Magnetron sputtered nanocrystalline metastable (V,Al)(C,N) hard coatings

Nanocrystalline hard coatings of the system V-Al-C-N with an f.c.c. metastable solid solution (V,Al)(N,C) microstructure were deposited by non-reactive r.f.-magnetron sputtering of a ceramic compound target (composition: 60 mol.% VC and 40 mol.% AIN) in a pure argon discharge at 1.1 Pa. The chemical composition of the as-deposited coatings was determined by electron probe micro analysis (EPMA). The microstructure of the thin films was characterized by scanning electron microscopy (SEM), X-ray diffraction (XRD), transmission electron microscopy (TEM), and selected area electron diffraction (SAED). The influence of a moderate argon ion bombardment during thin film deposition, realized through the variation of the argon ion energy in the range 20 eV-170 eV, as a means to adjust the adatom surface mobility and surface diffusion processes, on the microstructure evolution and on the Vickers micro-hardness is discussed. The conditions for the formation of a metastable solid solution f.c.c. (V,AI)(C,N) thin film microstructure are described in terms of surface processes during film growth and thermodynamic considerations. It was demonstrated, that a metastable phase formation in the quaternary material system V-Al-C-N can easily be adjusted in magnetron sputter deposition.     

Effect of the aluminium content and the bias voltage on the microstructure formation in Ti1 − xAlxN protective coatings grown by cathodic arc evaporation

The effect of aluminium contents and bias voltage on the microstructure of cathodic arc evaporated Ti_1 − xAl_xN coatings was investigated with the aid of X-ray diffraction experiments and transmission electron microscopy. The coatings were deposited from mixed Ti-Al targets with different Ti:Al ratios (60:40, 50:50, 40:60 and 33:67) at bias voltages ranging between − 20 V and − 120 V. The microstructure of the coatings was described in terms of the phase composition, crystallite size and residual stress and related to the indentation hardness. The microstructure features were found to be related to the uniformity of the local distribution of Ti and Al in (Ti,Al)N, which was controlled, for a certain overall chemical composition of the coatings, by the bias voltage. The consequences of large local fluctuations of the Ti and Al concentrations in Ti_1 − xAl_xN that occurred at higher bias voltages were the phase segregation, which was indicated through the formation of the fcc-(Ti,Al)N/fcc-AlN nanocomposites and the increase of the compressive residual stress in the face-centred cubic (Ti,Al)N. Concurrently, the increasing bias voltage contributed significantly to the reduction of the crystallite size. Higher residual stress and smaller crystallite size increased the hardness of the coatings. The overall chemical composition of the coatings influenced mainly their phase composition. The high concentration of Al in (Ti,Al)N led to the formation of wurtzitic AlN in the coatings.     

Surface protection of titanium and titanium–aluminum alloys against environmental degradation at elevated temperatures

Experiments have been undertaken to explore the possibility of creating an oxygen barrier coating, which is effective in preventing oxidation and oxygen embrittlement of Ti and several low-Al content Ti-base alloys during exposure to oxidizing environments at elevated temperatures. The fabrication process has involved three steps, namely co-deposition of Ti and Al by magnetron sputtering onto a substrate material to be protected, followed by vacuum annealing and plasma immersion ion implantation of fluorine. The first two steps produce an overlay of γ-TiAl while the last step provides the necessary conditions for bringing about the halogen effect upon subsequent high-temperature oxidation. Analysis techniques such as cross-sectional transmission electron microscopy (XTEM) in conjunction with electron energy loss spectroscopy (EELS), energy-dispersive X-ray spectroscopy (EDX), X-ray diffraction (XRD), and elastic recoil detection (ERD) have been used to study the microstructure, phase formation and depth distribution of the elements in the coating material. Following oxidation in air at 600 °C for 100 h, specimens have been prepared for metallographic analysis, and their cross sections have been characterized by scanning electron microscopy (SEM) in combination with EDX, and electron probe microanalysis (EPMA). The results obtained show that during oxidation exposure the coating is capable of forming a protective alumina-containing scale which serves as an oxygen barrier, thereby preventing oxygen embrittlement. In addition, since the only constituents of the coating are Ti and Al, it exhibits excellent chemical substrate compatibility.     

Structure of Al–Fe alloys prepared by different methods after severe plastic deformation under pressure

Al–Fe alloys prepared by casting, rapid quenching from the melt, and mechanical alloying from elemental powders have been studied using X-ray diffraction analysis, optical metallography, transmission electron microscopy, and microhardness measurements in the initial state and after severe plastic deformation by high-pressure torsion using Bridgman anvils. The relationship between the phase composition, microstructure, and the microhardness of the investigated alloys has been established.     

Protective behavior of an SO2/CO2 gas mixture for molten AZ91D alloy

The protective behavior for a molten AZ91D alloy in an open melting furnace was investigated under a protective gas mixture containing 3% SO2 and 97% CO2, and the protection mechanism was discussed. Experimental results show that the gas mixture provides effective protection for AZ91D melt in the temperature range from 680 oC to 730 oC. The microstructure, chemical composition and phase composition of the surface film formed on the molten AZ91D alloy were analyzed using scanning electron microscopy (SEM) with energy dispersive spectrometer (EDS) and X-ray diffraction (XRD). The SEM results demonstrate that the surface films with an average thickness between 0.5 μm and 2 μm are dense and coherent in the protected temperature range. The EDS results reveal that the surface film mainly contains elements S, C, O, Al and Mg. The XRD results show that the surface film consists of MgO, MgS and a small amount of C phase.     

B_4C/BN纳米复合粉末的制备与显微结构的研究

利用H38O3和CO(NH2)2在高温下发生化学反应生成纳米BN,并且形成纳米BN包覆B4C颗粒的B4C/BN纳米复合粉末.利用X射线衍射(XRD),透射电镜(TEM)和选区电子衍射(SAED)对所制备的复合粉末的物相组成和显微结构进行了研究,并且对热压烧结块材的物相组成进行了研究.物相组成和显微结构的研究结果表明,在850℃氮气气氛下热处理6 h所得到的复合粉末主要是非晶态纳米BN涂层包覆在B4C颗粒表面所形成的B4C/BN纳米复合粉末,而且非晶态BN包覆层的厚度为300～500 nm.此非晶态BN相在1850℃,30 MPa,1 h的热压烧结工艺条件下完全转变成晶态的h-BN相.     

Effects of Ti_(0.5)Al_(0.5)N coatings on the protecting against oxidation for titanium alloys

Ti0.5Al0.5N coatings were deposited on TC11(Ti-6.5Al-3.5Mo-1.5Zr-0.3Si) and silicon substrates using a cathode arc ion-plating system.The microstructure, composition, phase structure, and oxidation-resistance of the alloys and nitride coatings were investigated by scanning electron microscopy, X-ray diffraction, transmission electron microscopy, Auger electron spectroscopy, and thermal analyzer.The results show that the oxidation resistance of the titanium alloy is relatively limited;the compound structures of Ti mixed with Al oxides are formed during the heating process.The phases of the Ti0.5Al0.5N coatings are composed of a TiN solid solution phase.The oxidation kinetics obeys the parabolic law.During the oxidation process, the selective oxidation of Al occurs, thus protecting the underlying coating and substrate.     

定向凝固下Ti-48Al合金与不同氧化物铸型涂层界面反应的研究

通过SEM、EDS以及XRD等检测方法对Ti-48Al合金分别与Al2O3、Y2O3、ZrO2铸型涂层的界面反应处的微观组织、元素分布以及界面处的相组成等进行检测;同时结合对界面处的硬度测量,得到界面反应层厚度。结果表明,合金熔体与不同铸型涂层均发生了界面反应。铸型涂层材料不同,界面反应剧烈程度也不同。反应过程中在熔体和扩散元素的冲击下,物理侵蚀和化学反应同时存在形成了反应层,反应的强弱则与涂层材料有关。更值得注意的是,对钛铝合金与铸型涂层的热力学性质进行了计算。研究还表明,熔体在界面处的反应层主要由涂层材料的脱落扩散程度控制,涂层中的元素尤其是O元素的扩散是控制界面反应进程的重要因素。     

35CrMo钢表面电火花沉积NiCr合金强化层特性的研究

采用电火花沉积技术,以NiCr合金为堆焊电极,在35CrMo钢表面沉积NiCr合金强化涂层。用显微硬度计测试了涂层的显微硬度,用SEM,EDX,XRD等方法表征了涂层的微观结构、化学成分分布及相组成。结果表明:涂层的表面显微硬度约为基体的2倍;涂层与基体的主要元素发生了相互扩散,涂层是由基体与NiCr合金电极发生反应形成的冶金结合层,主要成分为NiCrFe和FeNi。     

Investigating the microstructure and composition of cold gas-dynamic spray (CGDS) Ti powder deposited on Al 6063 substrate

The compositional variation, morphology and microstructure of cold gas-dynamic spray are of great importance for its proper application. This study investigates titanium powder deposition on an Al 6063 substrate using light optical microscopy, scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The composition was examined using energy dispersive X-ray spectroscopy (EDX), X-ray diffraction, X-ray photoelectron spectroscopy (XPS) and time-of-flight secondary ion mass spectrometry (ToF SIMS). Optical and electron microscopy revealed heavily deformed Ti powder particles penetrating 10 to 30 μm into the Al substrate. Examination using TEM did not reveal any evidence of second phases at the interface suggesting a sharp transition between the two metals. The presence of nanocrystals and grain refinement of both the coating and the substrate suggest the formation of a partial hetero-epitaxy condition near the interface. EDX results from a dedicated high-resolution scanning transmission electron microscope showed a sharp compositional change with a maximum inter-diffusion region of about 5 nm. Bonding of the coating to the substrate is therefore thought to be achieved by the particle/substrate interlocking and direct metal to metal bonding. However, it is most likely that the refine crystalline structure near the interface will be beneficial to the adhesion of the coating. XPS and ToF SIMS provided evidence of nitrogen pick-up during the spray process in the form of N and TiN even when utilizing Helium as the gas carrier. The presence of TiN suggests reaction of the Ti with the entrained air during spraying which explains the occurrence of flashing jet outside the nozzle. Investigation of the material properties using nanoindentation showed reasonably consistent hardness and elastic modulus values throughout the titanium coating and at the transition region. The hardness was slightly higher than typical commercially available bulk Ti.     

Thin Yttria-Stabilized Zirconia Coatings Deposited by Low-Energy Plasma Spraying Under Very Low Pressure Condition

In recent decades, very low pressure plasma spraying (VLPPS) technology (less than 10 mbar), as a next-generation coating process, has been extensively studied, because it can fully evaporate the materials to deposit dense, thin, and columnar grain coatings. This research aims at applying VLPPS with low-energy plasma source to melt or evaporate ceramic materials to develop high-quality thermal barrier coatings. Thin and homogeneous yttria-stabilized zirconia coatings were deposited successfully on a stainless steel substrate using low-power plasma spraying torch F100 (23 kW maximal) under very low pressure (1 mbar). The optical emission spectroscopy was used to analyze the properties of the plasma jet. The phase composition and the microstructure of the coatings were characterized by x-ray diffraction and scanning electron microscopy. The results showed that the YSZ powder was fully melted and partially evaporated, and the coatings had a hybrid microstructure that was combined with the condensation of the YSZ vapor and the melted particles. In addition, the porosity and microhardness of the coatings were evaluated.     

Evolution of microstructure,hardness, and corrosion properties of high-entropy Al0.5CoCrFeNi alloy

In this study, we investigate the microstructure, hardness, and corrosion properties of as-cast Al_0.5CoCrFeNi alloy as well as Al_0.5CoCrFeNi alloys aged at temperatures of 350 °C, 500 °C, 650 °C, 800 °C, and 950 °C for 24 h. The microstructures of the various specimens are investigated using X-ray diffraction (XRD), scanning electron microscopy (SEM), and electron probe X-ray microanalysis (EPMA). The results show that the microstructure of as-cast Al_0.5CoCrFeNi comprises an FCC solid solution matrix and droplet-shaped phases (Al–Ni rich phases). At aging temperatures of between 350 and 950 °C, the alloy microstructure comprises an FCC + BCC solid solution with a matrix, droplet-shaped phases (Al–Ni rich phase), wall-shaped phases, and needle-shaped phases (Al–(Ni, Co, Cr, Fe) phase). The aging process induces a spinodal decomposition reaction which reduces the amount of the Al–Ni rich phase in the aged microstructure and increases the amount of the Al–(Ni, Co, Cr, Fe) phase. The hardness of the Al_0.5CoCrFeNi alloy increases after aging. The optimal hardness is obtained at aging temperatures in the range 350–800 °C, and the hardening effect decreases at higher temperatures. Both the as-cast and aged specimens are considerably corroded when immersed in a 3.5% NaCl solution because of the segregation of the Al–Ni rich phase precipitate formed in the FCC matrix. Cl^? ions preferentially attack the Al–Ni rich phase, which is a sensitive zone exhibiting an appreciable potential difference, with consequent galvanic action.     

Microstructure and synthesis mechanism of Al-Ti-C-Sr master alloy

Al-5Ti-0.5C-8Sr (mass fraction,%) master alloy was prepared using a melt reaction method.The microstructure and synthetic process of the master alloy were investigated by optical microscopy,X-ray diffraction,scanning electron microscopy and X-ray energy-dispersive spectrum.The results show that the master alloy is composed of α(Al),TiAl3,TiC,Al4Sr and Al-Ti-Sr phases.The synthesis mechanisms of the master alloy are as follows:TiAl3 is formed through the reaction between K2TiF6 and Al melt at 850 ℃;when the melt was heated up to 1 200?1 300 ℃,TiC was formed through the reaction:Ti+C(s)=TiC(s);Al4Sr was formed through the binary uniform reaction when Sr was added into the melt;after the following solidification process in the peritectic reaction:L(Al,Sr)+α(TiAl3)→β(Al-Ti-Sr),the enwrapped structure was formed with the outer layer of Al-Ti-Sr phase and the internal layer of TiAl3 phase.     

热浸镀铝硅镀层微观组织结构表征

目的 研究热成形钢热浸镀铝硅镀层的微观组织与物相组成.方法 利用扫描电镜(SEM)和能谱仪(EDS)分析铝硅镀层表面与截面的微观组织形貌与成分,利用X射线衍射(XRD)和电子背散射衍射技术(EBSD)分析铝硅镀层的物相组成与比例.结果 热浸镀铝硅镀层表面由富Al相、少量的富Fe相以及树枝晶网状分布的高Si相构成,截面是由内外两层组成,其靠近铁基体的内层为Fe-Al-Si合金层,外层为Al-Si层.进一步的研究显示,Al-Si层由富Al相、少量的富Fe相以及柱状分布的高Si相构成,高Si相主要存在于合金层与铝硅层界面以及Al-Si层中.结论 热浸镀铝硅镀层中富Al相、富Fe相、高Si相和Fe-Al-Si三元合金层的物相分别为Al、Al13Fe4、Si和Al8Fe2Si.对热浸镀铝硅镀层中高Si相的研究显示,分布于合金层与铝硅层界面处的高Si相,可以有效阻碍镀层的生长,而分布于铝硅层中的高Si相在空间中以立体网状骨架的结构形式存在,这种立体网状结构形式作为镀层的主体框架,可以有效地提高镀层的强韧性和成形性能.     

ANALYSIS OF HOT IMPREGNATED Al-Si COATINGS

The microstructure and chemical composition of the hot impregnated Al-Si coating on 08Alsteel sheet were analysed by SEM,EPMA and X-ray diffraction.The coating consists ofthree parts:the outer is an α-Al solid solution enriched Si and γ-(Fe,Al,Si)phases;the in-termediate FeAl_3 and Fe_2Al_5 phases mainly and the inner neighbouring the substrate mainlyFe_2Al_5 phase.     

Ti-Al-N 涂层的组织结构与摩擦学性能

目的采用多元等离子体注入与沉积(MPIIID)技术制备Ti-Al-N涂层,系统研究涂层的微观组织结构、力学性能与摩擦学特性。方法借助XRD,XPS,SEM和TEM等,观察分析Ti-Al-N涂层的微观组织结构与物相组成,采用纳米压入试验仪、布氏硬度试验仪、摩擦磨损试验仪和激光共聚焦显微镜等测试分析Ti-Al-N涂层的力学性能、膜基结合力和摩擦磨损性能。结果 Ti-Al-N涂层表现出较高的膜-基结合强度。Al元素掺杂诱发Ti-Al-N涂层发生严重晶格畸变。当Al原子数分数为6.18%时,Ti-Al-N涂层以c-TiAlN相结构为主,表现出超高硬度(达到39.83 GPa);随着Al元素含量增加,涂层中的软质h-TiAlN相结构增多,硬度随之下降。摩擦试验结果表明,低Al含量Ti-Al-N涂层的抗磨损能力良好,其主要磨损机制为磨粒磨损;高Al含量Ti-Al-N涂层的抗磨损能力较差,其主要磨损机制倾向粘着磨损。结论 MPIIID技术成功实现了Ti-Al-N涂层的低温制备与成分调控,低Al含量的Ti-Al-N涂层具有优良的力学性能和优异的抗磨损能力。     

激光原位合成Ni3Al金属间化合物覆层及其高温摩擦学性能

利用激光熔覆技术在不锈钢基材表面原位合成了Ni3Al金属间化合物覆层。用XRD和SEM分析了覆层的相组成和组织结构。在CSM栓-盘摩擦磨损试验机上对覆层的高温摩擦磨损性能进行了测试。结果表明:覆层由单相Ni3Al金属间化合物组成;覆层与基材呈良好的冶金结合;覆层的摩擦因数和磨损率在500℃时具有最低值,分别为0.51和1.38×10-4mm3/Nm。     

Microstructure and thermal stability behavior of a rapidly solidified Al—Ti—Fe—Cr alloy

A rapidly solidified Al-2.5Ti-2.5Fe-2.5Cr(mass fraction in%) alloy was prepared by melt spinning.Asquenched and as-annealed microstructures were studied by X-ray diffractometry(XRD),transmission electron microseopy(TEM),high-resolution transmission electron microscopy(HREM) and energy dispersive spersive spectrum(EDS) analysis,The microhardness of the alloy at different annealing temperatures was measured.The results obtained indicate that the microhardness of the rapidly solidified Al-2.5Ti-2.5Fe-2.5Cr alloy does not vary with differnet annealing temperatures.The as-quenched microstructure of the alloy includes two kinds of dispersed primary phases:Al3Ti and Al13(Cr,Fe)2,After annealing at 400℃ for 10h,the stable phase Al13Fe4 appears in the microstructure.     

Constitution of Ni–Al–Ti system studied by scanning electron microscopy

The Ni–Al–Ti system is one of the key model systems for technically important materials based on nickel and titanium aluminides. A recent critical literature review by Schuster stated a lack of experimental data apart from corners of the composition triangle. This work is focused on several alloys of Ni–Al–Ti system from the central part of the composition triangle, where numerous intermetallic phases coexist. The microstructure of alloys was studied and quantified after long term annealing at 1050 °C by means of scanning electron microscopy with an energy dispersive X-ray analysis and electron backscatter diffraction. Experimental results were compared with existing literature data. In order to compare experimental knowledge on phase equilibria with results of thermodynamic modelling, phase diagram was calculated using the software package ThermoCalc and two different thermodynamic databases.     

Properties of the TiN coatings on previously Ti ion-implanted magnesium alloy substrate

To enhance the mechanical properties of TiN coating on magnesium alloy, metal vapor vacuum arc (MEVVA) ion implantation was performed to modify magnesium alloy substrate before TiN film deposition. Implantation energy was fixed at 45 keV and dose was at 9 × 10¹⁷ cm^− 2. TiN coatings were deposited by magnetically filtered vacuum-arc plasma source on unimplanted and implanted substrate. The microstructure composition distribution and phase structure were analyzed using scanning electron microscopy (SEM) and X-ray diffraction (XRD). The chemical states of some typical elements of the TiN coating were analyzed by means of X-ray photoelectron spectroscopy (XPS). The properties of corrosion resistance of TiN coatings were studied by CS300P electrochemical-corrosion workstation, and the mechanism of the corrosion resistance was also discussed.