Synthesis, structure and physical properties of Ru ferrites: BaMRu5O11 (M=Li and Cu) and BaM′2Ru4O11 (M′=Mn, Fe and Co)

The synthesis, structure, and physical properties of five R-type Ru ferrites with chemical formula BaMRu₅O₁₁ (M=Li and Cu) and BaM′₂Ru₄O₁₁ (M′=Mn, Fe and Co) are reported. All the ferrites crystallize in space group P6₃/mmc and consist of layers of edge sharing octahedra interconnected by pairs of face sharing octahedra and isolated trigonal bipyramids. For M=Li and Cu, the ferrites are paramagnetic metals with the M atoms found on the trigonal bipyramid sites exclusively. For M′=Mn, Fe and Co, the ferrites are soft ferromagnetic metals. For M′=Mn, the Mn atoms are mixed randomly with Ru atoms on different sites. The magnetic structure for BaMn₂Ru₄O₁₁ is reported.     

氧化锰团簇粒子在有序多孔氧化锆孔道中的组装及其特殊性能研究

利用醇溶液浸渍法及后续的热处理工艺成功实现了氧化锰团簇粒子在有序多孔氧化锆孔道中的组装，借助XRD，TEM，UV-vis，EPR以及O~2-TPD等分析手段进行样品结构表征及性能分析。研究表明，氧化锰团簇粒子能比较均匀地分散于规则的孔道中；团簇粒子的生长随着热处理温度的提高受到孔道大小的限制；孔道中的氧化锰团簇粒子能显示出与较大尺寸氧化锰粒子完全不同的强顺磁信号，并且还具有优异的表面氧吸附特性。     

2-巯基苯并咪唑保护的铜纳米团簇的制备及银离子检测

以2-巯基苯并咪唑为保护剂,聚乙烯吡咯烷酮为稳定剂,水合肼为还原剂,“一锅法”合成2-巯基苯并咪唑保护的,高稳定性、强荧光、大斯托克斯位移的铜纳米团簇(Cu NCs),并用于检测水样中的银离子含量。采用透射电子显微镜(TEM)和X射线光电子能谱(XPS)对铜纳米团簇的结构进行表征,通过荧光光谱和紫外可见光谱对其光学性能进行研究。研究表明:该铜纳米团簇的最大激发和发射波长分别为340和558 nm,在日光灯和紫外灯下分别为无色和橙色。Cu NCs具有较高的分散性,尺寸大小为2~3 nm。在最佳反应条件下,铜纳米团簇可以选择性地被银离子猝灭,且灵敏度高,线性范围为1~40μmol/L,检测限为0.5μmol/L。该方法用于检测实际水样(自来水、湖水)中银离子的浓度,结果令人满意,表明在环境监测中有非常高的应用价值。     

Thermal behavior of short-range-order in quenched Cu-12 at% Mn assessed by DSC

Summary The ordering behavior of quenched Cu-12 at% Mn was investigated by differential scanning calorimetry (DSC) under increasing temperature conditions. The ordering process can be better explained in terms of a homogeneous short-range-order (SRO) rather than a disperse-short-range-order (DSRO) model as for concentrated Cu-γMn solid solutions. At the employed high quench rates ordering is established in one stage here termed stage 1, assisted by excess vacancies. This stage obeys a first order kinetics law, being the effective activation energy consistent with a weighed average sum of the activation energy for migration of free and bound vacancies. An estimated solute-vacancy binding energy of 15 kJ mol^-1 seems quite reasonable for this alloy together with the assessed activation energy for complex migration of 92.6 kJ mol^-1. By adopting a first SRO order parameter based in quasi-chemical theory in pair approximation and using boundary values calculated from displayed features of DSC traces, the retained degree of quenched-in order at room temperature was calculated. This procedure also enabled to estimate an ordering energy of -2.7 kJ mol^-1. The effect of quenching temperature demonstrate that for smaller vacancy sink densities, the retained degree of order at room temperature goes through a minimum.     

PbO~2纳米粉体的固相合成及其对MnO~2电极材料的改性作用

利用固相氧化反应制备了PbO~2纳米粉体样品，借助XRD，TEM以及循环伏安测试对其性质进行了表征。同时，对反应条件的选择进行了讨论。将所得样品用于改性MnO~2电极，恒流放电测试结果表明，样品掺杂量在1.25%～5.00%间对MnO~2有良好的改性效果，可使改性MnO~2的放电容量得到极大提高。循环伏安测试结果表明，铅的掺入改变了MnO~2的放电机理。在循环扫描过程中，掺杂物与MnO~2均不再以单纯氧化物的形式存在，而是形成了一系列Pb(X)(X=0,Ⅱ)Mn(Y)(Y=Ⅳ，Ⅲ，Ⅱ)复合物的共氧化与共还原，抑制了电化学惰性物质Mn~3O~4的生成和积累，从而有望改善MnO~2的可充性能。纳米PbO~2与常粒径PbO~2与常粒径PbO~2(标记为S)对MnO~2的改性机理类似。但前者对MnO~2的改性效果明显优于后者，当恒流放电至-1.0V时，其放电容量较S样改性MnO~2的放电容量平均高出约30%。     

Improvement of direct determination of Cu and Mn in seawater by GFAAS and total elimination of the saline matrix with the use of hydrofluoric acid

Hydrofluoric acid, added to seawater, can assist in the removal of chloride in the drying step by precipitating fluoride salts, thus suppressing the chloride interference effects induced on the atomization signals of Cu and Mn. By adding HF to seawater before the analysis, MgF₂ and CaF₂ are precipitated at the bottom of the sampling flask, without precipitating Cu and Mn, and are consequently not introduced into the graphite furnace. Because sodium salts are eliminated at the pretreatment step, the whole seawater matrix is eliminated before the atomization of Cu or Mn. Therefore, the analyzed volume of seawater can be increased by using the multi-injection procedure without degradation of the limit of detection and risks of spectral interferences. The limit of detection obtained for Cu and Mn are 0.05 and 0.01 μg L⁻¹, respectively, for a 50 μL analyzed seawater volume.     

DNA为模板的铂纳米团簇沉积

Platinum nanoclusters were deposited along the supercoiled DNA strands after incubation of cis-(trans-1R，2R-diaminocyclohexane)(dl-camphorato)platinum(Ⅱ) (Cdp)， an analogue of the anti-tumor drug-carboplatin， with DNA and K₂PtCl₄ for 600 min and then through reduction of dimethylaminoborane (DMAB). The decrease of absorption of DNA at 260 nm indicates the coordination of Cdp and DNA. TEM and AFM were employed to characterize the morphologies and structures of platinum nanoclusters.     

STUDY OF Cu-Mu CATALYST FOR THE SYNTHESIS OF METHYL FORMATE AND METHANOL FROM SYNTHESIS GAS

将一种新型的ＣｕＭｎ催化剂用于由合成气合成甲酸甲酯和甲醇，该催化剂表现出良好的反应活性和甲酸甲酯选择性。考察了反应温度、合成气压力及催化剂制备方法等对合成甲酸甲酯和甲醇的反应活性及选择性的影响。在反应条件下，产物收率最高达６０．１０ｇ／（Ｌ·ｈ），产物甲酸甲酯的选择性很高。用ＢＥＴ、ＸＲＤ及ＸＰＳＡｕｇｅｒ等测试方法对催化剂的比表面、晶相组成以及铜、锰在催化剂中的价态进行了表征，并探讨了催化剂失活的原因。     

X-射线荧光光谱法测定钛铁中的硅、锰、磷、铝

介绍用X-射线荧光光谱仪测定钛铁中Si、Mn、P、Al含量的方法,通过试验确定了合适的研磨时间、压力和保压时间,用压片法制样,建立了各元素的工作曲线,各元素的测定范围分别为Si3.00%～6.00%,Mn1.00%～3.00%,P0.030%～0.070%,Al5.00%～9.00%。通过强度测量得到测定Si、Mn、P、Al的相对标准偏差分别为0.074%、0.308%、0.383%、0.040%,精密度满足测试要求。将该方法测定结果与化学法比对,准确度满足国家标准方法分析误差的要求。     

Study of short-lived silver isotopes with a laser ion source

The continuum part of the⁶Li (a,a)⁶Li (1.47–2.47 MeV) scattering data at E_a=50 MeV are extracted in two discretized bins. Coupled-channel calculations are carried out coupling the 1⁺ ground state of⁶Li with both the resonant, 3⁺ ₁ state, and two non-resonant continuum states. The discretized continuum of the⁶Li (p,p)⁶Li (1.75–3.25 MeV) scattering data at E_p=65 MeV are also analysed on the same footing. In both the cases the effect of coupling is found to be minimal.