HA-316L不锈钢纤维非对称功能梯度生物材料制备与显微组织

用低压热等静压方法在1100℃下制备了HA(ZrO₂)-316L不锈钢纤维非对称FGM,其中316L不锈钢纤维含量按体积比20%→15%→10%→5%呈非对称梯度变化.并通过金相显微镜、SEM、EDXA分析了材料的微观结构和微区元素含量.结果表明,HA(ZrO₂)-316L不锈钢纤维非对称FGM微观上表现为316L不锈钢纤维在FGM中呈无序、均匀分布状态,316L不锈钢纤维包裹于HA(ZrO₂)基体中,两者结合紧密,界面表现为部分凹凸不平,316L不锈钢纤维与HA(ZrO₂)基体紧紧的咬合在一起.在FGM基体中发生了微量的韧化相Fe元素扩散,韧化相316L不锈钢纤维不发生基体相Ca、P元素的扩散,基体与韧化相均相对独立,二者之间不发生任何化学反应.随着HA含量增加,HA(ZrO₂)-316L不锈钢纤维复合材料的断裂韧性和弹性模量逐渐减小,体现了FGM中各梯度层的力学性能缓和设计.HA(ZrO₂)-316L不锈钢纤维FGM中,分析认为,增韧机理主要为纤维拔出增韧和层间裂纹偏转增韧.     

真空烧结制备316L不锈钢纤维/HA复合生物材料及其理化性能

用真空烧结成功制备了不同成分316L不锈钢纤维/HA复合生物材料和316L不锈钢纤维/HA-ZrO₂ (CaO) 复合生物材料,并通过金相显微镜、SEM、EDXA分析了材料的微观结构、断裂性能和微区元素含量。结果表明:不锈钢纤维和纳米ZrO₂ (CaO) 粒子对复合材料具有增强和增韧的作用。综合考虑认为,20% 316L不锈钢纤维/HA-ZrO₂ (CaO) 复合材料的性能最优,其抗弯强度和抗压强度分别为140.1MPa和348.9MPa。316L不锈钢纤维/HA-ZrO₂ (CaO) 复合材料抗弯强度随316L 不锈钢纤维直径和长度减小而增大,且纤维长度对抗弯强度的影响略大于纤维直径的影响。复合材料微观组织随HA粉末和316L不锈钢纤维成分变化呈规律性变化,没有出现明显的裂纹或孔隙,HA和316L不锈钢纤维结合紧密,界面平整,两相融合程度较高。5% 316L不锈钢纤维复合材料表现为脆性断裂,而10%、20%、40% 316L不锈钢纤维复合材料均表现为韧性断裂,且韧性程度随316L不锈钢纤维含量依次增加。基体与韧化相均相对独立,二者之间不发生任何化学反应,基体HA中发生微量的Fe元素扩散,但在316L不锈钢中不发生基体的扩散。      

热压制备硅酸铝纤维/TCP生物FGM的微观结构与性能

采用热压工艺制备了硅酸铝纤维/TCP生物功能梯度材料(FGM)。采用X射线衍射分析、扫描电镜、EDAX线扫描能谱分析、密度分析及洛氏硬度分析对FGM进行了研究,结果表明：纤维含量分布呈轴向对称梯度变化。FGM整体完好,无破损或裂纹出现。FGM在宏观上呈现较模糊的梯度分布,微观上则表现出成分的连续变化。TCP基体与纤维结合紧密。FGM中TCP与硅酸铝纤维及热压模之间均未发生化学反应生成杂质化合物,HA至TCP的相变是因为羟基磷灰石的分解产生。随纤维含量增加,FGM各梯度层的断裂形式由脆性断裂逐渐转变为韧性断裂,且韧性程度随纤维含量增加而增强。各梯度层硬度和相对密度随纤维含量的增加而提高,且在纤维含量为60 vol%时达到最高,分别为92.7 MPa和86.5%。     

316L纤维尺寸和含量对HA-ZrO2(CaO)/316L纤维复合生物材料性能的影响

研究了316L纤维的长度、直径与含量对HA-ZrO_2（CaO）/316L纤维生物复合材料的力学性能的影响规律.结果表明：纤维直径为40μm的复合材料力学性能优于纤维直径为50μm的复合材料;纤维长度为0.8～1.2mm的复合材料力学性能优于纤维长度为2～3mm的复合材料;随着纤维体积分数增大,纤维之间相互接触而导致在复合材料中形成的微孔增多,并成为微裂纹源,导致材料力学性能下降.含20vol%直径为40μm、长度为0.8～1.2mm的316L纤维的HA-ZrO_2（CaO）/316L纤维生物复合材料的综合力学性能最佳,其抗弯强度、杨氏模量、断裂韧性和相对密度分别为140.1MPa、117.8GPa、5.81MPa·m~（1/2）和87.1%.复合材料微观组织随HA粉末和316L纤维成分的变化呈规律性变化,没有出现明显的裂纹或孔隙,316L纤维与HA-ZrO_2（CaO）基体紧紧地咬合在一起,其结合主要靠基体对316L纤维的物理附着力所致.基体中发生微量Fe元素扩散,但在316L纤维中不发生基体Ca、P元素的扩散.含5%316L纤维复合材料表现为脆性断裂,而含10%、20%、40%316L纤维复合材料均表现为韧性断裂,且韧性程度随316L纤维含量的增加而增大.     

流延法制备管状ZrO_2/SUS316L功能梯度材料

结合流延法和辊压成型技术制备梯度变化为10%和20%(体积分数)的管状ZrO2/SUS316L梯度材料,优化了管状梯度材料的制备工艺,对其截面形貌进行了表征,利用有限元模拟其应力分布,并结合压缩和循环热震实验对管状梯度材料的径向力学性能和热冲击行为进行了研究。结果表明,所制备的管状ZrO2/SUS316L梯度材料成分梯度过渡良好;径向压缩时最大拉应力产生于外壁不锈钢层,20%(体积分数)管状梯度材料的抗压缩变形的能力较高,但是断裂功较低,而10%(体积分数)管状梯度材料接近于塑性断裂方式;随着梯度变化降低,管状梯度材料的热冲击性能提高,梯度变化10%(体积分数)时500~25℃最大循环热震次数为78。     

HA／ZrO2功能梯度涂层中羟基磷灰石的超微结构分析

利用净能量控制的PRAXAIR 4500型等离子喷涂系统，在钛合金基体上制备出HA／ZrO2功能梯度涂层，采用HTEM、XRD、SEM和表面轮廓仪等对涂层表面HA的显微结构和相结构特征进行分析。结果表明：（1）喷涂态涂层表面HA主要以非晶相存在，存在微量的纳米HA晶体；（2）大气气氛700℃晶化处理显著提高涂层表面HA结晶度，涂层以结晶的HA相存在，且晶体结构完整；（3）HA／ZrO2功能梯度涂层表面粗糙多孔，呈现“二级窝洞”的形貌特征，有利于材料与骨组织间的结合。     

ZrO_2增韧Al_2O_3陶瓷的力学性能和增韧机制

对通过热压烧结法制备的3种陶瓷99.5vol%Al2O3(AD995)、ZrO2(15vol%)/Al2O3和ZrO2(25vol%)/Al2O3的力学性能和增韧机制进行了实验和理论研究。基于复合材料细观力学理论并考虑ZrO2的相变特性,建立了描述ZrO2/Al2O3陶瓷力学性能的本构模型。结果表明:ZrO2的加入细化了基体Al2O3晶粒,ZrO2/Al2O3陶瓷的致密性得到提高;3种陶瓷试件的破坏呈现小变形到脆性破坏的特点,压缩加载下试件应力-应变曲线近似为线性关系;AD995陶瓷的断裂韧性为5.65 MPa·m1/2,ZrO2(25vol%)/Al2O3陶瓷的断裂韧性为8.42 MPa·m1/2,提高了近50%;随ZrO2增韧相含量的增加,ZrO2/Al2O3陶瓷的弹性模量降低而断裂韧性增加,这一变化趋势与实验结果有良好的一致性。     

离心凝胶注模技术制备梯度ZrO_2/HA复合材料

采用离心-凝胶注模成型技术制备梯度ZrO2/HA复合材料,研究浆料固相含量、ZrO2含量对浆料粘度的影响。观察ZrO2/HA浆料的凝胶固化过程,分析离心成型工艺参数对ZrO2/HA生坯密度梯度的影响。观察烧结产物的显微组织并对复合材料的力学性能进行测试。结果表明,浆料固相含量为40%(质量分数),ZrO2含量为15%(质量分数)时,ZrO2/HA浆料粘度为223.5mPa·s,具有良好的分散性。当催化剂含量为1.5%(质量分数)和引发剂含量均为0.6%(质量分数)时,起始凝胶和终止固化时间与离心成型工艺相匹配。当在1 500r/min的转数下离心10min后,离心-凝胶注模成型所得生坯具有良好的密度梯度,经1 200℃烧结2h后试样顶部、中部和底部中ZrO2形成良好的梯度。当ZrO2含量为15%(质量分数)时,复合材料的抗弯强度和断裂韧性达到最大值84.2 MPa和1.76MPa·m1/2,比基体提高了159.8%和117.2%。     

氧化锆增韧HA/ZrO2功能梯度涂层的TEM分析

利用净能量控制的PRAXAIR4500型等离子喷涂系统,在钛合金基体上制备出HA/ZrO2功能梯度涂层,采用HTEM、XRD、SEM等对涂层过渡层ZrO2相的结构特征进行分析.结果表明:(1)富锆的过渡层存在ZrO2 3种晶型,主要以四方氧化锆为主,含有少量的立方氧化锆及微量的单斜氧化锆和CaZrO3,单斜氧化锆的出现说明材料内发生了四方氧化锆向单斜氧化锆马氏体相变,这种马氏体相变有利于提高HA材料的韧性;(2)生物活性功能涂层的富锆过渡层致密,与钛合金基体结合紧密,纯羟基磷灰石的表面层具有典型的多孔结构特征,整个涂层沿垂直基体方向从过渡层致密结构向表面层多孔结构过渡;涂层的这种结构特征有利于改善功能梯度涂层的综合性能,提高涂层与基体的结合强度,其结合强度达到48.6MPa.     

316L不锈钢表面激光熔覆Stellite6合金组织及其耐液态铅铋腐蚀性能

为提高316L不锈钢耐高温液态铅铋的腐蚀能力,通过使用同轴送粉的激光熔覆方式,在316L不锈钢表面制备一层Stellite6合金涂层,将其放入400℃的高温液态铅铋中进行500 h高速流腐蚀试验,其中相对流速设置为2.56 m/s.分析涂层的微观组织、物相组成、元素分布、显微硬度值等的变化规律,以及该涂层耐液态铅铋的腐蚀性能.涂层组织由等轴晶、树枝晶、胞状晶及平面晶组成,搭接区晶粒沿不同方向长大;涂层主要有γ-Co、CoCx、(Cr,Fe)7 C3及M23 C6等物相;各组分元素在涂层表面均匀分布,Co、Cr与Fe等元素在基体316L与涂层之间发生明显扩散;Stellite6涂层的硬度平均值为基体材料316L的2.3倍,且最高达到556.8HV.在进行高温液态铅铋高速流腐蚀后,316L不锈钢表面生成了大面积且连续的氧化物,存在大量微型腐蚀坑,Stellite6涂层表面仅存在少量氧化物,未发现明显的腐蚀坑,较好地维持了原貌;Stellite6涂层表面粗糙度值为1.0μm,而316L经腐蚀后的表面粗糙度为2.4μm.Stellite6合金涂层能够有效地提高316L不锈钢基体在高温液态铅铋合金中的耐腐蚀性能.     

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.