Post‐oxidizing effects on surface characteristics of salt bath nitrocarburized AISI 02 tool steel type

The effect of post‐oxidizing treatment on the characteristics of modified surface layers produced by salt bath nitrocarburizing on the industrial American Iron and Steel Institute (AISI) 02 tool steel types is investigated. Nitrocarburizing treatment is performed for 6 h and 8 h at 570 °C and post‐oxidizing treatment for 30, 60 and 90 min at 520 °C, using argon–steam mixture. Formed layers are characterized by their basic properties such as thickness layer, depth, surface hardness and wear resistance. Detailed estimation of the modified metal surface quality, in terms of chemical composition, formed phases, microstructures and diffusion mechanisms are performed by metallographic techniques, EDX, X‐ray diffraction, scanning electron microscopy (SEM) and glow discharge optical electron spectroscopy (GDOES). The corrosion resistance was investigated in 0.4 M H₂SO₄ solutions, using steady‐state electrochemical polarization methods. The obtained results revealed the existence of a superficial oxide layer which consists of magnetite (Fe₃O₄) and hematite (Fe₂O₃) and the presence of an ε‐phase associated with a small amount of γ′‐phase. Important improvements in wear, microhardness and corrosion resistance occur after these treatments and it is specifically concluded that the sole application of a nitrocarburizing treatment does not significantly ameliorate the corrosion resistance of the as‐received steel. In fact, post‐oxidation treatment contributes to increase corrosion resistance by forming a dense magnetite layer and at the same time, it partially covers the compound layer pores. Copyright © 2009 John Wiley & Sons, Ltd.     

Surface modification and wear test of carbon steel by plasma electrolytic nitrocarburizing

Plasma electrolytic nitrocarburizing (PEN/C) was applied to the surface of carbon steel under the boiling condition of saturated urea electrolyte. In addition to the general effect of the bath temperature, different applied voltages and processing times were also considered in this new process. Optical and scanning electron microscopy, X‐ray diffraction, microhardness and pin‐on‐disc wear tests were used to characterize the PEN/C‐treated surfaces. A mixture of θ‐(Fe₃C) and ε‐(Fe_2–3N) was found in the compound layers. At certain conditions, dense surface layers with minimum porosity were observed at the top of the samples. The boiling condition resulted in special character of the compound layers on the surface. The layers consisted of some irregularities grown inward the samples andaffected the characteristics of the surface layers. The microhardness of the PEN/C‐treated layers increased up to 1280 HV0.1, which was 3 to 4 times higher than that for untreated material and higher than that obtained by other investigators (750 HV0.1). PEN/C decreased the wear loss of carbon steel significantly due to the change of the adhesive wear of untreated material to the abrasive mode of treated surfaces. The major advantage of this technique was a higher growth rate of the nitrocarburized layers and a more significant improvement in the tribological performance of the treated samples if compared to similarly oriented surface treatments. Copyright © 2011 John Wiley & Sons, Ltd.     

Surface behavior and film formation analysis of sisal fiber coated by poly(methyl methacrylate) ultrathin film

Admicellar polymerization was used to modify a sisal fiber surface with poly(methyl methacrylate) (PMMA) in order to improve the compatibility between the sisal fiber and the surrounding polymeric matrix in a composite. The effect of the amount of monomer (methyl methacrylate) and initiator (sodium persulfate) on the hydrophobicity behavior and PMMA film formation of the admicellar-treated sisal surface was studied. The increase in the hydrophobicity of the admicellar-treated sisal fiber was examined by flotation testing, moisture absorption, and electrostatic charge or zeta (ζ) potential. The amount of PMMA film formed on the sisal surface was investigated by the weight loss of the admicellar-treated sisal extracted by acetone and chloroform; and the thermal degradation was studied by thermogravimetric analyses. The admicellar-treated sisal could float on the surface of water for longer than half an hour, and its moisture absorption decreased. The ζ potential of its surface also showed a significant change compared to the untreated sisal. The results from the weight loss indicated that the amount of PMMA formed on the sisal fiber surface depended on the amount of monomer and initiator. The Fourier transform infrared spectrum of the admicellar-treated sisal showed the characteristic peaks of PMMA and the scanning electron micrograph of the treated sisal was clearly different from the untreated sisal, confirming that there was a thin film coating on the admicellar-treated sisal fiber.     

Study of the spectroscopic characteristics of methyl (ligand) cobaloximes and their antibacterial activity

Spectroscopic characterization (IR, NMR and electronic spectra) of methyl (ligand) cobaloxime was done, where ligand = pyrazole, dimethyl pyrazole, alanine and alanine methyl ester. The frequency changes in the IR spectra and shifts in the NMR were explained on the basis of basicity of the ligand, steric hindrance, HSAB principle and dπ-pπ back-bonding from metal to ligand. Alanine and alanine methyl ester form more stable complexes than pyrazole and dimethyl pyrazole. Based on their IR and ¹H NMR spectra it is inferred that pyrazole and dimethylpyrazole bind to Co (III) via N-2 ring nitrogen, i.e. monodentate coordination.     

Theoretical Studies on Adsorption and Diffusion of Hydrogen Atom on Pd（311） and Ni（311） Stepped Surface

The adsorption and diffusion of hydrogen atom on open rough Pd(311) and Ni(311) stepped surface were investigated in detail using 5-parameter Morse Potential (5-MP for short) method. The results on theoretical studies indicate that only threefold adsorption states exist at low coverage, and fourfold states are annihilated on the top layer which become the diffusion channels between threefold adsorption states due to strong competition and repulsion between hydrogen adatoms.     

Surface characterization of laser-treated poly(ethylene terephthalate) by optical profilometry and scanning tunneling microscopy

Characteristic changes in the surface topography due to UV laser treatment are of high significance for the determination of material destruction thresholds and surface structure development. E.g. irradiation of poly(ethylene terephthalate) (PET) film with pulsed UV laser light of 248 nm modifies the smoth surface of the polymer into a well oriented structured surface. The development of these structures were studied with scanning tunneling microscopy (STM) and high resolution optical profilometry. Three dimensional data of the surface were taken from the samples after each laser pulse. A change of topographic data was found in relation to fluence and number of pulses applied. © 1993 John Wilcy & Sons, Inc.     

Surface characterization of polybutadiene and natural rubbers oxidized by silver(II)

Silver (II) ion is a powerful oxidizing mediator that was used for surface modification of vulcanized polybutadiene rubber (BR) and natural rubber (NR) through mediated electrochemical oxidation (MEO). Scanning electron microscopy (SEM) pictures showed that surface morphology of the oxidized rubbers was changed so that some cracks and holes appeared on the surface in macroscopic scale. This is possibly due to chain scission caused by alkane group formation which is in turn in accordance with the attenuated total reflection Fourier transform infrared (ATR-FTIR) spectra. The amounts of hydroxyl and carbonyl type surface functional groups were also increased in both oxidized rubbers. The results obtained by atomic force microscopy (AFM) showed that the surface roughness for both rubbers was changed significantly from nano- to micro-scale. Energy dispersive X-ray analysis (EDXA) expresses that surface concentration of atomic oxygen for both BR and NR was increased significantly. Also surface polarity of the treated rubbers was enhanced based on contact angle measurements leading to a higher hydrophilicity. Finally it was found that silver(II) has a somewhat greater oxidation impact on the surface of natural rubber than polybutadiene rubber.     

新型二茂铁甲基季铵盐离子液体的合成与表征

以二茂铁与二甲胺为原料合成了碘化二茂铁甲基季铵盐,再经复分解反应得到乙酸二茂铁甲基季铵盐离子液体;表征了离子液体的结构,测定了其熔点和溶解性.结果表明,合成的乙酸二茂铁甲基季铵盐离子化合物熔点低于100℃,是一种新型的二茂铁甲基季铵盐离子液体.     

Spectrophotometric determination of iron(III) and total iron by sequential injection analysis technique

A procedure for determination of concentrations of iron(III) and total iron by sequential injection analysis is described. The method is based on the strong blue-colored complexes formed between iron(III) and tiron. The absorbance of the complexes is measured spectrophotometrically at 635 nm. Oxidation of iron(II) and masking of interfering fluoride is simultaneously done by injecting one zone of hydrogen peroxide and one of thorium(IV) between the sample and reagent zones. Concentration of iron(III) and total iron, in the range 0.002–0.026 M, in diluted samples from a pickle bath were determined. The relative standard deviation was 0.4% (n=7). The method was also used in a pilot plant of a zinc process for determination of iron(III) in the range 0.2–3.0 g l⁻¹. The sample throughput is approximately 17 samples per hour, including three repetitive determinations of each sample.     

Crystallographic and electrochemical characteristics of La(0.7)Mg(0.3)Ni(5.0-x)(Al(0.5)Mo(0.5)x hydrogen-storage alloys.

The structure, hydrogen-storage property and electrochemical characteristics of La(0.7)Mg(0.3)Ni(5.0-x)(Al(0.5)Mo(0.5))x (x = 0-0.8) hydrogen-storage alloys have been studied systematically. X-ray diffraction Rietveld analysis shows that all the alloys consist of an La (La,Mg)2Ni9 phase and an LaNi5 phase. The pressure-composition isotherms indicate that the hydrogen-storage capacity first increases and then decreases with increasing x, and the equilibrium pressure decreases with increasing x. Electrochemical measurements show that the maximum discharge capacity and the exchange-current density of the alloy electrodes increase as x increases from 0 to 0.6 and then decrease when x increases further from 0.6 to 0.8. Moreover, the low-temperature dischargeability of the alloy electrodes increases monotonically with increasing x in the alloys.     

改性酚氧树脂/聚(甲基丙烯酸丁酯-co-4-乙烯基吡啶)共混物的相容-络合行为和表面表征

合成了一系列不同4-乙烯基吡啶含量的聚(甲基丙烯酸丁酯-co-4-乙烯基吡啶)(BVPy)共聚物,并对酚氧树脂(Phenoxy)的仲羟基进行了不同乙酰化程度的改性.用粘度法和激光光散射(LLS)研究了BVPy/改性Phenoxy共混物在溶液中的络合行为对氢键相互作用基团密度的依赖性,并用DSC研究了共混体系在本体中的相容性.将粘度法及LLS的结果结合起来,得到了改性Phenoxy/BVPy共混体系的不相容-相容-络合转变相图.在此基础上,用XPS初步考察了共混物的相容性对其表面组成的影响.结果表明,大分子间的络合相互作用可抑制共混物的表面富集.     

硝酸铈及热处理对化学镀Ni-W-P合金的性能影响

为提高化学镀Ni-W-P镀层的耐蚀性和耐磨性,拓宽其应用,采用电化学方法和热处理等手段,研究了镀液中添加剂硝酸铈(Ce(NO3)3)的质量分数和热处理对化学镀Ni-W-P镀层的沉积速度、孔隙率、失重腐蚀速度、腐蚀电位、腐蚀电流、交流阻抗、显微硬度、摩擦系数等性能的影响。结果表明:添加1.0 wt%Ce(NO3)3时,所得镀层的沉积速度最大(36.5 g/m2·h),孔隙率最低(0.8个/cm2),耐腐蚀性能最好。镀层的组织均匀、致密、无缺陷和非晶态结构是其耐蚀性能高的重要原因。100~600℃热处理后,镀层硬度和耐磨性有所提高,而400℃热处理之后,合金显微硬度高达1100 HV,是镀态的1.8倍。     

Thickness dependence of the structural,mechanical and electrical properties of Ni films deposited on polyimide by ion beam‐assisted deposition (IBAD)

Ni thin films with different thicknesses were deposited on pre‐treated polyimide substrates by ion beam‐assisted deposition. Dependence of structural, mechanical and electrical properties of the Ni films on their thickness was investigated. The results showed a clear correlation between film properties and film thickness. The inter‐diffusion at the interface regions of the films with different deposition time were demonstrated by transmission electron microscopy and X‐ray photoelectron spectroscopy. With increasing film thickness, surface roughness of the Ni films firstly decreased and then increased, while the grain size gradually increased. Residual stress of the Ni thin films decreased with increasing Ni film thickness up to 202 nm and then slightly increased as the film thickness further increased. Resistivity decreased, and temperature coefficient of resistivity (TCR) increased with increasing film thickness due to the enhancement of crystallization degree and the increase in grain size. The decrease in surface roughness and residual stress also contributed to the decrease of resistivity and the increase of TCR of the films. An optimal film thickness is suggested, which yielded a relatively high TCR value and low levels of both surface roughness and residual stress. Copyright © 2012 John Wiley & Sons, Ltd.     

Ni(115)台阶面对氢表面微观动力学行为的影响

用５参数Ｍｏｒｓｅ势模拟氢－镍表面体系相互作用势，考察了氢原子在Ｎｉ（１１５）台面上吸附扩散行为。同时构造了氢分子与Ｎｉ（１００）和Ｎｉ（１１５）台阶面 相互作用推广的ＬＥＰＳ势面面，考察了氢分子解离化学吸附的微观动力学性质。     

XPS and AES surface analysis of WC-Co-(Cr) cemented carbide after immersion in neutral solution

The binder phase Co in WC-Co cemented carbide is dissolved easily in corrosive media (even in neutral solution), which has limited its application in a wider range. In this paper, the influence of Cr on corrosion resistance of WC-Co immersed in neutral solution was studied, with a focus on the surface chemistry of the corrosion product. The results show that in neutral solution, the corrosion is mainly caused by the selective dissolution of Co and the dominant surface corrosion product after immersion is Co (OH)₂. The corrosion resistance of WC-Co cemented carbide can be improved by the addition of Cr. This can be explained by the formation of more protective chromium containing oxide on the binder phase of WC-Co-Cr alloy, leading to reduced corrosion rate.     

Surface segregation measurements of In and S impurities from a dilute Cu(In,S) ternary alloy

The surface segregation of In and S from a dilute Cu(In,S) ternary alloy were measured using Auger electron spectroscopy coupled with a linear programmed heater. The alloy was linearly heated and cooled at constant rates. Segregation data of a linear heat run showed surface segregation of In that reached a maximum surface coverage of 25% followed by S, which reached a coverage of 30%. It was found that after In had reached a maximum surface coverage, it started to desegregate as soon as the S enriched the surface until In was completely replaced by S. The segregation parameters, namely, the pre‐exponential factor (D₀), activation energy (Q), segregation energy (ΔG?) and interaction energy (Ω) were extracted from the measured segregation data for both In and S segregation in Cu by simulating the measured segregation data with a theoretical segregation model (modified Darken model). The segregation parameters obtained for In segregation in Cu are D₀ = 1.8 ± 0.5 × 10^?5 m² s^?1, Q = 184.3 ± 1.0 kJ.mol^?1, ΔG? = ?61.4 ± 1.4 kJ.mol^‐1, Ω_Cu?In = 3.0 ± 0.4 kJ.mol^?1; for S segregation in Cu the parameters are D₀ = 8.9 ± 0.5 × 10^?3 m² s^?1, Q = 212.8 ± 3.0 kJ.mol^?1, ΔG? = ?120.0 ± 3.5 kJ.mol^?1, Ω_Cu?S = 23.0 ± 2.0 kJ mol^?1 and the In and S interaction parameter is Ω_In?S = ?4.0 ± 0.5 kJ.mol^?1. The initial parameters used for the Darken calculations were extracted from fits performed with the Fick's and Guttmann model. Copyright © 2013 John Wiley & Sons, Ltd.     

Surface and mechanical analysis of metallized poly(dimethylsiloxane) gel for varifocal micromirrors

Varifocal micromirrors are alternative and miniaturized mirror systems that are used for imaging procedures in biomedical diagnostics, mirror-based tunable lenses, or the correction of spherical aberration. In this study, we demonstrate a new concept for focal length variation by electrostatic mirror deformation of a compact and integrated electroactive polymer actuator based on metallized poly(dimethylsiloxane) (PDMS) gel thin films. The varifocal micromirrors have a lateral size of 70 × 70 μm² and are capable of deforming in either convex or concave direction, depending on a defined surface treatment by O₂-plasma or UV/ozone of the PDMS prior to metallization by physical vapor deposition (PVD). Surface and interface analysis by wetting experiments, sputter depth-profiling X-ray photoelectron spectroscopy (XPS) combined with scanning electron microscopy (SEM) on cross-sections processed with focused ion beam (FIB) as well as polymer and metal surfaces are used to understand and to improve the metal film growth and quality with respect to high reflectivity and conductivity. In addition to the high quality of the metallic mirror layer, the mirror displacement is important and inevitably depends on the gel stiffness of the actuator. Therefore, we investigate the gel mechanics and the performance of the actuator with rheology, confocal microscopy, and image formation on the electrically deformed mirrors. Our concept of varifocal micromirrors offers a wide range of applications for tunable mirror-based optics due to their simple and compact design.     

The structure and electrochemical characteristics of La0.67Mg0.33 (Ni0.8Co0.1Mn0.1) x (x=2.5–5.0) multiphase alloys for nickel-metal hydride batteries

This paper presents results concerning structure and electrochemical characteristics of the La_0.67Mg_0.33 (Ni_0.8Co_0.1Mn_0.1) _x (x=2.5–5.0) alloy. It can be found from the result of the Rietveld analyses that the structures of the alloys change obviously with increasing x from 2.5 to 5.0. The main phase of the alloys with x=2.5–3.5 is LaMg₂Ni₉ phase with a PuNi₃-type rhombohedral structure, but the main phase of the alloys with x=4.0–5.0 is LaNi₅phase with a CaCu₅-type hexagonal structure. Furthermore, the phase ratio, lattice parameter and cell volume of the LaMg₂Ni₉phase and the LaNi₅ phase change with increasing x. The electrochemical studies show that the maximum discharge capacity increases from 214.7 mAh/g (x=2.5) to 391.1 mAh/g (x=3.5) and then decreases to 238.5 mAh/g (x=5.0). As the discharge current density is 1,200 mA/g, the high rate dischargeability (HRD) increases from 51.1% (x=2.5) to 83.7% (x=3.5) and then decreases to 71.6% (x=5.0). Moreover, the exchange current density (I ₀) of the alloy electrodes first increases and then decrease with increasing x from 2.5 to 5.0, which is consistent with the variation of the HRD. The cell volume reduces with increasing x in the alloys, which is detrimental to hydrogen diffusion and accordingly decreases the low-temperature dischargeability of the alloy electrodes.     

Hydrogel networks of poly(ethylene oxide) star-molecules supported by expanded polytetrafluoroethylene membranes: characterization, biocompatibility evaluation and glucose diffusion characteristics

The present work discusses the grafting by electron beam irradiation of poly(ethylene oxide) (PEO) star-shaped polymers onto porous expanded polytetrafluoroethylene (EXPTFE) surfaces. The resulting materials are intended to combine the good biocompatible properties of PEO with the outstanding mechanical properties of PTFE. The star-shaped PEOs were synthesized via anionic polymerization. 3 Mev electron beam irradiation was applied to graft these PEO stars onto porous EXPTFE surfaces. The hydrophobic EXPTFE surface had to be pre-modified with N-vinylpyrrolidone. ESCA was used to quantify the amount of grafted star-shaped PEO. Unmodified EXPTFE surfaces are well known, when implanted in a body, to be rapidly covered by a layer of cells and fibrin. The EXPTFE coated with PEO were implanted in the peritoneal cavity of rats (or under the back skin). This implantation did not induce any inflammation reactions and SEM analysis had attested the absence of adsorbed cells and fibrin. The glucose diffusion properties of these membranes were studied by a lag time analysis method and compared to those of pure PEO hydrogels. As expected, glucose diffuses through the hydrogel coated membrane and diffusion is not affected by the presence of the EXPTFE membrane.