人类胚胎低温保存溶液EFSh40实现玻璃化工况条件的实验研究

实验研究了溶液EFSh40实现玻璃化的工况条件以及人类胚胎低温保存中采用双层麦管的可行性。研究结果表明,玻璃化溶液EFSh40在降温速率高于100K/min时能够玻璃化,复温速率高于200K／min时没有反玻璃化现象。本研究也实现了双层麦管中溶液EFSh40的玻璃化。采用双层麦管不但避免了潜在的污染问题,而且简化了操作程序。     

不同保护剂浓度和不同降温速率对脂质体玻璃化转变温度的影响

玻璃化转变是动力学的非平衡过程,玻璃化转变量温度是和过程有关的参数。测量了在降温速率分别为５℃/min和１０℃/miｎ,升温速率为１０℃／ｍｉｎ条件下,葡萄糖、蔗糖、甘露醇、海藻糖浓度为５％（Ｗ／Ｖ）的脂质体悬浮的玻璃化转变温度Ｔ‘g,在降温速率为５℃ｍｉｎ、升温为１０℃/min条件下,测量了葡萄糖、蔗糖、甘露醇、海藻糖浓度为１５％（Ｗ／Ｖ）的脂质体的Ｔ’ｇ;并分析了不同降温速率和不同保护剂浓度对脂质体玻璃化转变温度Ｔ’g的影响因素。     

新型低温保存装置性能的实验研究

低温保存装置是实现生物材料长期储存的关键设备之一.采用自复叠制冷、自动化控制和最新低温生物技术的冻结线跟踪法开发了一种新型低温保存装置.利用该装置对甘油、丙二醇、二甲亚砜这三种常用的低温保护剂溶液进行了程序控制的变浓度降温和复温实验,使溶液的最终浓度达到玻璃化所需的浓度,最低温度降到-80℃以下.实验表明,新装置性能符合低温保存要求,在生物材料的玻璃化保存领域有良好的应用前景.     

非晶聚合物玻璃化转变温度Tg附近的转变过程

从弛豫理论出发，在不同的时效时间和不同降温速率下对非晶聚合物PVC玻璃化转变过程中与时间参量密切相关的。α峰峰温（Tα）和用热膨胀法标定的玻璃化转变温度（Tg）进行了对比测量，得出α内耗峰是非晶态聚合物热平衡态下的特征内耗峰，其弛豫机制是在热平衡态下独立存在的Tg是热平衡态到非平衡态的转变温度点，两者都与非晶态结构的存在紧密相关，它们的表观行为取决于非晶聚合物热平衡态下的同一个本征弛豫时间，但它们的表征是完全不同的两种物理过程     

冷冻干燥过程中溶液冻结特性的DSC研究

利用差示扫描量热仪(DSC)研究了蔗糖水溶液的冻结特性,分析了溶液浓度和热历史对冻干过程的影响.DSC实验结果表明,过冷度和最大冻结浓缩溶液的玻璃化转变温度Tg'均与热历史有关;降温时溶液中的水分能否充分结晶受浓度和降温速率的共同影响.降温过程中的结晶热可用来确定溶液降温后的冻结水含量以及最大冻结浓缩溶液中的水分含量.     

羟基磷灰石纳米微粒对不同种类低温保护剂反玻璃化结晶的影响

为了研究羟基磷灰石（HA）纳米微粒对不同种类低温保护剂[渗透性丙三醇（60%,w/w）和非渗透性PEG-600（50%,w/w）]反玻璃化结晶的影响,利用低温显微镜研究了含有不同粒径（20nm、40nm、60nm）和不同质量浓度（0.1%、0.5%）HA纳米微粒的丙三醇和PEG-600溶液在反玻璃化过程中的结晶现象。实验结果表明：丙三醇和PEG-600溶液在反玻璃化过程中的冰晶形貌分别为枝状和球形,且形貌都不随添加纳米微粒而改变。与未添加纳米微粒的丙三醇溶液相比,添加60nm、0.5%纳米微粒溶液的析晶分数仅为未添加溶液的1/7。PEG-600溶液在-64℃～-52℃区间内的析晶分数显著增加,其中添加40nm、0.5%纳米微粒的PEG-600溶液的析晶分数增加了90%。冰晶的生长速率存在两个极大值现象,而添加40nm、0.5%纳米微粒的丙三醇溶液、未添加和添加60nm纳米微粒的PEG-600溶液的冰晶生长速率都只有一个极大值。     

渗透性低温保护剂玻璃化转变临界降温速率的实验确定

从Boutron结晶动力学半经验公式出发，结合他人的修正结果，利用差示量热扫描仪(DSC)的实验数据，不必构造TTT和ccT曲线，获得了若干常用低温保护剂实现玻璃化转变的临界降温速率，测定了渗透性低温保护剂实现玻璃化转变的临界结晶率，修正了临界降温速率的计算公式，实验还说明了Bourton模型对非渗透性保护剂降温结晶过程的局限性。     

低温保护剂溶液固化性质的DSC研究

利用差示扫描量热仪,研究了乙二醇、丙三醇、1,3丙二醇、1,3丁二醇和2,3丁二醇水溶液的水合性质、玻璃化转变温度和反玻璃化转变温度,得出了这些性质与溶液浓度的关系.研究发现未冻水含量在低浓度时没有明显的规律性,而在中高浓度则随着溶液浓度的增大而增大.对于玻璃化转变,中低浓度区溶液形成的是部分晶体的玻璃态,紧接着在高浓度区溶液形成完全的玻璃态.部分玻璃化的温度不随浓度变化,而玻璃化的温度随浓度增大而升高.形成反玻璃化的浓度范围比较小,反玻璃化的温度随浓度增大而升高.保护剂在玻璃化转变温度和反玻璃化转变温度的明显差异,则反映它们在玻璃化能力方面的强与弱.     

控制降温对近空间升华法沉积CdZnTe薄膜形貌与结构的影响

采用场发射扫描电镜和X射线衍射技术研究了生长结束后的降温过程对以近空间升华法生长的CdZnTe薄膜形貌与结构的影响。分析了快速(炉冷,673K以上-8K/min)和慢速(-2K/min)两种降温速率下获得的CdZnTe薄膜的结构与形貌,并考察了降温中是否阻断生长源向薄膜的传质的影响。结果表明,所得到的薄膜均为闪锌矿结构,降温时薄膜的持续生长将抑制晶粒在平面内铺展而使其棱角钝化的趋势,以较慢的速率降温和降温时阻断传质均有利于提高薄膜的致密度,降低粗糙度及薄膜的织构强度。     

冷冻载体Cryotop降温速率的测量及系统优化

Cryotop法是玻璃化保存卵母细胞较有效的方法之一。当Cryotop载体插入液氮时,降温速度极高,几乎瞬间完成,常规的方法无法测量。实验使用数字示波器、线径25μm 的T型热电偶建立起高速测温系统,测量了Cryotop法用于卵母细胞低温保存时的降温速率。通过改变载体材料、厚度、冷源温度等条件,提高Cryotop的降温速率。结果发现当使用60μm的铜质载板,使用浆状液氮作为冷源时,降温速度最高,可达到37130±1336 K/min,较商品化的Cryotop的降温速度（11982±1936 K/min）提高了2倍。     

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.     

Degradation behaviour of sputtered Co–Al coatings on superalloy

Degradation behaviour of sputtered Co–Al coatings on Superni-718 substrate has been investigated. Cyclic high temperature oxidation tests were conducted on uncoated and coated samples at peak temperatures of 900 °C for up to 100 thermal cycles between the peak and room temperatures. The results showed that a dense scale formed on the coated samples during thermal cycling at the peak temperature of 900 °C. The external scale exhibited good spallation resistance during cyclic oxidation testing at both temperatures. The improvement in oxide scale spallation resistance is believed to be related to the fine-grained structure of the coating. Nanostructured Co–Al coatings on Superni-718 substrate were deposited by DC/RF magnetron sputtering. FE-SEM/EDS, AFM, and XRD were used to characterize the morphology and formation of different phases in the coatings, respectively. The Co–Al coating on superalloy substrate showed better performance of cyclic high temperature oxidation resistance due to its possession of β-CoAl phase as Al reservoir and the formation of Al₂O₃ and spinel phases such as CoCr₂O₄ and CoAl₂O₄ in scale. The oxidation results confirmed an improved oxidation resistance of the Co–Al coating on superalloy as compare to bare substrate in air at 900 °C temperature up to 100 cycles.     

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.     

Thermal Stability of Amorphous Hydride Mg_(50)Ni_(50)H_(54) and Mg_(30)Ni_(70)H_(45)

The thermal stability of amorphous ternary hydrides Mg_(50)Ni_(50)H_(54) and Mg_(30)Ni_(70)H_(45) and their corre-sponding amorphous binary alloys Mg_(50)Ni_(50) and Mg_(30)Ni_(70) were studied with X-ray diffraction(XRD) and differential scanning calorimetry(DSC). Samples of the amorphous alloys were preparedby mechanical alloying and the amorphous hydrides were obtained by charging the alloys with gas-eous hydrogen at 3.0 MPa and 423 K. It was found that the amorphous hydrides released most oftheir hydrogen before the crystallization of the essentially hydrogen depleted amorphous alloy. Thecrystallization temperature of amorphous Mg_(50)Ni_(50)H_(54) elevated and that of amorphousMg_(30)Ni_(70)H_(45) did not change in relation to the original binary amorphous alloy. This is very excep-tional for amorphous hydrides. The reason for the effects of hydrogen absorption/desorption on thecrystallization of amorphous alloys was discussed.     

长余辉材料Sr_4Al_(14)O_(25)∶Eu~(2+),Nd~(3+)的溶胶凝胶法制备及性能研究

首次研究了以Nd~(3+)离子为辅助激活剂,对Eu~(2+)掺杂的发光材料Sr_4Al_(14)O_(25):Eu~(2+)余辉性能的影响.用溶胶凝胶法合成了Eu~(2+), Nd~(3+)共掺杂的Sr_4Al_(14)O_(25):Eu~(2+),Nd~(3+)发光粉末,并用扫描电镜、X射线衍射计、荧光分光光度计、余辉亮度测试仪、热释光剂量计等手段对粉末样品进行了表征.结果表明,在1350℃得到了单一的Sr_4Al_(14)O_(25)相,粉末颗粒平均粒度在1μm左右.Eu~(2+), Nd~(3+)共掺杂的Sr_4Al_(14)O_(25):Eu~(2+),Nd~(3+)发光粉末有402和485nm两个发射峰,与Eu~(2+)单掺杂的Sr_4Al_(14)O_(25):Eu~(2+)相比,发射峰位置没有变化,但适量的掺杂可以大大提高余辉时间和余辉亮度,余辉时间可达18h以上.最后通过对热释光谱的分析解释了双掺杂发光粉余辉性能增强的原因,适宜深度的陷阱可以有效存储光能,增强余辉的时间和强度.     

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.     

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.     

Percolation and the resistive transition of the critical temperature Tc of Nb3Sn

The relationship between the distribution of the critical temperature, the percolation function, and the resistive transition of the critical temperature is explored for polycrystalline Nb₃Sn. In the neighborhood of the critical temperature, Nb₃Sn is assumed to be a random mixture of superconducting and normal grains. Percolation concepts are applied to a study of the resistivity. A general analysis is made showing that the onset and shape of the resistive transition for composite conductors are determined by the percolation function and the distribution of the critical temperature. An approximate form of the percolation function is determined based on a linear FEM analysis. Example resistive transitions are calculated for an assumed normal distribution of the critical temperature. An argument is presented that relates grain orientation and strain dependence in Nb₃Sn. It is noted that a dependence of the distribution of T_c with strain, in addition to the usual shift in T_c with strain, would be the result of a strain dependence that is a function of grain orientation. The analysis shows the extent to which the slope of the resistive transition is a measure of the distribution of the critical temperature, and therefore a measure of the grain orientation strain sensitivity. Finally, a method is described to determine the percolation function experimentally.