制备参数对氧化铌涂层晶相成分与结合性能的影响

为探讨制备参数对直流反应溅射氧化铌涂层晶相成分与结合性能的影响规律,采用不同的氧气流量、功率和沉积时间,通过直流反应溅射技术在AZ31镁合金表面制备了氧化铌涂层。利用X射线衍射仪和X射线光电子能谱仪对涂层进行表征,采用划痕仪测定了涂层的结合力。结果表明：当氧气流量为0.5~3.0 mL/min、功率为60~100 W、沉积时间为3~7 h时,制备参数对氧化铌涂层的晶相结构和化学价态没有影响,但是对涂层的结合性能影响显著。涂层结合力随氧气流量的增大而减小,随溅射功率和沉积时间的增加而先增大后减小。当溅射功率为80 W（W3试样）和沉积时间为300 min（T3试样）时,涂层的结合力分别为最大。     

AZ31和Ti6Al4V表面Nb2O5涂层的微观结构与性能研究

采用射频溅射技术在AZ31镁合金和Ti6Al4V钛合金表面分别沉积Nb2O5陶瓷涂层,对比研究其微观结构、残余应力、附着力和耐腐蚀性能。研究结果表明：两种涂层试样表面组织致密,颗粒大小均匀,无明显的裂纹和孔洞等缺陷。当Nb2O5涂层的厚度为1.98 μm时,Ti6Al4V涂层试样的残余应力（27.1 MPa）比AZ31涂层试样的小65.1%,附着力（9.24 N）比AZ31涂层试样的大13.2倍。Nb2O5陶瓷涂层能明显提高Ti6Al4V和AZ31的耐腐蚀性能,但在腐蚀电流密度的降低幅度、极化电阻的增大程度和保护效率方面,镁合金涂层试样优于钛合金涂层试样。     

电化学沉积法制备镁基Ca-P生物陶瓷涂层的研究

利用电化学沉积法在AZ31镁合金表面制备了Ca-P基生物涂层,使用扫描电子显微镜观察了经不同沉积时间处理后的涂层形貌,采用X射线衍射和能谱分析了涂层的结构和成分,通过电化学测试技术研究了在Hank’s仿生溶液中AZ31镁合金及其Ca-P涂层的腐蚀行为。结果表明,镁合金表面在Ca(NO3)2和NH4H2PO4电解液中电化学沉积形成Ca-P涂层由DCPD(CaHPO4·2H2O)片状晶体组成。且涂层形貌随时间发生变化。AZ31镁合金表面的钙磷涂层提高了镁合金的自腐蚀电位,显著地减小了镁合金的腐蚀电流密度。这表明经钙磷涂层处理的AZ31镁合金耐蚀性能得到明显的提高。钙磷涂层的形貌和结晶程度影响AZ31镁合金的耐蚀性。     

溅射工艺参数对氧化铌涂层微观结构与耐蚀性的影响

为揭示溅射工艺参数对氧化铌涂层耐蚀性的影响规律,采用直流反应溅射技术在AZ31镁合金表面制备了不同工艺参数的氧化铌涂层,并通过扫描电镜和电化学工作站对涂层进行微观结构及耐蚀性测试。结果表明：氧气流量对涂层微观结构的影响不显著,但涂层的耐蚀性随氧气流量的增加而降低;当溅射功率由60 W增大到100 W时,涂层表面的致密性变差,甚至出现裂纹,耐蚀性则先增强后减弱;随着沉积时间由180 min增加到420min,涂层的厚度增加、致密性下降,对基底的腐蚀保护效果先增强后减弱。     

新型Mg-Zn-Y-Nd-Zr镁合金表面复合涂层的耐腐蚀性能

为了控制镁材及镁合金在人体中的生物降解速率,采用微弧氧化法、电化学沉积法及微弧氧化+电化学沉积法在新型Mg-Zn-Y-Nd-Zr镁合金表面制备了3种涂层。利用JSM-5610V扫描电子显微镜、TESCANTS5130 SB能谱分析仪、Bruker D8 ADVANCE X射线衍射仪、VS-2005涂层附着力自动划痕仪、RST200F电化学工作站对3种涂层的形貌、成分、结构、厚度、结合力以及电化学性能进行了检测。结果表明:3种涂层均能提高新型Mg-Zn-Y-Nd-Zr镁合金的电化学性能,改善其耐蚀性;微弧氧化+电化学沉积层较单一微弧氧化层及电化学沉积层在致密性、结晶度、厚度、结合力、耐腐蚀性能方面都具有更强的指标。     

退火温度对镁合金表面Nb2O5涂层微观结构与 性能的影响

采用直流反应溅射技术在AZ31镁合金表面制备了Nb2O5涂层,并在不同的温度下对涂层进行退火处理,通过扫描电子显微镜（SEM）、X射线衍射仪（XRD）、划痕仪和电化学工作站对Nb2O5涂层的微观形貌、晶相结构、结合性能和耐腐蚀性能进行测试与表征。研究结果表明,退火温度为100~400 ℃时,Nb2O5涂层的晶相未发生变化,且为非晶结构;而退火温度为500 ℃时,出现了六方晶相。随着退火温度的升高,涂层表面开裂现象加剧,涂层的结合力减小,耐腐蚀性能下降。     

不同磷源制备的镁合金微弧氧化生物陶瓷膜的性能比较

镁合金较差的静蚀性、耐磨性限制了其在生物医学方面的应用。为此,采用微弧氧化技术在AZ31B镁合金表面生成了富含钙、磷的生物陶瓷膜,采用扫描电镜（SEM）、X射线衍射仪（XRD）、X射线荧光光谱仪（XRF）、涂层测厚仪及电化学工作站测试了陶瓷膜的表面形貌、相组成、钙磷原子比、膜厚以及耐蚀性,探讨了电解液中5种磷源对陶瓷膜...     

表面改性后AZ31B镁合金在不同模拟体液中的降解性能研究

采用化学沉积法在AZ31B镁合金表面制备了钙磷陶瓷涂层,通过浸泡试验和电化学试验研究了其在3种不同模拟体液(生理盐水、PBS、Hank′s)中的降解性能。结果表明,沉积处理改变了AZ31B镁合金在模拟体液中的降解性能,明显抑制了其降解速度;浸泡后溶液的pH值变化结果和电化学实验结果均表明,在3种不同模拟体液中,表面处理后AZ31B镁合金显示出不同的降解速度,顺序依次为:生理盐水>PBS溶液>Hank′s溶液。     

AZ31镁合金表面磁控溅射Zr(Al,Ti)-SiN_x复合薄膜及其耐蚀性能

镁合金表面沉积薄膜可以提高其耐蚀性,但现有的几种沉积方法得到的膜疏松、与基体结合力差,影响了其耐腐蚀性能.为此,采用磁控溅射法在AZ31镁合金表面制备了Al,Zr,Ti膜及其与SiN_x的复合薄膜.用扫描电镜、X射线衍射、XPS研究了金属膜及其与SiNi_x复合薄膜的晶体结构、表面形貌和化学成分.结果表明:所制备的SiN_x薄膜为非晶态的富N膜;Zr膜的耐腐蚀性最好,Al膜的保护性最差;Zr-SiN_x复合薄膜比AZ31镁合金的腐蚀电流密度降低了3个数量级,Ti-SiN_x复合薄膜在阳极极化区出现了钝化.SiN_x复合薄膜的耐腐蚀性优于AZ31镁合金和单一金属膜.     

生物医用AZ31B镁合金表面氧化锰转化涂层制备及性能研究

采用转化处理的方式,在AZ31B镁合金表面成功制备一层氧化锰转化涂层,以提高合金表面耐蚀性能。SEM研究表明,氧化锰转化涂层均匀分布在AZ31B镁合金表面,涂层中无规分布着微裂纹,涂层厚度为10~12μm。XRD研究表明,氧化锰转化涂层的主要成分包括MgO、MnO和Mn2O3。电化学和腐蚀浸泡实验结果表明,氧化锰转化涂层能够有效改善AZ31B镁合金的体外耐蚀性能。     

Growth and corrosion of aluminum PVD-coating on AZ31 magnesium alloy

Magnetron sputtering was applied to prepare aluminum coating on a mechanically polished AZ31 magnesium alloy. A loose oxide film was spontaneously formed on the surface of AZ31 magnesium alloy during polishing process. The aluminum coating, which was subsequently deposited on this oxide layer, presented a developed columnar microstructure. Attributed to the barrier effect of Al coating, the Al coated AZ31 showed a higher corrosion resistance than bare AZ31 in corrosion tests. Generally, Al coating is cathodically protected by magnesium alloy substrate. But it is interesting in this study that Al coating still suffered from severe corrosion due to the occurrence of the alkalization effect.     

退火处理对AZ31镁合金表面Ni-Mo-P镀层组织与耐腐蚀性能的影响

为了进一步提高镁合金表面Ni-Mo-P镀层的耐蚀性,采用0M、XRD和浸泡试验等方法,研究了退火处理对AZ31镁合金表面Ni-Mo-P镀层组织与腐蚀性能的影响。结果表明:AZ31镁合金阳极氧化-化学镀Ni-Mo-P镀层表面为“胞状”组织,随着退火温度的升高或退火时间的延长,AZ31镁合金阳极氧化-化学镀Ni-Mo-P镀层的胞状组织逐渐细化,但镀层厚度降低,同时,非晶态Ni-Mo-P镀层组织逐渐向晶态转变,350℃退火1.0h具有较高的非晶化程度,退火处理后的Ni-Mo-P镀层由Mg、MgO、Mg2SiO4、Ni和Ni3P组成;退火使AZ31镁合金阳极氧化-化学镀Ni-Mo-P镀层耐蚀性降低,350℃退火1.0 h镀层具有相对较好的耐蚀性,这与镀层的厚度和非晶化程度有关。     

AZ31镁合金酸性化学镀Ni-Co-P层的耐腐蚀性能

为了提高镁合金的耐蚀性,以酸性化学镀的方法在AZ31镁合金表面制备了Ni-Co-P镀层。分别用XRD,SEM和EDS对镀层的结构、表面形貌和成分进行了分析,并用点滴试验和电化学方法测试了镀层的耐蚀性。结果表明:酸性化学镀Ni-Co-P层为非晶态胞状结构,镀层中P含量可高达9.41%,远高于碱性镀层;AZ31镁合金镀覆Ni-Co-P合金层后腐蚀电流比基体降低3个数量级,其耐蚀性能显著提高。     

Formation by reactive magnetron sputtering of TiN coating on Ti-implanted magnesium alloy

Reactive magnetron sputtering method was used to deposit TiN coating on Ti-implanted magnesium alloy. FESEM, GIXRD and AES were used to investigate this surface system's micro-morphology, crystalline structure and chemical composition, respectively. It showed that TiN coating took on a compact surface morphology and existed as a columnar crystalline structure. The results of the electrochemical test and immersion test showed that the corrosion resistance of AZ31 was greatly improved in 3.5 wt.% NaCl solution by this kind of surface treatment technique. It was mainly due to the combined effect of the dense TiN coating, the Ti-implanted layer and the good adhesion between coating and substrate.     

Fabrication of Al and Al/Ti coatings on magnesium alloy by sputtering

Multi-magnetron sputtering was applied to prepare aluminum coating and aluminum/titanium multilayer coating on AZ31 magnesium alloy. FESEM, AFM and XRD were used to investigate the morphology and phase structure of these obtained coatings. Aluminum coating presented a (111) preferred texture and this texture was strongly strengthened with the Ti(002) plane as template in Al/Ti multilayer coating. The top surface of Al/Ti-coated sample took on a round roof-like morphology compared to the pyramid-like morphology of Al-coated sample. The result of polarization tests showed that both Al coating and Al/Ti multilayer coating could improve the corrosion resistance of AZ31 magnesium alloy in 3.5 wt.% NaCl solution.     

The effect of PVD coatings on the corrosion behaviour of AZ91 magnesium alloy

In this study, multilayered AlN (AlN + AlN + AlN) and AlN + TiN were coated on AZ91 magnesium alloy using physical vapour deposition (PVD) technique of DC magnetron sputtering, and the influence of the coatings on the corrosion behaviour of the AZ91 alloy was examined. A PVD system for coating processes, a potentiostat for electrochemical corrosion tests, X-ray difractometer for compositional analysis of the coatings, and scanning electron microscopy for surface examinations were used. It was determined that PVD coatings deposited on AZ91 magnesium alloy increased the corrosion resistance of the alloy, and AlN + AlN + AlN coating increased the corrosion resistance much more than AlN + TiN coating. However, it was observed that, in the coating layers, small structural defects e.g., pores, pinholes, cracks that could arise from the coating process or substrate and get the ability of protection from corrosion worsened were present.     

Fluoride Conversion Coating on Biodegradable AZ31B Magnesium Alloy

A fluoride conversion coating was successfully prepared on AZ31B magnesium alloy by chemical reaction in hydrofluoric acid. Morphologies, composition, bonding strength, corrosion properties, in vitro cytotoxicity and antibacterial properties of the coating were investigated, respectively. The scanning electron microscopy observations revealed a dense coating with some irregular pores. The thin-film X-ray diffraction analysis indicated that the coating was mainly composed of MgO and MgF2. The electrochemical impedance spectroscopy results showed that the fluoride conversion coating significantly improved the corrosion resistance of AZ31B. The hydroxyapatite formed on the surface of the fluoride coated AZ31 B after being immersed in the simulated blood plasma indicated the good bioactivity of the material. The in vitro cytotoxicity test showed that the fluoride coated AZ31B alloy was not toxic to BMMSCs （human bone marrow-derived mesenchymal stem cells）. It was also found that the fluoride coated AZ31 B alloy had antibacterial capability.     

AZ31镁合金无铬阳极氧化新工艺

为了提高镁合金的耐腐蚀性能,采用直流阳极氧化工艺研究了一种新型无Cr环保型镁合金阳极氧化配方及工艺.溶液主要成分包含NaOH、Na3PO4、KF、铝盐和适量添加剂.结果表明,氧化膜主要由MgO和MgAl2O4组成;该环保型阳极氧化新工艺所获得的膜层的耐腐蚀性能等级为9级,优于传统的HAE工艺(8级),对AZ31镁合金能提供更有效的保护.