Ti基体上形成微弧氧化膜组成和结构的研究

在甘油磷酸钙和醋酸钙电解液中采用直流电源对纯Ti进行了微弧氧化。采用微弧氧化方法所制备的氧化膜具有粗糙多孔的结构,且微孔直径随着电压的增加而增大。AES分析表明在基体与氧化膜界面发生了扩散,从基体钛到氧化膜的表面氧的浓度逐渐增大,钛的浓度逐渐减小。XPS分析表明氧化膜的组成随着所施加的微弧氧化电压而改变,微弧氧化电压为200V时TiO2、Ti2O3和TiO占Ti的原子百分比分别为72．61％、22．08％和5.31％;当微弧氧化电压为350V时氧化膜表面Ti元素只由TiO2、Ti2O3组成,且占Ti的原子百分比分别为85．48％、14．52％。     

微弧氧化和水热合成在钛基上制备羟基磷灰石

在含有0.04mol/L的磷酸二氢钠和0.01mol/L的醋酸钙电解液中对T i进行微弧氧化,生成含Ca和P很高的氧化膜。氧化膜粗糙多孔。然后,将样品放在220℃的高压釜中进行4h的水热处理,羟基磷灰石晶体在氧化膜表面沉积。用XRD检测氧化膜的晶体结构,用XPS研究氧化膜表面的化学成份,用SEM-EDS观察样品表面形貌。     

Effects of electrolytic concentration on properties of micro-arc film on Ti6A14V alloy

To study the effect of electrolytic concentration, bioactive ceramic films containing Ca and P on the surface of the Ti6Al4V alloy were prepared by micro-arc oxidation (MAO) in aqueous solutions of different concentrations. Composition, mi-cro-morphology, wettability of the films and their corrosion behavior in a Hank's SBF were studied. Our experimental results show that the film is mainly composed of anatase, ruffle and amorphous phases. With an increase in electrolytic concentration, the ratio of ruffle in films enlarge and small amounts of calcium phosphate (Ca3(PO4)2) and hydroxyapatite (HA) appear. The number of mi-cropores in films increases but their dimensions decrease and their porosities increase slightly. As the surface roughness of MAO film increases with concentration, the wettablility of the oxide film improves continually, while micro-hardness increases at first and then decreases. MAO treatment clearly improves the corrosion resistance of substrates in a Hank's SBF.     

Ti6Al4V合金表面纳米管阵列的制备

以氢氟酸和铬酸为电解液,采用阳极氧化法在Ti6Al4V合金表面制备高密度的纳米管阵列.利用场发射扫描电镜、X射线衍射仪和X射线光电子能谱对多孔氧化膜的形貌和结构进行分析,利用极化曲线和电化学阻抗谱研究了电解液中CrO3的作用机理.结果表明:电解液种类决定能否形成多孔氧化膜,而电解液的浓度影响多孔氧化膜的形貌和孔径大小;纳米管阵列氧化膜主要由大部分非晶态组织的TiO2,Al2O3和少部分晶态的Al2TiO5,Al3Ti5O2,Al2O3组成,氧化膜内的Al,Ti原子比高于基体中的Al,Ti原子比;CrO3浓度的高低会影响氧化膜的结构.     

Characterization of Ti-Cu Films Deposited by HPPMS and Effect on NO Catalytic Release and Platelet Adhesion Behavior

Ti-Cu films with different Cu concentrations were fabricated by high-power pulsed magnetron sputtering(HPPMS) to release copper ions and catalyze NO to improve the blood compatibility. The Cu concentrations of films were 25.7 at% and 68.8 at%. Pure Ti films were also fabricated. Copper release, catalytic release of nitric oxide(NO), and blood platelet adhesion of Ti-Cu films were studied. Ti-Cu films released copper ions in PBS solution and more Cu ions were released from films with 68.8 at% Cu. Ti-Cu films had excellent ability of catalytical decomposition of exogenous donor S-nitroso-N-acetyl-DL-penicillamine(SNAP) and as a result, nitric oxide(NO) was generated. The NO generation catalyzed by Ti-Cu films was significantly higher than that by pure Ti films. This was more eminent in the Ti-Cu films with 68.8 at% Cu. The platelet adhesion and activation of Ti-Cu films were significantly inhibited compared to that of pure Ti films in the presence of SNAP. The Ti-Cu film fabricated by HPPMS showed the ability of releasing Cu ions to catalyze SNAP to generate NO to inhibit platelet adhesion and activation.     

曙红敏化微弧氧化TiO2膜光催化研究

以钛片为原料,以磷酸钠为电解液,采用微弧氧化法在钛片上制备钛基二氧化钛膜(TiO2/Ti).用20W的紫外灯光催化降解苯酚模拟废水,采用敏化后处理对二氧化钛膜进行改性实验,考察了敏化剂、敏化剂浓度、微弧氧化时间、pH等条件对二氧化钛膜的影响.实验结果表明:在微弧氧化电压为300V,电解液浓度为8g/L,微弧氧化时间为5m in,光催化时间为2h,曙红为敏化剂的浓度为20 mg/L,pH为6,敏化时间为10h,光催化效率由原来的31.5(提高到52.2(.     

Ti6Al4V钛合金微弧氧化工艺研究

采用直流稳压电源,选用3种不同PH值的碱性微弧氧化电解液,在Ti6Al4V钛合金表面制备微弧氧化膜层;应用扫描电子显微镜分析微弧氧化膜层形貌特征。结果表明,钛合金微弧氧化膜层表面凹凸不平,带有微米级和亚微米级的孔洞,孔洞周围呈现火山丘状形貌特征;微弧氧化电解液PH值越大,火花放电时间越长;在给定电压条件下,电解液PH值越大,微弧氧化膜层厚度越大。     

The effect of anodizing temperature on the structure and electrical properties of Al-Ti composite oxide film

The tendency in high capacitance and small volume of aluminum electrolytic capaci-tors that act as the key components in the electrical complex strongly requires increasing specific capacitance of anodic aluminum foils. The electric capacitance, C, of electro-lytic capacitors is expressed by C=ε0ε r S/d, where ε 0 is the dielectric constant of vacuum atmosphere, ε r represents the relative dielectric constant of the anodic oxide film, S is on behalf of the effective surface area, and d is…     

Analyses of Microarc Oxidation Coating Formed on AZ91D Alloy in Phosphate Electrolytes

This paper studied the appearance transition of microdischarges, the phase composition and the morphology evolution of the oxide film formed by microarc oxidation on AZ91D magnesium alloy. The appearance of microdischarges population experienced apparent changes in size, spatial density and color, which was related with the changes of the type and quantity of the disintegrated gas bubbles generated at the interface between the electrolyte and substrate. Correspondingly, the diameter of micropores together with net-like fine microcracks increased when a higher voltage was employed. The coating was composed of MgO, MgAl2O4 and there existed a fluoride-enriched zone of about 3-5μm at the film/substrate interface.     

Preparation of Hydroxyapatite-titanium Dioxide Coating on Ti6Al4V Substrates using Hydrothermal-electrochemical Method

Ti6Al4V substrates were anodized in a 0.5 mol/L H_2SO_4 solution at applied voltages of 90-140 V.A hydroxyapatite-titanium oxide(HA-TiO2)coating was then deposited on the anodized Ti6Al4 V substrates via a hydrothermal-electrochemicalmethod at a constant current.The obtained films and coatings were characterized by X-ray diffraction,scanning electron microscopy,energy-dispersive X-ray spectroscopy,and Fourier-transform infrared spectrometry.The microstructures of the porous films on the Ti6Al4 V substrates were studied to investigate the effect of the anodizing voltage on the phase and morphology of the HATiO_2 coating.The results indicated that both the phase composition and the morphology of the coatings were significantly influenced by changes in the anodizing voltage.HA-TiO_2 was directly precipitated onto the surface of the substrate when the applied voltage was between 110 and 140 V.The coatings had a gradient structure and the HA exhibited both needle-like and cotton-like structures.The amount of cotton-like HA structures decreased with an increase in voltage from 90 to 120 V,and then increased slightly when the voltage was higher than 120 V.The orientation index of the(002)plane of the coating was at a minimum when the Ti6Al4 V substrate was pretreated at 120 V.     

β钛合金微弧氧化膜制备及其在人体模拟液中腐蚀性能研究

采用微弧氧化技术在TiNbZrFe合金表面制备出含钙磷成分的多孔氧化膜,通过人体模拟液浸泡的方法诱导生成羟基磷灰石,并利用电化学阻抗谱（EIS）研究其在人体模拟液中浸泡不同时间后的耐腐蚀性能．结果表明,经400V电压微弧氧化后TiNbZrFe合金表面氧化膜的形貌与成分达到最优化,且明显有α-Ca3（PO4）2 相生成;α-Ca3（PO4）2 相能够起到良好的诱导生成羟基磷灰石（HA）的作用,在人体模拟液中浸泡1d后,通过XRD检测出有HA相生成,导致微弧氧化膜层表面的微孔被诱导生成物覆盖填充明显,较小微孔完全消失;随着浸泡时间的延长,经过微弧氧化膜诱导生成的HA涂层不断增厚,EIS结果表明其具有良好的隔绝渗透作用,能够阻碍腐蚀性介质在溶液和金属界面之间扩散和迁移,从而起到保护基体抗腐蚀的作用．     

多孔型阳极氧化铝膜的制备及微观分析

在硫酸电解液、草酸和磷酸电解液中,采用阳极氧化方法制备多孔型氧化铝膜。通过扫描电子显微镜对多孔型氧化铝膜进行形貌表征。根据试验得到:当0.3mol/L硫酸中,恒压25V阳极氧化1h可得到孔径约为40～60nm多孔氧化铝膜。在电解液为10.0g/L草酸与3.0ml/L磷酸混合液中,恒压140V二次阳极氧化可得到孔径为160～190nm多孔氧化铝膜。讨论了高温退火及磷酸处理对多孔氧化铝膜的影响,并进行了机理分析。     

A combinatorial approach of developing alloy thin films using co-sputtering technique for displays

In this study we have used a combinatorial approach for producing binary and ternary alloy thin film libraries using a lab-scale RF co-sputtering system. Initially we used two elemental sputtering targets, i.e. aluminum (Al) target and neodymium (Nd) target, to produce a film library of varying composition and successfully identified a suitable composition range (1.95―2.38 at% Nd) in which resistance to hillock formation and resistivity of the film spots were found to be satisfactory in annealed state (350℃, 30 min). In another case, in order to form ternary alloy composition library we have used two sputtering targets, i.e. an Al-0.5 at% Nd alloy target and an elemental Ni target. Though, co-sputtered Al-0.6 at% Nd-0.9 at% Ni alloy films showed satisfactory resistance to hillock formation and low resistivity after annealing, film deposited from a ternary alloy target with the same composition failed to show satis- factory resistance to hillock formation during annealing. In case of Al-0.6 at% Nd-0.9 at% Ni alloy target, 250 nm thick film showed poor resistance to hillock formation than the 500 nm thick film. This clearly showed thickness-dependent hillock performance of Al-0.6 at% Nd-0.9 at% Ni alloy. In this study it was found that, in addition to the process variables, metallurgical microstructure of the alloy sputtering targets had significant effect on the film properties which was not obvious from the results of films deposited using co-sputtering of the individual elemental targets.     

Sol-gel derived bioactive hydroxyapatite/titania composite films on Ti6Al4V

The composite films consisting of the titania gel impregnated with hydroxyapatite （HAP） submicron particles were prepared on commercial Ti6A14V plates processed by a sol-gel route. HAP powders were synthesized based on wet chemical precipitation method with Ca（NO3）2.4H2O and （NH4）2HPO4 as starting reagents. After being calcined at 900℃, HAP powders were ultrasonically scattered in ethanol to produce HAP sol. The titania sol was prepared using titanium （IV） isopropoxide {Ti[OCH（CH3）2]4} as precursor. Both the titania sol and the HAP/titania mixture were sequentially spin-coated on the substrates and calcined at various temperatures. The characteristics and mechanical adhesion of the composite films were investigated. The results show that the as-prepared films are dense, homogeneous, well-crystallized, and there is a good interfacial adhesion between the film and the substrate. The in vitro bioactivities of these films were discussed based on the analysis of the variations of Ca and P concentrations in the simulated body fluid and their surface morphologies against immersion time.     

铸造纯钛表面微弧氧化工艺研究

微弧氧化技术可以有效地改善钛合金的表面性能.实验以Na3PO4.12H2O为电解质对铸造纯钛进行微弧氧化.结果表明,不同电压的微弧氧化效果不同,铸造纯钛的微弧氧化的最佳工艺参数为电压275V,电解质浓度15g/L,时间15min.纯钛微弧氧化后表面为一层为致密和一层带有微孔的双层TiO2氧化膜,氧化膜是由于火花放电和排出气体形成的.     

Structural and mechanical properties of amorphous carbon films deposited by the dual plasma technique

Direct current metal filtered cathodic vacuum are (FCVA) and acetylene gas (C2H2) were wielded to synthesize Ti-containing amorphous carbon films on Si (100). The influence of substrate bias voltage and acetylene gas on the microstructure and mechanical properties of the films were investigated. The results show that the phase of TiC in the (111) preferential crystallo-graphic orientation exists in the film, and rite main existing pattern of carbon is sp2. With increasing the acetylene flow rate, the con-tents of Ti and TiC phase of the film gradually reduce; however, the thickness of the film increases. When the substrate bias voltage reaches -600 V, the internal stress of the film reaches 1.6 GPa. The micro-hardness and elastic modulus of the film can reach 33.9 and 237.6 GPa, respectively, and the friction coefficient of the film is 0.25.     

固定态TiO2薄膜制备及光催化氧化性能研究

以TAi钛合金为原料,在不同的成膜电压及电流密度下,用阳极氧化法在基体表面原位生长TiO2薄膜,应用于光催化氧化及光电催化氧化反应体系降解水中的罗丹明B,采用X射线衍射法和扫描电镜对薄膜的粒径、物相进行了表征,结果表明：当成膜电压为160V,电流密度为160mA／cm^2时,薄膜中二氧化钛晶型以锐钛矿型为主,粒径45～50nm;在光催化氧化水中罗丹明B的实验中,90min去除率达到93．5％,该薄膜表现了很好的光催化活性;同时,外加一定的偏压,在降解的最初60min时,外加偏压0．6V比未加偏压(OV)的薄膜电极罗丹明B的去除率提高了33．4％,表明外加偏压可以提高光催化氧化的效率。     

工艺参数对LY12铝合金复合涂层的影响

以恒压模式在NaOH-Na2SiO3电解液中对LY12铝合金进行微弧氧化实验,然后用强流脉冲电子束轰击,采用扫描电镜、XRD、涂层测厚仪等检测手段,研究电参数对复合涂层的影响.结果表明：电压越高,氧化时间越长,微弧氧化膜越厚;电子柬复合处理后,涂层变得平整、致密,新相α-Al2O3峰值变高,耐摩擦磨损性能增加.     

Synergistic Corrosion Inhibition Effect of Molybdate and Phosphate Ions for Anodic Oxidation Film Formed on 2024 Aluminum Alloy

In order to effectively improve the corrosion resistance of aluminum alloys, anodic oxidation technique was used to generate the oxide film. We investigated the influences of two inorganic corrosion inhibitors(ammonium dihydrogen phosphate and sodium molybdate) on the corrosion resistance of anodic oxidation films on 2024 aluminum alloy, and studied the synergistic effect of two corrosion inhibitors. The corrosion resistance of anodic oxidation film in 3.5 wt% NaCl solution was evaluated by electrochemical impedance spectroscopy(EIS) and potentiodynamic polarization curves. Results show that, after adding the single ammonium dihydrogen phosphate or sodium molybdate of 0.01 M to oxalic acid electrolyte, inhibition efficiencies of the anodized samples are 10% and 47%, respectively. However, in the presence of two inhibitors with the same concentration of 0.01 M, inhibition efficiency can be as high as 92%. Therefore, we observed the significantly synergistic corrosion inhibition effect of molybdate and phosphate ions for anodic oxidation film formed on 2024 aluminum alloy.     

铝合金基体厚度对硬质阳极氧化膜的影响

选用不同厚度、相同表面积的6061铝合金板材试样,在相同工艺参数下对各试样进行硬质阳极氧化,动态采集其在氧化过程中的氧化电压,测量各试样氧化膜的厚度和硬度,并对测试结果进行比较分析。结果显示,基体厚度越大,在致密层形成后氧化膜生长速度越快,且额定氧化时间后获得的膜层越厚、硬度值越高。