抗菌元素对纳米TiO2涂层结构和性能的影响

目的为克服纳米氧化钛在黑暗条件下不具有抗菌效果这一缺点,使用抗菌金属元素Cu、Zn和Ag掺杂以提高其抗菌性能。方法利用大气等离子喷涂技术在钛合金表面制备Cu、Zn和Ag掺杂的TiO_2复合涂层。利用X射线衍射仪(XRD)、拉曼光谱仪(Raman)和场发射扫描电子显微镜(FE-SEM),对涂层的物相组成和表面形貌进行表征。利用接触角测量仪、三位轮廓仪、电化学工作站和电感耦合等离子体原子发射光谱,对涂层的亲水性、表面粗糙度、耐腐蚀性能和抗菌离子释放情况进行表征。利用细菌和涂层共培养实验来评价涂层的抗菌效果。结果抗菌金属元素掺杂没有改变TiO_2涂层的主要相结构,涂层主要由金红石相组成。涂层具有微米级的表面粗糙度,表面由粒径小于50 nm的粒子组成。掺杂使TiO_2涂层的亲水性略有降低。Cu掺杂的涂层的耐腐蚀性能大幅提升,抗菌金属离子在各涂层中都可以释放,且Cu掺杂涂层中的释放量最高。与细菌共培养24 h之后,TiO_2涂层没有显示出抗菌效果,掺杂后涂层表现出优异的抗菌性能。在有水存在的条件下进行紫外光预辐照,可以显著提高TiO_2涂层的抗菌性能,且掺杂后的涂层在经过预辐照后抗菌性能的提升大于TiO_2涂层。结论抗菌金属元素掺杂不改变涂层结构,同时大幅提高了等离子喷涂TiO_2涂层在黑暗条件下的抗菌性能,紫外预辐照处理能够使没有抗菌性能的TiO_2涂层具备抗菌效果,也能进一步提升掺杂涂层的抗菌效果。     

悬浮液等离子喷涂制备FHA/CS复合涂层

目的 采用悬浮液等离子喷涂技术（SPS）在纯钛表面制备氟代羟基磷灰石/硅酸钙（FHA/CS）生物复合涂层。方法 利用X射线衍射仪（XRD）、傅里叶红外光谱仪（FT-IR）、扫描电子显微镜（SEM）及能谱仪（EDS）对复合涂层的物相组成、组织结构和显微形貌进行分析。通过动电位极化测试和体外生物活性测试,分析复合涂层在模拟体液（SBF）中的腐蚀行为和类骨磷灰石形成能力。通过电感耦合等离子体光谱仪（ICP）分析涂层中Ca2+的释放行为,评估复合涂层的化学稳定性。采用划痕法表征涂层的结合强度。结果 SPS制备的复合涂层具有粗糙的表面和层片堆叠结构。涂层中FHA和CS两相分布均匀,结晶性良好。复合涂层临界载荷达到111.43 N,比单一FHA涂层提高62.5%。与纯钛相比,涂层样品具有较高的腐蚀电位（Ecorr）和较低的腐蚀电流密度（Jcorr）。在SBF溶液中浸泡3天,涂层样品表面被类骨磷灰石完全覆盖。ICP结果表明,复合涂层中Ca2+释放速率低于单一CS涂层。结论 通过SPS在纯钛表面制备的FHA/CS复合涂层具有良好的生物活性、耐腐蚀性能和与基体的结合强度,复合涂层中FHA组分的存在有利于提高涂层的化学稳定性。     

镁合金表面等离子喷涂Al2O3-TiO2陶瓷涂层的耐腐蚀性研究

采用等离子喷涂技术在AZ31镁合金表面制备Al2O3-13％TiO2陶瓷复合涂层,对涂层的微观组织进行了观察分析,测试了涂层的表面硬度.通过极化曲线和浸泡腐蚀试验,对比研究了镁合金基材及喷涂陶瓷涂层的试样在5％ NaCl溶液中的耐腐蚀性能.结果表明:涂层镁合金试样的硬度和耐腐蚀性优于基体镁合金,但当腐蚀液透过涂层孔隙时...     

微束等离子喷涂氧化锆增韧羟基磷灰石复合涂层

采用微束等离子喷涂方法,在Ti-6Al-4V基体上制备了羟基磷灰石 氧化锆(70HA-30ZrO2,质量分数,%)复合涂层.将复合涂层置于模拟体液中分别浸泡了3,7,14,28 d并观察表面磷灰石的生长情况以评价涂层生物活性.采用扫描电镜(SEM)和X射线衍射(XRD)分析技术对涂层浸泡前后的表面形貌和相组成进行了研究.结果表明,涂层中ZrO2主要以立方相存在;喷涂过程中羟基磷灰石(HA)出现了一定的分解,产生大量的α-Ca3(PO4)2杂质相.HA涂层熔化效果很好,但涂层中有未熔化的ZrO2颗粒.涂层在模拟体液中浸泡28 d后表面可以形成磷灰石,说明涂层具有很好的生物活性.     

镁合金等离子喷涂Al/Al_2O_3涂层的耐腐蚀性能

采用等离子喷涂技术在AZ31镁合金表面制备Al/Al_2O_3复合涂层,测试了镁合金及表面喷涂有Al/Al_2O_3复合涂层的镁合金试样的极化曲线,研究了没有涂层、经封孔处理和未经封孔处理的喷涂有复合涂层的镁合金三种试样在浸泡腐蚀和5%NaCl盐雾腐蚀情况下的耐腐蚀性能及其腐蚀行为.结果表明,经封孔处理的Al/Al_2O_3复合涂层镁合金试样在上述腐蚀条件下的耐腐蚀性均优于镁合金和涂层未封孔处理的试样,在浸泡试验中未封孔处理的涂层试样比镁合金腐蚀更加严重,在盐雾试验中却优于镁合金.     

活塞杆表面制备CoNiCrAl/Cr_2O_3·SiO_2·TiO_2复合涂层的性能研究

采用超音速火焰喷涂与高焓等离子喷涂相结合的方法,在启闭机活塞杆用45钢表面制备了CoNiCrAl/Cr_2O_3·SiO_2·TiO_2复合涂层。分析了该涂层的微观组织结构、显微硬度、孔隙率、结合强度、抗磨损性能和电化学性能等,并分析了涂层的磨损机理。结果表明:涂层的孔隙率为0.57%,涂层的平均显微硬度达1332.3HV0.2,涂层结合强度均值达到63.7MPa,涂层的抗摩擦磨损性能是基体45钢的84.3倍,CoNiCrAl/Cr_2O_3·SiO_2·TiO_2涂层具有优良的抗磨损性能。CoNiCrAl/Cr_2O_3·SiO_2·TiO_2涂层的抗电化学腐蚀能力强于基体的。利用超音速火焰喷涂与高焓等离子喷涂相结合制备的CoNiCrAl/Cr_2O_3·SiO_2·TiO_2涂层具有优良好的应用前景。     

镍离子掺杂TiO2涂层的制备及亲水性研究

目的 研究不同含量的镍离子掺杂对TiO2纳米涂层亲水性能的影响.方法 采用溶胶-凝胶法制备不同含量Ni2+掺杂TiO2纳米复合溶胶,通过浸渍提拉法在载玻片上成膜,经过热处理后,得到不同含量Ni2+掺杂TiO2复合涂层.通过X射线衍射仪(XRD)、扫描电子显微镜(SEM)、紫外-可见光分光光度计(UV-Vis)、傅里叶变换红外光谱仪(FT-IR)和表面接触角仪,对掺杂不同浓度Ni2+后TiO2的晶型、涂层微观形貌、光吸收性能、结构组成和涂层亲水性等进行表征分析,从而确定最佳Ni2+浓度的复合涂层材料配方.结果 制备的TiO2主要由锐钛矿相和少量金红石相组成,Ni掺杂抑制了锐钛矿相向金红石相的转变.随着Ni含量的增加,TiO2晶粒尺寸逐渐降低.适量掺杂Ni2+制备的TiO2纳米涂层表面形貌光滑,粒子分布致密均匀.掺杂使吸收波长阈值向长波方向偏移,禁带宽度减小,在一定程度上提高了TiO2涂层的亲水性.当Ni2+掺杂质量分数为1.5％时,TiO2涂层亲水性最佳.结论 采用溶胶-凝胶法实现了镍离子掺杂TiO2的改性,掺杂Ni2+后,Ni2+/TiO2复合涂层的亲水性能明显提高.     

Si掺杂对溶液等离子喷涂TiO2涂层结构及光催化性能的影响

目的采用溶液前驱体等离子喷涂制备TiO_2以及Si掺杂TiO_2涂层,并分别研究H2流量和Si掺杂对TiO_2涂层光催化性能的影响。方法通过X射线衍射、扫描电子显微镜、拉曼光谱和傅里叶变换近红外光谱表征样品的晶相、表面形貌以及化学结构,然后以甲基橙为目标物,借此模拟有机污染物,利用光化学反应仪测试TiO_2以及Si掺杂TiO_2涂层的光催化性能。结果适量Si掺杂可以细化晶粒,提升TiO_2涂层中锐钛相含量(从7.4%提高到49%),同时形成Ti—O—Si键,Si掺TiO_2涂层甲基橙的降解率达到95%左右,高于纯TiO_2涂层80%的降解率。随着H2流量增加,TiO_2涂层中的晶粒明显粗化,主要以金红石相的形式存在,H2流量为8 L/min的TiO_2涂层甲基橙降解率达到82%,要远高于H2流量为4、10 L/min的52%和33%。结论 Si掺杂TiO_2涂层比纯TiO_2涂层的光催化性能更优,当H2流量为8 L/min时,光催化性能最好。     

AZ91镁合金表面复合涂层的组织与性能研究

采用火焰喷涂和等离子喷涂相结合的方法,在AZ91镁合金表面制备复合CoCrAlY-Al2O3/TiO2涂层,研究了复合涂层的微观形貌、结合强度、耐磨性能和耐腐蚀性能。结果表明,复合喷涂CoCrAlY-Al2O3/TiO2涂层后,AZ91镁合金的耐磨性和耐腐蚀性能得到明显提高。     

280 简易快速的表面超疏水涂层制备及其性能

目的 低成本简易快速地制备出耐腐蚀超疏水涂层,并研究表面喷砂对超疏水涂层的影响。方法 利用喷砂和抛光这2种表面处理方式和喷涂工艺在5050铝合金板基体表面构建出具有多级结构的超疏水表面。通过润湿性、电化学腐蚀、耐磨性、浸泡耐久性和自清洁测试等试验,分别评价制备样品表面的润湿性、耐海水腐蚀、耐磨性、耐长时间浸泡性能和自清洁性能,并通过扫描电子显微镜和能谱仪对表面形貌和元素成分进行分析。结果 制备的样品表面具有优异的超疏水性能。在30次喷涂次数下,喷砂基底的涂层表面的水滴静态接触角为(153.9±1)°,动态滚动角为(2.99±0.5)°。电化学腐蚀测试结果表明,喷涂氟硅树脂/SiO2涂层可以有效增强铝合金表面的耐腐蚀性能。试验中,样品在25次砂纸摩擦后,抛光基底的涂层表面的接触角为(97±1)°,喷砂基底的涂层表面的接触角为(102.4±1)°。样品在NaCl溶液浸泡10 d后,抛光基底的涂层表面的接触角为(69.4±1)°,喷砂基底的涂层表面的接触角为(113.7±1)°。结论 所制备的喷砂和抛光基体在经过不同次数的喷涂氟硅树脂/SiO2复合涂料后具备超疏水性能,且喷砂基底的涂层表面具有更低的滚动角。涂层修饰的表面在NaCl溶液中的耐腐蚀性能随着喷涂次数的提升而增强。在相同的喷涂条件下,喷砂处理基体能提高超疏水表面的耐腐蚀性、耐磨性和耐久性。     

Effects of plasma treatment on bioactivity of TiO2 coatings

In this work, nano-TiO₂ powders were deposited on titanium alloy substrates by atmospheric plasma spraying, followed by plasma immersion ion implantation (PIII) using hydrogen, oxygen and ammonia gases. The bioactivities of PIII-treated TiO₂ coatings were evaluated by the formation of apatite on their surface after soaked in simulated body fluids (SBF) for a period of time. As-sprayed TiO₂ coating is composed of rutile, anatase and TiO_2−x (most of them is Ti₃O₅). After immersion in SBF for two weeks, the hydrogen PIII-treated TiO₂ coating can induce bone-like apatite formation on its surface but apatite cannot be formed on the surface of as-sprayed and oxygen, ammonia PIII-treated TiO₂ coatings. The results obtained indicated that a hydrogenated surface plays a very important role to induce bioactivity of TiO₂ coatings.     

Characterization of bioactive ceramic coatings prepared on titanium implants by micro-arc oxidation

Micro-arc oxidation （MAO） is an enhanced chemical technology in an electrolyte medium to obtain coating structures on valve-metal surfaces. Titanium oxide films obtained by MAO in the sodium phosphate electrolyte were investigated. The films were composed mainly of TiO2 phases in the form of anatase and mille and enriched with Na and P elements at the surface. Their apafite-inducing ability was evaluated in a simulated body fluid （SBF）. When immersing in SBF for over 30 d, a preferential carbonated-hydroxyapatite was formed on the surfaces of the films, which suggests that the MAO-treated titanium has a promising positive biological response.     

复合活化处理镍钛合金及磷灰石层的仿生沉积

利用H2O2和NaOH溶液对近等原子比NiTi记忆合金（SMA）进行复合活化处理,并采用XRD,SEM,XPS,FTIR等研究了活化处理后NiTi SMA的表面结构及其在模拟体液（SBF）中磷灰石涂层的仿生沉积过程.结果表明：复合活化处理后NiTi SMA表面为贫Ni、富含Ti-OH的蠕虫状活性层,由结晶度较低的TiO2,钛酸纳（Na2TiO3）及少量的Ni2O3组成,在SBF中表面活性层诱导磷灰石形核及生长,短期内在镍钛基体表面获得了理想的磷灰石层.     

纯钛表面微弧氧化TiO2-B4C复合陶瓷膜耐磨耐蚀性研究

采用微弧氧化工艺,并掺杂B4C颗粒来制备耐磨耐蚀性优异的复合陶瓷膜,系统研究掺杂B4C含量对陶瓷膜微观形貌、物相组成、与基体结合力、显微硬度、粗糙度、耐磨性与耐蚀性的影响。结果表明:相比TiO2陶瓷膜,掺杂B4C颗粒的复合陶瓷膜更均匀致密,且由金红石型TiO2、锐钛矿型TiO2和B4C组成。随B4C浓度增大,陶瓷膜的膜层结合力、耐磨性与耐蚀性均先增强后减弱。由于具有最致密的表面形貌,TiO2-0.9B4C复合陶瓷膜的膜层结合力最大,为22.6 N。TiO2-0.9B4C复合陶瓷膜的破损时间最长,磨痕宽度最小,分别为19.24 min和384.53μm,耐磨性最好,其磨损机理为磨粒磨损与疲劳磨损。其自腐蚀电位与极化电阻最大,腐蚀电流密度最小,分别为-213.38 mV、5.47×10^4Ω·cm^2和2.37×10^-6A·.cm^2,耐蚀性最好。由Bode相图可知,陶瓷膜均由致密内层和疏松表层组成。     

Microstructure and in vitro bioactivity of laser-cladded bioceramic coating on titanium alloy in a simulated body fluid

In order to obtain bioactivity on the surface of titanium alloy, the bioceramic coating on Ti–6Al–4V was designed and fabricated by laser cladding. The microstructure and bioactivity of laser-cladded bioceramic coating were investigated in vitro via soaking in a simulated body fluid (SBF). The results indicated that the laser-cladded bioceramic coating was metallurgically bonded to the substrate and contained such bioactive phases as hydroxyapatite (HA) and β-tricalcium phosphate (β-TCP). A bone-like apatite layer was spontaneously formed on the surface of laser-cladded coating merely soaked in SBF for 7 days. And the appearance of flake-like and cotton-like morphology, which is the characteristic morphology of apatite, offered an advantageous condition for osseo-connection. The formation ability of apatite was remarkably accelerated on the surface of laser-cladded bioceramic coating compared with the untreated titanium alloy substrate.     

New generation hopeite coating on Ti6Al4V (TC4) by radio frequency magnetron sputtering for prosthetic-orthopaedic implant applications: synthesis and characterisation

ABSTRACT

Bioceramic coatings with multifunctionality have emerged as an effective alternative to conventional coatings, owing to their combination of various properties that are essential for bio-implants, such as osseointegration and antibacterial character. In the present study, thin hopeite coatings were synthesised by radio frequency magnetron sputtering on TC4 substrates. The obtained hopeite coatings were thermally treated at 500°C in ambient air and characterised in terms of surface morphology, phase composition, surface roughness, adhesion strength, antibacterial efficacy, apatite forming ability, surface wettability and corrosion resistance by Scanning Electron Microscopy (SEM), X-ray diffraction (XRD), Atomic Force Microscopy(AFM), Tensometer, Fluorescence-Activated Cell Sorting (FACS), Simulated Body Fluid (SBF) immersion, Contact Angle Goniometer and potentiostatic polarisation respectively. It was observed that the post-deposition annealing increases the crystallinity of the synthesised hopeite coatings. SEM analysis showed deposited particles are spherical in shape and small in dimensions (<1?μm in diameter). XRD results confirm the deposited coating is crystalline in nature. AFM analysis reveals deposited hopeite coating has an average surface roughness value of 8.66?nm. Tensile pullout experiments indicated that the adhesive strength of the hopeite coating is 21.75?±?2.1?MPa. FACS study confirms the deposited hopeite coating possesses antibacterial character. SBF immersion experiments clearly demonstrate apatite growth on the surface of the deposited hopeite coating. The surface wettability test showed that the deposited coatings are hydrophobic in character having an average contact angle value of 136.65°. Potentiodynamic polarisation experiments in SBF showed a significant improvement in corrosion resistance (R_p?=?7945.87?Ω?cm²) of hopeite coated samples. In summary, it can be concluded that the new generation multifunctional hopeite coating synthesised by an alternative new process route of radio frequency magnetron sputtering on TC4 substrates is an effective alternative to conventional coatings. This is largely attributed to the strong osseointegration and antibacterial character of deposited hopeite coating ensuring the overall stability of metallic orthopaedic implants.     

沉积时间对AZ91D合金表面Ni-P-SiC复合镀层性能的影响

目的提高镁合金的耐蚀性和耐磨性。方法以AZ91D镁合金为基体,采用SiC颗粒质量浓度为3 g/L的Ni-P化学镀溶液,在其表面沉积不同时间,制备Ni-P-SiC复合镀层。通过扫描电子显微镜(SEM)、显微硬度测试、粗糙度仪、电化学腐蚀和磨损等试验来分析和评价Ni-P-SiC复合镀层的厚度、表面粗糙度、显微硬度、耐腐蚀性能和耐磨性能。结果 Ni-P-SiC复合镀层的厚度和表面粗糙度随沉积时间增加而增加,沉积时间为150 min时,镀层厚度可达53μm,表面粗糙度为2.5μm。沉积时间为120 min时,镀层的显微硬度最高,为641HV,此时复合镀层的耐蚀性和耐磨性最好,自腐蚀电位高达-0.73 V,腐蚀电流密度为0.78μA/cm~2,磨损体积最小,为1.04×10~(-3)mm~3。与AZ91D镁合金基体相比,沉积复合镀层后的样品更耐蚀,说明复合镀层有效改善了镁合金基体的耐蚀性。结论沉积时间对Ni-P-SiC复合镀层的性能有一定影响,在沉积时间为120 min时获得的复合镀层具有较好的耐蚀性和耐磨性。