oxygen noncooperatively with no Bohr effect

The relationship between the structure and function of haemoglobin has mainly been studied by comparing its X-ray crystal structures with its function in solutions. To make a direct comparison we have studied the functional properties of haemoglobin in single crystals, an approach that has been an important part of the investigation of several enzyme mechanisms. Here we report on the oxygen binding by single crystals of human haemoglobin grown in solutions of polyethylene glycol. Unlike haemoglobin crystals formed in concentrated salt solution, which crack and become disordered on oxygenation, crystals grown in polyethylene glycol remain intact. X-ray studies have shown that the T (deoxy) quaternary structure of haemoglobin in this crystal at pH 7.0 is maintained at atmospheric oxygen pressure, and that the salt-bridges are not broken. We find striking differences between oxygen binding by haemoglobin in this crystal and by haemoglobin in solution. Not only is oxygenation of the crystal noncooperative, but the oxygen affinity is independent of pH in the range 6.0-8.5, and is much lower than that of the T state in solution. The lack of cooperativity without a change in quaternary structure is predicted by the two-state allosteric model of Monod, Wyman and Changeux. The absence of a Bohr effect without breakage of salt-bridges is predicted by Perutz's stereochemical mechanism. In contrast to the X-ray result that oxygen binds only to the alpha haems, our measurements show that the alpha haems have only a slightly higher affinity than the beta haems.