中国液态锂铅包层材料研究进展

液态锂铅包层是国际上普遍关注和最有发展潜力的聚变堆包层概念设计之一,而包层材料是液态锂铅包层的核心问题之一.目前,液态锂铅包层普遍选用低活化铁素体/马氏体钢(RAFM钢)作为结构材料,液态锂铅作为中子倍增剂及氚增殖剂.另外,部分设计采用了耐高温、电绝缘流道插件作为功能材料,以降低磁流体动力学效应及提高冷却剂出口温度(高于700℃).为适应液态包层的发展需求,中国科学院等离子体物理研究所FDS团队联合国内外相关研究单位,进行了具有中国自主知识产权的中国低活化马氏体钢(CLAM钢)及液态锂铅包层功能材料研发,并开展了锂铅热对流及强迫对流回路的设计、研制及腐蚀实验研究,以研究液态金属锂铅的流动特性及其与结构和功能材料的相容性.同时建立了聚变堆材料数据库平台,为促进中国聚变堆液态包层及材料技术的研究和发展提供数据支持.     

Transmission electron microscopic observations of the decomposition process of lithium alanate

The thermal decomposition process of lithium alanate (LiAlH₄) was investigated by TEM, TG-DTA and XRD. It was shown that LiAlH₄ decomposes through a two-step reaction: a liquid-to-solid phase transition in the first step of the decomposition and a solid-to-solid reaction in the second step of the decomposition, both steps accompanied by hydrogen release. The particle size of the aluminum (Al), which formed in the first decomposition step, was much larger than that in the second decomposition step. In addition, Al particles formed in the liquid phase of LiAlH₄ in the first decomposition step, while, they form in solid phase of Li₃AlH₆ in the second decomposition step, resulting in the kinetics of the first decomposition step being faster than that of the second decomposition step. The investigation clearly demonstrated the reaction model of the decomposition of LiAlH₄ in the nano-scale, showing different diffusion processes of Al in each of the decomposition steps.     

Variable temperature neutron diffraction studies of single crystals of LiND2

We have synthesized a single crystal of lithium amide (LiNH₂, LiND₂) by melting method, and performed neutron diffraction of the single crystal at variable temperature. LiND₂ is tetragonal structure and I-4 space group. Lattice parameters and unit cell volume of LiND₂ at room temperature, 50 °C, 100 °C, 150 °C and 200 °C were determined. Both of the lattice parameters and the unit cell volume increase with increase of temperature. From these results, we have estimated coefficient of volumetric thermal expansion α_V of LiND₂ to be 222 × 10⁻⁶/K. With increase of temperature, all thermal ellipsoids gradually expand because of thermal vibration.     

注氘低活化马氏体钢在电子辐照下的缺陷行为

低活化铁素体/马氏体(RAFM)钢被视为国际热核聚变反应堆以及聚变反应堆的第1壁候选结构材料之一,很多国家均在研究不同的RAFM钢,中国低活化马氏体(CLAM)钢的研究亦正在进行。核聚变会产生氢、氦、氘及氚,这些气体元素与辐照缺陷结合在一起,对材料的辐照性能会产生较大影响。本文对注氘后不同温度下的辐照后微观结构进行研究。试验利用日本北海道大学的JEOL-1300高压电子显微镜研究注氘CLAM钢从室温到873K在1250keV电子辐照下的微观结构变化。研究结果表明,在电子辐照下,注氘产生的缺陷团会出现消失和长大两种现象,意味着间隙型与空位型位错环在注氘过程中同时产生。并研究了注氘产生的空洞。     

Microstructure and hydrogen desorption characteristics of hydrogenated ScH2–MBn (M = Mg and Ca) systems synthesized by mechanical milling

The mixtures of scandium hydride ScH₂ and metal boride MB_n, which is MgB₂ or CaB₆, were hydrogenated by mechanical milling under hydrogen pressure at room temperature. ScH₂–MgB₂ and ScH₂–CaB₆ desorbed 3.4 and 2.3 mass% of H₂, respectively, with peaks below 300 °C. The results of synchrotron radiation X-ray powder diffraction and X-ray absorption spectroscopy at the Sc K-edge indicated that ScB₂ was produced by milling. Fourier-transform infrared spectroscopy suggested that hydrogen was stored as B–H bonds in the as-milled samples. Nuclear magnetic resonance spectroscopy clarified the presence of metal borohydrides M(BH₄)₂ (M = Mg and Ca) in the as-milled ScH₂–MB_n mixtures. These results indicate that M(BH₄)₂ is synthesized by milling the ScH₂–MB_n mixtures under hydrogen pressure at room temperature, and hydrogen was desorbed from M(BH₄)₂. The by-products of M(BH₄)₂ are MgH₂ in the M = Mg case, which was observed by transmission electron microscopy, and ScB₂ in both cases.     

硅对低活化马氏体钢电子辐照行为的影响

利用超高压透射电子显微镜研究了两种成分的低活化马氏体钢(CLAM钢)的辐照损伤行为。结果表明：电子辐照能在未添加硅的CLAM钢中产生辐照空洞;在450℃下辐照至14dpa时,空洞数密度约为8.7×10²¹m^－3,辐照肿胀率约为0.26％;在450℃下的辐照肿胀率明显比500℃下的高;当损伤率为2×10^－3dpa/s时,添加合金元素硅能显著提高CLAM钢的抗辐照肿胀能力,未在添加硅的CLAM钢中实验观察到辐照空洞的形成。在450℃下进行辐照时,添加硅的CLAM钢出现明显的辐照共格析出现象。     

Effect of Deuterium Ion Implantation on Microstructures of Fe-M （M=V,W, Ta） Alloys

To study the effect of tungsten, vanadium and tantalum on the microstructures in CLAM (China Low Activation Martensitic) steel after irradiation respectively, the microstructures of Fe-M (M= V ,W, Ta) model alloys were investigated after implanted deuterium ions using an ion accelerator at 773 K. After implanted deuterium ion, TEM (Transmission Electron Microscope) observation and EDX (Energy Dispersive X-ray Spectrom) analysis have been carried out. The result showed that tiny voids were observed in all model alloys after implanted the same dose of deuterium ions. The swelling rate in FeTa alloy was the smallest among the three alloys. Unlike FeW and FeV alloys, there was the segregation in FeTa alloy under a fluence of 5×1017 D + /cm2 at 773 K. A theoretical analysis showed that the void growth in FeTa alloy slowed down due to tantalum segregation near voids. It indicates that tantalum plays an important role in the improved irradiation resistance of CLAM steel.     

Plastic bag method for active sample loading into transmission electron microscope

A plastic bag method was developed to observe air-sensitive samples on microstructure and phase distribution without exposure to air during the holder transfer process into the transmission electron microscope (TEM). As an example, a type of lithium aluminum hydride (Li(3)AlH(6)) was observed in the TEM to demonstrate the effectiveness of this method. Results show that the plastic bag method is a simple and practical TEM transfer method utilized to reduce air contact for a series of air-sensitive materials.     

中国低活化马氏体钢在电子辐照下产生位错环的原位观察

高流强的中子辐照在结构材料内部产生严重的级联离位损伤,使得材料性能下降,而辐照缺陷是聚变堆材料性能下降的根本原因.为了研究结构材料在高辐照剂量下的损伤机理,针对中国低活化马氏体钢(CLAM钢),通过使用高能电子辐照来模拟中子对材料造成的高剂量辐照损伤,并对微观结构进行原位观察.进行了辐照下产生的位错环随辐照剂量的演化过程的观察,并分析了位错环浓度和尺寸随辐照剂量和温度的变化规律.