Preparation of ceramic coatings on inner surface of steel tubes using a combined technique of hot-dipping and plasma electrolytic oxidation

A new method for inner surface modification of steel tubes, named a combined technique of hot-dipping and plasma electrolytic oxidation (PEO) was proposed and demonstrated in this paper. In this work, metallurgically bonded ceramic coatings on inner surface of steel tubes were obtained using this method. In the combined process, aluminum coatings on steel were firstly prepared by the hot-dip process and then metallurgically bonded ceramic coatings were obtained on the aluminum coatings by PEO. The element distribution, phase composition and morphology of the aluminide layer and the ceramic coatings were characterized by SEM/EDX and XRD. The corrosion resistance of the ceramic coatings were also studied. The results show that, after hot-dip treatment, the coating layers consist of two layers, where Al, Fe_xAl _(1−x) were detected from external topcoat to the aluminide/steel substrate. Then after PEO process, uniform Al₂O₃ ceramic coatings have been deposited on inner surface of steel tubes. The ceramic coatings are mainly composed of -Al₂O₃ and γ-Al₂O₃ phase. The compound coatings show favorable corrosion resistance property. The investigations indicate that the combination of hot-dipping and plasma electrolytic oxidation proves a promising technique for inner surface modification of steel tubes for protective purposes.     

Surface modification of die casting mold steel by a composite technique of hot-dipping and plasma electrolytic oxidation

The hot dipping process of pure aluminum on H13 steel substrates followed by plasma electrolytic oxidation（PEO） was studied to form alumina ceramic coatings for protective purpose.H13 steel bars were first dipped in pure aluminum melts,and then,a reactive iron-aluminum intermetallic layer grew at the interface between the melt and the steel substrate.The reactive layer was mainly composed of intermetallic Fe-Al（Fe₂Al₅）;the thickness of aluminum layer and Fe-Al intermetallic layer were mainly influenced by dipping time（1.5～12.0 min） and dipping temperature（710～760 ℃）.After PEO process,uniform Al₂O₃ ceramic coatings were deposited on the surface of aluminized steel.The element distribution,phase composition and morphology of the aluminized layer,and the ceramic coatings were characterized by SEM/EDS and XRD.The distribution of hardness across the composite coating is demonstrated,and the maximum value reaches 1864 HV.The thermal shock resistance of the coated sample is also well improved.     

非阀金属的等离子体电解氧化研究进展

等离子体电解氧化技术通常用于Al、Mg、Ti等阀金属表面形成高性能陶瓷层,较少涉及非阀金属。主要介绍了碳钢、铜、锌及其合金等“非阀金属”的等离子体电解氧化技术的最新进展。列举了碳钢在不同的电解液成分、电参数、氧化时间等工艺参数条件下制备所得涂层的相关性能,阐述了碳钢在等离子体电解氧化过程中绝缘膜击穿优于气膜击穿的成膜理论。分析了铜及其合金在硅酸盐、铝酸盐、磷酸盐及其混合电解液中的等离子体电解氧化行为,并探究了涂层的耐腐蚀和耐摩擦性能及形成机理。阐述了在不同的工艺参数下锌及其合金在耐腐蚀、耐摩擦、气敏传感和生物降解性的研究,并且论述了阀金属与非阀金属成膜的差异所在。最后,对非阀金属等离子体电解氧化技术后续的发展进行了展望。     

Finite element analysis on stresses field of normalized layer thickness within ceramic coating on aluminized steel

Multilayer ceramic coatings were fabricated on steel substrate using a combined technique of hot dipping aluminum（HDA） and plasma electrolytic oxidation（PEO）. A triangle of normalized layer thickness was created for describing thickness ratios of HDA/PEO coatings. Then, the effect of thickness ratio on stresses field of HDA/PEO coatings subjected to uniform normal contact load was investigated by finite element method. Results show that the surface tensile stress is mainly affected by the thickness ratio of AI layer when the total thickness of coating is unchanged. With the increase of AI layer thickness, the surface tensile stress rises quickly. When Al2O3 layer thickness increases, surface tensile stress is diminished. ＇Meanwhile, the maximum shear stress moves rapidly towards internal part of HDA/PEO coatings. Shear stress at the Al2O3/Al interface is minimal when Al2O3 layer and AI layer have the same thickness.     

H13热作模具钢微弧氧化复合陶瓷层的组织和性能

通过热浸镀铝/微弧氧化复合工艺对H13模具钢进行表面改性以提高模具表面质量。在热浸镀铝过程中,将H13钢基体浸入710℃纯铝液6 min,得到了以Fe2Al5为主中间合金层,使得镀层与基体紧密结合。经过微弧氧化处理后,镀铝试样表面铝层转化为氧化铝陶瓷,主要由α-Al2O3和γ-Al2O3相组成。用带有能谱分析装置(EDX)的扫描电镜(SEM)、X射线衍射(XRD)分析了膜层的形貌、成分和相组成。微弧氧化陶瓷层主要由Al、O、Si元素组成,其中O、Si主要来源于硅酸盐电解液。     

阴极电流密度对6061铝合金在含Na2WO4电解液中微弧氧化膜结构和耐磨性能的影响

目的 研究恒流模式下阴极电流密度对6061铝合金在含Na2WO4的电解液中制备的微弧氧化膜厚度、形貌、相组成及耐磨性能的影响。方法 固定阳极电流密度为5.0 A/dm²,阴极电流密度分别为0、1.25、2.5、3.75、5.0 A/dm²,对6061铝合金进行微弧氧化40 min。用涡流测厚仪测量了氧化膜的厚度,用扫描电镜观察了微弧氧化膜的表面形貌和截面形貌,用能谱分析仪分析了氧化膜的表面成分,用X射线衍射分析仪分析了微弧氧化膜的相组成,用往复式摩擦磨损试验机测试了氧化膜的耐磨性能。结果 随着阴极电流密度的增加,氧化膜内的W含量逐渐减少,氧化膜颜色逐渐变浅,氧化膜厚度逐渐增加。微弧氧化膜的主要组成相为α-Al2O3和γ-Al2O3。当阴极电流密度从0 A/dm²增加到3.75 A/dm²时,氧化膜内孔洞的数量和尺寸逐渐减少,孔洞到氧化膜/基体界面的距离逐渐增加,氧化膜的耐磨性能逐渐提升。当阴极电流密度为3.75 A/dm²时,氧化膜的磨损率最低,仅为1.07×10^‒4 mm³/(N.m)。但阴极电流密度增加到5.0 A/dm²时,氧化膜表层出现孔洞和剥落,耐磨性能下降。结论 阴极电流的加入有助于增加6061铝合金微弧氧化膜的厚度,提高氧化膜的致密性和耐磨性能,但过高的阴极电流会导致氧化膜表层出现孔洞,降低耐磨性能。     

Wettability and Corrosion Behavior of Chemically Modified Plasma Electrolytic Oxidation Nanocomposite Coating

The aim of this paper was to investigate the effect of potassium stearate on the wettability behavior, corrosion resistance, roughness and thickness of reinforced and unreinforced plasma electrolytic oxidation (PEO) coatings with Si₃N₄ nanopowders. Morphological characteristic, corrosion behavior and wetting properties of the coatings were evaluated using SEM, cyclic polarization and Wilhelmy plate method, respectively. In order to obtain a better evaluation of the contact angle, roughness of the coatings was studied by AFM. The results indicated that the nanocomposite hydrophobic coatings have the best corrosion resistance. Potassium stearate could repel water from the holes of coating by reacting with aluminum and producing aluminum stearate. The contact angle of nanocomposite and normal PEO coatings was increased up to 65° due to the addition of potassium stearate. This additive could also increase the hysteresis contact angle up to 51°.     

Growth mechanism and corrosion behavior of ceramic coatings on aluminum produced by autocontrol AC pulse PEO

Ceramic coatings are produced on aluminum alloy by autocontrol AC pulse Plasma Electrolytic Oxidation (PEO) with stabilized average current. Transient signal gathering system is used to study the current, voltage, and the transient wave during the PEO process. SEM, OM, XRD and EDS are used to study the coatings evolution of morphologies, composition and structure. TEM is used to study the micro profile of the outer looser layer and inner compact layer. Polarization test is used to study the corrosion property of PEO coatings in NaCl solution. According to the test results, AC pulse PEO process can be divided into four stages with different aspects of discharge phenomena, voltage and current. The growth mechanism of AC PEO coating is characterized as anodic reaction and discharge sintering effect. PEO coating can increase the corrosion resistance of aluminum alloy by one order or two; however, too long process time is not necessarily needed to increase the corrosion resistance. In condition of this paper, PEO coating at 60 min is the most protective coating for aluminum alloy substrate.     

球铁浸镀微弧氧化陶瓷层的制备与组织分析

通过热浸镀铝及微弧氧化的方法在球墨铸铁表面上获得了陶瓷层,并对该涂层进行了XRD、SEM分析.研究结果表明:浸镀温度越高,镀层越厚,直到达到一峰值;浸镀时间越长,镀层越厚.球墨铸铁浸镀微弧氧化获得的涂层由涂层表面至基体依次为陶瓷层、纯铝层、扩散层、基体.陶瓷层主要为Al2O3相,扩散层由FeAl3、Fe2Al5相组成.     

Correlation between discharging property and coatings microstructure during plasma electrolytic oxidation

1 Introduction Plasma electrolytic oxidation (PEO) is a new technology in surface engineering[1- 8]. A deep under- standing of discharge property during the process will be veryhelpful for revealing the mechanism of PEO and for developing new surface modi…     

Investigation of wear and corrosion resistance of nanocomposite coating formed on AZ31B Mg alloy by plasma electrolytic oxidation

Ceramic-WC coatings were prepared on AZ31 B Mg alloy by plasma electrolytic oxidation (PEO) from a phosphate based bath containing suspended tungsten carbide nanoparticles at various process times. Scanning electron microscope results indicated that increase of coating time and incorporation of tungsten carbide into the ceramic coating during the PEO process led to a decrease in the number and diameter of coating pores. Phase analysis showed that the nanocomposite coating was composed of MgO, Mg₃(PO₄)₂ and WC. Tribological properties and corrosion behaviour of uncoated AZ31 B Mg alloy and ceramic coatings were evaluated using a pin-on-disc tribometer and potentiodynamic polarisation technique in 3.5% NaCl solution, respectively. The wear and electrochemical tests showed that wear and corrosion resistance of ceramic-WC nanocomposite coatings were better than ceramic only ones. In addition, wear and corrosion behaviour of coatings improved with increasing the coating time.     

Fundamental and practical evaluations of PEO coatings of titanium

Abstract

Plasma electrolytic oxidation (PEO) enables fabrication of high performance ceramic surfaces on the light metals, with thickness, topography, composition and structure controllable by the process parameters. The growth of anodic coatings on titanium has been investigated at a fundamental level, and understanding of coating growth has been enhanced. Discrete thickening at sites of dielectric breakdown, local growth at the metal/oxide interface and destruction of earlier formed oxide were shown, offering a new perspective on coating processes, including those aspects affecting coating efficiency. Routes to tailored coating compositions for enhanced biocompatibility have been developed, and carried through to in vitro evaluation. Fabrication of amorphous oxide, which is beneficial to biocompatibility, was achieved through anodising at controlled current densities and with use of complexing agents. Corrosion tests of the coatings revealed low titanium release into physiological solution, which is important to avoid adverse tissue reaction. In vitro tests confirmed good attachment of human osteoblast cells to the fabricated titanium oxide coatings.     

铝合金微弧氧化陶瓷涂层研究进展

简述了微弧氧化技术的基本原理和优点,着重介绍了实验参量,如电源模式、电解液组成、电压、频率、占空比、氧化时间、基材成分等对铝合金微弧氧化的影响,总结和分析了铝合金微弧氧化陶瓷涂层微观结构与性能的特点及其关系。最后,针对目前铝合金微弧氧化陶瓷涂层研究领域存在的问题,提出了今后的研究方向。     

微弧氧化处理对铝合金耐霉菌腐蚀特性的影响

在2A12铝合金表面制备了微弧氧化膜层,按照国家军用标准霉菌测试方法对微弧氧化膜层的耐腐蚀性能进行了测试,通过扫描电镜(SEM)、X射线衍射分析(XRD)对铝合金基体及微弧氧化膜层霉菌腐蚀前后的微观结构、相组成进行了表征。结果表明,未经过微弧氧化处理的铝合金表面有少量的霉菌生长,表面产生了一定数量的点蚀坑,长霉等级为1级。经过微弧氧化处理试样表面未发现霉菌生长,长霉等级为0级。微弧氧化处理可以有效提高铝合金表面耐霉菌腐蚀性能,扩大其应用范围。     

微弧氧化技术述评

微弧氧化(MAO)又称为微等离子体氧化(MPO)、阳极火花沉积(ASD)或火花放电阳极氧化(SDAO),它是一种直接在有色金属表面原位生长陶瓷膜层的表面处理新技术.该技术突破了传统阳极氧化的诸多不足之处,通过对工艺过程的控制,可以使金属表面陶瓷化,生成的陶瓷薄膜具有优异的耐磨和耐蚀性能、较高的硬度和绝缘电阻.基于目前微弧氧化技术在Al、Mg、Ti及其合金表面改性方面的广泛应用和进展,综述了微弧氧化技术的工艺原理、技术特点、微弧氧化膜层的性质和影响因素以及该技术的应用现状.     

316L表面激光熔覆复合等离子体电解氧化制备多孔陶瓷涂层及其生物应用（英文）

为了提高316L不锈钢的生物活性,采用激光熔覆(LC)技术在316L不锈钢表面制备钛层,然后利用等离子体电解氧化(PEO)技术在钛层上形成多孔陶瓷涂层。采用三维表面轮廓仪、SEM、EDS、XRD和XPS等测试方法对涂层试样的形貌、微观结构和组成进行表征。通过动电位极化曲线和模拟体液(SBF)浸泡试验,分别对涂层的耐腐蚀性和生物活性进行评价。结果表明,多孔陶瓷涂层主要由锐钛矿和金红石组成,并检测到高结晶HA。陶瓷涂层的主要元素为Ca、P、Ti和O。在模拟体液中,LC+PEO复合生物涂层比316L基质具有更优异的耐腐蚀性,并且复合涂层能有效提高316L不锈钢的生物活性。     

Structure and corrosion resistance of ZrO2 ceramic coatings on AZ91D Mg alloys by plasma electrolytic oxidation

The aim of this work is to study the structure and the corrosion resistance of the plasma electrolytic oxidation ZrO₂ ceramic coatings on Mg alloys. The ceramic coatings were prepared on AZ91D Mg alloy in Na₅P₃O₁₀ and K₂ZrF₆ solution by pulsed single-polar plasma electrolytic oxidation (PEO). The phase composition, morphology and element distribution in the coating were investigated by X-ray diffractometry, scanning electron microscopy and energy distribution spectroscopy, respectively. The results show that the coating thickness and surface roughness were increased with the increase of the reaction time. The ceramic coatings were of double-layer structure with the loose and porous outer layer and the compact inner layer. And the coating was composed of P, Zr, Mg and K, of which P and Zr were the main elements in the coating. P in the coating existed in the form of amorphous state, while Zr crystallized in the form of t-ZrO₂ and a little c-ZrO₂ in the coating. Electrochemical impedance spectra (EIS) and the polarizing curve tests of the coatings were measured through CHI604 electrochemical analyzer in 3.5% NaCl solution to evaluate the corrosion resistance. The polarization resistance obtained from the equivalent circuit of the EIS was consistent with the results of the polarizing curves tests.     

Microstructure and corrosion resistance of modified 2024 Al alloy using surface mechanical attrition treatment combined with microarc oxidation process

A top ceramic coating was fabricated on the surface mechanical attrition treatment (SMAT) modified nanocrystalline layer of 2024 Al alloy by microarc oxidation (MAO) process. The corrosion resistance of the SMAT-MAO composite coating was studied by EIS. The results show that SMAT-MAO composite coating with 10 μm top ceramic coating exhibited better corrosion resistance, while the SMAT-MAO coating with the thickness of 15 μm showed worse corrosion resistance compared with those simple MAO coatings with same thickness. The formation of a dense passive film at the damaged region caused by the bottom nanocrystalline interface contributed to the improved corrosion resistance property.     

Nd对镁合金微弧氧化陶瓷层厚度及表观质量的影响

为了研究Nd对AZ31D铗合金微弧氧化陶瓷层的厚度及表观质量的影响作用,通过在磷酸盐体系电解液中添加不同量的Nd(NO3)3,采用恒压方式对AZ31D镁合金进行微弧氧化得到的陶瓷层,并对获得的陶瓷层进行膜厚测试和XRD、EDAX及SEM检测分析.结果表明:在添加0.005mol/L Nd(NO3Nd2O3和Nd(OH)3的形式存在于陶瓷层中;能够增厚陶瓷层和优化表面质量等结论.最后探讨了Nd对镁合金微弧氧化陶瓷层的厚度及表观质量的作用机理.     

Study on wear behavior of plasma electrolytic oxidation coatings on aluminum alloy

Thick and hard ceramic coatings were fabricated on A356 aluminum alloy by using plasma electrolytic oxidation(PEO) technique.The microstructure and phase composition of the PEO coatings were examined by using SEM and XRD method.It is found that the PEO coatings are mainly composed of crystalline α-Al2O3 and mullite.The dry sliding wear test of PEO coatings were carried out on a ring-on-ring wear machine.Results shows that there is hardly no wear loss of polished PEO coatings while the wear rate of uncoated aluminum alloy is 4.3×10-5 mm3·(N·m)-1 at a speed of 0.52 m·s-1 and a load of 40 N.