化学计量及其进展

扼要介绍了化学计量主要研究内容和量传方法。并从化学计量技术机构,基准、标准装置,标准物质,检定规程和化学计量学等方面,叙述了化学计量的进展概况。     

N,N-二甲基甲酰胺中电沉积制备镁镍储氢合金

采用恒电位沉积法, 选用适宜的添加剂和络合剂, 成功地从N,N-二甲基甲酰胺(DMF)中沉积出致密的黑色Mg-Ni储氢合金膜. 并初步探讨了其共沉积机理. XRD显示沉积层中含有非晶态Mg-Ni相和微晶态Mg相. SEM图及相应能谱图分析表明合金颗粒以团聚状态存在, 合金成分不是很均匀. AAS分析表明沉积合金中Mg的原子摩尔分数达27.3%. LAND电池测试系统测得所镀合金膜的放电比容量最高为172.4 mAh/g.     

2A12-T6铝合金表面双-(γ-三乙氧基硅丙基)四硫化物薄膜的特性

采用傅立叶变换红外光谱分析了2A12-T6铝合金表面自组装双-(!-三乙氧基硅丙基)四硫化物硅烷偶联剂(SCA)薄膜结构特征,并采用电化学极化曲线评价了薄膜的耐蚀性能.结果表明,铝材表面自然晾干,SCA薄膜分子之间主要通过氢键连接,腐蚀电流密度减小1个数量级以上.120℃的加热处理促进铝板表面通过SiOSi链接而形成SCA网状薄膜结构,并通过在界面上形成SiOAl界面相结构而与铝板表面牢固连接,腐蚀电流密度降低2个数量级以上.SCA乙醇溶液浸泡处理10min比浸泡2s～1min的铝板表面SCA薄膜内氢键缔合羟基要多.     

混合稀土对共晶Al-2%Fe合金组织形态的影响

研究了富La混合稀土对共晶Al-2?合金组织形态的影响. 当混合稀土加入量较少时, 合金中的α-Al相为明显的胞状枝晶;随着混合稀土加入量的增加, α-Al枝晶优先形核生长得到抑制, 共晶Al3Fe相得到细化;当稀土加入量增至0.6% (质量分数)共晶Al3Fe相尺寸逐渐增大. 并对混合稀土对共晶Al-2?合金组织形态的影响机制进行了探讨.     

氢化物发生石墨炉原位富集直接测定高温镍基合金中碲

通过选择碲的氢化物发生条件，克服了高含量镍对碲的干扰，把氢化物富集在涂钯石墨管里，然后再原子化，成功地测定了高温镍基合金中碲。     

Segregation of Sn in the binary CuSn and ternary CuSnSb alloy systems

Progression studies have been followed from Cu(111)‐ and Cu(100)Sn binaries to Cu(111)‐ and Cu(100)SnSb ternary‐alloy systems under the same experimental conditions. The segregation behaviour of Sn in the two orientations are explained. It is found that the kinetic segregation profiles of Sn in the ternary alloys shift to lower temperatures as compared to that in the binary. The Sn profile shift is mainly due to the decrease in the activation energy of Sn in the ternary systems. For a particular Cu orientation, the other segregation parameters that the Sn profiles depend on, like the pre‐exponential factor, segregation energy and the interaction coefficient, are found to be the same in the two systems. There is also a change in the equilibrium segregation profiles of Sn. In the ternary system, site competition between Sn and Sb causes the Sn to suffer exponential desegregation and eventual displacement from the surface. Copyright © 2006 John Wiley & Sons, Ltd.     

New mixed tellurides of nickel and Group 13–14 metals Ni<Subscript>3−δ</Subscript>MTe<Subscript>2</Subscript> (M = Sn,In, Ga)

Three new mixed tellurides of nickel and group 13–14 metals Ni_3−δMTe₂ (M = Sn, In, Ga) were prepared by high-temperature ampoule synthesis and studied by powder X-ray diffraction analysis. The compound Ni_3−δSnTe₂ was also studied by single crystal X-ray diffraction analysis. The structural model of this phase and two analogs was described as consisting of layers with nickel-main group metal bonds confined from the above by tellurium atoms. The van der Waals gap formed through contacts between the tellurium atoms of neighboring layers is partially occupied by nickel atoms. Published in Russian in Izvestiya Akademii Nauk. Seriya Khimicheskaya, No. 10, pp. 1879–1881, October, 2007.     

电化学合成镍配合物的研究

采用金属镍为“牺牲”阳极，首次在无隔膜电解槽中，电化学溶解金属镍一步 制备了纳米NiO前驱体Ni(Oet)2,Ni(Obu)2,Ni(Oet)2(acac)2，Ni(Obu)2(acac)2 [acac为乙酰丙酮基].产物通过红外光谱（FT-IR）、拉曼光谱（Raman spectrum） 进行表征。同时讨论了影响电合成镍醇盐及其配合物的关键因素。实验表明，防止 阳极钝化，温度控制在30-40℃，采用有机胺溴化物为导电盐，可以提高电合成效 率。     

Die Kristallstruktur von Na2NiAlF7—ein Beitrag zum Problem der wahren Raumgruppe orthorhombischer Weberite

The Crystal Structure of Na₂NiAlF₇ — a Contribution to the Problem of the True Space Group of Orthorhombic Weberites The X-ray single crystal structure determination of the orthorhombic weberite Na₂NiAlF₇ (a = 707.4(2), b = 1003.8(2), c = 731.5(1) pm; Z = 4) was performed in space group Imma, after all reflections hk0 with h(k) = 2n + 1 could be eliminated, as they proved simulated by Renninger effect and/or λ/2 reflections. The alternative space groups Imm2 resp. I2₁2₁2₁ of former weberite structure determinations thus became obsolete. The refinement using 880 independent reflections ended at wR = 0.0232. The resulting average distances within the framework of octahedra are Ni? F = 197.3, Al? F = 180.4 pm.