多弧离子镀制备的耐事故燃料包壳铬涂层晶粒结构研究

本文通过从几十微米到几埃的多尺度表征展示了多弧离子镀制备铬涂层的详细结构.经XRD, SEM, FIB, TEM和HRTEM表征，结果显示该涂层是一种多重结构，包括表面上的微米级颗粒、缺陷带钉扎的微米或次微米级液滴、以堆垛层错为晶界的柱状晶、以刃位错和螺型位错为区分的微晶、位错末端的原子畸变以及原子排列无序化的区域.这些结构通过改变涂层的结晶度，影响了晶格常数、表面粗化和FIB溅射裂纹.此外，通过分析HTEM照片，确定了这些堆垛层错和位错的类型.最后，讨论了沉积参数对这些晶粒结构的影响.     

硅凝胶体系中碳酸钙晶体生长实验

为了得到不同晶型的碳酸钙晶体，采用凝胶法生长出了碳酸钙的三种同质异象体：方解石、文石、球霰石．讨论了反应物浓度和杂质离子（Na^＋）对碳酸钙晶体生长的影响．结果表明：通过改变反应物浓度和利用不同的反应物可以生长出不同晶型的碳酸钙晶体．同时，利用原子力显微镜对生长的方解石晶体表面的形貌观察发现：晶体生长是以台阶簇（大台阶）的方式推进，不同高度的堆垛层错呈现在表面上．     

原位合成增强体TiB层错的透射电镜分析

利用透射电镜和高分辨率透射电镜研究了原位合成钛基复合材料增强体TiB的堆垛层错结构。结果表明，堆垛层错容易在TiB的（100）面上形成，平行于TiB的生长方向[010]，并贯穿整个增强体。堆垛层错在TiB形核与长大的过程中形成，并且与增强体TiB的B27晶体结构有关。由于TiB的B27结构，在（100）面上容易形成B原子的不足而导致原子错排，并且在（100）面上形成堆垛层错有利于减少增强体与基体合金间的晶格畸变。     

Influence of stacking fault energy on formation of long period stacking ordered structures in Mg–Zn–Y–Zr alloys

The influence of alloying elements on the stacking fault energy (SFE) of Mg–Y–Zn–Zr alloys was calculated by using first-principles, and the microstructure of as-cast Mg-1.05Y-0.79Zn-0.07Zr (mole fraction, %) alloy prepared by conventional casting was investigated by SEM, TEM and HRTEM. The block-like long period stacking ordered (LPSO) phase, the lamellar LPSO phase and stacking faults were observed simultaneously and the lamellar LPSO structure and stacking faults were both formed on (0001)_α-Mg habit plane and grown or extended along [01i0]_α-Mg direction. The calculation results by the first-principles showed that the addition of Y can sharply decrease the stacking fault energy of the Mg–Zn–Y–Zr alloy, while Zn slightly increases the stacking fault energy of the alloy. The influence of stacking fault energy on the formation of LPSO was discussed. It shows that LPSO may nucleate directly through stacking faults and the lower stacking fault energy was in favor of formation of LPSO.     

疏水冷面霜晶生长的有限扩散凝聚模型

为了深入了解霜晶的动态生长过程,以有限扩散凝聚模型为基础建立了疏水冷面霜晶二维生长模型.通过在表面上设置不同冰珠数量来模拟冷面不同疏水性能,无涂层金属表面则布满冰珠;采用粒子在网格节点上随机移动来描述水蒸气分子的运动,粒子沿各方向移动的概率相同.数值结果表明,霜晶动态生长的可视化结果与实验图像在形态上保持一致;树枝状霜晶具有分形特征,相应的分形维数为1.44～1.78,与实验值相近.疏水冷面霜晶生长缓慢且分布稀疏;采用疏水效果不好的冷面的结霜情况与金属表面相似.     

吸水性涂层在霜层生长初期的抑霜

研究吸水性涂层对霜层生长过程的影响,以寻求抑制结霜的有效方法.通过自行设计的试验设备对吸水性涂层表面上霜层生长特性进行试验研究,获取了不同时段霜层的显微图片,采用数字图像处理方法对其分析,与无涂层的铜表面进行对比.结果表明,吸水性涂层使得结霜时间推迟,霜层高度下降,冰晶体分布稀疏.此外霜层生长初期冰晶体的结构发生了变化,晶体呈倒立状,在某个时段内持续这种状态.对列固含率的分析表明,吸水性涂层的表面在初期有些位置冰晶体含量较高,但有些位置则接近于零,这样的霜层在生长初期甚至加强了热传递.最后通过对比不同表面霜层高度随时间的变化规律发现:吸水性涂层在初期抑霜效果最好,随着时间的推移其抑霜能力逐渐下降.     

TEM observation of oxidation of CuZnAlMnNi shape memory alloy

The atmospheric oxidation of a quenched CuZnAlMnNi alloy after ion-polishing was examined by transmission electron microscopy (TEM). It was found that a lot of oxide grains with various sizes yield homogeneously on the surface of the alloy after exposure at room temperature for 90 d. The grains mainly form along the planes of stacking fault, meanwhile, they can also be observed at the stacking fault tetrahedrals or around the dislocation lines. The formation of the oxides gives rise to the reduction of the stacking faults, and even complete disappearance in some zones, which is partly responsible for the decrement of shape memory effect (SME) of the alloy quenched during long-term holding at room temperature.     

新型金纳米薄片的制备与生长研究

在表面活性剂PVP的辅助下,利用高温溶剂热法,合成了星形、盾形和多边形等新型Au纳米薄片.对其结构分析表明,Au纳米薄片均为单晶,边长为数微米,厚度约40 nm.这些新型的Au纳米片的形成可以理解为(111)面沿着〈211〉和其他高指数面的生长.不同晶面表面能的理论模拟可以很好解释(111)晶面沿高指数方向生长的可能性.利用堆垛层错引导晶体生长可以很好地解释选区电子衍射中的分数衍射及晶面间距.     

铝合金表面有色钛/锆转化膜的成膜机理及性能

为了解决工业生产中钛/锆转化膜无色的问题,通过向含钛/锆的处理液中加入单宁酸及成膜促进剂,在铝合金表面制备了有色钛/锆转化膜.采用X射线能谱仪、扫描电镜、傅里叶变换红外光谱仪、X射线衍射仪、X射线光电子能谱仪和电化学工作站对转化膜的形成过程、形貌、组织结构、耐蚀性等进行了分析.结果表明:在铝合金表面成功制备出了金黄色、耐蚀性优异的转化膜,其主要成分是Na3AlF6,其次是单宁酸水解产物的金属络合物以及少量Al2O3.3H2O、TiO2等;膜的形成可分为Na3AlF6晶体成核、生长和金属络合物的沉积3个阶段;转化膜的腐蚀电流密度由基体的5.894μA/cm2下降到0.283μA/cm2,耐蚀性明显提高.     

高应变率拉伸下纳米空洞的成核与早期生长

利用分子动力学方法研究了单晶铜中纳米空洞的成核与早期生长过程.研究结果表明：高应变率拉伸作用下,在缺陷原子或空位密集区首先启动（111）-[211],（111）-[211],（111）-[211],（111）-[211]4个滑移系的位错.空洞在特定滑移系层错交叠,即（111）-[211]和（111）-[211]滑移系的层错交叠以及（111）-[211]和（111）-[211]滑移系的层错交叠形成的空穴串处成核.这些空穴串分别沿[011]和[011]方向,与加载方向垂直.相对于其他的滑移系交叠,这种滑移系交叠形成的空穴串的截面积最大.此后,空洞通过发射位错长大,形状类似长条形;伴随其他类型位错的生长,空洞逐渐演化为柱形-椭球形-类球形.对于含双空洞的单晶铜体系,受已存空洞周围应力分布的影响,多个滑移体系同时启动,空洞在3个滑移系的层错交汇点的空穴处成核,其形状受交汇处位错线运动方向的影响,类似扁三角形,并在位错的滑移和攀移作用下逐渐演化为类球形.我们根据畸变场计算了3个层错面交叠处的空穴体积,发现108个不同交叠构型中,只有4种构型的交叠引起的空穴体积最大,空洞成核容易,其他情况不能使空洞成核.     

马来二睛基二硫烯过渡金属配合物分子间的弱相互作用

制备并用元素分析、红外光谱表征了两种马来二睛基二硫烯过渡金属配合物。通过测定配合物的单晶结构 ,研究了两种配合物中阳离子间的 π… π或 N O2 … π相互作用。     

Preparing Ca-P coating on biodegradable magnesium alloy by hydrothermal method: In vitro degradation behavior

Magnesium alloys are potentially attractive biodegradable materials.However,their rapid corrosion rate limits their biomedical application.To slow down the rate of biodegradation,a protective calcium-phosphate coating was formed on a magnesium alloy substrate by a hydrothermal method.Scanning electron microscope results showed that the coating consisted of two layers with different crystalline characteristics.The loose outer layer showed a prism-like crystal structure,while the compact inner layer is a dense ultra-fine regular di-pyramid-like structure with an average grain dimension of ～200 nm.The compositions of the inner layer and outer layer were calcium-deficient hydroxyapatite (Ca-def HA) and dicalcium phosphate (DCPa),respectively.The coating adhered well to the substrate with a thickness of about 15 m.Immersion in Hank’s solution indicated that the coating could significantly improve the degradation properties of magnesium alloy.The pH of the solution containing the coated samples increased much more slowly than the untreated control.After 8 d immersion,the uncoated sample had corroded seriously while the coated sample was much less corroded.The Ca/P atom ratio in both the layers of the coating increased and the coating was still protecting the substrate.The two layers of the coating corroded differently because of differences in solubility.The outer layer was more severely attacked and many holes were formed on the surface,the inner layer suffered less attack.In addition,a growth of precipitate on the inner layer was observed,indicating that surface bioactivity was improved by the coating.Thus,magnesium alloys coated with a Ca-P coating prepared by a hydrothermal method are promising candidate biodegradable biomaterials,and further investigation of in vivo degradation behavior is suggested.     

Hydrothermal synthesis of hydroxyapatite coating on the surface of medical magnesium alloy and its corrosion resistance

The early corrosion control of biomedical magnesium alloy is an important measure to determine its good performance during implantation into human body. The deposition of calcium phosphate biological coating is the most effective solution at present. In this paper, hydroxyapatite (HAP) coating was hydrothermal synthesized on the surface of AZ31B magnesium alloy, and the influence mechanism of hydrothermal synthesis temperature, time and solution concentration was investigated. The synthesis conditions and deposition mechanism of hydroxyapatite coating without DCPA (CaHPO₄) were proposed. The surface morphology of the coating was observed by field emission electron scanning microscope (FESEM). The types and contents of microelements in the material were analyzed by energy disperse spectroscopy (EDS). Fourier transform infrared spectroscopy (FTIR) was used to analyze the functional group information of the coating surface. The corrosion resistance of different experimental groups was studied by electrochemical test. The results showed that when the calcium phosphate solution concentration was 0.1 ?mol/L and the calcium/phosphorus ratio was 1.67, the coating had better morphology structure and corrosion resistance, and the calcium/phosphorus ratio of HAP crystals reached 1.58, the epit of the prepared AZ31B-HAP coating by bare metal increased from ?1.51 ?V to ?1.18 ?V, the impedance value reached 1.0 ?× ?10⁵ ?Ω?cm², and the early corrosion of magnesium alloy substrate was effectively delayed.     

异型纳米AlOOH微观晶体结构

利用RTO金属包埋切片微米--纳米表征法,通过高分辨透射电镜观察了γ--AlOOH薄膜切片中的晶格点阵条纹像,分析了添加复合添加剂后异型纳米AlOOH的微观晶体结构,从原子层面揭示了由于铁离子的同晶替代以及硫酸根离子的插层而导致的晶格畸变.阐述了极性添加剂在晶须生长过程中首先形成复合的高聚体、进而定向生长的诱导机理,并指出了非极性表面活性剂对异型纳米AlOOH晶体形貌表面的修复和"美容"作用.用能谱及红外光谱佐证了复合多聚体的存在.     

氧化铈对玻璃涂层与金属基体密着性的影响

利用冲击试验、热震试验和扫描电镜等方法研究了添加氧化铈对玻璃涂层与金属基体密着性的影响规律。试验结果表明 ,加入氧化铈可以改善玻璃涂层与金属基体的密着性 ,提高涂层的抗冲击和抗热震性能。氧化铈含量在 1%～ 5 %内 ,氧化铈加入量越多 ,瓷层的抗冲击和抗热震性能越好。由于氧化铈的存在能加剧瓷层与金属基体的界面反应 ,从而在界面上形成了更多的Ni Fe键和铁的枝晶体。Ni Fe键能提高瓷层的弹性 ,铁的枝晶体能增强瓷层与基体的连接作用。界面反应使界面上的孔洞消失 ,形成明显的密着层 ,因而提高了界面的结合强度。     

PM Al—Li合金高应变速率超塑变形过程中的孔洞行为

用扫描电子显微镜及拉伸试验研究了PMAl—Li合金高应变速率超塑变形过程中孔洞的形核、长大及其影响因素．结果表明，孔洞主要在三角晶界和晶界突起处形核，其长大由周围的塑性变形控制，随应变速率的提高，孔洞的形核率和长大速率增加；随变形温度的升高，孔洞的长大速率增加，材料对孔洞容纳性提高．     

EB-PVD制备ZrO2涂层的微观组织结构研究

采用电子束物理气相沉积法在不锈钢基体上制备了氧化钇部分稳定氧化锆陶瓷涂层。利用XRD、XPS、SEM、AFM对涂层的相结构、化学成分、表面形貌进行了实验分析。结果表明,氧化锆涂层为四方相氧化锆,并不同程度存在织构现象。随着基体温度的升高,涂层中的晶粒尺寸在逐渐长大。涂层表面的小颗粒为柱状晶的上表面,涂层表面的粗糙度随着靶基距的升高而变小。涂层表面Zr-O结合态为Zr4+,而涂层内部存在少量的缺氧现象。     

β′—Sialon陶瓷的晶体生长机制

本文从分析试验现象入手,探索了β′-Sialon陶瓷的晶体生长机制。分析结果表明,β′-Sialon陶瓷的晶体生长速度由界面反应速度控制,晶粒的表面形态由界面能控制。     

Evolutionary mechanism of b-oriented TS-1 film on porous α-Al2O3 supported chitosan surface in hydrothermal reactions

The acid-base titration, atomic force microscopy (AFM), contact angle technique, energy dispersive X-ray (EDX) and electron probe microanalysis (EPMA) were performed to check the existence of the gel-layer on the chitosan surface after it was dipped in aqueous TPAOH solution as well as in TS-1 synthesis solution. The evolution of TS-1 monolayer and multi-layered film on the chitosan surface was studied using SEM imaging at different stages during hydrothermal reactions. Experimental evidence for the formation mechanism of supported zeolite films and membranes revealed that a gel-layer enriched with TPA cations and TS-1 precursors was first formed on the chitosan surface, followed by the nucleation within the gel-layer especially on the chitosan surface. The nuclei formed on the chitosan surface were further transformed into crystalline particles and TS-1 crystal grains. The nuclei beyond the chitosan surface subsequently grew up, leading to the formation of multi-layered TS-1 film with preferential b-orientation. The result is significant for engineering the microstructure of supported zeolite films and membranes in hydrothermal reactions.     

Study on growth of coarse grains of diamond with high quality under HPHT

The growth of coarse grains of diamond was observed with graphite as carbon source and Fe₈₀Ni₂₀ alloy powder as catalyst at HPHT in a China-type SPD 6×1670T cubic high-pressure apparatus with highly exact control system. To synthesize coarse grains of diamond crystal with high quality, advanced indirect heat assembly, powder catalyst technology and catalyst with optimal granularity were used. Especially the nucleation of diamond and the growth rate were strictly controlled by the optimized synthesis craft. At last, diamond crystals (about 0.85 mm) in the perfect hex-octahedron shape were successfully synthesized at ~5.4 GPa and ~1360℃ in 60 min. The characteristic of crystal growth with powder catalyst technology under HPHT was discussed. The results and techniques might be useful for production of coarse grains of diamond.