在空间微重力下生长碲镉汞晶体

本文叙述了我国首次在空间微重力下进行的碲镉汞(MCT)晶体生长试验及一些观测结果。生长是从熔体进行的。在空间90min的加热时间内,将MCT多晶试样熔化,然后随炉冷却,最后在地面上再结晶。于是,生长出约3cm长的晶体,其表面光滑.结构致密,无孔洞,由1～3个大晶粒组成,其中单晶占74%。X射线能量色散分析(EDS)表明,其径向组分均匀性优于±0.02,其中约1cm长的一段晶体的径向组分均匀性优于±0.01。电学特性与地面上生长的样品基本相同。     

THE SPACE EXPERIMENT OF PROTEIN CRYSTALLIZATION ABOARD THE CHINESE SPACECRAFT SZ-3

Using a new flight hardware, a Chinese mission of space protein crystallization has been performed on the Chinese spacecraft SZ-3 for seven days from March 25 to Apr. 1, 2002. The rate of yielding crystals in the 60 samples is 75%, a little higher than the ground control experiment. Preliminary analysis of the experimental results have shown that among the 16 proteins involved in the mission, about 4 kinds of better diffraction-quality protein crystals were produced in space. At least one kind of protein crystals, i.e. crystals of cytochrome b5 mutant could diffract X ray beyond the highest resolution reported so far. In addition, some rules derived from our numerical studies of the liquid/liquid diffusion protein crystallization were proved by the crystallization of lysozyme as model protein in this space experiment,which also clearly showed the advantages and disadvantages of the gelled protein solution used in microgravity growth of protein crystals. In order to exploit this mission, more diffraction work with the grown crystals and detailed analysis of data to be obtained will be done in the next few months.     

微重力下胶原蛋白纤维化及羟基磷灰石结晶的初步研究

在长期空间飞行过程中, 骨质丢失是一个严重问题. 羟基磷灰石(HAP)晶体是骨骼的主要成分, 骨骼中的胶原蛋白纤维在HAP生长结晶过程中起到关键作用. 研究了胶原蛋白纤维化过程在模拟微重力和常重力条件下的变化, 对以胶原 蛋白纤维作为模板生长出的HAP晶体形貌进行了观察. 结果表明, 不同浓度胶原蛋白溶液中形成的胶原蛋白纤维, 其内部孔隙数量和尺寸在模拟微重力条件下要明显大于常重力条件下, 胶原蛋白纤维内部孔隙的分布也不同于常重力条 件下的结果. 以模拟微重力条件下形成的胶原蛋白纤维为模板生长出的HAP 晶体主要为立方体状, 而以常重力条件下形成的胶原蛋白纤维为模板生长出的 HAP晶体形貌主要为板状. 该结果有助于未来进一步阐明空间骨质丢失的机理.      

EFFECTS OF CONVECTIVE FLUID MOTION UPON OXIDE CRYSTAL GROWTH IN HIGH TEMPERATURE SOLUTION

For understanding of the influence of convective flow on crystal growth, space high temperature in situ observation instrument (SHITISOI) is dedicated to visualize and record the whole growth process of oxide crystals in high temperature up to 1000°C. Model experiments using transparent liquids such as KNbO3 and a mix ture of Li2B4O7+KNbO3 were chosen to investigate effects on ground and in space.On the earth, an investigation of growth kinetics of KNbO3 crystal related to two different states of convection: diffusive-advective flow and diffusive-convective flow,has been performed. The per unit length of a step e is calculated from the exper imental data for two different states of convection. Analyses of these data show the effect of buoyancy convection is to enhance the sharpness of the interface. The growth of KNbO3 crystals from solution of KNbO3+Li2B4O7 was investigated in space. The streamlines of the steady thermocapillary convection in Li2B4O7 solvent was observed. Due to thermocapillary convection, KNbO3 crystal grains grew and filled the whole solution homogeneously. Earth-based quenching experiments are de signed in order to study polyhedral instability of KNbO3 crystal, which is controlled by diffusion mechanism limitation. In all cases, when the crystal was nucleated near air/solution surface, it lost its polyhedral stability and varied from polyhedrons to dedrites. The thickness of diffusion mechanism limitation layer is about 60μm.     

Experimental study of morphological and convective instabilities: The MEPHISTO space program

It is now well established that the morphological instability, i.e. the transition during solidification from a planar L/S interface to a cellular one, is strongly influenced by convection. The most recent theories on this topic, which are very advanced, suffer from the lack of experimental tests because uncontrolled convective effects cannot be avoid on the ground. Moreover the check of all the pertinent solidification parameters are not controlled in the same time or measured in real time. After a review of the main 1g experiments and their own limitations, we describe a new apparatus (MEPHISTO) which allows :

• •in-situ measurements of the main solidification parameters and in particular the undercooling at the solidification front in real time by a non perturbative method.
• •real time supervision of convective motions influence on crystal growth. First results obtained under 1g condition are presented :
  • ◦hydrodynamic scaling laws testing,
  • ◦instabilities detection,
  • ◦transient phenomena.

Main space results are then anticipated including the role of g-jitters.     

CsI(Eu)晶体空间生长地面实验

人工晶体在高技术领域具有十分重要的应用.在多组分晶体生长过程中,由于分凝的存在,会导致成分沿晶体生长方向产生变化,从而影响到晶体性能的均匀性,对应用产生不利影响.为研究微重力对多组分晶体分凝的影响,利用天宫二号卫星进行空间晶体生长实验.结合晶体生长特性和天宫二号综合材料实验装置的技术条件,确定以铕掺杂CsI晶体为研究对象.在地面研制阶段,CsI（Eu）晶体样品顺利通过力学环模试验,并在地面实验中生长出质量较高的CsI晶体,样品中存在明显的组分分凝.      

Protein crystal growth aboard the U.S. space shuttle flights STS-31 and STS-32.

The first microgravity protein crystal growth experiments were performed on Spacelab I by Littke and John. These experiments indicated that the space grown crystals, which were obtained using a liquid-liquid diffusion system, were larger than crystals obtained by the same experimental system on earth. Subsequent experiments were performed by other investigators on a series of space shuttle missions from 1985 through 1990. The results from two of these shuttle flights (STS-26 and STS-29) have been described previously. The results from these missions indicated that the microgravity grown crystals for a number of different proteins were larger, displayed more uniform morphologies, and yielded diffraction data to significantly higher resolutions than the best crystals of these proteins grown on earth. This paper presents the results obtained from shuttle flight STS-32 (flown in January, 1990) and preliminary results from the most recent shuttle flight, STS-31 (flown in April, 1990).     

天宫二号碲化锌晶体生长

在天宫二号飞船综合材料实验炉六工位采用碲熔剂法生长了碲化锌晶体,生长时最高温度为800℃,以0.5mm·h-1的提拉速度向炉膛内部提拉生长晶体.飞行实验后,用相同实验参数在地面进行了对比实验.结果发现,空间样品尾部有一个非常大的橙色结晶区域（约10mm×6mm×2mm）,而地面生长样品中碲化锌晶体尺寸仅为约3mm×3mm×1mm,空间生长的碲化锌晶粒尺寸明显优于地面.空间微重力环境下,由于毛细作用,空间样品的塞子处有Te和ZnTe的外延膜生成.而地面生长的锭条在塞子处只有零星点状气相生产物.因此微重力条件有利于碲化锌晶体材料的生长.      

Progress in Space Material Researches

New progress in the post researches on space grown materials, the development of experiment facilities, and the experiment techniques for space materials researches were introduced. Besides the conventional materials, such as alloys, semiconductors, and optical crystals, new materials have also been prepared on the ground.     

The influence of microgravity on the growth of metals and alloys—The project of Czechoslovak experiment

The crystal growth under near-zero gravity conditions may lead to materials of better crystalline and compositional perfection [1]. Unidirectional solidification of metals is a part of Czechoslovak programme on space research within the framework of Interkosmos [2]. On the model-like systems of metals grown in the space we want to study the effect of foreign atoms on the surface tension and the lattice defects density. The objectives of our ground-based and space experiments are discussed.     

空间低温溶液晶体生长的地基实验

首次使用疏水型聚四氟乙烯微孔滤膜,利用其透气不透水的特性,密封晶体生长容器,采用恒温蒸发法进行晶体生长.溶剂通过蒸发离开生长容器后,被生长容器外的吸附剂吸附,使得溶液维持一定过饱和度,以实现单晶的连续生长.在此基础上研制出一套空间低温溶液晶体生长地基模拟装置.利用此装置进行了一系列地基模拟实验,获得一批高质量α-LiIO₃单晶,证实了该生长装置的溶剂蒸发量和容器密封性能够满足空间低温溶液晶体生长需要,为未来空间低温溶液晶体生长实验奠定了基础.      

Strong magnetic field effect on the dissolution process of tetragonal lysozyme crystals.

Either a homogeneous or inhomogeneous magnetic field has been known to dampen the protein crystal growth. To date the mechanism is not clear. However, it was generally proposed that the magnetic field may dampen the convection in the solution, resulting in a reduced crystal growth rate and possibly a good crystal quality, similar to the case of protein crystal growth in space. To understand the mechanism of the magnetic field effect on protein crystal growth, further explorations on the magnetic field effect on protein solution, on the processes of crystal growth and dissolution, and on different crystallization (solution) systems, should be valuable. In this paper we present our recent efforts to study magnetic field effects on the dissolution processes of tetragonal lysozyme crystals under a strong magnetic field. A layer of oriented tetragonal lysozyme crystals was prepared under a temperature gradient and magnetic field, after that the crystals were dissolved by increasing the temperature of the solution. The lysozyme molecules will diffuse upwards due to the steep concentration gradient at the lower side of the cell caused by the dissolution. The evolution of the concentration in the solution was measured in-situ using a Mach-Zehnder interferometer. The results confirmed that the dissolution process of the crystals was slowed by the magnetic field. Judging from the concentration evolution versus time at different positions in the solution, we concluded that the apparent diffusion coefficient of lysozyme molecules was decreased by the magnetic field. The results were discussed using a suspended crystal model in the initial dissolution stage.     

A space instrument for fundamental materials science problems: The MEPHISTO program

Keeping planar the L/S interface during solidification and controling heat and mass transfers in the liquid phase are 2 important constraints which need to be satisfied to grow suitable single crystals. In the first part of this paper we describe performances of the MEPHISTO instrument which allows :

— On line in-situ measurements of the real undercooling of a solidification front by a non-perturbative thermoelectric method.

— On line supervision of convective motions influence on crystal growth. In the second part, we present the first main results obtained during the ground testing of the space mock-up and we quantify the scientific results accuracy concerning both the onset of the morphological stability and the interface response to unsteady perturbations.     

Crystallisation of alpha-crustacyanin, the lobster carapace astaxanthin-protein: results from EURECA.

Crystallisation of alpha-crustacyanin, the lobster carapace astaxanthin-protein was attempted under microgravity conditions in EURECA satellite using liquid-liquid diffusion with polyethyleneglycol (PEG) as precipitant; in a second reaction chamber phenol and dioxan were used as additives to prevent composite crystal growth. Crystals of alpha-crustacyanin grown under microgravity from PEG were larger than those grown terrestrially in the same apparatus under otherwise identical conditions. On retrieval, the crystals from PEG were shown to be composite and gave a powder diffraction pattern. The second reaction chamber showed leakage on retrieval and had also been subjected to rapid temperature variation during flight. Crystal fragments were nevertheless recovered but showed a powder diffraction pattern. It is concluded, certainly for liquid-liquid diffusion using PEG alone, that, for crustacyanin, although microgravity conditions resulted in an increase in dimensions of crystals, a measurable improvement in molecular ordering was not achieved.     

Solidification and Crystal Growth on the SJ-10 Recoverable Scientific Experiment Satellite

The low-gravity environment aboard the space provides a unique platform for understanding crystal-growth-related phenomena that are masked by gravity on the Earth and for exploring new crystal growth techniques. We have characterized the wetting behavior of metal alloys and carried out melt growth of compound semiconductors under the support of materials science program in the SJ-10 recoverable satellite. We found that interfacial reaction plays a significant role in the interfacial evolution of Sn-based alloys. Detached growth of InAsSb was realized under microgravity, whereas during the terrestrial experiment the crystal and the crucible wall contact with each other. Moreover, the suppression of buoyancy-driven convection results in a more uniform composition distribution in the InGaSb and Bi₂Te₃-based semiconductor alloys.      

微重力条件下红外材料的空间生长

根据近年红外材料在空间生长的研究概况,分析了涵盖熔体、气相、液相外延和分子束外延等生长方法及各个方法生长红外材料的基本原理,在地面生长遇到的问题,以及在空间微重力环境中进行红外材料生长的优势.同时基于中国利用熔体法在天宫二号上已经进行的ZnTe:Cu晶体的空间生长科学实验及地基实验结果,通过对空间和地面实验结果进行对比,提出了在超高真空环境下,利用分子束外延方式生长高性能、大尺寸红外材料的可能性,以及未来在空间微重力条件下进行红外材料生长的研究方向及具体应用.      

Farming in space: environmental and biophysical concerns.

The colonization of space will depend on our ability to routinely provide for the metabolic needs (oxygen, water, and food) of a crew with minimal re-supply from Earth. On Earth, these functions are facilitated by the cultivation of plant crops, thus it is important to develop plant-based food production systems to sustain the presence of mankind in space. Farming practices on earth have evolved for thousands of years to meet both the demands of an ever-increasing population and the availability of scarce resources, and now these practices must adapt to accommodate the effects of global warming. Similar challenges are expected when earth-based agricultural practices are adapted for space-based agriculture. A key variable in space is gravity; planets (e.g. Mars, 1/3 g) and moons (e.g. Earth's moon, 1/6 g) differ from spacecraft orbiting the Earth (e.g. Space stations) or orbital transfer vehicles that are subject to microgravity. The movement of heat, water vapor, CO2 and O2 between plant surfaces and their environment is also affected by gravity. In microgravity, these processes may also be affected by reduced mass transport and thicker boundary layers around plant organs caused by the absence of buoyancy dependent convective transport. Future space farmers will have to adapt their practices to accommodate microgravity, high and low extremes in ambient temperatures, reduced atmospheric pressures, atmospheres containing high volatile organic carbon contents, and elevated to super-elevated CO2 concentrations. Farming in space must also be carried out within power-, volume-, and mass-limited life support systems and must share resources with manned crews. Improved lighting and sensor technologies will have to be developed and tested for use in space. These developments should also help make crop production in terrestrial controlled environments (plant growth chambers and greenhouses) more efficient and, therefore, make these alternative agricultural systems more economically feasible food production systems.     

抗振晶体振荡器的仿真设计CSCD

本文介绍了利用仿真软件进行抗振晶体振荡器设计的方法,通过建立晶体振荡器结构仿真模型,对其力学特性进行深入细致的分析,并在此基础上对比分析减振材料的剪切模量和被减振物质量对晶体振荡器抗振性能的影响,优化晶体振荡器减振结构。然后,根据仿真设计制做了抗振晶体振荡器,并进行了随机振动试验。结果表明,试验现象与仿真结果基本一致,验证了仿真分析的有效性,且振动下晶体振荡器相位噪声达到-145d Bc/Hz@1k Hz,极大地提高了晶体振荡器的抗振性能。     

空间毛细管式蛋白质结晶室样品加载技术研究

采用X-elax射线衍射技术研究蛋白质分子结构与功能的必要前提是获得高质量的蛋白质晶体.空间微重力环境是生长优质蛋白质晶体的理想场所.蛋白质样品的加载工艺对于空间蛋白质结晶实验的成效具有重要影响.针对为神舟八号飞船空间实验新研制的毛细管式空间蛋白质结晶室,结合样品加载基本流程,对加载工艺和伴随的气泡缺陷问题进行了系统和深入分析,确定了针头形状、毛细管封口质量和硅化效果、样品加载工具以及毛细管夹持方式等影响因素,并获得了实验测试验证.在此基础上,通过改进毛细管烧制工艺和样品加载工具,研制和使用专用毛细管夹具等措施,简化了蛋白质样品加载工艺,消除了气泡缺陷,提高了加载效率.新工艺的实施保证了空间实验任务的顺利完成.      

用国产装置进行的空间蛋白质结晶实验

使用国内研制的管式汽相扩散结晶装置,在我国返回式卫星上,成功地完成了两次空间蛋白质晶体生长实验,10种不同种类的蛋白质配制的48个样品在空间的出晶率分别达52%和80%,其中少数蛋白质生长出了较高质量的蛋白质晶体。结果表明,空间的微重力环境利于改善蛋白质晶体的生长,而且在结晶条件优化足够好的条件下,在空间里能生长出比地面晶体尺寸较大、形态较好和内部有序性较高的蛋白质晶体。本文还就微重力对蛋白质晶体生长的具体作用及其开发利用做了讨论。