Enhanced corrosion resistance of porous NiTi with plasma sprayed alumina coating

In this study, corrosion behaviour of porous NiTi modified by plasma sprayed alumina coating has been investigated. Scanning electron microscopy and X-ray diffraction techniques were applied for the morphology and microstructure characterisation, while linear sweep voltammetry and electrochemical impedance spectroscopy were used for investigation of corrosion behaviour of coated and uncoated NiTi specimens. Induced couple plasma was conducted to measure ion release of the specimens in simulated body fluid at 37°C. The plasma sprayed Al₂O₃ coating on the porous NiTi improved the surface characteristics for biomedical applications. The alumina coating significantly hampered Ni ion release from the surface. In spite of slight decrease in corrosion resistance of the coated specimens, the corrosion mechanism changed from pitting to general corrosion. The breakdown phenomenon was not detected in the coated specimens, as well. Overall, it can be concluded the longevity of the coated specimen in the simulated biological system was enhanced, comparing to bare NiTi specimens.     

Microstructural analysis of YSZ and YSZ/Al2O3 plasma sprayed thermal barrier coatings after high temperature oxidation

Air plasma sprayed TBCs usually include lamellar structure with high interconnected porosities which transfer oxygen from YSZ layer towards bond coat and cause TGO growth and internal oxidation of bond coat.The growth of thermally grown oxide (TGO) at the interface of bond coat and ceramic layer and internal oxidation of bond coat are considered as the main destructive factors in thermal barrier coatings.Oxidation phenomena of two types of plasma sprayed TBC were evaluated: (a) usual YSZ (yttria stabilized zirconia), (b) layer composite of (YSZ/Al₂O₃) which Al₂O₃ is as a top coat over YSZ coating. Oxidation tests were carried out on these coatings at 1100°C for 22, 42 and 100h. Microstructure studies by SEM demonstrated the growth of TGO underneath usual YSZ coating is higher than for YSZ/Al₂O₃ coating. Also cracking was observed in usual YSZ coating at the YSZ/bond coat interface. In addition severe internal oxidation of the bond coat occurred for usual YSZ coating and micro-XRD analysis revealed the formation of the oxides such as NiCr₂O₄, NiCrO₃ and NiCrO₄ which are accompanied with rapid volume increase, but internal oxidation of the bond coat for YSZ/Al₂O₃ coating was lower and the mentioned oxides were not detected.     

Thermal shock behavior of nanostructured and conventional Al2O3/13 wt%TiO2 coatings fabricated by plasma spraying

The thermal shock behavior of three kinds of Al₂O₃/13 wt%TiO₂ coatings fabricated by plasma spraying was studied in this paper. One kind of those coatings was derived from conventional fused and crushed feedstock powder available commercially; the other two kinds of coatings were derived from nanostructured agglomerated feedstock powders. These two nano coatings possess moderate pores and pre-existing microcracks, they were composed of fused structure and three-dimensional net or skeleton-like structure. For conventional coatings, the pores and pre-existing cracks were bigger, sharp-point and mostly distributed between splats. Thermal shock tests for the three coatings were performed by water quenching method. Testing result showed the two kinds of nano coatings had much higher thermal shock resistance than the conventional coatings. The improved thermal shock resistance for nano coatings could attribute to their improved microstructure and crack propagation mode. The damage evolution and failure mechanism of coatings was quite different at thermal shock temperature of 650 °C and 850 °C, which was explained by a simple model. Different crack propagating modes in nanostructured and conventional coatings during thermal shock tests were due to their different microstructures in these two kinds coatings. The stress state of coating surfaces during the thermal cycles was also discussed in this paper.     

溶液等离子喷涂铈酸镧热障涂层的制备及表征

采用溶液前驱体等离子喷涂(solution precursor plasma spray,SPPS)方法制备了La2Ce2O7涂层。通过SEM、XRD、EDS、激光导热仪对制备的涂层进行了表征,应用STA-FTIR-QMS联用技术对La2Ce2O7干燥前驱体的分解过程进行了研究,分析了前驱体的分解温度及分解过程,从而确定了喷涂温度为450℃。通过正交实验确定了雾化压力0.1MPa、电流700A、送液速率23 mL/min为最佳喷涂工艺参数,用此参数喷涂20遍制备的La2Ce2O7涂层厚度达到121μm,相对密度为92.4%,硬度为2.1 GPa。结果表明,得到了热导率较低、元素分布均匀、具有萤石结构的La2Ce2O7热障涂层。     

Toughening and strengthening mechanism of plasma sprayed nanostructured Al2O3–13 wt.%TiO2 coatings

The starting materials of Al₂O₃, TiO₂, ZrO₂ and CeO₂ nanoparticles were agglomerated into sprayable feedstock powders and plasma sprayed to form nanostructured coatings. There were net structures and fused structures in plasma sprayed nanostructured Al₂O₃–13 wt.%TiO₂ coatings. The net structures were derived from partially melted feedstock powders and the fused structures were derived from fully melted feedstock powders. The nanostructured Al₂O₃–13 wt.%TiO₂ coatings possessed higher hardness, bonding strength and crack growth resistance than conventional Metco 130 coatings which were mainly composed of lamellar fused structures. The higher toughness and strength of nanostructured Al₂O₃–13 wt.%TiO₂ coatings were mainly related to the obtained net structures.     

TiB2涂层熔盐电沉积制备与表征

炭阴极在铝电解槽中受熔盐和铝液腐蚀而影响寿命,而TiB₂涂层是铝电解槽理想的阴极材料。本文以石墨为基体,在KF-KCl-K₂TiF₆-KBF₄熔盐中以0.4-0.7A.cm_-2^{电流密度、}700-800℃温度电沉积TiB₂涂层,通过XRD衍射仪、SEM-EDS、表面粗糙度测量仪及附着力测试仪对不同电流密度和温度下制备的涂层进行表征。结果表明：在石墨基体上可以得到均匀连贯的TiB₂涂层;增大电流密度、降低电解温度可以细化涂层晶粒,提高涂层致密性;在0.6 A.cm_-²、750℃最优电沉积条件下制得的TiB₂涂层的厚度为229 μm,择优取向为<110>,表面粗糙度为14.85 μm,涂层与石墨基体的结合力为6.39 MPa。     

Thermal stability of bulk Zr2Al4C5 ceramic at elevated temperatures

Thermal expansion analysis is applied to the study of phase segregation of Zr₂Al₄C₅ at elevated temperatures (20-2000 °C) under flowing argon. Such information would be useful for the detection of phase decomposition temperature and thermal stability of materials. The detected phase-decomposition temperature of Zr₂Al₄C₅ is approximately 1900 °C. The presented thermal expansion analysis results are in good agreement with the X-ray diffraction (XRD) and SEM results. The results indicate that Zr₂Al₄C₅ is susceptible to decomposition through sublimation of high vapor pressure of Al and weaker covalent bonds between ZrC slabs and Al₄C₃ layers. Thus, minimal amounts of Al, Zr₂Al₃C₅, Al₄C₃ and ZrC form on the surface layer. Zr₂Al₃C₅ further decomposes to ZrC_1 − x and Al₄C₃ at 2000 °C. However, the amount of decomposing phase slowly increases, and the structural shape of bulk Zr₂Al₄C₅ ceramic is always kept stable during heat treatment.     

Synthesis and characterization of Y3Al5O12 and ZrO2-Y2O3 thermal barrier coatings by combustion spray pyrolysis

Y₃Al₅O₁₂ and ZrO₂-Y₂O₃ (8 mol% YSZ) coatings for potential application as thermal barrier coatings were prepared by combustion spray pyrolysis. Thermal cycling of as deposited coatings on stainless steel and FeCrAlY bond coat substrates was carried out at 1000 °C and 1200 °C to determine the thermal fatigue response. Structural and morphological studies on Y₃Al₅O₁₂ and 8 mol% YSZ coatings before and after thermal cycling have been carried out. It has been noted that the coatings on FeCrAlY substrates remain intact after 50 cycles between room temperature and 1200 °C, whereas the coatings on stainless steel show some minor damage such as peeling off near the periphery after 50 cycles at 1000 °C. Thermal diffusivity values of Y₃Al₅O₁₂ and 8 mol% YSZ films were measured by using photo thermal deflection spectroscopy and the values are lower than those of coatings produced by conventional techniques such as EBPVD and APS.     

The effect of plasma spray parameters on the cavitation erosion of Al2O3-TiO2 coatings

This paper reports a study of how the choice of plasma spray parameters, used during deposition of Al₂O₃-13%TiO₂ coatings on carbon steel, influences the cavitation erosion properties of such coatings. The parameters studied are the power feeding rate and hydrogen flow rate. The surface and cross section of coatings before and after cavitation were also observed by scanning electron microscopy (SEM). The phases present in the coatings were characterized by X-ray diffraction method (XRD). The microscopic observations were used to study the inter-lamellar connection, porosity, unmelted particles and so on inside the coating. We also measured the roughness, microhardness, adhesion strength and cavitation erosion of the coatings. The XRD results showed that the coating includes different allotropes of Al₂O₃ such as α and γ. The cavitation erosion studies of the coatings were conducted by ultrasonic cavitation testing on the basis of ASTM G32 standard. It was found that cavitation erosion is accelerated around the unmelted particles and porosities. The results reveal that the cavitation resistance of the coating is determined by its microstructure and that increasing discontinuities (inside the coating) reduce its cavitation resistance. We have found that the coating obtained at hydrogen gas flow rate of 16 L/min and powder feeding rate of 20 g/min has the best cavitation resistance.     

Effects of critical plasma spray parameter and spray distance on wear resistance of Al2O3-8 wt.%TiO2 coatings plasma-sprayed with nanopowders

Effects of plasma spraying conditions on wear resistance of nanostructured Al₂O₃-8 wt.%TiO₂ coatings plasma-sprayed with nanopowders were investigated in this study. Five kinds of nanostructured coatings were plasma-sprayed on a low-carbon steel substrate by varying critical plasma spray parameter (CPSP) and spray distance. The coatings consisted of fully melted region of γ-Al₂O₃ and partially melted region, and the fraction of the partially melted regions and pores decreased with increasing CPSP or decreasing spray distance. The hardness and wear test results revealed that the hardness of the coatings increased with increasing CPSP or decreasing spray distance, and that the hardness increase generally led to the increase in wear resistance, although the hardness and wear resistance were not correlated in the coating fabricated with the low CPSP. The main wear mechanism was a delamination one in the coatings, but an abrasive wear mode also appeared in the coating fabricated with the low CPSP. According to these wear mechanisms, the improvement of wear resistance in the coating fabricated with the low CPSP could be explained because the improved resistance to fracture due to the presence of partially melted regions might compensate a deleterious effect of the hardness decrease.     

Preparation and wear performance of NiCr/Cr3C2-NiCr/hBN plasma sprayed composite coating

NiCr clad hexagonal BN powder (NiCr/hBN) was added to NiCr/Cr₃C₂ feedstock to improve the tribological properties of chromium carbide nichrome coating. The microstructure, flowability and apparent density of the composite powder, as well as the structure and mechanical properties of the plasma sprayed coating were characterized. The friction and wear behavior of the NiCr/Cr₃C₂-NiCr/hBN coating from ambient temperature up to 800 °C was evaluated on a ball-on-disk wear tester and compared with that of NiCr/Cr₃C₂ coating and NiCr/Cr₃C₂-NiCr/BaF₂·CaF₂ coating. The results show that NiCr cladding can reduce the decarburization of Cr₃C₂ and oxidation of hBN during the thermal spray. The main wear mechanisms of the NiCr/Cr₃C₂-NiCr/hBN composite coating are ploughing and adhesive wear. Layered hexagonal BN particle reduce the direct contact and severe adhesion between friction pairs, thus decreasing the friction coefficient. The NiCr/Cr₃C₂-NiCr/hBN composite coating shows a promising application in the high temperature environment with the request of both wear resistance and friction reduction.     

In-situ TiB2 and Al2O3 formation by DC plasma spraying

In-situ plasma spraying (IPS) is a promising process to fabricate composite coatings with in-situ formed thermodynamically stable phases. In the present study, mechanically alloyed Al-12Si, B₂O₃ and TiO₂ powder was deposited onto an aluminum substrate using atmospheric plasma spraying (APS). It has been observed that, during the coating process, TiB₂ and Al₂O₃ are in-situ formed through the reaction between starting powders and finely dispersed in hypereutectic Al-Si matrix alloy. Also, obtained results demonstrate that in-situ reaction intensity strongly depends on spray conditions.     

Fe2O4催化纤维素水热法制备 Fe2O3/ 碳纳米复合材料

目的在较为温和的条件下制备氧化铁/碳纳米复合材料。方法以纳米Fe3O4粉体为催化剂,水热催化纤维素碳化,并借助扫描电镜、透射电镜、X射线光电子能谱仪和X射线衍射仪对碳化产物进行表征分析。结果获得了粒径约为150 nm的枣核形氧化铁/碳纳米复合材料。结论通过相对温和的水热反应,纤维素被碳化形成了壳核结构的纳米产物,Fe3O4催化剂在反应过程中被氧化并成为壳核结构产物的核心。     

Hot corrosion behaviour of plasma sprayed YSZ/Al2O3 dispersed NiCrAlY coatings on Inconel-718 superalloy

Oxide dispersed NiCrAlY bond coatings have been developed for enhancing thermal life cycles of thermal barrier coatings (TBCs). However, the role of dispersed oxides on high temperature corrosion, in particular hot corrosion, has not been sufficiently studied. Therefore, the present study aims to improve the understanding of the effect of YSZ dispersion on the hot corrosion behaviour of NiCrAlY bond coat. For this, NiCrAlY, NiCrAlY + 25 wt.% YSZ, NiCrAlY + 50 wt.% YSZ and NiCrAlY + 75 wt.% YSZ were deposited onto Inconel-718 using the air plasma spraying (APS) process. Hot corrosion studies were conducted at 800 °C on these coatings after covering them with a 1:1 weight ratio of Na₂SO₄ and V₂O₅ salt film. Hot corrosion kinetics were determined by measuring the weight gain of the specimens at regular intervals for a duration of 51 h. X-ray diffraction, scanning electron microscopy and energy dispersive spectroscopy techniques were used to determine the nature of phases formed, examine the surface attack and to carry out microanalysis of the hot corroded coatings respectively. The results show that YSZ dispersion causes enhanced hot corrosion of the NiCrAlY coating. Leaching of yttria leads not only to the formation of the YVO₄ phase but also the destabilization of the YSZ by hot corrosion. For the sake of comparison, the hot corrosion behaviour of a NiCrAlY + 25 wt.% Al₂O₃ coating was also examined. The study shows that the alumina dispersed NiCrAlY bond coat offers better hot corrosion resistance than the YSZ dispersed NiCrAlY bond coat, although it is also inferior compared to the plain NiCrAlY bond coat.     

Photocatalytic performance of nano-photocatalyst from TiO2 and Fe2O3 by mechanochemical synthesis

Nano-particles of homogeneous solid solution between TiO₂ and Fe₂O₃ (up to 10 mol%) have been prepared by mechanochemical milling of TiO₂ and yellow Fe₂O₃/red Fe₂O₃/precipitated Fe (OH)₃ using a planetary ball mill. Such novel solid solution cannot be prepared by conventional co-precipitation technique. A preliminary investigation of photocatalytic activity of mixed oxide (TiO₂/Fe₂O₃) on photo-oxidation of different organic dyes like Rhodamine B (RB), Methyl orange (MO), Thymol blue (TB) and Bromocresol green (BG) under visible light (300-W Xe lamp; λ > 420 nm) showed that TiO₂ having 5 mol% of Fe₂O₃ (YFT1) is 3-5 times higher photoactive than that of P25 TiO₂. The XRD result did not show the peaks assigned to the Fe components (for example Fe₂O₃, Fe₃O₄, FeO₃, and Fe metal) on the external surface of the anatase structure in the Fe₂O₃/TiO₂ attained through mechanochemical treatment. This meant that Fe components were well incorporated into the TiO₂ anatase structure. The average crystallite size and particle size of YFT1 were found to be 12 nm and 30 ± 5 nm respectively measured from XRD and TEM conforming to nanodimensions. Together with the Fe component, they absorbed wavelength of above 387 nm. The band slightly shifted to the right without tail broadness, which was the UV absorption of Fe oxide in the Fe₂O₃/TiO₂ particle attained through mechanochemical method. This meant that Fe components were well inserted into the framework of the TiO₂ anatase structure. EPR and magnetic susceptibility show that Fe³⁺ is in low spin state corresponding to μ_B = 1.8 BM. The temperature variation of μ_B shows that Fe³⁺ is well separated from each other and does not have any antiferromagnetic or ferromagnetic interaction. The evidence of Fe³⁺ in TiO₂/Fe₂O₃ alloy is also proved by a new method that is redox titration which is again support by the XPS spectrum.     

Characterization of plasma-sprayed Y2O3 coating and investigation of its visual aspect change

Yttria (Y₂O₃) has been commonly used as a protective coating material because it has strong resistance to plasma erosion with reducing the amount of reaction products generated during the semiconductor/LCD fabrication process. We have investigated the visual aspect of the plasma-sprayed Y₂O₃ coating both experimentally and numerically to propose the process conditions proper for white Y₂O₃ coating. It was demonstrated that heating of the particle surface in oxygen deficient plasma jet core resulted in the reduction of coating materials associated with the formation of black spots, while the re-oxidation of reduced feed stock materials at long spray distance, where they were exposed to relatively lower temperature of plasma and abundant oxygen, caused the whitening of coating. Based on the results, we proposed a spray coating condition proper for reducing the black spots formed in protective Y₂O₃ ceramic coating.     

P-type transparent conducting SnO2:Zn film derived from thermal diffusion of Zn/SnO2/Zn multilayer thin films

Highly transparent, p-type conducting SnO₂:Zn thin films are prepared from the thermal diffusion of a sandwich structure of Zn/SnO₂/Zn multilayer thin films deposited on quartz glass substrate by direct current (DC) and radio frequency (RF) magnetron sputtering using Zn and SnO₂ targets. The deposited films were annealed at various temperatures for thermal diffusion. The effect of annealing temperature and time on the structural, electrical and optical performances of SnO₂:Zn films was studied. XRD results show that all p-type conducting films possessed polycrystalline SnO₂ with tetragonal rutile structure. Hall effect results indicate that the treatment at 400 °C for 6 h was the optimum annealing parameters for p-type SnO₂:Zn films which have relatively high hole concentration and low resistivity of 2.389 × 10¹⁷ cm^− 3 and 7.436 Ω cm, respectively. The average transmission of the p-type SnO₂:Zn films was above 80% in the visible light range.     

Fe2O3-CaO-TiO2 体系下铁酸钙的合成过程及TiO2 和CaTiO3 的影响

为了确定高钛型钒钛磁铁矿烧结过程中铁酸钙的生成是受TiO₂还是TiO₂和CaO形成的CaTiO₃影响,首先利用Fe₂O₃和CaO的纯试剂合成了铁酸钙,并研究了TiO₂和CaTiO₃对钛铁酸钙 （FCT） 形成的影响。在Factsage 7.0软件进行热力学计算的基础上,通过在空气气氛下进行烧结,获得了在1023~1423 K温度范围内、不同烧结时间的不同样品。通过X射线衍射和扫描电镜-能谱分析等表征手段,对烧结样品的物相转变和微观结构变化进行了表征。发现FCT的形成过程主要分为2个阶段：前一阶段为1023~1223 K温度范围内Fe₂O₃与CaO之间的反应,合成产物为Ca₂Fe₂O₅,反应方程式为“Fe₂O₃(s)+ 2CaO(s)= Ca₂Fe₂O₅(s)”;后一阶段为1223~1423 K温度范围内Ca₂Fe₂O₅和Fe₂O₃的反应,主要产物为CaFe₂O₄,反应为“Ca₂Fe₂O₅(s)+ Fe₂O₃(s)= 2CaFe₂O₄(s)”,该阶段尤其是温度为1423 K时,反应速率显著加快,随温度的升高CaTiO₃显著增加。然而,Ti元素在铁酸钙中的固溶很难实现,TiO₂与铁酸钙之间的反应不是形成FCT的有效途径。随着保温时间的延长,CaTiO₃和FCT相界中Fe元素含量增加。FCT主要是通过Fe组分在CaTiO₃中固溶形成的,主要反应是“Fe₂O₃+CaTiO₃(s)=FCT(s)”。     

The corrosion behavior of two-phase Ni-Dy alloys in a eutectic (Li,K)2CO3 mixture at 650 °C

The corrosion behavior of binary Ni-Dy alloys containing 1, 3 and 5 wt.% Dy in a eutectic (0.62Li,0.38K)₂CO₃ mixture at 650 °C has been investigated. The alloys are two-phase composed of α-Ni solid solution and intermetallic compound Dy₂Ni₁₇. The experimental results indicate that the corrosion rate of the three Ni-Dy alloys is significantly lower than that of pure Ni, forming a scale mainly composed of NiO together with a small amount of dysprosium oxides. The weight gain of the alloys changes little with the content of dysprosium, while the thickness of the scale decreases with increasing content of dysprosium. The presence of Dy can promote the lithiation process of NiO during immersion in the melt. The corrosion mechanism of the alloys is also discussed.     

Mechanical and tribological performance of Al2O3-TiO2 coatings elaborated by flame and plasma spraying

Mechanical properties and wear rates of Al₂O₃-13 wt.% TiO₂ (AT-13) and Al₂O₃-43 wt.% TiO₂ (AT-43) coatings obtained by flame and atmospheric plasma spraying were studied. The feed stock was either ceramic cords or powders. Results show that the wear resistance of AT-13 coatings is higher than that of AT-43 and it seems that the effect of hardness on wear resistance is more important than that of toughness. Additionally, it was established that, according to conditions used to elaborate coatings and the sliding tribological test chosen, spray processes do not seem to have an important effect on the wear resistance of these coatings.