碱热处理对TC4合金微弧氧化膜生物活性的影响

利用微弧氧化技术在Ti6Al4V合金表面制备含钙、磷的多孔TiO_2涂层(记为MAO),并对涂层进行碱热处理(记为MAONH).结果表明:MAONH膜层的相结构和MAO膜层的大有不同,它主要由TiO_2(金红石型和锐钛矿型)、钛酸钙相组成.钙和磷离子在MAONH膜层表面比在MAO膜层表面更容易沉积,其原因是钛酸钙在模拟体液浸泡时发生水解,生成大量的Ca~(2+)和OH~- 离子,Na~+和OH~-离子同模拟体液中的Ca~(2+)和PO_4~(3-)离子发生离子交换,导致磷灰石在MAONH膜层表面沉积.     

Effect of K_2TiO(C_2O_4)_2 Addition in Electrolyte on the Microstructure and Tribological Behavior of Micro-Arc Oxidation Coatings on Aluminum Alloy

Micro-arc oxidation(MAO)coatings with different concentrations of K_2TiO(C_2O_4)_2 in the sodium silicate base electrolyte were prepared on 6061 aluminum alloy with the aim of promoting a better understanding of the formation mechanisms and tribological behaviors of the coatings.Scanning electron microscopy(SEM)assisted with energy-dispersive X-ray spectroscopy(EDS),X-ray photoelectron spectroscopy(XPS)and friction test were employed to characterize the MAO processes and microstructure of the resultant coatings.Results showed that the composition and microstructure of the coatings were significantly affected by the addition of K_2TiO(C_2O_4)_2.A sealing microstructure of MAO coating was obtained with the addition of K_2TiO(C_2O_4)_2.Ti element from K_2TiO(C_2O_4)_2 was only absorbed into the defects of micropores under surface energy in the early stage,while in the later stage,Ti element was predominant in the micropores and distributed on the coatings under plasma discharge to form TiO_2.It was demonstrated that Ti and Si elements from the electrolyte could interact with each other during the MAO process and the interaction mechanism was systematically analyzed.Wear resistance of the MAO coatings with K_2TiO(C_2O_4)_2 addition was significantly improved compared with that of the MAO coatings without K_2TiO(C_2O_4)_2 addition.     

6061铝合金表面新型黄色微弧氧化陶瓷层的制备与表征

目的 研究6061铝合金表面新型微弧氧化黄色陶瓷层的制备工艺,并对其微观结构、成分、硬度、耐蚀性能等进行表征。方法 在以Na2SiO3为基础的电解液中加入Na2SnO3进行微弧氧化处理,制备出黄色微弧氧化陶瓷层,并与传统白色、黄色、黑色微弧氧化陶瓷层作对比。采用SEM和EDS分析膜层表面形貌和元素分布,借用XPS对膜层进行成分表征,使用硬度计测试其表面硬度,采用电化学工作站和人造海水腐蚀实验评价陶瓷层的抗腐蚀性能。结果 随着电解液中Na2SnO3浓度的增加,陶瓷层中Sn元素含量增加,Si元素含量减少,陶瓷层黄色饱和度不断增强。黄色含Sn陶瓷层制备过程中,电解液中的SnO32-在高温高压下转化为SnO2,导致陶瓷层硬度达到365HV,高于白色与黑色陶瓷层。在3.5% NaCl溶液中进行电化学测试,黄色含Sn陶瓷层的腐蚀电流密度与腐蚀电位分别为9.34×10-9 A/cm2和-0.34 V,耐蚀性优于白色和黄色含Mn陶瓷层。结论 在电解液中添加Na2SnO3可在铝合金表面生成具有较高硬度和耐蚀性能良好的类似沙漠黄色的陶瓷层,为铝及其合金在多领域的应用奠定了一定的实验基础。     

Ti6Al4V微弧氧化TiO2/W复合膜的制备及摩擦学性能

目的提高Ti6Al4V合金的摩擦学性能。方法在硅酸盐-磷酸盐电解液中添加不同浓度的纳米W粉,利用微弧氧化技术在Ti6Al4V基体表面制备出氧化陶瓷膜。利用FE-SEM、EDS和XRD研究了在不同浓度W粉参与下的微弧氧化膜表截面微观形貌、元素分布及膜层相组成。通过旋转摩擦磨损试验评估了膜层的摩擦学性能。结果电解液中加入纳米W粉可以促进膜厚增长,尤其在含0.5～2 g/L纳米W粉时,膜厚呈近似线性增长;但W粉在膜层表面的附着会导致粗糙度的增大。在纳米W粉参与下,微弧氧化膜中除了锐钛矿、金红石和Al_2TiO_5相之外,W含量也随电解液中颗粒含量的增加而提高。在6 g/L纳米W粉复合下,微弧氧化膜的摩擦系数、比磨损率分别减小了约13.33%和3.53%。结论 W粉颗粒以机械啮合附着在氧化膜表面,部分颗粒随熔融氧化物包裹进入膜层并发现熔化迹象。W粉含量为6 g/L时,制备的氧化膜表面质量有所改善,即微孔和裂纹等有所减少,耐磨性较佳,摩擦系数和比磨损率较不含W粉的膜层均有所减小。     

甘油磷酸钙浓度对钛合金MAO涂层性能的影响

目的 提高医用钛合金的生物活性。方法 在含葡萄糖酸钙(Ca Glu₂)、葡萄糖酸镁(MgGlu₂)、植酸钠(Na₁₂Phy)和磷酸(H₃PO₄)的基本溶液中,分别添加8、10、12 g/L甘油磷酸钙(Ca-GP),采用MAO方法在Ti-6Al-4V表面制备3种涂层。使用SEM、EDS、XRD、XPS和AFM检测涂层表面形貌、化学成分、物相结构、元素存在状态和表面粗糙度,并测试涂层的接触角、结合强度以及体外生物活性。结果 经过MAO处理后,钛合金表面可成功生长出多孔陶瓷涂层,Ca-GP参与了MAO涂层形成。当Ca-GP的质量浓度为8 g/L时,涂层非常粗糙,Ca和Mg的原子数分数分别为7.56%和1.74%。随着Ca-GP浓度的增加,微孔均匀性变好,表面微裂纹减少,且钙磷原子比(Ca/P)显著提高。在含8、10 g/L的Ca-GP溶液中,制备的涂层以Ti、锐钛矿和金红石型Ti O2组成为主;在12g/L的Ca-GP溶液中生成的涂层,Ca/P原子比可达1.77,含有Ti P     

Na2SiO3系溶液中Ti6A14V微弧氧化陶瓷膜的结构与力学性能

采用交流微弧氧化法于Na2SiO3-KOH-（NaPO3)6-NaAlO2溶液中在Ti6A14V表面形成了氧化物陶瓷膜。用扫描电镜和X射线衍射研究了陶瓷膜的组织形貌和相组成，用Nano IndenterXP系统研究膜层的力学特性。结果表明：氧化膜分为3层，即过渡层、致密层与疏松层。膜层主要由金红石相TiO2及少量锐钛矿相TiO2组成。膜层中致密层与基底的弹性回复分别为40.5%和14.9%，硬度分别为8.54GPa和5.5GPa，弹性模量分别为87.4GPa和150GPa，膜层表现出明显的陶瓷特征。     

Effects of additives on corrosion and wear resistance of micro-arc oxidation coatings on TiAl alloy

Ceramic coating was deposited on TiAl alloy substrate by micro-arc oxidation(MAO)in a silicate-aluminate electrolyte solution with additives including sodium citrate,graphite and sodium tungstate.The microstructures and compositions were analyzed by SEM,EDX and XRD.The corrosion and wear properties of the coatings were investigated by potentiodynamic polarization and ball-on-disc wear test,respectively.The results show that the MAO coatings consist of WO3,Ti2O3,graphite and Al2O3 besides Al2TiO5 and Al2SiO5.With additives in the electrolyte,the working voltage at the micro-arc discharge stage decreases,and the ceramic coating gets smoother and more compact.The corrosion current density of MAO coating is much lower than that of TiAl substrate.It can be reduced from 9.81×10-8A/cm 2to 3.02×10-10A/cm 2 .The MAO coatings composed of hard Al2O3,WO3 and Ti2O3 obviously improve the wear resistance of TiAl alloy.The wear rate is-3.27×10-7g/(N·m).     

ZnHA/TiO2复合涂层的制备及生物相容性

为改善羟基磷灰石(HA)涂层与Ti基体的结合性能及成骨性能,在纯Ti表面先通过微弧氧化方法形成多孔TiO2,然后通过溶胶-凝胶法在其上形成ZnHA生物涂层.利用SEM和XRD观察和分析样品的表面形貌和物相组成,采用火焰原子吸收分光光度法测量Zn2十的释放浓度.将MG-63细胞直接接种于样品表面,评价成骨细胞在样品表面的...     

Effect of voltage on microstructure and corrosion resistance of microarc oxidation coatings on CP-Ti

The surface modification of commercially pure titanium (CP-Ti) by microarc oxidation (MAO) under different voltages was investigated using 1%H₃PO₄ solution as an electrolyte. The microstructure, phase composition and elemental distribution of ceramic coatings were investigated using scanning electron microscopy (SEM) and X-ray diffraction. The corrosion behaviour of the coating was also examined by potentiodynamic polarisation testing in a 3·5 wt-%NaCl solution. Micropore oxide films were formed on all the sample groups by MAO. The thickness and micropore size of the MAO coating increased with the increasing voltage. Energy dispersive X-ray spectroscopy results indicate that Ti, O and P became incorporated into the MAO coatings. At a low voltage of 250 V, the MAO coatings were composed of amorphous, P₂O₅, TiP₂O₇ and titania phases (rutile and anatase). Variation of treatment voltages increased the ceramic coatings from an amorphous structure to a phase structure, and the P₂O₅ phase disappeared. The corrosion potential Φ_corr of the MAO sample shifted towards nobler directions, and the corrosion density I_corr fell significantly compared with that of the bare CP-Ti. Corrosion testing showed that the sizes of the micropore of the MAO samples obviously decrease, and the MAO surface becomes smooth.     

Ti2AlNb合金微弧氧化电解液优化及耐磨性研究

目的优化Ti_2AlNb合金微弧氧化的电解液配方,提高Ti_2AlNb合金微弧氧化膜的耐磨性。方法借助SEM、EDS、XRD研究硅酸盐-磷酸盐电解液体系中Na_2MoO_4浓度对Ti_2AlNb合金微弧氧化膜形貌、成分及相结构的影响。利用CFT-I型磨损试验机测试不同微弧氧化膜的摩擦磨损性能。结果电解液中添加Na_2MoO_4后,微弧氧化膜的生长速率增加,膜层中出现了Mo元素且含量也逐渐增加。Na_2MoO_4的加入降低了Ti_2AlNb合金微弧氧化膜的摩擦系数及比磨损率,但微弧氧化膜的耐磨性并非随Na_2MoO_4含量线性提高。含6 g/L Na_2MoO_4的体系中,微弧氧化膜摩擦系数低至0.25左右,比磨损率仅为1.20×10~(-3) mm~3/(N·m),表面呈轻微磨粒磨损特征。结论电解液中的Na_2MoO_4参与了成膜过程,对Ti_2AlNb合金微弧氧化膜的生长有显著的促进作用,有效地改善了Ti_2AlNb合金微弧氧化膜的耐磨性。     

钛合金表面GO/HA/MAO复合膜层的制备及其性能

为了改善钛合金种植体在体液中的腐蚀及摩擦腐蚀行为,延长其在人体环境中的服役时间,在微弧氧化 (MAO)膜层上采用溶胶凝胶(Sol-gel)法于羟基磷灰石(HA)和氧化石墨烯(GO)的混合溶胶中浸渍提拉成膜,从而在 Ti6Al4V 合金表面成功地制备了 GO/ HA/ MAO 复合膜层。 结果表明,MAO 膜层表面的微孔及微球被 GO/ HA 薄膜有效的覆盖且较为致密;膜层的物相组成主要为金红石相及锐钛矿相的 TiO₂、HA、SiO₂ 和GO;根据电化学腐蚀和摩擦腐蚀结果分析知,GO/ HA/ MAO 复合膜层在模拟体液(SBF)中的耐蚀性及耐摩擦腐蚀性相比于 MAO 膜层和 Ti6Al4V 基体均得到了显著提高。     

Antifouling properties of micro arc oxidation coatings containing Cu2O/ZnO nanoparticles on Ti6Al4V

Micro arc oxidation (MAO), as a new special surface treatment method, has been introduced to the marine antifouling field for titanium alloys because of the anatase and rutile TiO₂ with antibacterial effects obtained during the oxidation process. Despite this, metallic oxide antifouling additives have been added into MAO coatings to improve the antibacterial and antifouling abilities of titanium alloy. In this study, MAO coatings containing nanometer particles were obtained by adding nano Cu₂O and nano ZnO into the electrolyte. Structure, morphology, phase constitution and chemical composition of the MAO coating film were studied by SEM, XRD and EDS. The antibacterial properties of the film were evaluated by exposing the specimens to Escherichia coli and comparing the Ti-MAO and Ti-bared controls. The results showed that the MAO process on Ti6Al4V has an outstanding antibacterial property which can be further enhanced by nano Cu₂O and nano ZnO. The Ti-MAO–Cu₂O group had the best antibacterial ability. These findings indicate that by means of this process adding nanometer metallic oxide into an MAO coating film via an electrolyte is useful for enhancing the antibacterial and antifouling abilities of titanium.     

交流脉冲参数对TC4钛合金微弧氧化陶瓷膜的影响

为了研究交流脉冲占空比和频率对微弧氧化膜的影响.采用恒电流方式对TC4钛合金进行微弧氧化,用扫描电镜和X衍射仪分析膜层的表面形貌及相结构.结果表明:随占空比的增大,微弧氧化膜层的生长速率增大,金红石相TiO2相对含量增加;随频率的增大,微弧氧化膜层的生长速率减小,表面趋于平整,锐钛矿相和金红石相TiO2相对含量与处理频率无关.     

AZ91D压铸镁合金激光局部重熔区气孔的形成机制

采用扫描电镜(SEM)、X光电子能谱分析仪(XPS)等分析手段,研究了NiTi合金表面绝缘膜的结构及成分,从而探讨非阀金属NiTi合金表面微弧氧化陶瓷膜层的形成机制.结果表明,NiTi合金微弧氧化过程中的电流密度-时间曲线与纯钛形状基本一致,也可分为3个阶段,但其最大的电流密度为后者的13倍;NiTi合金表面的绝缘膜主要是通过电化学沉积形成的Al2O3及少量的TiO2、Ni2O3和磷酸盐薄膜,这一绝缘膜就相当于阀金属的阳极氧化膜,为NiTi合金进行微弧氧化处理提供了前提条件;NiTi合金表面的陶瓷膜层主要来源于电解液中的铝酸根离子和少量的基体Ni和Ti(包括固态的和溶解于电解液中离子态的),经反复的放电、熔融、喷射、冷却、凝固,发生一系列的电化学、等离子体化学和热化学反应最终形成表面粗糙多孔陶瓷膜层.     

Compound Ceramic Coatings on Ti-6Al-4V by Micro-Plasma Oxidation in NaAlO2 Solution

MICRO PLASMA OXIDATION(MPO)technique,bywhich compound ceramic coating can be grown in situon Al,Ti,Mg and many other valve-metals,has apromising application prospect in the fields likemilitary,aerospace,textile,automobile,hospital,decoration aspects,and so on tl"3).Although there aretwo much work on the composition and the structure ofthe coatings l4"61,the application of ElectrochemicalImpedance Spectroscopy(EIS)technique on suchcoatings is seldom reported.And EIS is a powerfulan…     

电解液成分对纯钛表面微弧氧化膜结构与生物活性的影响

采用微弧氧化处理技术,在纯钛TA2表面制备了含钙磷的多孔复合氧化膜,用SEM、XRD、EPMA等分析了电解液成分对氧化膜形貌、成分、相构成及生物活性的影响。结果表明:纯钛表面微弧氧化后原位生成的含钙磷多孔性复合氧化膜由锐钛矿相TiO2,金红石相TiO2和基体Ti组成;随电解液中钙磷摩尔比(Ca/P)值的增大,表面孔洞数量增多、直径变小,膜中Ca/P值增大,锐钛矿相TiO2减少、金红石相TiO2增多;当电解液中Ca/P=5时得到的氧化膜的Ca/P值为1.528,将该样品经碱液处理后再在快速钙化溶液(FCS)中浸泡2 d后即有羟基磷灰石HA形成,表明其具有良好的生物活性。     

镁合金微弧氧化黑色膜的制备工艺和结构

用微弧氧化的方法,通过两种电解液体系在AZ91D镁合金基体上获得颜色均匀、致密性好的黑色陶瓷层,研究了在这两种体系中,着色盐成分、浓度,以及氧化电压和处理时间对氧化陶瓷层的影响。结果表明：试样在两种电解液体系中皆能得到黑色陶瓷层,不同的基础电解液所需加的着色盐不同,在硅酸盐体系中以CuSO4为主要着色盐,在磷酸盐体系中以CoSO4为主要着色盐。着色盐浓度和氧化电压对膜层颜色影响较大,在一定范围内,随着氧化电压的上升,膜层颜色有所加深,而相同条件下氧化时间的改变对颜色变化影响较为缓和。通过比较,发现在磷酸盐体系中膜层表面质量最好。     

纯铜表面热化学反应陶瓷涂层耐磨性研究

在工业纯铜表面分别用料浆法和热化学反应法制备陶瓷涂层,陶瓷涂层骨料为Al_2O_3、TiO_2和ZnO,粘接剂为钠水玻璃.研究了该涂层与基体的结合强度、涂层的抗热震性能、耐磨性,用SEM观察了涂层表面和截面的形貌.用X射线衍射法分析了涂层的相组成.结果表明,热化学反应法制备的陶瓷涂层热同化后,涂层内有NiAl_2O_4、Al_2SiO_5,新相.且这新相增加了涂层与基体的结合强度.热化学反应法制备的陶瓷涂层磨粒磨损和粘着磨损的相对耐磨性分别是基体的11.26倍和7.97倍.     

Ti6Al4V合金微弧氧化/Cr2O3复合膜的生长特征与摩擦学性能

在电解液中加入Cr2O3微粒,以共生沉积方式在Ti6Al4V表面制备微弧氧化/Cr2O3复合膜。利用SEM、XRD、EDS等研究复合膜的生长规律及Cr2O3微粒的沉积方式,通过摩擦试验分析不同生长阶段的复合膜的摩擦磨损性能。结果表明:在0~30min内,复合膜呈近线性增长,之后生长速率明显变缓,膜层表面也出现了大块Cr2O3团聚体。复合膜主要由金红石TiO2、锐钛矿TiO2及Cr2O3相组成。随氧化时间的延长,锐钛矿TiO2逐渐减少,金红石TiO2含量先增加后趋于稳定,而Cr2O3的衍射峰一直增强,复合膜的耐磨性也先增后降;氧化20min时,复合膜的耐磨性最好,摩擦系数最小,仅为0.05~0.2。在微弧氧化过程中,Cr2O3微粒或直接吸附在熔融态的氧化膜表面,或被捕捉、锁定到氧化膜的表面微孔中;也有部分Cr2O3微粒被高温放电产生的熔融物裹覆并一起遇冷凝固到氧化膜中。     

TC4 合金表面微弧氧化制备抗高温氧化涂层

目的寻求最佳的微弧氧化工艺参数,提高钛合金的高温抗氧化性能。方法进行3因素3水平正交试验(3因素包括电压、氧化反应时间和电解液浓度),通过XRD和SEM表征微弧氧化涂层的物相和显微结构,采用650℃×100 h循环氧化试验评价涂层的抗高温氧化性能,最终利用极差分析法分析各因素对涂层试样氧化增重的影响主次,并得到最优参数组合。利用回归分析建立氧化增重与试验各参数之间的数学模型,并分析模型的显著性。结果不同工艺参数下制得的微弧氧化涂层表面形貌特征不同,涂层物相以金红石相和锐钛矿相二氧化钛为主。3个因素对涂层抗高温氧化性的影响由大到小依次为:电压时间电解液浓度。建立的氧化增重W与各参数(电压V、反应时间t、电解液浓度E)间的二次函数方程模型为:W=0.008 39(V-396.6)+0.1698t-64.5E-0.000 108(V-396.6)2-0.0044t2+700E2+0.0017。结论最佳参数组合为:电压480 V,时间25 min,电解液浓度0.04 mol/L。通过回归分析得到的氧化增重与各参数间的数学模型显著。