低温生长硅基碳化硅薄膜研究

在850℃的低温下，在Si（100）衬底上生长了3C－SiC薄膜，气源为SiH4和C2H4混合气体。用X射线衍射、X射线光电子能谱和傅立叶红外吸收谱分析了薄膜的晶体结构、组分以及键能随深度的变化。研究表明薄膜为富硅的3C－SiC结晶层，其中的Si/C比约为1.2。     

Si(001)衬底上方形3 C-SiC岛的LPCVD生长

Si衬底上SiC的异质外延生长深受关注,为了了解Si衬底上的成核及长大过程,采用PLCVD方法在Si(001)衬底上生长出了方形3C-SiC岛,利用Nomarski光学显微镜和扫描电子显微镜（SEM）观察了SiC岛的形状,尺寸,密度和界面形貌,结果表明,3C－SiC岛生长所需的Si原子来自反应气源,衬底上的Si原子不发生迁移或外扩散,气相中C原子浓度决定了SiC岛的生长过程。     

Si基β-SiC薄膜外延生长技术研究

采用SiH4-C3H8-H2气体反应体系,通过常压化学气相淀积（APCVD）工艺在P型Si(100)衬底上进行了β-SiC薄膜异质外延生长。利用俄歇电子能谱、SEM及X射线衍射能谱进行了生长薄膜微结构分析。提出并讨论了外延生长β－SiC薄膜的最佳工艺条件及其生长机理。     

ZnO/SiC/Si异质结构的特性

用MOCVD方法在p型单晶Si（100）基片上外延SiC层,再用直流溅射在SiC层上生长ZnO薄膜,制备出ZnO／SiC／Si异质结构,用XRD和AFM分析了ZnO／SiC／Si和ZnO／Si异质结构中表层ZnO的结构和形貌的差别,研究了这种异质结构的特性．结果表明,在Si（100）基片上外延生长出的是高取向、高结晶质量的SiC（100）层．这个SiC层缓冲层使在Si基片上外延生长出了高质量ZnO薄膜,因为ZnO与SiC的晶格失配比ZnO与Si的晶格失配更低．     

硅碳比对Si(111)表面SSMBE异质外延SiC薄膜的影响

利用固源分子束外延(SSMBE)生长技术, 在不同的硅碳蒸发速率比(Si/C)条件下, 在Si(111)衬底上生长SiC单晶薄膜. 利用反射式高能电子衍射(RHEED)、X射线衍射(XRD)、原子力显微镜(AFM)和傅立叶变换红外光谱(FTIR)等实验技术, 对生长的样品形貌和结构进行了研究. 结果表明, 在Si/C比(1.1:1.0)下生长的薄膜样品, XRDω扫描得到半高宽为2.1°; RHEED结果表明薄膜具有微弱的衍射环, 有孪晶斑点. 在Si/C比(2.3:1.0)下生长的薄膜, XRDω扫描得到的半高宽为1.5°, RHEED显示具有Si的斑点和SiC的孪晶斑点. AFM显示在这两个Si/C比下生长的样品表面都有孔洞或者凹坑, 表面比较粗糙. 从红外光谱得出 薄膜存在着比较大的应力. 但在Si/C比(1.5:1.0)下生长的薄膜样品, XRDω 扫描得到的半高宽仅为1.1°; RHEED显示出清晰的SiC的衍射条纹, 并可看到SiC的3×3表面重构, 无孪晶斑点; AFM图像表明, 没有明显的空洞, 表面比较平整. FTIR谱的位置显示, 在此Si/C比下生长的薄膜内应力比较小. 因此可以认为, 存在着一个优化的Si/C比(1.5:1.0), 在这个Si/C比下, 生长的薄膜质量较好.     

Si(100)衬底上SiC的外延生长

在1050℃下用Si2H6和C2H4在Si(100)衬底上外延生长了3C-SiC,生长前只通入C2H4将Si衬底碳化形成SiC缓冲层.碳化过程中C2H4与Si表面反应形成了SiC孪晶,但随着生长时间的延长,外延层转变为单晶层,其表面呈现典型的单晶SiC的(2×1)再构.从外延层的Raman谱观察到明显的SiC的TO和LO声子模;SEM观测结果表明,外延层的表面比较平整.     

不同衬底上低温生长的ZnO晶体薄膜的结构及光学性质比较

采用电子束反应蒸发方法,在单晶Si（001）及玻璃衬底上低温外延生长了沿C轴高度取向的单晶ZnO薄膜,并对沉积的ZnO晶体薄膜的结构和光学性质进行了分析比较。通过对ZnO蒲膜的X射线衍射（XRD）分析及光致荧光激发谱（PLE）测量,研究了衬底材料结构特性、生长温度及反应气氛中充O2对ZnO薄膜的晶体结构和晶体光学吸收特性的影响。结果表明：①衬底温度对沉积的ZnO薄膜的晶体结构影响显,玻璃衬底上生长ZnO薄膜的最佳温度比Si(001)衬底上生长的最佳温度要高70℃;②虽在最佳生长条件下获得的ZnO薄膜的的XRD结果（半高宽和衍射强度）相近,但光学吸收特性有较大差异,Si(001)衬底上生长的ZnO薄膜优于玻璃衬底上生长的ZnO薄膜;③反应气氛中的O2分压对XRD结构影响不大,但对PLE谱影响显,充O2后能明显改善吸收边特性。     

蒸发速率对Si衬底上SSMBE外延SiC薄膜的影响

采用固源分子束外延（SSMBE）生长技术,用不同的蒸发速率,在Si（111）衬底上生长SiC薄膜。利用反射式高能电子衍射（RHEED）、X射线衍射（XRD）、原子力显微镜（AFM）等实验技术,对生长的样品的形貌和结构进行研究。结果表明,在优化的蒸发速率（1.0 nm·min^-1）下,所生长的薄膜质量最好。低的蒸发速率（0.25 nm·min^-1）难以抑制孔洞的形成,衬底的Si原子可通过这些孔洞扩散到样品表面,导致结晶质量变差。在高的蒸发速率（1.8 nm·min^-1）下,以岛状方式生长甚至以团簇聚集,表面的原子难以迁移到最佳取向的平衡位置,导致样品表面粗糙度变大,薄膜的结晶质量变差,甚至出现多晶。     

缓冲层对氮化镓二维生长的影响

报道了在射频等离子体（RF-Plasma)辅助的分子束外延（MBE）技术中，使用白宝石（0001）衬底，采用低温缓冲层工艺外延氮化镓（GaN)。通过原子力显微镜（AFM）的表面形貌比较及X射线双晶衍射（XRD）ω扫描摇摆曲线的分析，讨论了低温缓冲层成核机理及缓冲层生长温度与形成准二维生长的关系，确立了缓冲层的三维成核，准二维生长的生长机理，并在此基础上实现了氮化镓外延层更好地二维生长，进一步提高了氮化镓外延层的晶体质量。     

新型硅基双异质外延SOI材料Si/γ-Al2O3/Si制备

异质外延法是目前制备新型SOI材料的技术途径之一。采用低压化学气相沉积技术(LPCVD)在硅衬底上先外延γ-Al2O3绝缘单晶薄膜，制备出硅衬底上外延氧化物外延结构γ-Al2O3/Si(EOS)，然后采用类似SOS薄膜生长的常压CVD(APCVD)方法在EOS上外延硅单晶薄膜，形成新型硅基双异质SOI材料Si／γ-Al2O3／Si。利用反射高能电子衍射(RHEED)、X射线衍射(XRD)、俄歇电子能谱(AES)及MOS电学测量等技术表征分析了Si(100)／γ-Al2O3(100)／Si(100)SOI异质结构的晶体结构、组分和电学性能。测试结果表明，已成功实现了高质量的新型双异质外延SOI结构材料Si(100)／γ-Al2O3(100)／Si(100)，γ-Al2O3与Si外延薄膜均为单晶，γ-Al2O3薄膜具有良好绝缘性能，SOI结构界面清晰陡峭，该SOI材料可应用于CMOS电路的研制。     

Real gas choked flow conditions at low reduced-temperatures

Real gas choked mass flux is calculated for a frictionless stream expanding isentropically until it reaches the speed of sound and without phase changes. The other parameters associated with the choked state are the pressure, density, temperature ratios, and the speed of sound. Departure of the choked mass flux from the ideal gas model is discussed first in absolute terms and then in relative terms, using the Principle of Corresponding States, for gases with boiling points in the low temperature range. Reduced-stagnation pressures are examined up to values of 30 for hydrogen, neon, nitrogen, argon, methane, krypton, xenon, and R-14 and up to 100 for ⁴He. The corresponding reduced-stagnation temperatures go down to 1.4 and in some cases down to 1.2 for nitrogen and argon. Also discussed are the limiting values of stagnation parameters for which no phase change occurs in the choked state. Compared to the ideal gas, the mass flux may almost double and the critical pressure ratio may decrease by an order of magnitude. The relevance of results is discussed qualitatively and quantitatively for Joule-Thomson cryocooling.     

As-cast microstructures and behavior at high temperature of chromium-rich cobalt-based alloys containing hafnium carbides

Hafnium is often used to improve the high temperature oxidation resistance of superalloys but not to form carbides for strengthen them against creep. In this work hafnium was added in cobalt-based alloys for verifying that HfC can be obtained in cobalt-based alloys and for characterizing their behavior at a very temperature. Three Co–25Cr–0.25 and 0.50C alloys containing 3.7 and 7.4 Hf to promote HfC carbides, and four Co–25Cr– 0 to 1C alloys for comparison (all contents in wt.%), were cast and exposed at 1200 °C for 50 h in synthetic air. The HfC carbides formed instead chromium carbides during solidification, in eutectic with matrix and as dispersed compact particles. During the stage at 1200 °C the HfC carbides did not significantly evolve, even near the oxidation front despite oxidation early become very fast and generalized. At the same time the chromium carbides present in the Co–Cr–C alloys totally disappeared in the same conditions. Such HfC-alloys potentially bring efficient and sustainable mechanical strengthening at high temperature, but their hot oxidation resistance must be significantly improved.     

Chitosan-collagen/organomontmorillonite scaffold for bone tissue engineering

A novel composite scaffold based on chitosan-collagen/organomontmo-rillonite (CS-COL/OMMT) was prepared to improve swelling ratio, biodegradation ratio, biomineralization and mechanical properties for use in tissue engineering applications. In order to expend the basal spacing, montmorillonite (MMT) was modified with sodium dodecyl sulfate (SDS) and was characterized by XRD, TGA and FTIR. The results indicated that the anionic surfactants entered into interlayer of MMT and the basal spacing of MMT was expanded to 3.85 nm. The prepared composite scaffolds were characterized by FTIR, XRD and SEM. The swelling ratio, biodegradation ratio and mechanical properties of composite scaffolds were also studied. The results demonstrated that the scaffold decreased swelling ratio, degradation ratio and improved mechanical and biomineralization properties because of OMMT.     

Capacitance based mass metering for cryogenic fluids

This paper describes a method for measuring the mass of cryogenic fluids in on-board rocket propellant tanks or ground storage tanks. Linear approximations to the Clausius-Mossotti relationship serve as the foundation for a capacitance based mass sensor, regardless of fluid density stratification or tank shape. Sensor design considerations are presented along with the experimental results for a capacitance based mass gage tested in liquid nitrogen. This test data is shown to be consistent with theory resulting in a demonstrated mass measurement accuracy of ±0.75% and a deviation from linearity of less than ±0.30% of full scale mass. Theoretical accuracies are also shown to be ±0.73% for hydrogen and ±1.39% for oxygen for a select range of pressures and temperatures.     

Equipment using a “static-analytic” method for solubility measurements in potentially hazardous binary mixtures under cryogenic temperatures

A new apparatus designed to study, at cryogenic temperatures, thermodynamic equilibria of potentially explosive binary systems such as hydrocarbon-oxygen mixtures is described herein. This equipment has an equilibrium cell which was especially designed to minimize hazards while allowing accurate phase equilibrium measurements. Reliability of results, obtained with this equipment has been verified by working on the nitrogen-propane system, for which data are already available in literature, over a large range of compositions and at various temperatures. Four isothermal curves describing liquid phase compositions at 109.98, 113.77, 119.75 and 125.63 K have been determined. Our experimental data are represented within 2% in compositions and in pressures through the Peng-Robinson equation of state implying Mathias-Copeman alpha function and Huron-Vidal mixing rule. Comparisons to literature allow pointing out: good agreement is observed with Kremer and Knapp data (1983) while the three sets of Poon and Lu data (1974) presenting systematic positive deviation are consequently judged as suspicious.     

Gas gap thermal switches using neon or hydrogen and sorption pump

The very low pressure obtained thanks to adsorption phenomenon at low temperature can be used to build cryogenic heat switches, which offer the possibility to make or break thermal contact between two parts of a cryogenic system. The ON (conducting) and OFF (insulating) states of the switch are obtained by varying the gas pressure between two copper blocks separated by a gap of 100 μm. This pressure is controlled by acting upon the temperature of a small sorption pump (activated charcoal) connected to the gap space. For a “high” sorption pump temperature, the gas previously adsorbed in the sorption pump is released to the gap between the two blocks, allowing a good thermal conduction through the gas (ON state). On the opposite, cooling the sorption pump allows a very good vacuum between the copper blocks, which efficiently break the thermal contact (OFF state). Experimental thermal characteristics (Conductance in the ON and OFF state, ON-OFF switching temperature) of such a “Gas Gap Heat Switch” are described using hydrogen or neon as exchange gas and are compared with theoretical calculations.     

Development of No-Vent™ liquid hydrogen storage system for space applications

A number of technological advances required to store and maintain normal-boiling-point and densified cryogenic liquids, including liquid hydrogen, under zero boil-off conditions in-space, for long periods of time, have been developed. These technologies include (1) thermally optimized compact cryogen storage systems that reduce environmental heat leak to the lowest-temperature cryogen, which minimizes cryocooler size and input power, and (2) actively-cooled shields that surround the storage systems and intercept heat leak. The processes and tools used to develop these technologies are discussed. A zero boil-off liquid hydrogen storage system technology demonstrator for validating the actively-cooled shield technology is presented.     

Development of a miniature cryogenic fluid circuit and a cryogenic micropump

This article presents the development of a miniaturized cryogenic fluid circuit for distributed cooling of low-temperature tracking detectors in high-energy physics (HEP). The heart of the circuit is a prototype cryogenic micropump. This volumetric pump is compatible with cooling powers of about 10-100 W, and capable of producing pressure heads of up to around 0.3 MPa. Besides detector and electronics cooling in HEP, potential applications are found in the field of superconductor technology.     

Integrated Resonant Self-Pumped Loop and pulse tube cryocooler for cryogenic cooling distribution

Cooling distribution is a vital technology concerning cryogenic thermal management systems for many future space applications, such as in-space, zero boil-off, long-term propellant storage, cooling infrared sensors at multiple locations or at a distance from the cryocooler, and focal-plane arrays in telescopes. These applications require a cooling distribution technology that is able to efficiently and reliably deliver cooling power (generated by a cryocooler) to remote locations and uniformly distribute it over a large-surface area. On-going efforts by others under this technology development area have not shown any promising results.This paper introduces the concept of using a Resonant Self-Pumped Loop (RSPL) integrated with the proven, highly efficient pulse tube cryocooler. The RSPL and pulse tube cryocooler combination generates cooling power and provides a distributive cooling loop that can be extended long distances, has no moving parts, and is driven by a single linear compressor. The RSPL is fully coupled with the oscillating flow of the pulse tube working fluid and utilizes gas diodes to convert the oscillating flow to one-directional (DC) steady flow that circulates through the cooling loop. The proposed RSPL is extremely simple, lightweight, reliable, and flexible for packaging. There are several requirements for the RSPL to operate efficiently. These requirements will be presented in this paper. Compared to other distributive cooling technologies currently under development, the RSPL technology is unique.     

Helium liquefaction with a commercial 4 K Gifford-McMahon cryocooler

This paper describes helium liquefaction using a commercial cryocooler with 1.5 W cooling power at 4.2 K (Sumitomo model RDK415D with compressor CSW-71D, consuming 6.5 kW electrical power), equipped with heat exchangers for precooling the incoming gas. No additional cooling power of cryoliquids or additional Joule-Thomson stages were utilized. Measurements of the pressure dependence of the liquefaction rate were performed. A maximum value of 83.9 g/h was obtained for 2.25 bar stabilized input pressure. Including the time needed to cool the liquefied helium to 4.2 K at 1 bar after filling the bottle connected to the cold head, and correcting for heat screen influences, this results in a net liquefaction rate of 67.7 g/h. Maintaining a pressure close to 1 bar above the bath during liquefaction, a rate of 55.7 g/h was obtained. The simple design enables many applications of the apparatus.