高温原位XAFS研究NiB纳米非晶态合金催化剂的结构

原位XAFS方法研究NiB纳米非晶态合金在78K至573K温度范围的结构特点。结果表明：在78K时，NiB样品的第一配位峰的位置和强度分别为2．06A、396．4，其强度只有Ni箔第一配位峰强度的25％左右；300K时，第一配位峰的位置和强度分别2．08A、255．9；573K时，第一配位峰的位置和强度分别为1．87A、155．4。温度从78K升至300K，第一配位峰的位置变化不大，但峰强度降低35％左右：温度继续升至573K时，峰的位置较78K的向小的方向移动0．20A，并且强度降低了60％。这表明随着测量温度的升高，NiB纳米非晶态合金中Ni原子周围的热无序度显增加。     

高温原位XAFS研究NiB纳米非晶态合金催化剂的结构

原位XAFS方法研究NiB纳米非晶态合金在78K至573K温度范围的结构特点。结果表明：在78K时,NiB样品的第一配位峰的位置和强度分别为2．06A、396.4,其强度只有Ni箔第一配位峰强度的25％左右;300K时,第一配位峰的位置和强度分别2．08A、255．9;573K时,第一配位峰的位置和强度分别为1．87A、155．4。温度从78K升至300K,第一配位峰的位置变化不大,但峰强度降低35％左右;温度继续升至573K时,冷的位置较78K的向小的方向移动0．20A,并且强度降低了60％。这表明随着测量温度的升高,NiB纳米非晶态合金中Ni原子周围的热无序度显增加。     

高温原位XAFS研究熔态Sb的局域结构

利用高温原位XAFS技术研究了半金属Sb在固态和熔态时的局域结构特点。结果表明在893K高温时固态Sb的局域结构与常温(298K)时晶态Sb的相似,但其热无序度较大。随着温度再升高20K到熔化后的913K时,熔态Sb的主配位峰形状有较大变化,其强度仅为熔化前的70％左右。这一结果表明熔化导致Sb的结构无序显著增加,我们认为这是熔态Sb中Sb原子的第一近邻配位的大部分共价键断裂造成的。模型无关的Reverse Monte Carlo方法拟合计算结果也表明熔化引起Sb样品的第一近邻配位数由固态的6增加到熔态的9。当温度升高至1058K时,Sb样品的Sb原子的径向结构函数曲线的形状与913K的Sb样品的相似,说明在熔化后的100至200K的温度范围,熔态Sb中Sb原子的局域结构差别不大。     

Fe3O4纳米颗粒的制备和原位高压XRD研究

使用部分还原－共沉淀方法制备了平均粒径为3－11nm的球形Fe3O4纳米颗粒,以16：4：1的甲醇－乙醇－水混合溶液作为传压介质和均分散介质,利用金刚石对顶砧装置（DAC）研究了球形Fe3O4纳米颗粒的原位常温高压（0－31．8GPa)XRD谱和纳米颗粒的压致晶格结构变化。     

水溶液体系中光化学可控合成核壳结构磁性纳米凝胶

通过光化学方法合成并经进一步的Hoffmann降解获得了壳层带有伯胺基核壳结构磁性纳米凝胶,该磁性纳米凝胶粒径分布窄且粒径可控。由于磁性纳米凝胶的壳层水凝胶具有很好的亲水性和生物相容性,且反应过程中不加入任何表面活性剂,为该磁性纳米凝胶的生物应用奠定了良好的基础。通过光化学方法合成窄粒径分布且粒径可控的磁性纳米凝胶就我们认识而言尚未见到文献报道,有望为磁性纳米凝胶的合成提供一种新的方法。我们对合成的磁性纳米凝胶分别用傅立叶变换红外光谱（FTIR）、光子相关光谱（PCS）、原子力显微镜（AFM）和透射电子显微镜（TEM）进行了表征。     

核径迹-银纳米颗粒改性的CR-39材料制备及其抗红外反射性能

本工作用中国原子能科学研究院HI-13串列加速器提供的³²S离子辐照CR-39样品,产生潜径迹,用紫外灯敏化后在氢氧化钠溶液中蚀刻,使潜径迹成为具有一定孔径的孔（洞）。用真空充氩气的方法在核径迹孔样品表面镀银纳米颗粒。电子扫描电镜图片显示,氩气压强在50～100Pa之间时,银纳米颗粒直径约为60～100nm,纳米颗粒形成球状团簇的大小为3μm。在红外光区（2.5～25μm）测量镀膜样品的反射率,测量结果表明,CR-39表面的核径迹与银纳米颗粒能将红外光区（8.0～25μm）的反射率降低到0.9%,与未经改性的CR-39比较,减低了82%。在5.8和7.8μm处,CR-39的本底反射率分别从9.0%和130%降低到了5.0%和6.8%。     

光聚合一步可控合成表面氨化的核壳型超顺磁性纳米凝胶及其表征

用部分还原共沉淀结合离心分离合成超顺磁性Fe3O4纳米粒子,以其为核,N-（2-氨乙基）甲基丙烯酰胺盐酸盐N-（2-Aminoethyl）methacrylamide,AEM·HCI）为单体,N,N＇-亚甲基双丙烯酰胺（MSA）为交联剂,采用光聚合原位一步合成粒径可控的表面氨化的超顺磁性核壳型Fe3O4纳米凝胶。探索了单体、交联剂量及光照时间对纳米凝胶粒径的影响,并用动态光散射仪（DLS）、TEM、FTIR、TGA、UV、多功能磁测量仪等表征了纳米凝胶的粒径、粒径分布、形貌、结构、磁响应性及稳定性。结果表明：改变单体、交联剂量及光照时间可得到不同粒径、粒径分布均匀的超顺磁性纳米凝胶;与Fe3O4纳米粒子相比,纳米凝胶的磁饱和强度略有降低,但其高的Zeta电位使其稳定性大大提高。     

聚乙烯醇修饰Fe3O4纳米颗粒的制备表征及同步辐射X射线光电子能谱研究

采用水溶性高分子聚合物聚乙烯醇(PVA)对Fe3O4纳米颗粒表面进行功能化修饰,利用透射电镜(TEM)、紫外可见吸收光谱(UV-vis)、Zeta电位检测、电感耦合等离子体质谱(ICP-MS)和热重分析(TGA),对包被前后Fe3O4的粒径、分散稳定性、PVA的包覆效率及纳米颗粒进入细胞的量进行了表征研究.通过同步辐射...     

国产快堆包壳材料CW316(Ti)SS高温强度下降的微观机理分析

冷加工316(Ti)不锈钢CW 316(Ti)SS是我国首选的快堆包壳材料,国产材料的常规力学性能与国外数据相当,但高温蠕变和高温持久强度数据却较低.本项研究主要是通过观察、比较国产快堆包壳材料和俄罗斯快堆包壳材料在高温下微观结构的变化情况,并结合对国产材料高温持久断裂试验样品的断口形貌观察结果,分析得出:国产材料长时高温力学性能下降的主要原因是沿晶界的σ相析出.     

基于同步辐射原位拉伸XRD研究熔盐浸渗的核石墨IG-110微观结构演化

钍基熔盐堆(Thorium Molten Salt Reactor,TMSR)是第四代核反应堆的代表之一,其特点是以熔融氟盐作为冷却剂和燃料的载体。在熔盐堆中,熔盐容易浸渗到核石墨内部,引发核石墨局部高温,造成核石墨损伤程度增加,严重破坏核石墨的结构,从而影响核石墨材料的宏观性能和使用寿命。然而,熔盐浸渗对核石墨力学性能的微观机制以及熔盐浸渗引起的微结构损伤或破坏机制目前仍不清晰,因此有待进一步研究原位环境下(如力学加载、高温等)熔盐浸渗对核石墨微结构的影响,并揭示微结构演化的相关机制。本文基于同步辐射原位拉伸X射线衍射技术(Two Dimensional X-ray Diffraction,2D-XRD),开展了外部载荷为0 N、15 N、21 N、27 N和32 N时熔盐浸渗后的核石墨IG-110在拉伸断裂过程中的微观结构演化研究,以揭示外部载荷条件下的核石墨IG-110与熔盐之间的原位实时相互作用及材料断裂的微观机制。实验结果表明:在拉伸断裂过程中外部载荷使熔盐浸渗后的核石墨IG-110的结晶性变差、层间距变大,同时FLiNaK盐的结晶性也明显变差。这一发现将有助于解释熔盐浸渗后核石墨IG-110力学性能的变化,理解核石墨IG-110与FLiNaK熔盐间的相互作用机理,有利于高性能核石墨的制备和TMSR的安全可靠运行分析。     

基于固体探测器SDD的XAFS数据获取系统

X射线吸收精细结构谱学(X-ray Absorption Fine Structure,XAFS)的发展,提出了对低浓度(痕量)元素研究的需求,高灵敏度的固体探测器纷纷被应用到XAFS技术中来。硅漂移探测器(Silicon Drift Detector,SDD)是一种高计数率、高能量分辨率、采用半导体制冷的小型荧光探测器,其商业产品渐趋成熟。北京同步辐射装置1W2B实验站装备了这种小型SDD,并开发了相应采谱软件供用户使用。经过对含Cu 100 mg·L~(-1)浓度的CuSO_4溶液的测试,结果证明这套新的采谱系统可以满足1W2B实验站XAFS实验荧光模式的需求。     

北京同步辐射1W1B XAFS的实验控制和QXAFS的实现

1W1B的实验控制系统包括准直镜、单色器和聚焦镜的电动控制,光闸和束流位置监测器的控制,前狭缝和出口狭缝的电动控制,以及Labview开发的实验采谱软件等.利用新的实验控制系统可方便地进行光束线上各光学元件的姿态调整、束流监控、设置实验条件和采谱,为用户提供方便的实验环境.在1W1B X射线吸收精细结构谱(XAFS)实验站上除了可实现常规的透射、荧光和电子产额XAFS实验外,还发展了快速XAFS实验方法(QXAFS),可在2 min左右的时间里采集到信噪比较好的XAFS谱;随着采谱效率的进一步提高,可望在一些原位反应和对时间分辨要求较高的实验中得到应用.     

国家同步辐射实验室原子分子物理光束线气体滤波器的研制、安装和调试

为有效消除波荡器产生的高次谐波的影响,并维持光束线及储存环超高真空环境,根据原子分子物理光束线实际情况,采用二级差分抽气系统及大抽速的差分泵设计了气体滤波器系统.调试结果表明,在滤波气氩气压强Par<1.333×103 Pa时,光束线真空度维持在<4.933×10-7Pa,高次谐波滤波率>99.975%,满足了实验要求.     

基于LabVIEW的高能量分辨谱仪数据采集系统

在上海光源BL14W1线站,成功搭建一套基于Lab VIEW的高能量分辨谱仪运动控制和数据采集系统,该光谱仪系统可以实现高能量分辨荧光探测X射线吸收谱(High Energy Resolution Fluorescence Detected X-ray Absorption Spectroscopy,HERFD-XAS)、X射线发射谱(X-ray Emission Spectroscopy,XES)和共振X射线发射谱(Resonant X-ray Emission Spectroscopy,RXES)等主要实验功能,分辨率达到亚电子伏。硬件系统采用上海光源统一的VME运动控制硬件系统和硅漂移固体探测器;软件系统采用Lab VIEW编写用户操作界面,利用DSC(Data logging and Supervisory Control Module)模块实现与运动控制使用的实验与物理工业控制系统(Experimental and Physics Industrial Control System,EPICS)系统的数据交换。利用基于该运动控制和数据采集系统的光谱仪,开展了Mn化合物和Th O2锕系化合物的实验。结果表明,该系统可以满足高能量分辨率实验的需求。     

真空高温氢化法制备Pd-Zr复合膜

为了获得低成本、高渗氢率、长寿命、高强度的选择渗氢膜,耐熔金属锆(Zr)被选作复合膜的基体。在真空 4.0×10-4 Pa、温度 650 ℃的反应条件下,锆表面氧化 膜 松动 、分解 ,氧化膜被去除 ;再在氢气氛中使其洁净表面上生成一层氢化锆 保 护 膜 ; 在真空度为 6.6×10-6 Pa 下,采用离子溅射镀膜法,在锆片(φ 50 mm×0.23 mm)的双表面上分别镀上了一层厚约 400 nm 的钯(Pd)薄膜,钯膜均 、细 腻 、光洁 , 膜厚易控制 ;再经过退火处理 ,制得了 Pd-Zr复合膜, 膜面致密 , 钯膜与基体锆结合力强 ,内应力消失 。采用 X 射线衍射(XRD)和 X 光电子能谱(XPS)对锆表面及复合膜表面进行了分析。制备的 Pd-Zr 选择渗氢复合膜对核燃料和聚变燃料的纯化及反应堆增殖剂中氚的提取将具有很大的应用前景。     

Synthesis and characterization of SnO2 nanoparticles embedded in silica by ion implantation

Tin dioxide nanoparticles embedded in silica matrix were fabricated by ion implantation combined with thermal oxidation. Silica substrate was implanted with a 150 keV Sn⁺ ions beam with a fluence of 1.0 × 10¹⁷ ions/cm². The sample was annealed for 1 h in a conventional furnace at a temperature of 800 °C under flowing O₂ gas. According to the structural characterization performed by X-ray diffraction and transmission electron microscopy techniques, metallic tetragonal tin nanoparticles with a volume average size of 12.8 nm were formed in the as-implanted sample. The annealing in oxidizing atmosphere promotes the total oxidation of the tin nanoparticles into tin dioxide nanoparticles with a preferential migration toward the surface of the matrix, where large and coalesced nanoparticles were observed, and a small diffusion toward the bulk, where smaller nanoparticles were found.     

Current status and future development of coated fuel particles for high temperature gas-cooled reactors

The coated particles were first invented by Roy Huddle in Harwell 1957. Through five decades of development, the German UO₂ coated particle and US LEU UCO coated particle represent the highly successful coated particle designs up to now. In this paper, current status as well as the failure mechanisms of coated particle so far is reviewed and discussed. The challenges associated with high temperatures for coated particles applied in future VHTR are evaluated. And future development prospects of advanced coated particle suited for higher temperatures are presented. According to the past coated fuel particle development experience, it is unwise to make multiple simultaneous changes in the coated particle design. Two advanced designs which are modifications of standard German UO₂ coated particle (UO₂^∗ herein) and US UCO coated particle (TRIZO) are promising and feasible under the world-wide cooperations and efforts.     

Design of the material performance test apparatus for high temperature gas-cooled reactor

Most materials can be easily corroded or ineffective in carbonaceous atmospheres at high temperatures in the reactor core of the high temperature gas-cooled reactor （HTGR）. To solve the problem, a material performance test apparatus was built to provide reliable materials and technical support for relevant experiments of the HTGR. The apparatus uses a center high-purity graphite heater and surrounding thermal insulating layers made of carbon fiber felt to form a strong carbon reducing atmosphere inside the apparatus. Specially designed tungsten rhenium thermocouples which can endure high temperatures in carbonaceous atmospheres are used to control the temperature field. A typical experimental process was analyzed in the paper, which lasted 76 hours including seven stages. Experimental results showed the test apparatus could completely simulate the carbon reduction atmosphere and high temperature environment the same as that confronted in the real reactor and the performance of screened materials had been successfully tested and verified. Test temperature in the apparatus could be elevated up to 1600℃, which covered the whole temperature range of the normal operation and accident condition of HTGR and could fully meet the test reauirements of materials used in the reactor.     

Small-sized high temperature reactor (MHR-50) for electricity generation: Plant concept and characteristics

A new concept of Small-sized high temperature reactor (MHR-50) has been investigated toward the earliest commercialization in near future. Features of the MHR-50 are further different from the conventional light water reactors, and the MHR-50 is characterized by high passive safety, high thermal efficiency and smooth operability. When we selected plant basic parameters, we considered minimization of construction unit cost including R&D and of plant construction period as important issues. In the present study, the plant concept of the MHR-50 has been developed based on the above design philosophy.     

Development of high temperature gas-cooled reactor (HTGR) fuel in Japan

This paper describes experiences and present status of research and development works for the high temperature gas-cooled reactor (HTGR) fuel in Japan. Recently, Very High Temperature Reactor (VHTR) is evaluated highly worldwide, and is a principal candidate for the Generation IV reactor systems. In Japan, HTGR fuel fabrication technologies have been developed through the High Temperature Engineering Test Reactor (HTTR) project in Japan Atomic Energy Agency since 1960’s. In total about 2 tons of uranium of the HTTR fuel has been fabricated successfully and its excellent quality has been confirmed through the long-term high temperature operation. Based on the HTTR fuel technologies, SiC TRISO fuel has been newly developed for burnup extension targeted VHTR. For ZrC-TRISO coated fuel as an advanced fuel designs, R&Ds for fabrication and inspection have been carried out in JAEA. The irradiation with the Japanese uniform stoichiometric ZrC coating has been completed in the cooperation with Oak Ridge National Laboratory of the United States.