Zn^(2+)-壳聚糖螯合物的制备及其IR、XPS分析

以自制壳聚糖为原料 ,在 w=0 .0 5的醋酸水溶液中与 Zn2 + 配位 ,冷冻沉降后得 Zn2 + -壳聚糖高分子配合物 ,并用红外光谱 (IR)、光电子能谱 (XPS)研究了壳聚糖及 Zn2 + -壳聚糖螯合物表面的元素结构及其结合能的变化。结果表明 Zn2 + -壳聚糖螯合物的配位原子是— NH2 中的 N。

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.

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.

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.

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.

Characterization of Pyrolytic Lignin Extracted from Bio-oil

Bio-oil is a new liquid fuel produced by fast pyrolysis,which is a promising technology to convert bio-mass into liquid. Pyrolytic lignin extracted from bio-oil,a fine powder,contributes to the instability of bio-oil. The paper presents the structural features of three kinds of pyrolytic lignin extracted from bio-oil with different methods(WIF,HMM,and LMM) . The pyrolytic lignin samples are characterized by Fourier transform infrared spectrometer(FTIR) and X-ray photoelectron spectroscopy(XPS) . FTIR data indicate that the three pyrolytic lignin samples have similar functional groups,while the absorption intensity is different,and show characteristic vibra-tions of typical lignocellulosic material groups O H(3340-3380 cm-1) ,C H(2912-2929 cm-1) and C O(1652-1725 cm-1) . Comparison in the region(3340-3380 cm-1) indicates that WIF has more O H stretch groups than HMM and LMM. The carbon spectra are fitted to four peaks:C1,C C or C H,BE 283.5 eV;C2,C OR or C OH,BE 284.5-285.8 eV;C3,C O or HO C OR,BE 286.10-287.10 eV;C4,O C O,BE 287.5-287.7 eV. The absence of C1,C C or C H indicates the dominant polymerization structure of aro-matic carbon in pyrolytic lignin samples. For HMM and WIF,C2a and C2b can not be separated,so there is no free hydroxyl group in the samples. The oxygen peaks are also fitted to four peaks:O1,OH,BE = 530.3 eV;O2,RC O,BE 531.45-531.72 eV;O3,O C O,BE = 532.73-533.74 eV;O4,H2O,BE 535 eV. The absence of O1 and O4 indicates that little hydroxyl groups and adsorbed water are present in the samples.

Influence of oxygen partial pressure on properties of N-doped ZnO films deposited by magnetron sputtering

N-doped ZnO films were radio frequency(RF)sputtered on glass substrates and studied as a function of oxygen partial pressure(OPP)ranging from 3.0×10-4 to 9.5×10-3 Pa.X-ray diffraction patters confirmed the polycrystalline nature of the deposited films.The crystalline structure is influenced by the variation of OPP.Atomic force microscopy analysis confirmed the agglomeration of the neighboring spherical grains with a sharp increase of root mean square(RMS)roughness when the OPP is increased above 1.4×10-3 Pa.X-ray photoelectron spectroscopy analysis revealed that the incorporation of N content into the film is decreased with the increase of OPP,noticeably N 1s XPS peaks are hardly identified at 9.5×10-3 Pa.The average visible transmittance(380-700 nm) is increased with the increase of OPP(from～17%to 70%),and the optical absorption edge shifts towards the shorter wavelength.The films deposited with low OPP(≤3.0×10-4 Pa)show n-type conductivity and those deposited with high OPP(≥9.0×10-4 Pa)are highly resistive(>105Ω·cm)

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.

Effect of carbon on microstructure of CrAlC_xN_(1-x) coatings by hybrid coating system

A systematic investigation of the microstructure of CrA1CxN1-x coatings as a function of carbon contents was conducted. Quaternary CrA1CxN1-x coatings were deposited on Si wafers by a hybrid coating system combining an arc-ion plating technique and a DC reactive magnetron sputtering technique using Cr and AI targets in the Ar/N2/CH4 gaseous mixture. The effect of carbon content on microstructure of CrA1C^N~ x coatings was investigated with instrumental analyses of X-ray diffraction, X-ray photoelectron, and high-resolution transmission electron microscopy. The results show that the carbon content of CrA1CxN1-x coatings linearly increases with increasing CH4/（CH4/N2） gas flow rate ratio. The surface roughness of the CrA1CxN1-x coating layer decreases with the increase of carbon content.

Construction of a macromolecular structural model of Chinese lignite and analysis of its low-temperature oxidation behavior

The aim of this paper is to analyze the change in the active structure of lignite during the process of lowtemperature oxidation by constructing a molecular structure model for lignite. Using quantum computation combined with experimental results of proximate analysis, ultimate analysis, Fourier transform infrared spectroscopy(FTIR) and X-ray photoelectron spectroscopy(XPS), a structural model for the large molecular structure was constructed. By analyzing the bond lengths in the model molecule, the evolution law for the active structure of lignite was predicted for the process of low-temperature oxidation. In low-temperature oxidation,alkanes and hydroxyls are the primary active structures observed in lignite, though ether may also react. These active functional groups react with oxygen to release heat, thereby speeding up the reaction between coal and oxygen. Finally, the content of various functional groups in the process of lignite low-temperature oxidation was analyzed by infrared analysis, and the accuracy of the model was verified.

Carbon dioxide reforming of methane over bimetallic catalysts of Pt-Ru/γ-Al_2O_3 for thermochemical energy storage

The reaction of CO2 reforming of CH4 has been investigated with y-A1203-supported platinum and ruthenium bimetallic catalysts, with the specific purpose of thermochemical energy storage. The catalysts were prepared by using the wetness impregnation method. The prepared catalysts were characterized by a series of physico-chemical characterization techniques such as BET surface area, thermo-gravimetric （TG）, transmission electron microscope （TEM） and X-ray photoelectron spectroscopy （XPS）. In addition, the amount of carbon deposits on the surface of the catalysts and the type of the carbonaceous species were discussed by TG. It was found that the bimetallic Pt-Ru/7-A1203 catalysts exhibit both superior catalytic activity and remarkable stability by comparison of monometallic catalysts. During the 500 h stability test, the bimetallic catalyst showed a good performance at 800 ~C in CO2 reforming of CH4, exhibiting an excellent anti-carbon performance with the mass loss of less than 8.5%. The results also indicate that CO2 and CH4 have quite stable conversions of 96.0 % and 94.0 %, respectively. Also, the selectivity of the catalysts is excellent with the products ratio of CO/H2 maintaining at 1.02. Furthermore, it was found in TEM images that the active carbonaceous species were formed during the catalytic reaction, and well-distributed dot-shaped metallic particles with a relatively uniform size of about 3 nm as well as amorphous carbon structures were observed. Combined with BET, TG, TEM tests, it is concluded that the selected bimetallic catalysts can work continuously in a stable state at the high temperature, which has a potential to be utilized for the closed-loop cycle of the solar thermochemical energy storage in future industry applications.

Silica-gel Supported V Complexes： Preparation, Characterization and Catalytic Oxidative Desulfunzation

In this manuscript, a series of catalyst SG n-[VVO2-PAMAM-MSA] (SG silica gel, PAMAM polyamidoamine, MSA 5-methyl salicylaldehyde, n=0, 1, 2, 3) was prepared and their structures were fully characterized by Fourier transform-infrared spectroscopy (FT-IR), thermogravimetric analysis (TGA), X-ray photoelectron spectroscopy (XPS) and inductive coupled plasma emission spectrometer (ICP) etc. XPS revealed that the metal V and SG n-PAMAM-MSA combined more closely after the formation of Schiff base derivatives. Their catalytic activities for oxidation of dibenzothiophene were evaluated using tert-butyl hydroperoxide as oxidant. The results showed that the catalyst SG 2.0-[VVO2-PAMAM-MSA] presented good catalytic activity and recycling time. Meanwhile, the optimal condition for the catalytic oxidation of SG 2.0-[VVO2-PAMAM-MSA] was also investigated, which showed that when the oxidation temperature was 90 °C, time was 60 min, the O/S was 3:1, and the mass content of catalyst was 1%, the rate of desulfurization could reach 85.2%. Moreover, the catalyst can be recycled several times without significant decline in catalytic activity.

Low-Temperature Plasma Induced Grafting of 2-Methacryloyloxyethyl Phosphorylcholine onto Poly(tetrafluoroethylene) Films

Modification of poly(tetrafluoroethylene)(PTFE) films with 2-methacryloyloxyethyl phosphorylcholine(MPC) was performed by low-temperature plasma treatment and grafting polymerization.Surface properties of PTFE were characterized by attenuated total reflectance Fourier transform infrared(ATR-FTIR) spectra,X-ray photoelectron spectroscopy(XPS) ,and static contact angle.The results show that MPC has been grafted onto PTFE film surface successfully.Contact angle for the modified PTFE films in the water decreased from 108°to 58.25°,while surface energy increased from 17.52 mN/m to 45.47 mN/m.The effects of plasma treatment time,monomer concentration and grafting time on degree of grafting were determined.In the meanwhile,blood compatibility of the PTFE films was studied by checking thrombogenic time of blood plasma.

Applications of in-situ wide spectral range infrared absorption spectroscopy for CO oxidation over Pd/SiO_(2) and Cu/SiO_(2) catalysts

Infrared(IR)absorption spectroscopy has been widely used for dynamic characterization of catalysts and mechanism of catalytic reactions.However,due to the strong infrared absorption of heterogeneous catalysts(mainly oxides,or supported metal and metal oxides,etc.)below 1200 cm^(-1),and the intensity of regular infrared light source rapidly decays at low-wavenumber range,most in-situ infrared spectroscopy studies are limited to the detection of surface adsorbates in the range of 4000-900 cm^(-1).The change of catalytically active component itself(M-O,M-M bond,etc.,1200-50 cm^(-1))during the reaction is hard to be tracked under reaction conditions by in-situ IR.In this work,a home-made in-situ IR reactor was designed and a sample preparing method was developed.With such progresses,the changes of reactants,products,surface adsorbates,and catalysts themselves can be measured under the same reaction conditions with a spectral range of 4000-400 cm^(-1),providing a new opportunity for in-situ characterization of heterogeneous catalysis.CO oxidation on Pd/SiO_(2) and Cu/SiO_(2) catalysts were taken as examples,since both the two catalytic systems were extensively used commercially,and moreover reduction and oxidation of palladium and copper occur during the examined reaction conditions.The characteristic bands of Pd^(2+)-O(670,608 cm^(-1)),Cu^(+)-O(635 cm^(-1))and Cu^(2+)-O(595,535 cm^(-1))were observed by IR,and the changes during CO oxidation reaction were successfully monitored by IR.The oxidation/reduction of palladium and copper were also confirmed by ex-situ XPS.Moreover,Pd^(0) in Pd/SiO_(2) and Cu^(+)in Cu/SiO_(2) were found as the thermal dynamically stable phases under the examined conditions for CO oxidation.

Catalytic Performance of Graphite Oxide Supported Au Nanoparticles in Aerobic Oxidation of Benzyl Alcohol： Support Effect

Various Au/GO catalysts were prepared by depositing Au nanoparticles on thermally- and chemically-treated graphite oxide （GO） supports using a sol-immobilization method. The surface chemistry and structure of GO supports were characterized by a series of analytical techniques including X-ray photoelectron spectroscopy, temperature-programmed desorption and Raman spectroscopy. The results show that thermal and chemical treatments have large influence on the presence of surface oxygenated groups and the crystalline structure of GO supports. A strong support effect was observed on the catalytic activity of Au/GO catalysts in the liquid phase aerobic oxidation of benzyl alcohol. Compared to the amount and the type of surface oxygen functional groups, the ordered structure of GO supports may play a more important role in determining the catalytic performance of Au/GO catalysts.

Study on Deactivation by Sulfur and Regeneration of Pd/C Catalyst in Hydrogenation of N-（3-nitro-4-methoxyphenyl） Acetamide

Deactivation of Pd/C catalyst often occurs in liquid hydrogenation using industrial materials. For in-stance, the Pd/C catalyst is deactivated severely in the hydrogenation of N-(3-nitro-4-methoxyphenyl) acetamide. In this study, the chemisorption of sulfur on the surface of deactivated Pd/C was detected by energy dispersive spec-trometer and X-ray photoelectron spectroscopy. Sulfur compounds poison the Pd/C catalyst and increase the forma-tion of azo deposit, reducing the activity of catalyst. We report a mild method to regenerate the Pd/C catalyst: wash the deposit by N,N-dimethylformamide and oxidize the chemisorbed sulfur by hot air. The regenerated Pd/C cata-lyst can be reused at least ten runs with stable activity.

Room temperature gas sensor based on tube-like hydroxyapatite modified with gold nanoparticles

The main goal of this work is to explore the possibility of using Au-modified hydroxyapatite(HA) as a potential sensor material. Tube-like HA structure was fabricated with the aid of a Nafion N-117 cation exchange membrane and gold(Au) nanoparticles were added by a hydrothermal method. The morphology, structure and composition were characterized by scanning electron microscopy(SEM), transmission electron microscopy(TEM), X-ray diffraction(XRD), and X-ray photoelectron spectroscopy(XPS). The gas sensing properties were also investigated. Results show that Au nanoparticles are dispersed into the HA powder, which is tube-like, with rough inner and outer surfaces. Compared with pure HA, Au-modified HA exhibits improved sensing properties for NH_3. 5%(mass fraction) Au-modified HA shows the highest response with relatively short response/recovery time. The response is up to 79.2% when the corresponding sensor is exposed to 200×10^(-6) NH_3 at room temperature, and the response time and recovery time are 20 s and 25 s, respectively. For lower concentration, like 50×10^(-6), the response is still up to 70.8%. Good selectivity and repeatability are also observed. The sensing mechanism of high response and selectivity for NH_3 gas was also discussed. These results suggest that Au-HA composite is a promising material for NH_3 sensors operating at room temperature.

Evolution of Surface Oxide Film of Typical Aluminum Alloy During Medium-Temperature Brazing Process

The evolution of the surface oxide film along the depth direction of typical aluminum alloy under mediumtemperature brazing was investigated by means of X-ray photoelectron spectroscopy(XPS). For the alloy with Mg content below 2.0wt%, whether under cold rolling condition or during medium-temperature brazing process, the enrichment of Mg element on the surface was not detected and the oxide film was pure Al2O3. However, the oxide film grew obviously during medium-temperature brazing process, and the thickness was about 80 nm. For the alloy with Mg content above 2.0wt%, under cold rolling condition, the original surface oxide film was pure Al2O3. However, the Mg element was significantly enriched on the outermost surface during medium-temperature brazing process, and MgO-based oxide film mixed with small amount of MgAl2O4 was formed with a thickness of about 130 nm. The alloying elements of Mn and Si were not enriched on the surface neither under cold rolling condition nor during mediumtemperature brazing process for all the selected aluminum alloy, and the surface oxide film was similar to that of pure aluminum, which was almost entire Al2O3.