氢化物发生-原子荧光光谱法测定铜精矿中的砷、锑和铋

建立了氢化物发生-原子荧光光谱法同时测定铜精矿中砷、锑、铋的方法,采用了主量元素匹配法来消除基体干扰,优化了反应体系的酸度、还原剂浓度等条件进行了优化。砷、锑、铋的浓度在1—200μg·L~(-1)范围内与荧光强度呈线性关系。方法回收率为92%—101%,相对标准偏差为2.7%—5.5%。     

金矿石中高含量锑的断续流动氢化物发生-原子荧光光谱法快速测定

采用王水（1＋1）水浴分解样品,氢化物发生-原子荧光光谱法（HG-AFS）测定金矿石中高含量的锑.其方法回收率在95.0%-102.0%之间,相对标准偏差在1.0%-3.4%之间,方法检出限为3.0×10-10g/mL,经试验证实该方法可测范围宽、简便、快速、准确,实验室间对比分析结果吻合程度令人满意.     

Phase composition and phase transformation in Bi(Sb,Nb,Ta)O4 system

In this work Bi(Sb_xNb_yTa_z)O₄ (x + y + z = 1) samples are prepared using mixed-oxide method. A pseudo-ternary phase diagram of Bi(Sb,Nb,Ta)O₄ system is given below the melting point. It is composed of a monoclinic phase region, an orthorhombic phase region and a monoclinic–orthorhombic co-existing phase region. In the orthorhombic phase region, the transformation from orthorhombic to triclinic phase is found to be sensitive to the composition and sintering temperature. Both the transformation from monoclinic to orthorhombic structure and the transformation from orthorhombic to triclinic structure have been studied by the cell parameters.     

Improved thermoelectric performance in p-type Bi_(0.48)Sb_(1.52)Te_3 bulk material by adding MnSb_2Se_4

Bismuth telluride(Bi_2Te_3) based alloys, such as p-type Bi_(0.5)Sb_(1.5)Te_3, have been leading candidates for near room temperature thermoelectric applications. In this study, Bi_(0.48)Sb_(1.52)Te_3 bulk materials with MnSb_2Se_4 were prepared using high-energy ball milling and spark plasma sintering(SPS) process. The addition of MnSb_2Se_4 to Bi_(0.48)Sb_(1.52)Te_3 increased the hole concentration while slightly decreasing the Seebeck coefficient, thus optimising the electrical transport properties of the bulk material. In addition, the second phases of MnSb_2Se_4 and Bi_(0.48)Sb_(1.52)Te_3 were observed in the Bi_(0.48)Sb_(1.52)Te_3 matrix. The nanoparticles in the semi-coherent second phase of MnSb_2Se_4 behaved as scattering centres for phonons,yielding a reduction in the lattice thermal conductivity. Substantial enhancement of the figure of merit, ZT, has been achieved for Bi_(0.48)Sb_(1.52)Te_3 by adding an Mn_(0.8)Cu_(0.2)Sb_2Se_4(2mol%) sample, for a wide range of temperatures, with a peak value of 1.43 at 375 K, corresponding to ~40% improvement over its Bi_(0.48)Sb_(1.52)Te_3 counterpart. Such enhancement of the thermoelectric(TE) performance of p-type Bi_2Te_3 based materials is believed to be advantageous for practical applications.     

Determination of the surface states from the ultrafast electronic states in a thermoelectric material

We reveal the electronic structure in Yb Cd₂Sb₂,a thermoelectric material,by angle-resolved photoemission spectroscopy(ARPES)and time-resolved ARPES(tr ARPES).Specifically,three bulk bands at the vicinity of the Fermi level are evidenced near the Brillouin zone center,consistent with the density functional theory(DFT)calculation.It is interesting that the spin-unpolarized bulk bands respond unexpectedly to right-and left-handed circularly polarized probe.In addition,a hole band of surface states,which is not sensitive to the polarization of the probe beam and is not expected from the DFT calculation,is identified.We find that the non-equilibrium quasiparticle recovery rate is much smaller in the surface states than that of the bulk states.Our results demonstrate that the surface states can be distinguished from the bulk ones from a view of time scale in the nonequilibrium physics.     

Robustness of the unidirectional stripe order in the kagome superconductor CsV3Sb5

V-based kagome materials AV₃Sb₅ (A=K, Rb, Cs) have attracted much attention due to their novel properties such as unconventional superconductivity, giant anomalous Hall effect, charge density wave (CDW) and pair density wave. Except for the 2a₀×2a₀ CDW (charge density wave with in-plane 2×2 superlattice modulation) in AV₃Sb₅, an additional 1×4 (4a₀) unidirectional stripe order has been observed at the Sb surface of RbV₃Sb₅ and CsV₃Sb₅. However, the stability and electronic nature of the 4a₀ stripe order remain controversial and unclear. Here, by using low-temperature scanning tunneling microscopy/spectroscopy (STM/S), we systematically study the 4a₀ stripe order on the Sb-terminated surface of CsV₃Sb₅. We find that the 4a₀ stripe order is visible in a large energy range. The STM images with positive and negative bias show contrast inversion, which is the hallmark for the Peierls-type CDW. In addition, below the critical temperature about 60 K, the 4a₀ stripe order keeps unaffected against the topmost Cs atoms, point defects, step edges and magnetic field up to 8 T. Our results provide experimental evidences on the existence of unidirectional CDW in CsV₃Sb₅.     

电合成2,2-二羟甲基丙酸

制备Ti/SnO2+Sb2O4/PbO2电极,电极的组分及其价态由XRD和XPS表征;该电极可将2,2-二羟甲基丙醛直接电合成2,2-二羟甲基丙酸.应用高效液相色谱分析原料和产物,电化学方法研究电合成影响因素,包括:2,2-二羟甲基丙醛浓度、溶液pH值、反应温度和氧化电位等.在优化条件下(pH=1,C醛=0.10 mol.L-1,t=15℃,E=1.8 V)电合成2,2-二羟甲基丙酸的转化率为58%,选择性36%,电流效率28%.本法为该产物的合成提供了一种新的途径.     

In situ FTIRS studies of kinetics of HCOOH oxidation on Pt(110) electrode modified with antimony adatoms

The electrochemical behavior of irreversibly adsorbed antimony on a Pt(110) electrode (Pt(110)/Sb) with various coverages was studied using cyclic voltammetry. The kinetics of HCOOH oxidation via reactive intermediates on Pt(110)/Sb were investigated quantitatively by employing the potential step technique and in situ FTIR spectroscopy. The results demonstrated that Sb adatoms were stable on Pt(110) when the electrode potential was below 0.45 V (SCE). It has been revealed that the dissociative adsorption of formic acid can be inhibited by the presence of Sb_ad on the Pt(110) surface. The electrocatalytic effects of Sb_ad towards HCOOH oxidation consist in a negative shift of the oxidation potential (about 350 mV) and the enhancement of the oxidation current. Based on the data processing method of integration transform developed in our previous papers, the kinetics of HCOOH oxidation on Pt(110)/Sb electrodes of different θ_Sb have been investigated quantitatively, and both the rate constant k_f and the transfer coefficient β were determined and reported.     

Sb在Pt(100),Pt(110),Pt(111)及Pt(320)上不可逆吸附的电化学特性

研究了Sb在Pt(1 0 0 ) ,Pt(1 1 0 ) ,Pt(1 1 1 )和Pt(32 0 )单晶面上不可逆吸附的电化学特性 .发现当扫描电位的上限Eu≤ 0 .45V时 ,Sbad可以稳定地吸附在Pt(1 0 0 ) ,Pt(1 1 0 )和Pt(1 1 1 )表面 ,而Sbad在Pt(32 0 )表面稳定的电位较低 ,为Eu≤ 0 .40V .从饱和吸附Sb的铂单晶电极出发 ,通过改变电位扫描上限Eu 和电位扫描圈数可以获得不同Sb覆盖度 (θSb)的电极 .根据Sb和H在铂单晶电极表面共吸附的定量数据 ,对Sb在不同铂单晶面上饱和吸附的模型进行了初步探讨 .     

密闭高温高压溶样ICP-MS测定24个国际地质标样中的Sb和Bi

研究了ICP-MS分析中Bi,Sb,Te和As产生的记忆效应,其记忆效应Bi>Sb>Te>As。在低浓度硝酸介质中(0.01%～1%),贮存样品的聚丙烯瓶和ICP-MS的进样管道会对Bi元素产生严重的吸附作用。0.1%氢氟酸的清洗效果优于6%的硝酸,而6%的硝酸的清洗效果要优于0.1%高氯酸。在给定的仪器操作条件下,Sb和Bi的检出限分别为0.001和0.000 1 ng·mL-1。采用该清洗方法,结合密闭高温高压溶样,测定了24个国际地质标样中的Bi和Sb。大部分标样的测定结果与已有参考值吻合较好。文章还给出了国际标样AGV-2(安山岩)、BHVO-2(玄武岩)和BCR-2(玄武岩)中Bi和Sb的测定值。