自悬浮定向流法制备Ti纳米颗粒及结构表征

采用自悬浮定向流法制备钛纳米颗粒,并使用透射电镜、X射线衍射和X射线光电子能谱等方法,对钛纳米颗粒的形貌、粒度、结构及性能进行研究。结果表明：钛纳米颗粒呈球形,随着冷却气体Ar流速的增加,平均粒径逐渐减小,在流速为0.6、0.8和1.0 m³/h条件下,分别得到平均粒径为59、50和41 nm的钛纳米颗粒;在空气中,钛纳米颗粒极易氧化生成二氧化钛,同时能够与空气中的N₂和水蒸气发生反应,生成少量的氮化物及羟基基团。     

纳米AlNi金属间化合物的结构及其吸放氢行为

采用自悬浮定向流法制备AlNi纳米微粉。应用TEM、XRD和元素化学分析等检测手段对微粒材料的显微结构、相组成和成分构成进行了表征。结果表明,所制备的纳米颗粒为单相的AlNi,TEM形貌呈较规则的多边形,粒径分布范围为10～40nm。氢吸附实验表明：在3.43MPa氢压下,AlNi纳米微粉在90～100℃时有一释放氢过程,200℃时达到最大吸氢量,约为7.3%。     

单相纳米金属间化合物AINi的制备及其结构特征

采用自悬浮定向流法制备单相金属间化合物AINi的纳米微粉,通过TEM、XRD和元素化学分析等检测手段对微粒材料的显微结构、相组成和成分构成进行研究.所制备的纳米颗粒呈规则球形,粒径分布在10～40 nm之间,样品中的Al、Ni原子比为49:51,颗粒基本由单相AINi组成.实验证实,通过控制气相反应的工艺条件可有效避免单质Al和Ni的生成.     

单相纳米金属间化合物AlNi的制备及其结构特征

采用自悬浮定向流法制备单相金属间化合物AlNi的纳米微粉,通过TEM、XRD和元素化学分析等检测手段对微粒材料的显微结构、相组成和成分构成进行研究。所制备的纳米颗粒呈规则球形,粒径分布在10～40nm之间,样品中的Al、Ni原子比为49∶51,颗粒基本由单相AlNi组成。实验证实,通过控制气相反应的工艺条件可有效避免单质Al和Ni的生成。     

纳米晶Al的快中子辐照效应研究

采用真空热压技术将自悬浮定向流法制得的纳米Al粉压制成平均晶粒尺寸约为120nm的块体,并对其进行了注量为1.9×1012~7.2×1014 cm-2的快中子(E1 MeV)辐照。通过X射线衍射(XRD)分析、扫描电子显微镜与能谱(SEM-EDS)分析和显微硬度测试研究了快中子辐照对纳米晶Al的微观结构和显微硬度的影响。研究结果表明:快中子辐照同时造成了纳米晶Al的平均晶粒尺寸增大和显微硬度提高。随快中子辐照注量的增大,纳米晶Al的平均晶粒尺寸和显微硬度分别增大了2.09%~9.09%和3.54%~4.37%。纳米晶Al的平均晶粒尺寸的增长率随快中子注量的增加而增大。     

磁性纳米微粒的制备方法及其在放射免疫分析中的初步应用

采用化学共沉淀法合成水溶性正癸酸包覆的Fe3O4磁性纳米微粒,并以此为核心物理吸附羊抗兔IgG制备磁性纳米第二抗体,作为磁性分离载体用于放射免疫分析中。用光子相关光谱仪与透射电镜测定了磁性纳米微粒的粒径大小、粒径分布和多分散度等。研究了羊抗兔IgG包被磁性纳米微粒的包被介质的pH、羊抗兔IgG用量和包被时间等制备条件对磁性纳米微粒二抗免疫反应结合能力和非特异结合的影响。结果表明：化学共沉淀法制得的Fe3O4平均粒径约为10-20nm,吸附羊抗兔IgG后其平均粒径为1000nm左右,并可用于放射免疫分析中。提示羊抗兔IgG可通过物理吸附的方法固定在磁性纳米微粒上,其优点是制备方法简便、省时和成本低,在放射免疫分析中具有磁性分离的方便性,具有较大的医学应用价值。     

钴氧化物纳米催化剂的制备及对N2O的分解

用微乳液法制备了表面经硬脂酸（ST）修饰的4种不同价态的钴氧化合物纳米微粒。初步摸索了合成的最佳条件，利用XRD，TEM，IR等测试手段对制备的钴纳米催化剂的物相、粒子的形貌和粒度及钴氧化物纳米微粒与表面活性剂有机基团间的结合方式进行了表征，结果表明制得的纳米微粒呈球状、粒度随热处理温度升高而增大，COO－与Co(Ⅱ，Ⅲ）离子间以化学键相结合。利用流动法固定床反应器研究了钴氧化物纳米催化剂对N2O的催化分解活性，实验结果表明，在350℃焙烧制得的Co2O3纳米粒子对N2O的催化分解有较好的催化活性。     

电子束辐照制备的纳米硫化镉研究

在常温常压下，采用电子束辐照法在水溶液体系中合成了纳米硫化镉粒子。X射线衍射分析表明该产物为面心立方结构晶体的纳米硫化镉；透射电子显微镜分析表明该纳米粒子形貌呈球状颗粒，平均粒径为15nm；其光学性能研究表明，其紫外吸收光谱的吸收边波长为487nm；激发波长为350nm时，纳米粒子的荧光发射波长的峰值为476nm，主要为由带边发射引起的发光。用激光粒度仪研究了表面活性剂聚乙烯醇浓度对辐射制备纳米硫化镉粒径的影响，在一定范围内随着聚乙烯醇浓度的增大，纳米粒子的粒径相应减小。     

聚N-异丙基丙烯酰胺包覆Fe3O4磁导向纳米粒子的制备和表征

选择N-异丙基丙烯酰胺(N-isopropylacrylamide,NIPAM)为单体,N,N′-亚甲基双丙烯酰胺(Methylenebisacrylamide,MBA)为交联剂,用辐射化学方法合成了具有温敏的PNIPAM包覆Fe3O4磁导向纳米粒子。研究了NIPAM单体浓度、交联剂MBA用量、不同光照时间及温度对核壳结构磁性纳米粒子粒径的影响,发现在一定范围内随单体NIPAM浓度的增加、交联剂MBA浓度的减小、光照时间的增加,聚NIPAM包覆Fe3O4核壳结构纳米粒子的粒径增大。在25—39℃温度范围内PNIPAM包覆Fe3O4核壳结构纳米粒子具有最低临界溶解温度特性(Lowercriticalsolutiontemperature,LCST）。以SEM和动态激光光散射仪(PCS)对该核壳结构纳米粒子粒径进行测定,表明辐射化学方法合成的核壳结构纳米粒子比较均匀。     

热压纳米晶铜的硬度性能

采用自悬浮定向流法制备纳米铜粉末,利用不同的工艺参数在真空热压炉中压制成直径一定厚度不同的纳米晶体铜圆柱体。通过XRD、SEM、分析天平、硬度仪等分析测试手段,研究了块体硬度与晶粒大小、密度、晶体结构的关系。结果表明：较薄块体硬度随晶粒长大而降低,两者关系基本符合Hall-Petch经验公式;较厚块体各区域密度差异不明显,受表面缺陷状态及晶粒大小影响,其各处硬度差异较大（1.4～2.2GPa）。     

Dryout Heat Flux for Core Debris Bed, (I)

For gaining basic data on decay heat coolability of debris bed in the post-accident heat removal, measurement of dryout heat flux was made, with stagnant water as coolant, in a 50mm I. D. pyrex glass cylinder vessel. The fuel debris bed subjected to decay heat was simulated by steel ball particles which were inductively heated with a power supply of 20 kHz and 30 kW. The bed was made of homogeneous size particles. An emphasis was placed on the influence of system pressure and particle size. The experiment covered the ranges over the steel ball diameters of 0.3–4.0 mm and the system pressure of 0.02–0.5 MPa.

The experimental results, as a whole, agreed fairly well with the prediction based on Lipinski's 0-D model with respect to the dependence of dryout heat flux both on pressure and on particle size. In detail, however, the dryout heat flux deviates toward a lower value at a higher pressure while to a higher value for a smaller size particle bed. Comparison of the results between the free and fixed beds suggests that the deviation to the higher side will be attributed to the channeling and/or levitation.     

Experimental characterization of the effective particle diameter of a particulate bed packed with multi-diameter spheres

This paper is concerned with uncertainty reduction in coolability analysis of a debris bed formed in fuel-coolant interactions (FCI) during a postulated severe accident of LWRs. A test facility named POMECO-FL was designed and set up to investigate the friction laws of adiabatic single and two-phase flow through particulate beds which have the characteristics of the prototypical debris bed, such as packed with particles of multiple sizes or irregular shapes. The emphasis of the present study is placed on quantification of effective particle diameter of a particulate bed composed of multi-diameter spheres. Pressure drops are measured for water/air flow through the particulate beds packed with various combinations of spheres, and the effective particle diameters of the beds are obtained based on the pressure gradients and the Ergun equation. The results show that at low flowrate (Re < 7) the effective particle diameters can be represented by the area mean diameters of the particles in the beds, while at high velocity (Re > 7) the effective particle diameters are closer to the length mean diameters. If the area mean diameters are chosen as the effective particle diameters, the frictional pressure drops of two-phase flow in the beds can be predicted by the Reed model with good agreements.     

杯式连续沉淀器中草酸亚铁的沉淀工艺

采用着色法研究了杯式连续沉淀器中流场形状与性质，并采用加入颗粒、即时沉淀反应生成颗粒两种方式考察了沉淀颗粒在中心涡流区域的分布与扩散情况。在26 ℃时，采用杯式连续沉淀器研究了料液的加料方式、搅拌速率、表观反应时间等因素对生成的草酸亚铁沉淀颗粒粒径分布和平均粒径、对连续沉淀器和搅拌桨表面颗粒粘结的影响。当草酸料液与硫酸亚铁料液均从杯式连续沉淀器中心涡流区域加入时，可以有效避免沉淀器内壁产生颗粒粘附、结块现象，且所生成的颗粒平均粒径较大，其中生成的粒径为2～5 μm和小于10 μm的颗粒所占比例较小。当搅拌速率在500～800 r/min时，提高搅拌转速不利于生成粒径为2～5 μm和小于10 μm的沉淀颗粒，而草酸亚铁连续沉淀反应的表观反应时间大于30.0 min时，沉淀颗粒的生长速率逐渐变缓。     

同步辐射X射线小角散射法研究纳米ZnO和Fe2O3颗粒在分散介质中的尺寸和形态

为了准确评价纳米材料在生物体系中的作用,首先需要表征纳米材料在生物体系相关条件下的尺寸和团聚状态.本文应用同步辐射X射线小角散射技术测量了纳米ZnO和Fe2O3颗粒在1%羧甲基纤维素钠悬浮液中的粒径和形状,并与透射电镜的结果进行了比较.结果表明纳米颗粒在分散介质会发生聚集,聚集后的粒径大于单颗粒纳米ZnO和Fe2O3的粒径,但ZnO和Fe2O3在介质中的粒径未随着浓度的升高发生显著变化,表明纳米ZnO和Fe2O3颗粒在1%的羧甲基纤维素钠溶液中稳定.     

Growth of Aligned Carbon Nanotubes through Microwave Plasma Chemical Vapor Deposition

Aligned carbon nanotubes (CNTs) were synthesized on glass by microwave plasma chemical vapor deposition (MWPCVD) with a mixture of methane and hydrogen gases at the low temperature of 550~C. The experimental results show that both the self-bias potential and the density of the catalyst particles are responsible for the alignment of CNTs. When the catalyst particle density is high enough, strong interactions among the CNTs can inhibit CNTs from growing randomly and result in parallel alignment.     

杂质与粉末粒度对钛酸锶源芯性能的影响

90Sr放射源是一种能量较强的β放射源,在诸多领域有着广泛的应用。由于钛酸锶陶瓷源芯的性能对90Sr源的安全性和制造工艺难度有着重要的影响,因此需要研究杂质含量和粉末颗粒度对钛酸锶陶瓷源芯力学性能和烧结稳定性的影响规律。采用正交实验方法,将钙、钡、锆杂质含量和粉末粒度作为四个因素,按照正交表L9(3^4)设计对照实验。对不同杂质含量以及不同粉末粒度条件下压制烧结出的钛酸锶源芯的密度、尺寸、抗压强度和硬度进行测试。结果表明,在固定的冷压烧结工艺参数条件下,原料颗粒度和杂质元素锆的含量对钛酸锶陶瓷源芯性能的影响明显,原料最佳粒度为10μm,锆含量必须控制在1%以下,杂质元素钙和钡的影响较小,其含量只需分别控制在2%和4%以内即可。研究结果可为制定钛酸锶原料的纯化制备工艺以及钛酸锶源芯的冷压烧结工艺提供参考。     

包覆工艺对微球形燃料相弥散燃料混合均匀性的影响

针对微球形燃料相颗粒与基体粉末的流动性相差较大、难于混合均匀,建立了一种微球的包覆工艺,并研究了包覆工艺对混合均匀性的影响。采用直径约为100μm的不锈钢微球代替燃料微球,研究结果表明,在微球表面物理包覆一层基体粉末,可增加颗粒表面粗糙度,降低两组元粉末的密度差及颗粒沉降的距离,包覆层还能使颗粒间保持一定的间距,微观上形成连续的基体网络,减少甚至避免发生偏聚,有效地改善了混合均匀性。包覆工艺的最佳参数为:保温温度,76℃;保温时间,6min;黏结剂添加量,1%;粉末粒径,小于25μm。该方法可用于改善(U-Mo)-Al、(U-Mo)-Zr等微球形燃料相弥散燃料的混合均匀性。     

A theoretical model with variable masses for the molten fuel-sodium thermal interaction in a nuclear fast reactor

In the model proposed in this paper, the reaction has been asumed to occur in two successive phases, A and B.

1. Phase A. A given number (function of time) of fuel particles come into intimate contact with a given mass of liquid sodium (function of time). The heat transfer process is characterized by good direct thermal contact between the fuel and the liquid coolant, and by a large contact area due to the small size of the particles. The heat transfer coefficient decreases with time due to the formation of a temperature profile inside the fuel particles. The heated volume of sodium is constrained by the surrounding unheated coolant and by the other materials present in the core. The mechanical constraint is schematized by a sodium column of finite length which is contained in a channel located above the reaction volume. The sudden expansion of the heated volume first produces acoustic waves which travel along the sodium column. Later the sodium column behaves like a piston which is pushed inertially upwards. The pressure rises, reaches a maximum, and then falls as soon as the expansion of the liquid sodium becomes inportant. At the time at which the pressure reaches the saturation point, sodium boiling starts and phase B begins.

2. Phase B. The heat transfer process is now characterized by a very large contact area, and by thermal contact between the fuel and coolant which becomes increasingly worse with time, due to the formation of a sodium vapour layer at the external surface of the fuel fragments. The sodium will boil in a large quantity, and will therefore produce large volume changes. The sodium piston will be further accelerated and its movement will allow the pressure in the reaction volume to decrease.

The model accounts for the time history of the temperatures of each fuel particle by means of the use of specially averaged temperature values. The calculation of the heat transfer coefficient during phase B is based on experimental results. The presence of fission gases can also be taken into account. A size distribution of fuel particles has also been incorporated into the model as well as the effect of friction due to the channel walls and that of the pressure losses at the outlet of the channel. Numerical evaluations are also included and the results are discussed. It has been concluded that the total work produced decreases with the time scale of the vapour film layer around the particles and increases with the speed at which the fuel breaks down into fragments and mixes with the liquid sodium. The effect of sodium column length has also been investigated.     

Nb元素和Fe元素对锆合金耐腐蚀性能的影响

将几种成分不同的锆合金样品放入高压釜中,在350℃、16.8MPa、70μg/gLi+LiOH水溶液中腐蚀。结果显示:第二相几乎全是Zr-Nb-Fe粒子的3#样品耐腐蚀性能最好,而不含Zr-Nb-Fe粒子的1#和5#样品耐腐蚀性能很差,这说明Zr-Nb-Fe第二相粒子对改善锆合金耐腐蚀性能起着关键作用。只有合金中Nb元素和Fe元素配比合理,才可使合金中第二相主要是Zr-Nb-Fe粒子。     

还原温度对Pt/PTFE/泡沫SiC规整疏水催化剂性能的影响

为研究还原温度对Pt/PTFE/泡沫SiC规整疏水催化剂性能的影响,以200、225、250、275、300℃为还原温度,氯铂酸-乙醇溶液为浸渍溶液,采用浸渍-气相还原法制备Pt/PTFE/泡沫SiC规整疏水催化剂。利用接触角测试仪分析还原温度对催化剂疏水性能的影响,利用X射线衍射(XRD)、X射线光电子能谱(XPS)、透射电镜(TEM)等表征手段分析所得催化剂的结构与组成,并研究其氢-水液相催化交换(LPCE)性能。结果表明:还原温度的变化对催化剂疏水性能没有影响;还原温度200、225℃时催化剂中Pt粒子团聚现象严重,Pt粒子粒径大,分散性差;还原温度250、275、300℃时催化剂中Pt粒子粒径分散性较好;还原温度275℃时催化剂中Pt粒子粒径较窄,平均粒径最小,为6.2nm。Pt存在Pt(0)、Pt(Ⅱ)和Pt(Ⅳ)三种价态,还原温度275℃下催化剂中0价Pt所占比例高达72.50%,还原程度高。LPCE催化交换性能也表明,还原温度275℃时催化剂柱效率最高。揭示275℃是所选取还原温度中的最佳还原温度。