硬X射线磁圆二色实验方法的建立

在北京同步辐射装置(BSRF)1W1B光束线和XAFS实验站上国内首次建立了硬X射线波段的磁圆二色实验(XMCD)方法. 以单晶金刚石作为相位延迟片, 在透射劳埃(Laue)模式下, 利用衍射双折射效应, 将入射的单色线偏振光转变为相应的左旋和右旋圆偏振光, 测量磁化样品对左旋和右旋圆偏振光吸收的差异, 获得了XMCD信号. 本实验使用透射方法测量了Pt-Fe合金Pt L_2,3边的XMCD, 获得了XMCD信号. XMCD实验方法的建立, 为研究磁性材料尤其是磁性薄膜材料的电子结构和磁结构提供了实验基础.     

Modification of the surface state of rough substrates by two different varnishes and influence on the reflected light

Modification of the visual appearance when a rough surface is covered by a varnish is mostly attributed to the levelling of the substrate surface, which depends on the molecular weight of the varnish. The topography of varnished surfaces, however, has never been measured directly. Surfaces of varnishes applied over glass substrates of varying roughness were studied, therefore, using mechanical profilometry. Two different varnishes made with a low and a high molecular weight resin were studied. Both varnishes lower the r.m.s. roughness of the substrates and filter the high spatial frequencies. These results are amplified for the varnish containing the low molecular weight resin. The light reflected by the varnished samples is modelled from these topographical data. Its angular distribution, calculated from the probability density of slopes is presented, taking into account separately the air/varnish and the varnish/substrate interfaces. These analyses are presented in a back-scattering configuration. They show that varnishing significantly reduces the angular width of the reflected light and that this effect is magnified for the low molecular weight resin. Modelling furthermore shows that the influence of the roughness of the varnish/substrate interface is negligible in the total reflected light.     

Formation and hydrogenation of p(2 × 2)-N on Pt(1 1 1)

The formation of a well-ordered p(2 × 2) overlayer of atomic nitrogen on the Pt(1 1 1) surface and its reaction with hydrogen were characterized with reflection absorption infrared spectroscopy (RAIRS), temperature programmed desorption (TPD), low energy electron diffraction (LEED), Auger electron spectroscopy (AES), and X-ray photoelectron spectroscopy (XPS). The p(2 × 2)-N overlayer is formed by exposure of ammonia to a surface at 85 K that is covered with 0.44 monolayer (ML) of molecular oxygen and then heating to 400 K. The reaction between ammonia and oxygen produces water, which desorbs below 400 K. The only desorption product observed above 400 K is molecular nitrogen, which has a peak desorption temperature of 453 K. The absence of oxygen after the 400 K anneal is confirmed with AES. Although atomic nitrogen can also be produced on the surface through the reaction of ammonia with an atomic, rather than molecular, oxygen overlayer at a saturation coverage of 0.25 ML, the yield of surface nitrogen is significantly less, as indicated by the N₂ TPD peak area. Atomic nitrogen readily reacts with hydrogen to produce the NH species, which is characterized with RAIRS by an intense and narrow (FWHM ∼ 4 cm⁻¹) peak at 3322 cm⁻¹. The areas of the H₂ TPD peak associated with NH dissociation and the XPS N 1s peak associated with the NH species indicate that not all of the surface N atoms can be converted to NH by the methods used here.     

差分吸收光谱法测量大气污染的测量误差分析

差分吸收光谱技术被广泛地应用于测量大气中微量元素的浓度，尽管该技术利用最小二乘法来反演待测气体的浓度，能够得到很高的测量精度。但是，由于仪器本身的噪声以及测量波段其它气体的干扰等，使得仪器的测量有一定的误差，而且上述因素还决定着仪器的测量下限。对差分吸收光谱方法的测量误差以及引起误差的原因作了详细的分析。     

生长温度对碳纳米管阴极场发射性能的影响

碳纳米管(Carbon Nanotubes,CNTs)场发射平面显示器(Field Emission Display,FED)与其他显示器比较显示了其独特优点,被认为是未来理想的平面显示器之一。碳纳米管阴极作为器件的核心部分,其性能的好坏直接影响显示器的性能。针对30~60英寸(76.2~152.4cm)大屏幕显示器所用的厚膜工艺,即采用丝网印刷法制备了碳纳米管阴极阵列,研究了化学气相沉积法在不同温度下生长的CNTs的场发射电流-电压特性,找到了适合FED用碳纳米管的最佳生长温度。结果表明生长温度越高(750℃),CNTs场发射性能越好。并用荧光粉阳极测试这些CNTs的场发射发光显示效果,验证了上述结论。     

Sub-Doppler and Doppler spectroscopy of DCN isotopomers in the terahertz region: ground and first excited bending states (v1v2v3)=(0 1 0)

The rotational spectra of the deuterium cyanide isotopic species DCN, D¹³CN, DC¹⁵N, and D¹³C¹⁵N were recorded in the vibrational ground and first excited bending state (v₂=1) up to 2 THz. The R-branch transitions from J=3←2 to J=13←12 were measured with sub-Doppler resolution. These very high resolution (∼70 kHz) and precise (±3-10 kHz) saturation dip measurements allowed for resolving the underlying hyperfine structure due to the ¹⁴N nucleus in DCN and D¹³CN for transitions as high as J=10←9. Additional high JR-branch (J=25←24 to J=28←27) transitions around 2 THz and direct l-type (ΔJ=0, J=19 to J=25) transitions from 66 to 118 GHz were recorded in Doppler-limited resolution. For the ground state of D¹³C¹⁵N, the J=1←0 transition was measured for the first time. The transition frequency accuracies for the other deuterated species were significantly improved. These new experimental data, together with the available infrared rovibrational data and previously measured direct l-type transitions, were subjected to a global least squares analysis for each isotopomer. This yielded precise sets of molecular constants for the ground and first excited vibrational states, including the nuclear quadrupole and magnetic spin-rotation coupling constants of the ¹⁴N nucleus for DCN and D¹³CN. The hyperfine structure due to the D, ¹³C, and ¹⁵N nuclei have not been resolved, but led to a broadening of the observed saturation dips.     

Preparation, structure and properties of novel 1,3-dithiol-2-ylidene derivatives containing bis(ethynylpyridine) units

1,3-Dithiol-2-ylidene derivatives containing bis(ethynylpyridine) units were synthesized using a Pd-catalyzed reaction of the corresponding dibromide. X-Ray crystal analysis revealed unique crystal structures depending on the aromatic groups. The absorption spectra and redox properties indicated intramolecular charge-transfer interactions between the 1,3-dithiole unit and the pyridyl parts.     

差分吸收光谱法测量大气痕量气体浓度误差分析及改善方法

差分吸收光谱技术(DOAS)中采用线性最小二乘拟合方法,用痕量气体标准差分吸收截面对测量得到的差分吸收光谱进行拟合,得出大气中痕量气体的浓度.计算结果的准确性不仅取决于光谱的测量精度,而且受标准差分吸收截面以及仪器函数和温度等诸多因素的影响.详细地分析了计算误差的产生原因,提出了用高浓度样品池得到标准吸收截面的方法,针对光谱固有结构,以及温度对标准吸收截面的影响,改进了浓度反演算法.大量的实验表明,综合运用上述方法,即便对低浓度的样气,相对测量误差也能降低到10%以下.     

X-Ray Mapping and Interpretation of Scatter Diagrams

Electron beam induced quantitative X-ray mapping has become a very useful characterisation tool for determining the elemental distribution in materials, whether using energy dispersive spectroscopy or wavelength dispersive spectroscopy. The X-ray intensity distributions of the elements from an X-ray map allow us to generate two dimensional and ternary scatter diagrams thus converting spatial information into concentration dimensions, which is an important tool for displaying the spatial relationships of elements or correlated elements (phases) in materials. To best understand how to use this tool, we need to understand the production and features of the scatter diagram. The type of clustering observed in the scatter diagram, whether oval, linear or spherical, can give the major and trace element distributions within phases as well as qualitative and quantitative phase information. This paper demonstrates the generation of scatter diagrams, properties of scatter diagrams, interpretation of scatter diagrams and the advantages of scatter diagrams through the use of examples.     

An AFM, XPS and electrochemical study of molecular electroactive monolayers formed by wet chemistry functionalization of H-terminated Si(1 0 0) with vinylferrocene

Molecular electroactive monolayers have been produced from vinylferrocene (VFC) via light-assisted surface anchoring to H-terminated n- and p-Si(1 0 0) wafers prepared via wet chemistry, in a controlled atmosphere. The resulting Si-C bound hybrids have been characterized by means of XPS and AFM. Their performance as semiconductor functionalized electrodes and their surface composition have been followed by combining electrochemical and XPS measurements on the same samples, before and after use in an electrochemical cell. White-light photoactivated anchoring at short (1 h) exposure times has resulted in a mild route, with a very limited impact on the initial quality of the silicon substrate. In fact, the functionalized Si surface results negligibly oxidized, and the C/Fe atomic ratio is close to the value expected for the pure molecular species. The VFC/Si hybrids can be described as (η⁵-C₅H₅)Fe²⁺(η⁵-C₅H₄)-CH₂-CH₂-Si species, on the basis of XPS results. Electrochemical methods have been applied in order to investigate the role played by a robust, covalent Si-C anchoring mode towards substrate-molecule electronic communication, a crucial issue for a perspective development of molecular electronics devices. The response found from cyclic voltammograms for p-Si(1 0 0) functionalized electrodes, run in the dark and under illumination, has shown that the electron transfer is not limited by the number of charge carriers, confirming the occurrence of electron transfer via the Si valence band. The hybrids have shown a noticeable electrochemical stability and reversibility under cyclic voltammetry (cv), and the trend in peak current intensity vs. the scan rate was linear. The molecule-Si bond is preserved even after thousands of voltammetric cycles, although the surface coverage, evaluated from cv and XPS, decreases in the same sequence. An increasingly larger surface concentration of Fe³⁺ at the expenses of Fe²⁺ redox centers has been found at increasing number of cv’s, experimentally associated with the growth of silicon oxide. Surface SiO⁻ groups from deprotonated silanol termination, induced by the electrochemical treatments, are proposed as the associated counterions for the Fe³⁺ species. They could be responsible for the observed decrease in the electron transfer rate constant with electrode ageing.