用稀土多元渗法制备钾稀土钨青铜K_xLa_yWO_3的XPS研究

Potassium tungsten bronze KxLayWO3 (x>0.5 and y<0.01) was synthesized by rare earth co-permeation method using α-K7[SiMg3(OH2)3W9O37] as the precursor. Binding energies of La, W, O and C were determined by XPS. From the XPS data, a peak at 34.21 eV indicates that some W6+ turned into W5+ by rare earth co- permeation. The binding energies La3d were the same in the surface and inner of the composite, showing that rare earth element La could diffuse into the body of the composite and the compound of KxLayWO3 was formed at the same time. The binding energies of O1s in KxLayWO3 surface were 531.4 eV and 532.0 eV, respectively, while peak at 531.4 eV disappeared through etching process. The result implies that the binding energy of 531.4 eV was due to the adsorbent O. In addition, the binding energies of C1s in the surface were 283.5 eV, 285.0 eV and 286.7 eV respectively, while the inner had only one peak at 285.0 eV due to standard C1s. This proves that there was no C in the core.

硼碳氮薄膜的制备与表征

用电子束蒸发的方法在单晶硅(100)基片上制备了硼碳氮薄膜,通过椭圆偏振仪、X射线衍射仪(XRD)、X光电子能谱仪(XPS)、傅立叶红外光谱仪(FTIR),测试分析了薄膜厚度均匀性、成分与结构。结果表明,薄膜均匀性较好,薄膜的沉积速率非常慢;薄膜在衬底温度为常温下沉积已是晶态的,随着衬底温度升高到450℃,其结晶性逐渐增强;薄膜不是石墨与BN的混和膜而是C、B、N相互结合成键。

Characterization of atomic-layer MoS_2 synthesized using a hot filament chemical vapor deposition method

Atomic-layer MoS_2 ultrathin films are synthesized using a hot filament chemical vapor deposition method. A combination of atomic force microscopy（AFM）, x-ray diffraction（XRD）, high-resolution transition electron microscopy（HRTEM）, photoluminescence（PL）, and x-ray photoelectron spectroscopy（XPS） characterization methods is applied to investigate the crystal structures, valence states, and compositions of the ultrathin film areas. The nucleation particles show irregular morphology, while for a larger size somewhere, the films are granular and the grains have a triangle shape. The films grow in a preferred orientation（002）. The HRTEM images present the graphene-like structure of stacked layers with low density of stacking fault, and the interlayer distance of plane is measured to be about 0.63 nm. It shows a clear quasihoneycomb-like structure and 6-fold coordination symmetry. Room-temperature PL spectra for the atomic layer MoS_2 under the condition of right and left circular light show that for both cases, the A1 and B1 direct excitonic transitions can be observed. In the meantime, valley polarization resolved PL spectra are obtained. XPS measurements provide high-purity samples aside from some contaminations from the air, and confirm the presence of pure MoS_2. The stoichiometric mole ratio of S/Mo is about 2.0–2.1, suggesting that sulfur is abundant rather than deficient in the atomic layer MoS_2 under our experimental conditions.

Surface Analysis of ZIRLO Alloy Implanted with Carbon

ZIRLO alloy specimens were implanted with carbon ions with fluence range from 1×10 16 to 1×10 18ions·cm -2, using a MEVVA source at an extraction voltage of 40 kV at maximum temperature of 380 ℃. The surfaces of the implanted samples were then analyzed and the TRIM 96 computer code was used to simulate the depth distribution of carbon. The valences of elements in the implanted surface of ZIRLO alloy were analyzed by X-ray photoemission spectroscopy (XPS); and then the depth distributions of the elements on the surface of the samples were obtained by Auger electron spectroscopy (AES). Scanning electron microscopy (SEM) was used to examine the micro-morphology of implanted samples. Glancing angle X-ray diffraction (GAXRD) at 0.30 incident angles was employed to examine the phase transformations of implanted samples. It shows that the as-received ZIRLO alloy is mainly composed of hexagonal alpha zirconium, as for implanted samples, there appeared hexagonal zirconia (H-ZrO_ 0.35) and sigma zirconium carbide (δ-Zr_3C_2), and the δ-Zr_3C_2 increased when increasing the fluence. When the fluence reached 1×10 18 ions·cm -2, the concentration of δ-Zr_3C_2 is the maximum in all the samples. The micro-morphology of implanted samples are similar, there are many pits with diameters ranging from 1 to 3 μm on the implanted surfaces.

Influence of Aluminum Ions Implantation on Corrosion Behavior of Zircaloy-2 Alloy in 1 M H_2SO_4

The specimens were implanted with aluminum ions with fluence ranging from 1× 10^16 to 1× 10^17 ions/cm^2 to study the effect of aluminum ion implantation on the aqueous corrosion behavior of zircaloy-2 by metal vapor vacuum arc source （MEVVA） at an extraction voltage of 40 kV. The valence states and depth distributions of elements in the surface layer of the samples were analyzed by X-ray photoelectron spectroscopy （XPS） and Auger electron spectroscopy （AES）, respectively. Transmission electron microscopy （TEM） was used to examine the microstructure of the aluminum-implanted samples. Glancing angle X-ray diffraction （GAXRD） was employed to examine the phase transformation due to the aluminum ion implantation. The potentiodynamic polarization technique was employed to evaluate the aqueous corrosion resistance of implanted zircaloy-2 in a 1 M H2SO4 solution. It is found that a significant improvement was achieved in the aqueous corrosion resistance of zircaloy-2 implanted with aluminum ions. Finally, the mechanism of the corrosion behavior of aluminum- implanted zircaloy-2 was discussed.

Effect of copper ions implantation on the corrosion behavior of ZIRLO alloy in 1 mol/L H_2SO_4

In order to study the effect of copper ion implantation on the aqueous corrosion behavior of ZIRLO alloy, specimens were implanted with copper ions with fluences ranging from 1×10^16 to 1×10^ ions/cm^2, using a metal vapor vacuum arc source （MEVVA） at an extraction voltage of 40 kV, The valence states and depth distributions of elements in the surface layer of the samples were analyzed by X-ray photoelectron spectroscopy （XPS） and Auger electron spectroscopy （AES）, respectively. Glancing angle X-ray diffraction （GAXRD） was employed to examine the phase transformation due to the copper ion implantation. The potcntiodynamic polarization technique was used to evaluate the aqueous corrosion resistance of implanted ZIRLO alloy in a 1 mol/L H2SO4 solution. It was found that a significant improvement was achieved in the aqueous corrosion resistance of ZIRLO alloy implanted with copper ions when the fluence is 5×10^16 ions/cm^2. When the fluence is 1×10^16 or 1×10^17 ions/cm^2, the corrosion resistance of implanted sanaples was bad. Finally, the mechanism of the corrosion behavior of copper-implanted ZIRLO alloy was discussed.

Irradiation damage simulation of Zircaloy-4 using argon ions bombardment

To simulate irradiation damage, argon ion was implanted in the Zircaloy-4 with the fluence ranging from 1 × 10^16 to 1 × 10^17 cm^-2, using accelerating implanter at an extraction voltage of 190 kV and liquid nitrogen temperature. Then the influence of argon ion implantation on the aqueous corrosion behavior of Zircaloy-4 was studied. The valence states of elements in the surface layer of the samples were analyzed using X-ray photoelectron spectroscopy （XPS）. Transmission electron microscopy （TEM） was used to examine the microstructure of the argon-implanted samples. The potentiodynamic polarization technique was employed to evaluate the aqueous corrosion resistance of implanted Zircaloy-4 in 1 mol/L HzSO4 solution. It is found that there appear bubbles on the surface of the samples when the argon fluence is 1 × 10^16 cm^-2. The microstructure of argon-implanted samples changes from amorphous to partial amorphous, then to polycrystalline, and again to amorphous. The corrosion resistance of implanted samples linearly declines with the increase of fluence approximately, which is attributed to the linear increase of the irradiation damage.

Morphology and Properties of Hybrid Systems Comprising Gold Nanoparticles in CuPc Matrices

Transmission electron microscopy and surface- and bulk-sensitive spectroscopic methods were used to study the morphology and the electronic structure of a hybrid organic-inorganic system composed of gold nanoparticles （NP＇s） which were distributed in an organic matrix. Au atoms deposited onto a copper phthalocyanine （CuPc） surface diffuse into the organic matrix and self-assemble in well defined NP＇s with metallic properties. No formation of a continuous metallic Au film on top of the CuPc film is observed up to nominal coverages as large as 130 A.

Chemical composition and Mott-Schottky analysis of passive film formed on G3 alloy in bicarbonate/carbonate buffer solution

The chemical composition and semi-conductive properties of passive film on nickel- based alloy （G3 alloy） in bicarbonate/carbonate buffer solution were investigated by Auger electron spectroscopy （AES）, X-ray photoelectron spectroscopy （XPS）, elec- trochemical impedance spectra （EIS） and Mott-Schottky plot. AES and XPS results showed that the passive film appeared double-layer structure, in which the inner film was composed of nickel oxide, the mixed nickel-chromium-molybdenum-manganese oxides were the major component of the outer film. The electrochemical results revealed that the factors including frequency, potential, time, temperature and pH value can affect the semi-conductive property, the doping densities decreased with increasing potential and pH value, prolonging time and decreasing temperature. According to the above results, it can be concluded that the film protection on the substrate was enhanced with increasing potential and pH value, prolonging time and decreasing temperature.

Microstructure and Element Composition of Shell Plates of Liolophura japonica

The microstructure characteristics of shell plates of chiton Liolophura japonica Lischke were analyzed using environmental scanning electron microscopy （ESEM）. The results show that the internal structure of the shell plate of chiton Liolophurajaponica is composed of seven calcium layers which were crossed lamellar crystallites, homoge- neous structure, granular crystallites, and trabecular type crystallites. The element compositions of shell plates were analyzed using X-ray photoelectron spectroscopy （XPS）. The results determined by XPS show that the surface chemical states of various layers are different. There are 13 elements （Na, O, N, C, S, P, Ca, C1, Si, A1, K, Fe, Mg） on the shell plate of chiton L. japonica. Among the 13 elements, 11 are on the outside pigment layer except K and S. Among seven layers of shell plate, there is the largest quantity of elements on the outside pigment layer, and the least quantity of elements is on layer C （Articulamentum auctorum）. There are 7 elements on the layer C （Articulamentum auctorum）. Be- sides calcium carbonate, there are some inorganic compounds on the shell plate, such as NaC1, MgO, A1203, silicate, sulfate and phosphate. There are some organic chemical components, such as carbohydrate, organic sulfide, and organic nitride on the shell plates.

Thermal plasma synthesis of SiC

Synthesis of silicon carbide has been carried out using thermal plasma processing technique using SiO2 as the solid feed and CH4 as the gaseous reducing agent. Thermochemical calculations have been performed varying the molar ratio of silicon dioxide and methane to determine the feasibility of the reaction. Experiments using a molar ratio of SiO2：CH4 equal to 1：2 produced maximum yield of SiC of about 65 mol % at a solid feed rate of 5 g/min. Mostly spherical morphology with some nanorods has been observed. The presence of Si had been observed and was quantified using XRD, HRTEM, Raman spectroscopy and X-ray photoelectron microscopy （XPS）. Si acts as a nucleating agent for SiC nanorods to grow.