标准加入法测定锆铀合金中微量铪

应用标准加入ICP-AES测定锆铀合金中微量铪.当试样中锆的浓度为8mg/mL时,铪的测定范围是50-400μg/g,回收率为101%-106%,相对标准偏差(RSD,n=6)为3.7%-5.8%.     

双离子束溅射沉积HfO­­2光学薄膜的研究

用双离子束溅射沉积氧化铪光学薄膜,并对此工艺下制备的氧化铪薄膜进行了光学性质、残余应力、结构特性以及激光损伤特性的研究。实验结果表明,用双离子束溅射沉积的氧化铪薄膜不仅结构均匀,膜层致密,无定形结构,而且具有极低的散射和吸收,均匀的非晶结构,杂质缺陷少,激光损伤阈值高。     

用改进的重叠分辨率优化法于薄层色谱分离二茂铪化合物

在薄层色谱中分离一系列二茂铪化合物，首先利用黄金分割优选法优化二元展开剂体系，然后按优化结果把二元展开剂混合成四元溶剂体系，共用重叠分辨率法确定四元展开剂体系的最佳组成，分离结果令人满意，同时，本文还对等溶剂强度条件和不等溶剂强度条件下的优化结果做了比较和讨论。     

ICP—AES法测定高温合金中铌,钽,锆,铪——溶样及光谱干扰的进一步探讨

本文在原工作的基础上，继续探讨ＩＣＰ－ＡＥＳ法测定高温合金中Ｎｂ，Ｔａ，Ｚｒ和Ｈｆ能溶样与光谱干扰问题，通过试验研究表明，上述问题的解决在合金样品分析中具有实际意义。     

Ionization of Hafnium L—Shell by Electron Impact

A lower-energy electron beam has been directed on to a hafnium thin target with thick backing to investigate the process of L-shell ionization.By using a Si(Li) detector to count the x-rays from the L-subshell,the partial and total production cross sections and mean ionization cross sections versus electron energies have been deduced simultaneously (from threshold to 36keV),The influence of the electron reflected from the backing on measurements has been corrected.The path of the electron multi-scattered in the target itself has also been calculated by using the Monte Carlo programme(EGS4).A comparison with both theoretical predictions is given.     

Theoretical prediction of ion conductivity in solid state HfO2

A theoretical prediction of ion conductivity for solid state HfO2 is carried out in analogy to ZrO2 based on the density functional calculation. Geometric and electronic structures of pure bulks exhibit similarity for the two materials. Negative formation enthalpy and negative vacancy formation energy are found for YSH (yttria-stabilized hafnia) and YSZ (yttria- stabilized zirconia), suggesting the stability of both materials. Low activation energies (below 0.7 eV) of diffusion are found in both materials, and YSH’s is a little higher than that of YSZ. In addition, for both HfO2 and ZrO2 , the supercells with native oxygen vacancies are also studied. The so-called defect states are observed in the supercells with neutral and +1 charge native vacancy but not in the +2 charge one. It can give an explanation to the relatively lower activation energies of yttria-doped oxides and +2 charge vacancy supercells. A brief discussion is presented to explain the different YSH ion conductivities in the experiment and obtained by us, and we attribute this to the different ion vibrations at different temperatures.     

激光剥蚀-电感耦合等离子体质谱法测定高纯铪中10种杂质元素

高纯铪由于具有独特的理化性质,在核反应堆、等离子切割机、光学元件等方面有着重要的应用。高纯铪中杂质的种类和含量会影响高纯铪的物理化学性能,应用中对高纯铪纯度的要求也越来越高,这就对高纯铪的分析检测技术提出了更高的要求。激光剥蚀-电感耦合等离子体质谱法（LA-ICP-MS）是激光剥蚀进样技术与电感耦合等离子体质谱联用,可以直接分析固体样品,并且方法前处理简单,可以避免样品前处理过程中引入杂质,是一项高效、快速、精密的分析技术,在环境、地质、冶金、燃料能源、材料、生物医药、考古等领域广泛应用。所以,激光剥蚀-电感耦合等离子体质谱法（LA-ICP-MS）是高纯金属杂质元素最佳检测方法之一。还未见有应用LA-ICP-MS于高纯铪样品的报道。用LA-ICP-MS对高纯铪中10种杂质元素（Al,Sc,Ti,Fe,Ni,Cu,Mo,Ag,Sn,W）进行定量分析。为了降低激光剥蚀过程中元素的分馏效应,提高信号灵敏度和稳定度,对激光剥蚀参数进行优化实验。确定了激光剥蚀的最优仪器参数为：氦气流量600 mL·min-1,激光能量90%,剥蚀孔径150 μm,激光扫描速度60 μm·s-1,激光脉冲频率20 Hz。经实验优化后的ICP-MS仪器工作参数为：RF功率1 450 W,射频匹配电压1.8 V,载气流量0.85 L·min-1,冷却器流量0.85 L·min-1,采样深度7.5 mm。在最优参数条件下,利用内控标样建立工作曲线,各杂质元素标准曲线的线性相关系数为0.993 6～0.999 8。采集载气空白的信号强度,平行测定11次,以3倍空白信号的标准偏差所对应的含量作为元素的检出限,得到各元素的检出限为0.001~0.08 μg·g-1。将高纯铪制成尺寸合适的样品,用硝酸洗去样品表面的氧化物,将其装入剥蚀池中,运用线扫描剥蚀方式,在最佳仪器工作条件下,对三个高纯铪样品中的10种杂质元素进行定量分析。实验结果显示,杂质元素含量为0.17～36.76 μg·g-1,相对标准偏差为1.4%～20%,精密度良好。以184W为例,将LA-ICP-MS法和ICP-MS法的测定结果进行t检验,三个样品的t值分别为2.14,1.64和2.11,均小于显著性水平为0.05时的临界值（t_{0.05, 12}=2.18）,说明LA-ICP-MS法和ICP-MS法的测定结果在置信度为95%时没有显著性差异,即正确度良好。所以,该方法正确度和精密度良好,可用于高纯铪中杂质的定量分析。