Microstructure and growth kinetics of silicide coatings for TiAl alloy

In order to improve the oxidation resistance of Ti Al alloy, silicide coatings were prepared by pack cementation method at 1273, 1323, and 1373 K for 1-3 hours. Scanning electron microscopy(SEM), energy dispersive spectrometry(EDS) and X-ray diffraction(XRD) were employed to investigate the microstructures and phase constitutions of the coatings. The experimental results show that all silicon deposition coatings have multi-layer structure. The microstructure and composition of silicide coatings strongly depend on siliconizing temperatures. In order to investigate the rate controlling step of pack siliconizing on Ti Al alloy, coating growth kinetics was analyzed by measuring the mass gains per unit area of silicided samples as a function of time and temperature. The results showed that the rate controlling step was gas-phase diffusion step and the growth rate constant(k) ranged from 1.53 mg~2/(cm~4·h~2) to 2.3 mg~2/(cm~4·h~2). Activation energy(Q) for the process was calculated as 109 k J/mol, determined by Arrhenius' equation: k = k0 exp[–Q/(RT)].     

包渗法制备硅化物涂层的结构形貌及形成机理

采用包渗法在C-103铌合金基体上制备MoSi2涂层,通过X射线衍射、扫描电镜和能谱分析等手段研究涂层表面、截面形貌以及氧化后涂层结构变化,并分析硅化过程中涂层的形成机理。研究结果表明：包渗法制备硅化物涂层是通过反应扩散形成的,硅化过程服从抛物线规律;该涂层为复合结构：MoSi2相为主体层;以NbSi2相为主、并含少量Nb5Si3相的两相为过渡区;Nb5Si3相为扩散层。在高温氧化环境下,涂层表面生成致密的非晶氧化层,有效地阻止了氧向涂层内扩散。     

Microstructure and electrochemical behavior of laser cladded HA coating on pure titanium TA2

Hydroxyapatite (HA, Ca10(PO4)6(OH)2) coating was fabricated on pure Ti (TA2) by laser cladding technology. The phase structure, microstructure, microhardness and electrochemical behavior of the laser cladded HA coating in artificial body fluid were investigated. The results show that the HA coating is mainly composed of highly crystallized HA. A transitional layer between HA coating and Ti substrate is formed. Microhardness measurement shows the gradually increasing of microhardness from 150 HV at TA2 substrate to 600 HV at transitional layer, and followed by a decreasing to 400 HV at HA coated layer. Electrochemical corrosion tests show that the HA coating has higher open circuit potential , lower corrosion current density and corrosion rate in comparison to the TA2 substrate.     

Metallurgical microstructure control in metal-silicon reactions

A comprehensive review on interfacial reactions to form silicides between metal and Si nanowire or wafer is given.Formation of silicide contacts on Si wafers or Si nanowires is a building block needed in making current-based Si devices.Thus,the microstructure control of silicide formation on the basis of kinetics of nucleation and growth has relevant applications in microelectronic technology.Repeating events of homogeneous nucleation of epitaxial silicides of Ni and Co on Si in atomic layer reaction is presented.The chemical effort on intrinsic diffusivities in diffusion-controlled layer-typed intermetallic compound growth of Ni2Si is analyzed.     

SiC/Si-W-Mo coating for protection of C/C composites at 1873 K

In order to prevent carbon/carbon composites from oxidation at 1873 K, an efficient oxidation protective SiC/Si-W-Mo coating was prepared by a two-step pack cementation technique. The microstructures and the phase composition of the as-received multi-coating were examined by scanning electron microscopy （SEM） and X-ray diffraction （XRD）. It is seen that the compact multi-coating is composed of α-SiC, Si, and （WxMO1-x）Si2. Oxidation test shows that, after oxidation at 1873 K in air for 102 h and thermal cycling between 1873 K and room temperature for 10 times, the weight loss of the SiC/Si-W-Mo coated C/C composites is only 0.26%. The invalidation of the multi-coating is attributed to the formation of penetrable cracks in the coating. 2008 University of Science and Technology Beijing. All rights reserved.     

Microstructures and wear resistance of chromium coatings on P110 steel fabricated by pack cementation

In order to obtain a high-performance surface on P110 steel that can meet the requirements in oil/gas field environment, the chromium coatings were fabricated by pack cementation. The chromium coatings differed in with/without the addition of La₂O₃. Scanning electron microscope (SEM), energy dispersive X-ray spectrometer (EDS), X-ray diffractometer (XRD) and microhardness tester were employed to investigate the surface morphologies, surface element distributions, microstructures, phase constitutions and microhardness of the coatings. Friction-wear tests of the P110 steel substrate and the coatings were conducted in air at ambient temperature and humidity. The results show that uniform and continuous coatings are formed on P110 steel regardless of adding La₂O₃ or not. The chromium coatings consist of Cr₂₃C₆, Cr₇C₃, and (Cr, Fe)₇C₃. The La₂O₃-added chromium coating is more beneficial in terms of surface morphology, microstructure, thickness and microhardness as compared with the coating without adding La₂O₃. Chromizing treatment significantly improves the surface hardness and wear resistance of the P110 steel. The wear resistance of the tested samples can be sorted in the following sequence: La₂O₃-coating>no RE-coating>bare P110 steel.     

Modification of LiCo1/3Ni1/3Mn1/3O2 cathode material by CeO2-coating

LiCo_1/3Ni_1/3Mn_1/3O₂ was coated by a layer of 1.0 wt% CeO₂ via sol-gel method. The bared and coated LiMn_1/3Co_1/3Ni_1/3O₂ was characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), cyclic voltammogram (CV) and galvanotactic charge-discharge test. The results show that the coating layer has no effect on the crystal structure, only coating on the surface; the 1.0 wt% CeO₂-coated LiCo_1/3Ni_1/3Mn_1/3O₂ exhibits better discharge capacity and cycling performance than the bared LiCo_1/3Ni_1/3Mn_1/3O₂. The discharge capacity of 1.0 wt% CeO₂-coated cathode is 182.5 mAh·g⁻¹ at a current density of 20 mA·g⁻¹, in contrast to 165.8 mAh·g⁻¹of the bared sample. The discharge capacity retention of 1.0 wt% CeO₂-coated sample after 12 cycles reaches 93.2%, in comparison with 86.6% of the bared sample. CV results show that the CeO₂ coating could suppress phase transitions and prevent the surface of cathode material from direct contact with the electrolyte, thus enhance the electrochemical performance of the coated material.     

Corrosion resistance of plasma sprayed NiCrAl+(ZrO2+Y2O3) thermal barrier coating on 18-8 steel surface

The corrosion resistance of NiCrAl+(ZrO₂+Y₂O₃) thermal barrier coating, formed with the plasma spraying technique, on the 18 - 8 steel surface was investigated. The phase structure and morphology of the coating were analyzed by means of X-ray diffraction (XRD) and scanning electron microscopy (SEM). The electrochemical corrosion behavior of the coating in 1.0 mol/L H₂SO₄ solution was studied by using electrochemical measurement methods. The results show that the gradient plasma spraying coating is composed of the NiCrAlY coating and the (ZrO₂+Y₂O₃) top coating, and the coating thickness is 360 μm. The microhardness of coating reaches 1 100 HV. The corrosion resistance of the plasma sprayed coating of the 18 - 8 steel surface is about 5 times as great as that of the original pattern. The corrosion resistance of the coating is enhanced notably. Foundation item: Project (5040202140) supported by Scientific Research Common Program of Beijing Municipal Commission of Education     

铜表面气体渗硅后的滑动摩擦磨损研究

本文对用硅烷－氢（ＳｉＨ４／Ｈ２）混合气体在铜表面进行化学热处理获得的含硅表层进行了摩擦磨损研究．结果表明，在铜表面生成的含硅层可以降低摩擦系数；在低负荷干摩擦条件下，含硅表层的磨损率有较大程度的改善     

Influence of deposition voltage on phase, microstructure and antioxidation property of cristobalite aluminum phosphate coatings

Cristobalite aluminum phosphate (C-AlPO₄) coatings were prepared by a hydrothermal electrophoretic deposition process on SiC-coated C/C composites. Phase compositions and microstructures of the as-prepared coatings were characterized by XRD and SEM analyses. The influence of deposition voltage on the phase, microstructure and antioxidation property of the cristobalite aluminum phosphate coatings was investigated. Results show that the as-prepared coatings are composed of cristobalite aluminum phosphate crystallites. The thickness and density of cristobalite aluminum phosphate coatings are improved with the increase of deposition voltage. The deposition amount and bonding strength of the cristobalite aluminum phosphate coatings also increase with the increase of deposition voltage. The deposition mass per unit area of the coatings and the square root of the deposition time at different hydrothermal voltages satisfy linear relationship. The antioxidation property of the coated C/C composites is improved with the increase of deposition voltage. Compared with SiC coatings prepared by pack cementation, the multilayer coatings prepared by pack cementation with a later hydrothermal electrophoretic deposition process exhibit better antioxidation property. The as-prepared multi-coatings can effectively protect C/C composites from oxidation in air at 1 773 K for 37 h with a mass loss rate of 0.53%.     

Fabrication and microstructure of SiO2−GeO2 sol-gel glass coatings

SiO₂−GeO₂ sols and gel glass coatings with different contents of germanium dioxide were fabricated. Stable and transparent sols could only be obtained when the content of GeO₂ was under 35%. It is shown by SEM that only one continuous phase is observed in the coating of 65SiO₂·35GeO₂ and plenty of Ge, O and Si were all found in it. However, the separated phase is found in the coating of 60SiO₂·40GeO₂ and a large number of Ge and O. It is proved by the Raman scattering investigation that the separated phase in the coating of 60SiO₂ ·40GeO₂ is germanium dioxide. The congeries of hydrolystates of Cl₃ GeCH₂ CH₂ COOH play the main role in the formation of the separated phase when the proportion of GeO₂ is much higher. Si−O−Ge, Si−O−Si, and Ge−O−Ge bonds form in the coating of 65SiO₂·35GeO₂ and this coating is homogenous. Jing Cheng-bin: Born in 1974 This work was partly financially supported by the Foundation of Key Teachers of Ministry of Education, China     

Properties of plasma sprayed NiCrAlY+(ZrO2+Y2O3) coating on refractory steel surface

NiCrAlY+(ZrO₂+Y₂O₃) thermal barrier coating was prepared on the surface of refractory steel 1Cr18Ni9Ti with plasma spraying technique. The phases and microstructure of the thermal barrier coating were determined by scanning electron microscopy (SEM) and X-ray diffraction (XRD). The results show that the bonding between thermal barrier coating and substrate is sound. The surface hardness of 1Cr18Ni9Ti reaches up to 1 000 HV, but that of substrate is only 300 HV. The patterns sprayed with CoNiCrAlY+(ZrO₂+Y₂O₃) ceramic coating have a good heat insulation effect at 800 °C for heat insulation temperature difference reaches 54 °C, which increases the operating temperature and service life of refractory steel. Foundation item: Project (5040202140) supported by Scientific Research Common Program of Beijing Municipal Commission of Education     

The electronic structure and grain boundary segregation by boron addition

The electronic structure and grain boundary segregation caused by boron addition to Ni₃Al have been studied by X-ray photoelectron spectroscopy and Auger electron spectroscopy, respectively. The obtained results show that the Ni2p_3/2 electron binding energy rises gradually in the sequence of pure Ni<Ni₇₆Al₂₄<Ni₇₄Al₂₆<Ni₇₅Al₂₅, while it reduces monotonously with an increase in boron addition to Ni₃Al. Besides, it is found that the grain boundary segregation of boron occurring in Ni₃Al is a combined equilibrium and non-equilibrium type in nature. Based on the concept of the bonding environmental inhomogeneity, measured by the shift in Ni2p_3/2 electron binding energy from the nickel atoms in the simple substance nickel to those in the intermetallic compound Ni₃Al (ΔE _B), being responsible for the brittle behavior of the alloy, a binding energy shifting criterion for the brittle-ductile fracture transition in Ni₃Al is presented; when ΔE _B>0, the brittle failure occurs in Ni₃Al; when δE _B<0, the ductile one appears. Combined with the above experimental rules, the criterion predicts that pure Ni₃Al is brittle, and there exist the stoichiometric effect and concentration effect in the ductilization process for Ni₃Al by boron addition. Hence the criterion can be taken as a theoretical guide to alloy design in developing ductile intermetallics. Project supported by the National Natural Science Foundation of China.     

Synthesis and sintering of Mg<Subscript>2</Subscript>Si thermoelectric generator by spark plasma sintering

Raw Mg,Si powder were used to fabricate Mg2Si bulk thermoelectric generator by spark plasma sintering （SPS）.The optimum parameters to synthesize pure Mg2Si powder were found to be 823 K,0 MPa,10 min with excessive content of 10wt% Mg from the stoichiometric Mg2Si.Mg2Si bulk was synthesized and densified simultaneously at low temperature （823 K） and high pressure （higher than 100 MPa） from the raw powder,but Mg,Si could not react completely,and the sample was not very dense with some microcracks on the surface.Then,Mg,Si powder reacted at 823 K,0 MPa,10 min in SPS chamber to form Mg2Si green compact,again sintered by SPS at 1023 K,20 MPa,5 min.The fabricated sample only contained Mg2Si phase with fully relative density.     

Fabrication of W@Cu composite powders by direct electroless plating using a dripping method

A direct electroless copper (Cu) coating on tungsten powders method requiring no surface treatment or stabilizing agent and using glyoxylic acid (C₂H₂O₃) as a reducing agent was reported. The effects of copper sulfate concentration and the pH of the plating solution on the properties of the prepared W@Cu composite powders were assessed. The content of Cu in the composite powders was controlled by adjusting the concentration of copper sulfate in the electroless plating solution. A uniform, dense, and consistent Cu coating was obtained under the established optimum conditions (flow rate of C₂H₂O₃ = 5.01 mL/min, solution pH = 12.25 and reaction temperature 45.35 °C) by using central composite design method. In addition, the crystalline Cu coating was evenly dispersed within the W@Cu composite powders and Cu element in the coating existed as Cu0. The formation mechanism for the W@Cu composite powders by electroless plating in the absence of surface treatment and stabilizing agent was also proposed.     

Morphology and tribological properties of Ni/n-SiO2 composite coatings by pulse-reverse current brush-plating

Ni/n-SiO₂ composite coating was electrodeposited by brush-plating with pulse-reverse current(RC). The morphology, hardness, and tribological properties of the coating were investigated and compared with those of Ni and composite coatings electrodeposited with direct current (DC). The results indicate that Ni/n-SiO₂ composite coating electrodeposited by RC, because of RC and the nano powders, has denser coating, finer crystal grains, higher hardness (HV650.0, nearly 1.5 times higher than that of Ni coating electrodeposited by DC) and lower friction coefficient (nearly 0.62), as a result, in the wearing experiment, the Ni/n-SiO₂ composite coating electrodeposited by RC has the least worn loss. So this kind of coating has better wear resistance. And RC electro brush-plating can be used as a new technology of brush-plating in the area of wear resistance. Foundation item: Project (50235030) supported by the National Natural Science Foundation of China; Project (51489020104JS9102) supported by the National Key Laboratory for Remanufacturing     

Growth characteristics and kinetics of niobium carbide coating obtained on AISI 52100 by thermal-reactive diffusion technique

Niobium carbide coating was produced by thermal-reactive diffusion technique on AISI 52100 steel in salt bath at 1 123 K, 1 173 K, and 1 223 K for 1, 2, 4, and 6 hours. The salt consisted of borax, sodium fl uoride, boron carbide, and niobium pentoxide. The presence of NbC phase on the steel surface was confi rmed by X-ray diffraction analysis. Microscopic observation showed that niobium carbide coating formed on the substrate was smooth and compact. There was a distinct and fl at interface between the coating and substrate. The micro-hardness of niobium carbide coating was 2892±145HV. The thickness of coating ranged from 1.6 μm to 14μm. The forming kinetics of niobium carbide coating was revealed. Moreover, a contour diagram derived from experimental data was graphed for correct selection of process parameters. Some mathematical equations were built for predicting the coating thickness with predetermined processing temperature and time. The results showed that these mathematical equations are very practical as well as the kinetics equation.     

Graded materials of (TiB<Subscript>2</Subscript>)<Subscript>p</Subscript>Ni with nickel substrate prepared by field-activated pressure-assisted synthesis process

The preparation of functionally graded materials (FGMs) of (TiB₂)_pNi with an intermetallic compound media layer of Ni₃Al and a substrate of nickel by field-activated pressure-assisted synthesis process (FAPAS) was investigated. Ni₃Al was chosen as a layer of FGM for the first time due to its great deal of heat released during its synthesis from nickel and aluminium powder. The microstructure, phase composition of layers, micro-hardness and elemental concentration profiles across interfaces were characterized. The significant inter-diffusion of elements between layers showed the formation of good bonds. The measured micro-hardness values of the sample increased monotonically to more than 3 500 HK over a distance of 2 mm from the nickel substrate to the surface layer (TiB₂)_pNi. The results of this investigation demonstrate the feasibility of the FAPAS process for rapid formation of FGMs with good diffusion bonds.     

Effect of temperature on microstructure ofmolybdenum diffusion coating on titanium substrate

The halide-activated pack cementation process was used to form molybdenum diffusion coating on titanium substrate. The morphology, structure, elements diffusion distribution and microhardness of the coatings formed at different diffusion temperatures were studied. The results indicate that the coating is made up of deposition layer and diffusion layer, and the surface roughness of specimens is increased after diffusion. In the diffusion layer, the major phases are Mo and β-Ti phase with addition of α′-Ti phase and α″-Ti phase. And the phase composition of Mo →β→α″→α′ is formed for different Mo contents in the diffusion layer from outside to inside. The diffusion of Ti element is very obvious as well as Mo element. With increasing the diffusion temperature, the thickness of diffusion layer is increased rapidly, and the microhardness is changed more smoothly with diffusion depth, which shows the same distribution rules as the Mo content.     

Microstructure evolution of AS41 magnesium alloy fabricated by ultrasonic vibration

The effects of ultrasonic vibration on the grain size and morphology of Mg2Si in Mg-4 wt% Al-1 wt%Si(AS41) alloys designed were evaluated. The results show that the major constituents of the alloy include β-Mg17Al12 and Mg2Si phase, and no difference in the type of constituents between without ultrasonic vibration and with ultrasonic vibration. Without any ultrasonic vibration, the grain size and Mg2Si phase in AS41 alloy are coare structure. However, the microstructure with fine uniform grains and Mg2Si particles are achieved with ultrasonic vibration. The crystal grains and Mg2Si particles refine with increase in the ultrasonic vibration intensity. When the ultrasonic vibration intensity was too low or too high, coarse structures could be obtained. The analysis of refinement mechanism indicates that the acoustic cavitation and flows induced by ultrasonic vibration lead to the fine uniform microstructure.