铝合金微弧氧化过程中电学参量的特性研究

利用自制的数据采集系统研究了恒定电压下铝合金微弧氧化过程中有关电学参量随时间的变化规律.结果表明：通电回路中的阴极和阳极峰值电流随处理时间的变化明显分为5个阶段；陶瓷膜的动态正向电阻和电阻率随处理时间分阶段变化，而动态的反向电阻和电阻率随时间的变化不大.在微弧氧化过程中，各时刻的动态正、反向电阻值不同，一般情况下，动态正向电阻远大于反向电阻.对不同处理时间样品的扫描电子显微镜分析表明，陶瓷膜呈多孔结构并随处理时间分阶段变化. 关键词： 铝合金 微弧氧化 电学参量 陶瓷膜     

阴极电压脉冲占空比对钛合金微弧氧化膜特性的影响

利用自制多功能微弧氧化电源,在保持双极性电压脉冲幅度不变的条件下,研究了阴极电压脉冲占空比（d_c）对钛合金微弧氧化膜特性的影响.结果表明：阴、阳极的峰值电流随处理时间的变化分为几个不同阶段,各阶段的开始和结束时间与d_c密切相关.氧化膜主要由金红石和锐钛矿相TiO₂组成,金红石相TiO₂的相对含量在d_c=50%附近随d_c的 关键词： 微弧氧化 钛合金 占空比     

Al(OH)3溶胶浓度对TC4钛合金微弧氧化膜特性的影响

利用自制多功能微弧氧化(MAO)电源,在保持电学参数和处理时间不变的条件下对TC4钛合金表面进行了MAO处理,研究了Al(OH)₃溶胶浓度对钛合金MAO膜的生长特性、微观结构、相结构和电致变色特性的影响.结果表明:随着Al(OH)₃溶胶浓度(体积分数)C的增加,膜层的生长速率由慢到快逐渐增加,膜表面微孔尺寸和粗糙度逐渐增大,而微孔密度逐渐减小;当C≤10%时,膜层由锐钛矿相TiO₂组成,而当C>10%时,膜层中开始出现金红石相TiO₂并随着C的增加其相对含量逐渐增大,并在C=40%时,膜层全部由金红石相TiO₂组成;在pH＝2.0的HCl溶液中的循环伏安测试结果表明,C≤20%制备试样的膜层颜色变化不明显,随着C的进一步增加,制备试样的膜层颜色变化逐渐明显,并在C=40%时,其着色呈蓝色且色泽均匀;该试样在循环伏安测试过程中还表现出了良好的稳定性和可逆性. 关键词： 微弧氧化 氧化膜 微观结构 电致变色     

高性能微通道板除气过程中电阻的变化

比较了高性能微通道板和标准型微通道板在经过相同或类似制管工艺处理前、后电阻的变化，测定了高性能微通道板分别在真空烘烤和2个不同阶段电子清刷后电阻随电压及温度的变化关系。实验结果表明：高性能微通道板的热稳定性优于标准型微通道板，其电阻温度系数为-0.007/℃；经过第二阶段清刷后，电阻随电压的变化缓慢，电压系数为-1.11×10^-4V^-1；用这种材料和工艺制作的低电阻、大动态范围、高稳定性微通道板可满足特种探测器的需求。     

方块电阻法原位表征Cu薄膜氧化反应动力学规律

提出并建立了一种基于方块电阻测量的原位表征Cu薄膜氧化反应动力学规律的方法.利用Cu薄膜方块电阻随氧化时间的变化情况，得到氧化产物厚度与氧化时间的关系，反应动力学表征结果符合抛物线规律.还利用不同的氧化反应温度条件和对应的抛物线常数之间的关系得到体系的扩散激活能.结果表明，提出的表征方法适用于Cu薄膜氧化反应体系.     

聚丙烯孔洞驻极体膜的化学表面处理及电荷稳定性

利用热刺激放电(Thermally Stimulated Discharge, TSD)电流谱、在线电荷TSD、电荷等温衰减测量和衰减全反射(Attenuated Total Reflection, ATR)红外光谱分析，本文系统地研究了经化学表面处理(萃取、氧化及氢氟酸)的聚丙烯(PP)孔洞驻极体膜的电荷储存稳定性及电荷稳定性提高的原因.结果表明：经适当地氧化和氢氟酸室温处理试样的TSD电流谱中在温位约为184℃处出现原膜所没有的非常强的新峰，电荷热稳定性得到显著的提高，这一电荷热稳定性通过高温充电工艺得到进一步地改善；适当延长室温下氢氟酸处理的时间或延长氧化时间，都会使处理膜的电荷稳定性得到提高.理论分析表明在线电荷TSD测量法可给出线性升温过程中电荷重心及驻极体电荷量变化的综合信息，结合TSD电流谱和初始电荷重心位置的测量，可精确地考察线性升温过程中电荷重心的在线变化. 关键词： 聚丙烯孔洞膜 表面氧化 氢氟酸处理 电荷稳定性 在线电荷TSD     

电学参数对胶体中工业纯钛微弧氧化膜特性的影响

利用自制多功能微弧氧化(MAO)电源对处在胶体中的工业纯钛表面进行了MAO处理,比较系统地研究了电压脉冲的峰值(U)和占空比(d)对膜层的生长特性、微观结构、相结构和处理后试样耐腐蚀性能的影响.结果表明,随着U的增加或d的加大,膜厚几乎呈线性增加,膜表面微孔尺寸和粗糙度逐渐增大,微孔密度逐渐减小.膜层主要由致密层组成,除U=450V,d=10%时制备试样的膜层中含有少量锐钛矿相TiO2外,其他试样的膜层全由金红石相TiO2组成;在30%硫酸溶液中的耐腐蚀测试表明,MAO处理后试样的耐腐蚀性能与U和d密切相关,随着U的增加或d的加大,试样的耐腐蚀能力逐渐增强.     

金属薄膜电阻特性与厚度测量

考察不同沉积时间的金属铝与铜的薄膜的沉积态,电阻变化与厚度,厚度测量采用实验室光学干涉和透过率对比方法.金相显微与铝铜电阻变化的测量表明,不连续薄膜与连续过渡之间,电阻显著变化处不同.铝膜电阻随时间变化过程开始时存在波动状态.     

等离子体电解氧化过程中单个稳态微放电的热效应研究

详细回顾了有关等离子体电解氧化过程中单个稳态微放电热效应研究的现状；提出了处理过程中电解液/基体界面上离散气泡类型和数量上的变化造成了微放电外观的演化.基于微放电的圆柱形通道模型，并借鉴点热源的传热公式，估算了发生在通道内部及放电衰退过程中毗邻膜层的温度场，为膜层中存在的物相种类(MgAl₂O₄，Mg₂SiO₄等)及晶态类型提供了初步的理论分析. 关键词： 等离子体电解氧化 镁合金 微放电 热效应     

垂直腔面发射激光器湿法氧化工艺的实验研究

为实现对垂直腔面发射半导体激光器氧化孔径的精确控制,提高其光电特性,对湿法氧化工艺进行了实验研究.在不同的氧化温度下,对相同结构的垂直腔面发射半导体激光器模拟片进行湿法氧化.采用X射线能谱分析仪,对氧化后模拟片的氧化层按不同的氧化深度对其氧化生成物进行检测.依据氧化生成物中氧元素组分浓度的变化,对氧化过程进行了分析与讨论,推导出在一定的温度下,氧化速率随时间变化的一般规律.提出了在垂直腔面发射半导体激光器的湿法氧化工艺过程中,适当降低氧化温度,延长氧化时间,可减小氧化限制孔径的控制误差,提高氧化工艺的准确性与稳定性.     

Microstructure and corrosion resistance behavior of ceramic coatings on biomedical NiTi alloy prepared by micro-arc oxidation

In this paper, ceramic coatings were prepared on biomedical NiTi alloys by micro-arc oxidation (MAO) in constant voltage mode. The current density-time response was recorded during the MAO process. The microstructure, element distribution and phase composition of the coatings prepared at different MAO treatment times were investigated by scanning electron microscopy (SEM), energy dispersive X-ray spectrometer (EDS), thin-film X-ray diffraction (TF-XRD) and X-ray photoelectron spectroscopy (XPS). The corrosion behavior of the coatings in 0.9% NaCl solution was evaluated by the potentiodynamic polarization test. It is found that the coatings become more compact with increasing the MAO treatment time, and the growth rate of coating decreases. The results of TF-XRD, EDS and XPS indicate that the coatings are composed of a large amount of γ-Al₂O₃ and a little α-Al₂O₃, TiO₂ and Ni₂O₃. The Ni content of the coatings is about 3 at.%, which is greatly lower than that of NiTi substrate. The bonding strength of coating-substrate is higher than 40 MPa for all the samples in this study. The corrosion resistance of the coatings is about two orders of magnitude higher than that of the uncoated NiTi alloy.     

电流密度对铝合金微弧氧化膜物理化学特性的影响

利用微弧氧化(MAO)技术，在LYl2铝合金上沉积了显微硬度达42.14GPa的超硬陶瓷膜.采用x射线衍射仪和显微硬度计研究了阳极电流密度j_a和阴极、阳极电流密度比j_c/j_a对MAO膜相构成和力学特性的影响.此外，利用扫描电子显微镜和恒电位仪分别对膜的微结构和抗点腐蚀特性进行了分析.结果表明，高j_a制备的膜主要含α-Al₂O₃相，低j_a制备的膜主要含γ-Al₂O₃相.显微硬度测试表明，这类膜有较高的硬度，但以j_a=15A/dm²和j_c/j_a=0.7制备的陶瓷膜硬度最高.抗点腐蚀测试表明，j_c/j_a对陶瓷膜的微结构有很强的影响. 关键词： 微弧氧化 显微硬度 电流密度 抗点腐蚀     

Mechanical and corrosion resistance of hydrophilic sphene/titania composite coatings on titanium and deposition and release of cefazolin sodium/chitosan films

The mechanical and corrosion resistance of hydrophilic sphene/titania composite coatings on titanium formed by a hybid technique of microarc oxidation (MAO) and heat-treatment were investigated. The results indicated that the heat-treatment could improve the hardness, elastic modulus, elastic recovery and corrosion resistance of the MAO coatings, and reinforce the interface bonding between MAO coatings and titanium. A cefazolin sodium/chitosan drug film was prepared on the coating surfaces. The drug load procedures such as the addition of chitosan obviously increased the sustained-release ability of drug films. In addition, the increase of cefazolin sodium concentration could increase the accumulative release concentration of cefazolin sodium. The sustaining-release ability of drug films deposited on the MAO and heat-treated MAO coatings is similar. In the interior of drug film, the physical and chemical bonding reactions such as Coulombic interactions, van der Waals force and H-bonding etc. could be produced, through the chemical group interactions such as -OH and -NH₂ groups of chitosan with -CO of cefazolin sodium.     

Effects of Co and W alloying elements on the electrodeposition aspects and properties of nanocrystalline Ni alloy coatings

Depending on deposition current density and alloying elements, various types of surface structure (surface morphology and grain orientation) were observed for Ni and Ni alloy nanocrystalline coatings. It was found that the variation of surface morphology with current density is in a good agreement with the variation of grain orientation. An increase in the current density produced larger grains and also reduced the charge transfer resistance and growth inhibition intensity which may change the surface structure of the coatings. For Ni coatings, the effect of surface structure on the corrosion resistance was detected to be superior to that of grain size. In the case of Ni-Co coating and at different deposition current densities, Co content and surface structure were recognized as the major factors influencing the corrosion resistance. Surface structure was also a more important factor determining the corrosion resistance of Ni-W coatings. In Ni-Co-W coatings, surface structure and grain size of the coatings were found to be independent of deposition current density. This is believed to be due to the simultaneous contrary effects of Co and W elements.     

Influence of K2TiF6 in electrolyte on characteristics of the microarc oxidation coating on aluminum alloy

Black and gray microarc oxidation (MAO) coatings were prepared in a phosphate electrolyte with and without K₂TiF₆ on 2A70 aluminum alloy, respectively. Voltage–time curves were recorded during the MAO process. The effects of K₂TiF₆ on the morphology, composition, abrasive resistance and corrosion resistance of MAO coatings were investigated. The results showed that the MAO coating produced in the electrolyte with K₂TiF₆ was thicker, and more uniform than that produced in the electrolyte without K₂TiF₆. Ti was detected in the surface of the MAO coating formed in the electrolyte with K₂TiF₆. The results of abrasive resistance and corrosion resistance showed that the MAO coating formed in the electrolyte with K₂TiF₆ exhibited better abrasive resistance and corrosion resistance.     

Formation of Al2O3 coatings on NiTi alloy by micro-arc oxidation method

Rough and porous Al₂O₃ coatings containing Ca and P were prepared on Ti–50.8 at.% Ni alloy by micro-arc oxidation (MAO) technique. The microstructure, elemental and phase composition of the coatings were investigated by scanning electron microscopy (SEM), energy dispersive X-ray spectrometer (EDS) and thin-film X-ray diffraction (TF-XRD). The thickness of the coatings was measured by eddy current coating thickness gauge. The corrosion resistance and the nickel release of the coated and uncoated samples were examined by potentiodynamic polarization tests and immersion tests in Hank’s solution, respectively. The results show that the coatings are mainly composed of γ-Al₂O₃ crystal phase. The Ni content of the coatings is about 3.5 at.%, which is greatly lower than that of NiTi substrate. With increasing treatment time, both thickness and roughness of the coatings increase. The corrosion resistance of the coated samples is about two orders of magnitude higher than that of the uncoated NiTi alloy. The concentration of Ni released from coated NiTi samples is much lower than that of uncoated NiTi sample. It can be reduced in the factor of one-seventh compared with the uncoated NiTi sample after 3 weeks immersion in Hank’s solution.     

Formation and structure of sphene/titania composite coatings on titanium formed by a hybrid technique of microarc oxidation and heat-treatment

Sphene/titania composite coatings were fabricated on titanium by a hybrid technique of microarc oxidation (MAO) and heat treatment. The high-applied voltages promote the formation of sphene in the MAO coatings after heat-treatment. Heat treatment could change the surface morphology of the MAO coatings such as roughness, macropores size and density and the thickness of the MAO coatings. Increasing the heat-treatment temperature decreased the atomic concentration ratios of Ti/Si and Ti/Ca of the MAO coatings. The chemical states of Ti⁴⁺, Ca²⁺, Si²⁺ and O²⁻ were observed on all the coatings. Additionally, Ti²⁺ was detected in the MAO and heat-treated MAO coatings at 600 and 700 °C. The heat-treatment has obvious effect on the chemical states of Si, Ti and O elements due to the formation of sphene and oxidation of TiO phase of the MAO coating, but did not affect that of Ca. In the heat-treated MAO coatings at 800 °C (MAO-H8), the titanium surface shows a MAO top layer and oxidized interior layer. A concentration gradient in components in the MAO layer of the MAO-H8 coating was formed.     

Evolution of micro-arc oxidation behaviors of the hot-dipping aluminum coatings on Q235 steel substrate

Micro-arc oxidation (MAO) is not applicable to prepare ceramic coatings on the surface of steel directly. In this work, hybrid method of MAO and hot-dipping aluminum (HDA) were employed to fabricate composite ceramic coatings on the surface of Q235 steel. The evolution of MAO coatings, such as growth rate, thickness of the total coatings, ingrown and outgrown coatings, cross section and surface morphologies and phase composition of the ceramic coatings were studied. The results indicate that both the current density and the processing time can affect the total thickness, the growth rate and the ratio of ingrown and outgrown thickness of the ceramic coatings. The total thickness, outgrown thickness and growth rate have maximum values with the processing time prolonged. The time when the maximum value appears decreases and the ingrown dominant turns to outgrown dominant little by little with the current density increasing. The composite coatings obtained by this hybrid method consists of three layers from inside to outside, i.e. Fe-Al alloy layer next to the substrate, aluminum layer between the Fe-Al layer and the ceramic coatings which is as the top exterior layer. Metallurgical bonding was observed between every of the two layers. There are many micro-pores and micro-cracks, which act as discharge channels and result of quick and non-uniform cooling of melted sections in the MAO coatings. The phase composition of the ceramic coatings is mainly composed of amorphous phase and crystal Al₂O₃ oxides. The crystal Al₂O₃ phase includes κ-Al₂O₃, θ-Al₂O₃ and β-Al₂O₃. Compared with the others, the β-Al₂O₃ content is the least. The MAO process can be divided into three periods, namely the common anodic oxidation stage, the stable MAO stage and the ceramic coatings destroyed stage. The exterior loose part of the ceramic coatings was destroyed badly in the last period which should be avoided during the MAO process.