Analysis of PTCDA/ITO Surface and Interface Using X-ray Photoelectron Spectroscopy and Atomic Force Microscopy

The electronic states of the surface and interface of 3,4, 9, 10-perylenetetracarboxylic dianhydride （PTCDA）/indium-tin-oxide （ITO） thin film are investigated using X-ray photoelectron spectroscopy （XPS）. A- tomic force microscopy （AFM） is also applied to investigate the pattern of PTCDA/ITO film. XPS results show that there are two main peaks,which are associated with C atoms in the perylene rings and acid anhydride groups, located at 284.6 and 288.7eV, respectively,in the Cls spectrum of the original surface. It can be deduced from the emergence of a small peak at 290.4eV in the Cls spectrum that some C atoms are oxidized by O atoms from ITO. The binding energies of O atoms in C-O bonds and C--O---C bonds are 531.5 and 533.4eV respectively. At the interface,the peak at the high binding energy in the Cls spectrum disappears,and the peak value shifts about 0.2eV to lower binding energy, There is a significant 1.5eV chemical shift to lower binding energy in the Ols spectrum. These observations indicate that perylene rings inside PTCDA molecules are combined with In vacancies in the ITO at the interface. The AFM results show that PTCDA molecules formed an island-like structure a height of about 14nm. The sizes of the crystal grains are about 100--300nm. The island-like pattern comes from the delocalized π bonds of adjacent molecules in PTCDA and the combination of vacancies in ITO with perylene rings at the PTCDA/ITO interface.

Analysis of Wettability and X-ray Photoelectron Spectroscopy of Wheat Straw/SPI

[Objective] The aim was to improve the adhesive bonding property of wheat straw surface to prepare wheat straw particleboard of soy protein isolate （SPI） adhesive through chemical and enzyme treatments. [Method] Evaluation and analysis were made on wettability of wheat straws in the control group and treated groups （chemical and enzyme treatments） by means of measurement of contact angle and calculation of spreading-penetration parameters （K）. In addition, we made analysis on surface elements through X-ray photoelectron spectroscopy （XPS）. [Result] The re- sults showed that K value of straw treated with sodium hydroxide, hydrogen peroxide and lipase increased by 58.0%, 48.7% and 83.2% compared to that of control group, respectively. The XPS analysis indicated that rapid decrease of silicon content and destruction of wax layer greatly contributed to wettability improvement of wheat straw surface. [Conclusion] The chemical and lipase treatments of wheat straw provided technical support for manufacture of wheat straw particle boand.

Understanding fundamentals of electrochemical reactions with tender X-rays:A new lab-based operando X-ray photoelectron spectroscopy method for probing liquid/solid and gas/solid interfaces across a variety of electrochemical systems

Electrocatalysis is key to improving energy efficiency,reducing carbon emissions,and providing a sustainable way of meeting global energy needs.Therefore,elucidating electrochemical reaction mechanisms at the electrolyte/electrode interfaces is essential for developing advanced renewable energy technologies.However,the direct probing of real-time interfacial changes,i.e.,the surface intermediates,chemical environment,and electronic structure,under operating conditions is challenging and necessitates the use of in situ methods.Herein,we present a new lab-based instrument commissioned to perform in situ chemical analysis at liquid/solid interfaces using ambient pressure X-ray photoelectron spectroscopy(APXPS).This setup takes advantage of a chromium source of tender X-rays and is designed to study liquid/solid interfaces by the“dip and pull”method.Each of the main components was carefully described,and the results of performance tests are presented.Using a three-electrode setup,the system can probe the intermediate species and potential shifts across the liquid electrolyte/solid electrode interface.In addition,we demonstrate how this system allows the study of interfacial changes at gas/solid interfaces using a case study:a sodium–oxygen model battery.However,the use of APXPS in electrochemical studies is still in the early stages,so we summarize the current challenges and some developmental frontiers.Despite the challenges,we expect that joint efforts to improve instruments and the electrochemical setup will enable us to obtain a better understanding of the composition–reactivity relationship at electrochemical interfaces under realistic reaction conditions.

Hard X-ray Photoelectron Spectroscopy Study of Electron Spectral Structure beyond the Known Signal Electron Peak

HAXPES （hard X-ray photoelectron spectroscopy） is a powerful emerging instrument in surface analysis. It extended the photoelectron energy range up to 15,000 eV and opened the possibility to study much thicker films, buried layers and bulk electronic properties. In order to study these features, data for the electron IMFP （inelastic mean free path） at these energies is needed. To date, only calculated IMFP are available at energies above 5,000 eV and therefore experimental validation of these calculations are essential. In this paper, a new approach for using the HAXPES spectra is presented. This approach, treats the attenuated part of the electron spectrum as a whole to calculating the average electron energy loss. This average electron energy loss is the result of inelastic collisions in the material and hence, carry with it information about the electron transport poses. Carbon layers with thicknesses between 20 and 75 nanometer deposited over copper substrate were used to test this approach at the Spanish beam-line （Spline） in the ESRF （European synchrotron radiation facility）. The measured results showed good agreement with the predictions of the multiple inelastic scattering theory. In addition, an algorithm for the experimental evaluation of electron IMFP, using the measured energy loss, is proposed.

^(99m)Tc-环己二酮肟配合物甲硼酸加合物的合成与^(99)Tc的价态及其配位环境研究

目的 制备一种99mTc标记的心肌显像剂———99mTc 环己二酮肟配合物甲硼酸加合物 ,并对该显像剂99Tc的价态、99Tc的配位环境、放射化学纯度以及γ CD在药盒中的作用进行了研究。方法 使用X射线光电子能谱 (XPS)、纸层析法和循环伏安法 (CV)。结果 99Tc Teboroxime(由环己二酮肟、甲硼酸与SnCl2 还原了的99Tc形成的配合物 )是99Tc(Ⅲ ) ,且存在 :N99Tc和CL99Tc配位键。该配合物放置 6h ,XPS信号无明显变化。放置 8h ,99Tc3d5/ 2 的EB 值向高位能偏移 ,生成99Tc(Ⅳ )。其放化纯度较高且稳定 [平均放化纯度 (95 .19±3.13) % ]。此外 ,用循环伏安法显示 ,γ CD在药盒中有稳定的作用。结论 制备的心肌显像剂———99Tc 环己二酮肟配合物甲硼酸加合物是一种配位化合物 ,其稳定性良好 。

Fe-Mn/Al_2O_3 catalysts for low temperature selective catalytic reduction of NO with NH_3

A series of Fe‐Mn/Al2O3 catalysts were prepared and studied for low temperature selective catalytic reduction （SCR） of NO with NH3 in a fixed‐bed reactor. The effects of Fe and Mn on NO conversion and the deactivation of the catalysts were studied. N2 adsorption‐desorption, X‐ray diffraction, transmission electron microscopy, energy dispersive spectroscopy, H2 temperature‐programmed reduction, NH3 temperature‐programmed desorption, X‐ray photoelectron spectroscopy （XPS）, thermal gravimetric analysis and Fourier transform infrared spectroscopy were used to character‐ize the catalysts. The 8Fe‐8Mn/Al2O3 catalyst gave 99%of NO conversion at 150？？ and more than 92.6%NO conversion was obtained in a wide low temperature range of 90–210？？. XPS analysis demonstrated that the Fe3＋was the main iron valence state on the catalyst surface and the addition of Mn increased the accumulation of Fe on the surface. The higher specific surface area, enhanced dispersion of amorphous Fe and Mn, improved reduction properties and surface acidity, lower binding energy, higher Mn4＋/Mn3＋ratio and more adsorbed oxygen species resulted in higher NO conversion for the 8Fe‐8Mn/Al2O3 catalyst. In addition, the SCR activity of the 8Fe‐8Mn/Al2O3 cata‐lyst was only slightly decreased in the presence of H2O and SO2, which indicated that the catalyst had better tolerance to H2O and SO2. The reaction temperature was crucial for the SO2 resistance of catalyst and the decrease of catalytic activity caused by SO2 was mainly due to the sulfate salts formed on the catalyst.

Interface Reaction of SiO_2/Ta and Its Influence on Cu Diffusion

Ta/NiFe film is deposited on Si substrate precoated with SiO_2 by magnetron sputtering.SiO_2/Ta interface and Ta_5Si_3 standard sample are investigated by using X-ray photoelectron spectroscopy (XPS) and peak decomposition technique.The results show that there is a thermodynamically favorable reaction at the SiO_2/Ta interface:37Ta+15SiO_2=5Ta_5Si_3+6Ta_2O_5.The more stable products Ta_5Si_3 and Ta_2O_5 may be beneficial to stop the diffusion of Cu into SiO_2.

AFM and XPS Study on the Surface and Interface States of CuPc and SiO_2 Films

A CuPc/SiO2 sample is fabricated. Its morphology is characterized by atomic force microscopy, and the electron states are investigated by X-ray photoelectron spectroscopy. In order to investigate these spectra in detail, all of these spectra are normalized to the height of the most intense peak,and each component is fitted with a single Gaussian function. Analysis shows that the O element has great bearing on the electron states and that SiO2 layers produced by spurting technology are better than those produced by oxidation technology.

Effect of Rapid Thermal Annealing Ambient on Gettering Efficiency and Surface Microstructure in 300mm CZ Silicon Wafers

The effect of rapid thermal annealing （RTA） ambient on denuded zone and oxygen precipitates in Czochralski （CZ） silicon wafers is studied in this paper. N2 and a N2/NH3 mixture are used as RTA ambient. It is demonstrated that a high density of oxygen precipitates and thin denuded zone are obtained in N2/NH3 ambient,while a relatively lower density of oxygen precipitates and thicker denuded zone are observed in N2 ambient. As the RTA duration times increased, the oxygen precipitate density increased and the denuded zone depth decreased. X-ray photoelectron spectroscopy （XPS） data and atomic force microscope （AFM） results show that there RTA process,which can explain the different effect of RTA was a surface nitriding reaction during the N2/NH3 ambient ambient.

Visible-Light Activities of Erbium Doped BiVO4 Photocatalysts

Er-doped BiVO4 composite photocatalyst was hydrothermal synthesized and characterized by X-ray powder diffraction, scanning electron microscopy, energy-dispersive X-ray Spectroscopy, X-ray photoelectron spectroscopy, and UV-Vis diffuse reflectance spectra techniques. The activity of the catalyst was determined by oxidative decomposition of methyl orange in aqueous solution under visible-light irradiation. X-ray photoelectron spectroscopy and energy-dispersive X-ray Spectroscopy analysis revealed that the doped Er existed in the form of Er2O3. It also showed that the Er doping can enhance the visible-light absorption abilities of catalysts and their visible-light-driven photocatalytic activities in comparison with those of pure BiVO4.

The effect of the support on the surface composition of PtCu alloy nanocatalysts: In situ XPS and HS-LEIS studies

Supported PtCu alloys have been broadly applied in heterogeneous catalysis and electrocatalysis owing to their excellent catalytic performance and high CO tolerance. It is important to analyze the outermost surface composition of the supported alloy nanoparticles to understand the nature of the catalytically active sites. In this paper, homogeneous face-centered cubic PtCu nanoparticles with a narrow particle size distribution were successfully fabricated and dispersed on a high-surface-area Ti〇2 powder support. The samples were oxidized and reduced in situ and then introduced into the ultrahigh vacuum chamber to measure the topmost surface composition by high-sensitivity low-energy ion scattering spectroscopy, and to determine the oxidation states of the elements by X-ray photoelectron spectroscopy. The surface composition and morphology, elemental distribu-tion, and oxidation states of the components were found to be significantly affected by the support and treatment conditions. The PtCu is de-alloyed upon oxidation with CuO wetting on the TiO2 sur-face and re-alloyed upon reduction. Phase diagrams of the surface composition and the bulk com-position were plotted and compared for the supported and unsupported materials.

Catalytic Performance of Carbon Materials Supported Pd Nanoparticles in Selective Hydrogenation of Acetylene

Pd/C catalysts were prepared by deposited Pd nanoparticles （NPs） on different carbon supports including activated carbon （AC）, graphite oxide （GO）, and reduced graphite oxide （rGO） using sol-immobilization method. Through transmission electron microscopy, powder X-ray di raction, and X-ray photoelectron spectroscopy, the role of the carbon supports for the catalytic performances of Pd/C catalysts was examined in selective hydrogenation of acetylene. The results indicate that Pd/AC exhibited higher activity and selectivity than Pd/GO and Pd/rGO in the gas phase selective hydrogenation of acetylene. Thermal and chemical treatment of AC supports also have some effect on the catalytic performance of Pd/AC catalysts. The differences in the activity and selectivity of various Pd/C catalysts were partly attributed to the metal-support interaction.

Photocatalytic Activity of N-doped TiO2 Photocatalysts Prepared from the Molecular Precursor （NH4）2TiO（C2O4）2

We developed a novel approach for the preparation of N-doped TiO2 photocatalysts by calcining ammonium titanium oxalate at different temperatures. The structures of N-TiO2 were characterized by powder X-ray diffraction, infrared spectroscopy, thermogravimetric analysis, N2 adsorption-desorption isotherms, X-ray photoelectron spectroscopy, diffuse reflectance UV-Vis spectroscopy, and scanning electron microscope. The N-doped TiO2 photocatalysts calcined below 700 ℃ are the pure anatase phase but that calcined at 700 ℃ is a mixture of anatase and rutile phases. The doped N locates at the interstitial site of TiO2 which leads to the narrowing of bad gap of pure anatase N-TiO2. Among all photocatalysts, N-TiO2 photocatalysts calcined at 600 and 400 ℃ exhibit the best performance in the photodegradation of methyl orange under the UV light and all-wavelength light illuminations, respectively; however, because of the perfect crystallinity and the existence of anatase-rutile phase junctions, N-TiO2 photocatalyst calcined at 700 ℃ exhibits the highest specific photodegradation rate, i.e., the highest quantum yield, under both the UV light and all-wavelength light illuminations.

Effect and mechanism of dolomite with different size fractions on hematite flotation using sodium oleate as collector

The effect of dolomite with different particle size fractions on hematite flotation was studied using sodium oleate as collector at p H of about 9. The effect mechanism of dolomite on hematite flotation was investigated by means of solution chemistry, ultraviolet spectrophotometry(UV), inductively coupled plasma atomic emission spectrometry(ICP-AES) and X-ray photoelectron spectroscopy(XPS). It is observed that dolomite with different size fractions has depressing effect on hematite flotation using sodium oleate as collector, and dolomite could be the "mineral depressant" of hematite using sodium oleate as collector. The reasons for that are concerned with sodium oleate consumption and the adsorption onto hematite of dissolved species of dolomite.

Study on Relationship between Microstructure of Active Phase and HDS Performance of Sulfided Ni-Mo Catalysts: Effect of Metal Loading

Six Ni-Mo catalysts with different metal contents were prepared and characterized by N2 adsorption and X-ray diffi＇actometry. The active phase microstructure of these catalysts was examined by the Raman spectroscopy, temperature- programmed reduction （TPR）, X-ray photoelectron spectroscopy, and high-resolution transmission electron microscopy. Hydrodesulfurization （HDS） activity of catalyst samples were analyzed in a flow fixed-bed microreactor. The sulfidation degree of Mo and the length of the MoS2 slab slightly increased with the amount of metal loaded following sulfidation. This small change is attributed to polymolybdate species observed in all the oxidized catalysts. Weak metal-support interactions, as determined by the TPR technique, increased the NiSx sulfidation phase and MoS2 slab stacking. The HDS activity of the catalyst samples increased with the number of active sites. For high metal loading catalysts, their HDS activity was nearly identical because the sulfur atoms cannot easily approach active sites. This change is caused by the large number of stacked layers in the MoS2 slabs as well as the decrease in the specific surface area and pore volume of the catalyst samples with an increasing metal loading.

Carbonaceous Adsorbents Prepared from Sewage Sludge and Its Application for Hg^0 Adsorption in Simulated Flue Gas

The carbonaceous adsorbent was prepared from mixtures of dewatered sludge and sawdust with enhanced ZnCl2 chemical activation.Characteristics of the adsorbent were studied using scanning electron microscope(SEM) ,Fourier transform infrared spectroscopy(FT-IR) ,and adsorption of nitrogen.The surface analysis showed that the carbonaceous adsorbent had good specific surface and porosity(394 m 2 ·g-1of BET surface,0.12 and 0.10 ml·g-1of microporous and mesoporous volume,respectively) .The oxygen functional groups such as OH,C O and C O were found on the surface by FTIR and XPS(X-ray photoelectron spectroscopy) .The adsorption of elemental mercury(Hg0) on the carbonaceous adsorbent was studied in a fixed bed reactor.The dynamic adsorption capacity of carbonaceous adsorbent increased with influent mercury concentration,from 23.6μg·g-1at 12.58μg·m-3to 87.9μg·g-1at 72.50μg·m-3,and decreased as the adsorption temperature increased,from 246 μg·g-1 at 25°C to 61.3μg·g-1 at 140°C,when dry nitrogen was used as the carrier gas.The carbonaceous adsorbent presented higher dynamic adsorption capacity than activated carbon,which was 81.2μg·g-1and 53.8μg·g-1respectively.The adsorption data were fitted to the Langmuir adsorption model.The physical and chemical adsorption were identified on the adsorbent.

Inhibiting Effect of Ciprofloxacin,Norfloxacin and Ofloxacin on Corrosion of Mild Steel in Hydrochloric Acid

The inhibiting effect of ciprofloxacin,norfloxacin and ofloxacin on the corrosion of mild steel in 1 mol·L-1 HCl and the mechanism were studied at different temperatures using mass loss measurement,electrochemical method,and X-ray photoelectron spectroscopy(XPS) .Effective inhibition was shown by mass loss,potentiodynamic polarization and impedance spectroscopy measurement.The corrosion rate of the metal in the mass loss measurement,and the corrosion reaction on cathode and anode in the electrochemical measurement were accelerated when temperature was increased.XPS results showed that the inhibitors adsorbed effectively on the metal surface.

The correlation between nitrogen species in coke and NO_x formation during regeneration

Nitrogen oxides （NOx） emission during the regeneration ofcoked fluid catalytic cracking （FCC） catalysts is an en- vironmental issue. In order to identify the correlations between nitrogen species in coke and different nitrogen- containing products in tail gas, three coked catalysts with multilayer structural coke molecules were prepared in a fixed bed with model compounds （o-xylene and quinoline） at first. A series of characterization methods were used to analyze coke, including elemental analysis, FT-IR, XPS, and TG-MS. XPS characterization indicates all coked catalysts present two types of nitrogen species and the type with a higher binding energy is related with the inner part nitrogen atoms interacting with acid sites. Due to the stronger adsorption ability on acid sites for basic nitrogen compounds, the multilayer structural coke has unbalanced distribution of carbon and ni- trogen atoms between the inner part and the outer edge, which strongly affects gas product formation. At the early stage of regeneration, oxidation starts from the outer edge and the product NO can be reduced to N2 in high CO concentration. At the later stage, the inner part rich in nitrogen begins to be exposed to 02. At this period, the formation of CO decreases due to lack of carbon atoms, which is not beneficial to the reduction of NO. There- fore, nitrogen species in the inner part of multilayer structural coke contributes more to NOx formation. Based on the multilayer structure model of coke molecule and its oxidation behavior, a possible strategy to control NOx emission was discussed merely from concept.

Adsorption of cadmium ions from aqueous solutions by activated carbon with oxygen-containing functional groups

The adsorption of aqueous cadmium ions(Cd(Ⅱ)) have been investigated for modified activated carbon(AC-T)with oxygen-containing functional groups.The oxygen-containing groups of AC-T play an important role in Cd(Ⅱ) ion adsorption onto AC-T.The modified activated carbon is characterized by scanning electron microscopy,Fourier transform infrared spectroscopy(FT-IR) and X-ray photoelectron spectroscopy(XPS).The results of batch experiments indicate that the maximal adsorption could be achieved over the broad pH range of 4.5 to 6.5.Adsorption isotherms and kinetic study suggest that the sorption of Cd(Ⅱ) onto AC-T produces monolayer coverage and that adsorption is controlled by chemical adsorption.And the adsorbent has a good reusability.According to the FT-IR and XPS analyses,electrostatic attraction and cation exchange between Cd(Ⅱ) and oxygen-containing functional groups on AC-T are dominant mechanisms for Cd(Ⅱ) adsorption.

Tribological Performances of Fatty Acyl Amino Acids Used as Green Additives in Lubricating Oil

The friction and wear characteristics of lauroyl glutamine, lauroyl glycine and lauroyl alanine, used as green additives in HVI 350 mineral lubricating oil, were evaluated on a four-ball tribotester. The morphologies and chemical species of the worn surfaces were analyzed by scanning electron microscope （SEM） and X-ray photoelectron spectroscope （XPS）, respectively. The test results indicated that the three fatty acyl amino acids could effectively improve the anti-wear and friction-reducing abilities of the HVI 350 mineral oil. The improvement in anti-wear and friction-reducing abilities of the mineral oil by the related amino acids was mainly ascribed to the formation of a composite boundary lubrication film due to the adsorption of amino acids on the friction surfaces.