热处理后TiO2纳米管涂层的生物活性

采用阳极氧化法在钛种植体表面制备了TiO2纳米管涂层。考察了450℃热处理对TiO2纳米管涂层相结构及在模拟体液中抗腐蚀能力的影响,并探讨了成骨细胞在TiO2纳米管涂层表面的生长行为。结果表明,热处理后TiO2纳米管涂层的抗腐蚀能力及生物活性都有了明显的提高。     

悬浮液粉体含量对电泳沉积羟基磷灰石涂层的影响

从不同羟基磷灰石(hydroxyapatite,HA)粉体含量的悬浮液中,在钛表面电泳沉积HA涂层.采用扫描电镜、X射线衍射表征涂层的微观形貌及物相组成,通过黏结-拉伸实验测定涂层与基底的结合强度.结果表明:提高悬浮液的HA粉体含量,有助于提高电泳沉积HA涂层的致密性,改善其烧结性能,提高烧结致密化程度;HA涂层致密性的提高,有效地抑制了钛基底表面氧化反应,改善了涂层与基底的界面结合状态,使HA涂层与钛基底的结合强度从悬浮液HA粉体含量为5g/L时的4.54MPa,提高到悬浮液HA粉体含量为20g/L时的19.92MPa.     

微弧氧化和电泳沉积复合制备羟基磷灰石/TiO2复合涂层及其生物学特性

采用微弧氧化和电泳沉积复合的方法,在钛样品表面沉积了羟基磷灰石(hydroxyapatite,HA)/TiO2复合涂层.用扫描电子显微镜,能量散射X射线能谱分析和X射线衍射对复合涂层的表面形貌、形成过程、元素组成及含量变化、相组成进行了观察和分析.通过剪切粘结实验确定了复合涂层与基体的结合强度,并在高温消毒后,将成骨样细胞MC-3T3-E1接种于试件表面进行培养以评估HA/TiO2复合涂层的生物学性能.结果表明形成的复合涂层由内层致密的TiO2层、中间HA/TiO2混合过渡层和外层HA层构成,其中HA含量呈梯度变化,使TiO2层逐渐向HA层过渡.HA/TiO2复合涂层和基体间的结合强度约为(19.3±2.5)MPa.通过细胞免疫荧光染色观察到细胞在培养3 h就可附着于复合涂层表面并形成良好的铺展,而且随着培养时间的延长,细胞的形态更加舒展,附着在复合涂层表面的细胞数量亦逐渐增加,初步表明复合涂层具有较好的生物学和力学性能.     

复合电沉积制备HA/Ag生物陶瓷涂层

在电沉积羟基磷灰石(hydroxyapatite，HA)涂层的电解液中加入Ag粉，通过复合电沉积技术制备HA／Ag复合涂层，比较了不同工艺条件对涂层中Ag含量的影响，以及银对复合涂层结合强度、涂层组成和结构的影响。实验结果表明：复合涂层中Ag的含量随主盐浓度的减小、电流密度的减小和沉积时间的延长而增大。HA／Ag复合涂层经750℃烧结2h后的结合强度明显高于HA涂层，且随Ag含量的增加而提高，可达12．4MPa。当烧结温度高于750℃时，Ag起催化剂作用，促进HA发生了分解。     

羟基磷灰石/TiO_2复合涂层在模拟脑脊液中生物相容性(英文)

应用阳极氧化法在Ti-6Al-4V钛合金(TC4)表面制备了多孔TiO2涂层,在TiO2涂层表面电沉积制备了羟基磷灰石(hydroxyapatite,HA)/TiO2复合涂层,用实验用人工脑脊液(artificial cerebrospinal fluid,ACSF)体液模拟人体的脑脊液,以TC4和TiO2涂层为对比,研究了HA/TiO2涂层在浸泡过程中发生的物理化学变化,考察了HA/TiO2复合涂层抑制钛合金中元素Al和V的析出情况。结果表明:3种样品随浸泡时间的延长遵循的生长规律为:HA成核→HA晶粒长大→HA晶粒相互团簇形成一体→涂层逐渐扩大覆盖到整个基体表面;TC4,TiO2以及HA/TiO2涂层在ACSF中都能够诱导HA的生成,表现出了良好的生物活性。检测浸泡后溶液中Al和V的浓度可知,阳极氧化法制备的TiO2涂层对于Al,V元素的析出起到了一定的抑制作用,能够进一步提高钛合金的生物相容性。     

在非水溶液体系中电泳沉积Ti6Al4V/BG/HA梯度涂层

本工作的目的是探索制备钛合金表面生物活性梯度涂层的新方法 ,提高涂层的结合强度及稳定性 .通过诱导羟基磷灰石 (HA)在生物玻璃 (BG)颗粒表面的结晶 ,改变了生物玻璃表面的带电特性 ;采用电泳沉积 (EPD)法 ,在非水溶液体系中实现了BG和HA在阴极Ti6Al4V基体上的共沉积 ,经烧结获得了生物活性梯度陶瓷涂层 ,得到了一种制备生物活性梯度陶瓷涂层的新工艺 .用XRD对涂层的相组成进行了定性分析 ,结果表明涂层由HA ,榍石和玻璃组成 ;采用粘结拉伸法测定的涂层与基体结合强度大于 18MPa,用SEM观察涂层表面及断面的形貌 ,可见涂层表面较为平整 ,没有明显的裂纹 ;涂层与基体结合紧密 ,且存在一明显的界面梯度区域 .     

在非水溶液体系中电泳沉积Ti6Al4V/BG/IIA梯度涂层

本工作的目的是探索制备钛合金表面生物活性梯度涂层的新方法,提高涂层的结构强度及稳定性,通过诱导羟基磷灰石（HA）在生物玻璃（BG）颗粒表面的结晶,改变了生物玻璃表面的带电特性;采用电泳沉积（EPD）法,大非水溶液体系中实现了BG和HA在阴极Ti6Al4V基体上的共沉积,经烧结获得了生物活性梯度陶瓷涂层,得到了一种制备生物活性梯度陶瓷涂层的新工艺,用XRD对涂层的相组成进行了定性分析,结果表明涂层由HA,榍石和玻璃组成;采用粘结拉伸法测定的涂层与基体结合强度大于18MPa,用SEM观察涂层表面及断面的形貌,可见涂层表面较为平整,没有明显的裂纹;涂层与基体结合紧密,且存在一明显的界面梯度区域。     

改进酸碱联合处理法制备钛基羟基磷灰石活性涂层(英文)

为了制备理想的钛基羟基磷灰石(hydroxyapatite,HA)生物活性涂层,对钛合金表面分别采用酸处理、碱处理和酸碱联合处理,经过预钙化和热处理后,于模拟体液中进行HA沉积试验.采用X射线粉末衍射仪分析HA涂层的化学组成,以扫描电镜观察所得涂层的表面形态.结果表明:酸碱联合处理法是理想的钛合金表面处理法,所得表面呈多孔状,表面粗糙,对HA涂层沉积和结合强度的改善极为有利;模拟体液法所得涂层主要由HA组成,沉积物为云团状或球状;与相关文献比较,涂层HA含量高,没有裂纹,并且在钛基金属表面形成了片状晶体,均匀覆盖于金属表面,球状颗粒间有空隙存在,有利于新骨形成和牢固的结合.     

水热电沉积法制备羟基磷灰石/氧化钛复合涂层的研究

采用水热电沉积法．在钛金属基体￡：成功制备了羟基磷灰石(hydroxyapatite,HA)氧化钛(HA／TiO2)复合涂层．对涂层的表面形貌、相组成、TiO2共沉积量、热稳定性和结合强度进iir研究。实验结果表明：复合涂层具有较均匀的微观结构。TiO2的加入明显改善了涂层与基体的结合强度．涂层中TiO2含量越高．结合强度的提高也越显著。在200℃．100g／L TiO2条件下．电沉积制备的HA／TiO2复合涂层的结合强度为21.0MPa,约为纯HA涂层的2倍。TiO2共沉积量随电解液中TiO2浓度的提高逐渐增加;随电解液温度的提高先增后降,在160C达到最大。涂层经800℃热处理后,TiO2促使HA部分分解为β-磷酸钙(β-tricalciumphosphate,β-TCP)和CaO;经1200℃热处理后,HA和TiO2发生相互作用生成α-TCP和CaTiO3。     

电泳沉积和反应结合制备羟基磷灰石/氧化铝复合涂层

在金属表面用电泳沉积(electrophoretic deposition, EPD)法制备羟基磷灰石(hydroxyapatite, HA)涂层的主要问题是结合强度较低.为了提高HA涂层与基体的结合强度,先采用EPD在钛表面制得羟基磷灰石/铝(hydroxyapatite/aluminum, HA/Al)复合涂层,然后采用反应结合方法(reaction bonding process)制备羟基磷灰石/氧化铝(hydroxyapatite/aluminum oxide, HA/Al2O3)复合涂层,并与相同条件下制备的HA单一涂层进行比较研究.用扫描电镜表征涂层的表面和横截面形貌.用能量散射X射线衍射(X-ray diffraction, XRD)谱分析HA/Al2O3复合涂层的化学组成.用XRD仪研究涂层的物相组成和热稳定性.通过黏结-拉伸实验测定HA涂层与基体的结合强度.结果表明:通过850℃热处理,HA/Al复合涂层中的Al粉发生氧化反应生成Al2O3,经反应结合得到HA/Al2O3复合涂层;反应结合提高了HA涂层的致密化程度且降低了基底钛表面的氧化程度;与单一HA涂层相比,HA/Al2O3复合涂层与基底间的结合强度得到明显提高.     

Improvement in bioactivity and corrosion resistance of Ti by hydroxyapatite deposition using ultrasonic mechanical coating and armoring

In the present work, nanostructured hydroxyapatite (HA)-containing coating was prepared on a Ti surface by ultrasonic mechanical coating and armoring (UMCA). A Ti plate was pre-coated with HA slurry, followed by UMCA, which was achieved by high-frequency ZrO₂ ball bombardment. The UMCA process comprised several cycles of pre-coating and ball bombardment, providing high amounts of HA and good coating adhesion. The coating mainly consisted of nano-HA particles (less than 10 nm) and a small amount of Ti. Furthermore, the deformation structures of the Ti surface region were characterized in a nanocrystalline layer with a grain size of 50–200 nm. Additionally, the coating exhibited improved bioactivity and corrosion resistance in Hanks’ balanced salt solution than the Ti surface. Furthermore, the in vitro cytotoxicity test assessed that the HA-containing coating was non-cytotoxic.     

Preparation and corrosion resistance of a self-sealing hydroxyapatite- MgO coating on magnesium alloy by microarc oxidation

An ideal self-sealing hydroxyapatite (HA)-MgO coating was designed on an AZ31 Mg alloy by one-step microarc oxidation (MAO) with the addition of HA nanoparticles into a base electrolyte. The formation mechanism of the self-sealing HA-MAO coating was discussed. The effect of the nano-HA addition on the corrosion resistance of the MAO coating was evaluated by corrosion tests in Hank's solution. The results show that HA nanoparticles inertly incorporated into the MAO coating during the process of coating growth. HA and MgO were the main constituents of the HA-MAO coating. The HA nanoparticles were absent in the inner barrier layer but concentrated in the outer porous layer. In addition, HA nanoparticles accumulated much more inside coating defects than in the other zones, which resulted in the nearly ideal sealing of micropores on the coating surface. By forming a denser and more stable outer layer, the incorporation of HA nanoparticles greatly enhanced the anti-corrosion properties of the MAO coating.     

Characterization studies on plasma sprayed (AT/HA) bi-layered nano ceramics coating on biomedical commercially pure titanium dental implant

Hydroxyapatite (HA), Al₂O₃–13 wt%TiO₂ (AT) nanoparticles coated on bioactive commercially pure titanium (Cp-Ti) implant were fabricated by plasma spray coating technique. The fabricated monolayer AT, HA film of thickness 75 μm and bilayer (AT/HA) of thickness 150 μm and the coated film surface crystallinity, morphology and phases were investigated in terms of X-ray diffraction, SEM, FT-Raman spectroscopy. In this work, nanostructure AT, HA powders were plasma sprayed on the biomedical Cp-Ti implant surface improve corrosion resistance, and microhardness, surface roughness values compared to uncoated surface. Electrochemical corrosion test was carried out by simulated body fluid (SBF) with ionic concentrations comparable to that of human blood plasma and this result shows that improved corrosion resistance, for the bilayer (AT/HA) coated surface compared to a monolayer AT, HA coated surface. For Al₂O₃ addition with 13 wt%TiO₂ ceramics powder reinforced coating which can act as a barrier for the metal ion released from the implant surface. The in vitro analysis of the bilayer coated implant was good agreement with bone osteoinduction in the biological environment.     

Effect of transition layer on the performance of hydroxyapatite/titanium nitride coating developed on Ti-6Al-4V alloy by magnetron sputtering

A gradient transition multilayer hydroxyapatite/titanium nitride (HA/TiN) coating was prepared on the Ti-6Al-4V alloy by magnetron sputtering. The composition, surface topography, microstructure, adhesion strength and electrochemical properties of the as-deposited coatings were characterized by SEM/EDS, AFM, XRD, FT-IR and electrochemical workstation. The experimental results showed that the single TiN coating deposited at a partial pressure of nitrogen (N₂) of 0.08?Pa had the best internal stress and tribological performance, and its volume loss was only 0.89% of that of Ti-6Al-4V alloy. The introduction of the TiN transition layer greatly improved the wear resistance of the Ti-6Al-4V alloy, and the adhesion strength of the HA layer to the substrate increased from 6.50?±?0.5?N to 11.70?±?1.2?N, an increase of 56%. The HA/TiN coating surface consisted of uniform hemispherical particles with dense structure and invisible defects (micro-cracks and pores). For the HA surface layer, the crystal structure and active hydroxyl (-OH) group was restored after heat treatment. Potentiodynamic polarization experiments indicated that the HA/TiN coating achieved the lowest corrosion current density and the most positive corrosion potential compared to the single TiN layer and Ti-6Al-4V alloy. In summary, it can be conclude that the gradient transition layer can well improve the mechanical properties and electrochemical behavior of the titanium alloy, and largely ensuring the stability of the surface bioactive coating.     

Electrodeposition of hydroxyapatite coating on magnesium for biomedical applications

The effectiveness of hydroxyapatite (HA) coating prepared by electrodeposition technique in improving the corrosion resistance of commercially pure magnesium (CP-Mg) in simulated body fluid (SBF) is addressed. The coating formed in as-deposited condition is identified as dicalcium phosphate dehydrate (DCPD) (Brushite), which is converted to HA after immersion in 1?M NaOH at 80°C for 2?h. The XRD patterns and FTIR spectra confirm the formation of DCPD and HA. During electrodeposition, the H₂PO₄ ^? ion is reduced and the reaction between Ca²⁺ ions and the reduced phosphate ions leads to the formation of DCPD, which is converted to HA following treatment in NaOH. The deposition of HA coating enables a threefold increase in the corrosion resistance of CP-Mg. The ability to offer a significant improvement in corrosion resistance coupled with the bioactive characteristics of the HA coating establish that electrodeposition of HA is a viable approach to engineer the surface of CP-Mg in the development of Mg-based degradable implant materials.     

Anti-corrosive properties of waterborne polyurethane/poly(o-toluidine)-ZnO coatings in NaCl solution

The aim of this research was to prepare waterborne polyurethane (WPU) coating blended with a series of poly(o-toluidine)-nano ZnO composites and study its anti-corrosion performance after its application over carbon steel. The synthesized composites were characterized by X-ray diffractometry (XRD), Fourier transform infrared spectroscopy (FT-IR), X-ray photoelectron spectroscopy (XPS), and scanning electron microscopy (SEM). The corrosion resistance of coatings with and without nano ZnO were studied in 3.5% NaCl solution at a temperature of 25?°C, by electro-chemical techniques such as potentiodynamic polarization measurements and electrochemical impedance spectroscopy (EIS). It was observed that the composite coating containing 7% poly(o-toluidine)-nano ZnO composite had higher corrosion resistance than poly(o-toluidine) and 14% poly(o-toluidine)-nano ZnO composite. The presence of appropriate amount of ZnO significantly improved the corrosion resistance, due to the formation of passive layer on steel surface and the synergistic effects of poly(o-toluidine) along with a suitable amount of nano-ZnO reduced the porosity of the coating surface.     

机械泵旋片基材表面化学镀Ni-P/PTFE复合镀层

在机械泵旋片用45Mn钢板表面制备了化学镀Ni-P/PTFE复合镀层,并研究了PTFE的质量浓度对化学镀Ni-P/PTFE复合镀层的沉积速率、耐磨性、耐蚀性及表面形貌的影响。结果表明:适当增加PTFE的质量浓度,有利于加快沉积速率,提高化学镀Ni-P/PTFE复合镀层的耐磨性和耐蚀性。化学镀Ni-P/PTFE复合镀层表面呈胞状形貌,PTFE均匀分布在表面。当PTFE的质量浓度为8 g/L时,化学镀Ni-P/PTFE复合镀层具有最佳的耐磨性和耐蚀性。     

Characterization and corrosion behavior of plasma sprayed calcium silicate reinforced hydroxyapatite composite coatings for medical implant applications

Titanium and its alloys are widely used for medical implant applications, but their corrosion in the physiological environment leads to the discharge of metal ions, which can trigger severe health issues. In the present study, calcium silicate reinforced hydroxyapatite (HA-CS) coatings were deposited on the Ti6Al4V substrate by using atmospheric plasma spray (APS) process with an aim to improve the corrosion resistance and bioactivity. The coatings were prepared by varying the weight percentage (wt %) of calcium silicate (CS) reinforcement in hydroxyapatite (HA) as Ha/x CS (x = 0, 10, 20 wt %). The SEM analysis of the pure HA coating revealed the presence of surface microcracks, whereas HA-CS coatings displayed the crack-free surface morphology. The corrosion investigation revealed that with the progressive increment of CS content in HA coating, the corrosion resistance of HA-CS coatings improved. In addition, surface roughness, porosity, microhardness and crystallinity increased with the increase of CS content in HA. The findings of this study indicate that the development of plasma sprayed HA-CS coatings is a promising approach to improve the performance of Ti6Al4V alloy for medical implant applications.     

Structure and Properties of ZrO2 Ceramic Coatings on AZ91D Mg Alloy by Plasma Electrolytic Oxidation

ZrO₂ ceramic coatings were prepared in situ on an AZ91D Mg alloy by plasma electrolytic oxidation in a K₂ZrF₆ solution. The phase composition and the surface morphology of the coatings were examined with X-ray diffraction and scanning electron microscopy. The thermal shock resistance of the coatings was evaluated by a thermal shock test. The corrosion resistance of the coated samples was examined by the polarizing curve method in a 3.5% NaCl solution. The prepared coating was composed of t -ZrO₂ and a small amount of c -ZrO₂. There were many residual discharging channels on the coating surface. The coated samples showed excellent thermal shock resistance under 500°C, which improved with increasing frequency or decreasing current density or PEO time. Besides, the coating improved the corrosion resistance of AZ91D Mg alloy considerably. In the experiments, the corrosion current density of the coated samples prepared under 1000 Hz was the least, which also decreased with the current density during the PEO process.     

Influence of a hard transition layer on the microstructure and properties of diamond-like carbon/hydroxyapatite composite coating prepared by magnetron sputtering

The nanostructured diamond-like carbon/hydroxyapatite composite coating (DLC/HA) was deposited using magnetron sputtering technique with a densely packed columnar cross-sectional structure and a uniform granular surface morphology. After heat treatment, the amorphous structure of the coating was transformed into a crystal structure. Nanohardness and scratch tests results demonstrated the DLC transition layer significantly enhanced the nanohardness of Ti6Al4V substrates from 4.8 GPa to 10.4 GPa, and increased critical load from 16.6 N (pure HA layer) to 26.5 N (DLC layer) without obvious brittle fracture, flaking and delamination. Electrochemical and immersion tests results demonstrated that DLC/HA composite coatings with a dense gradient transition interlayer had better corrosion resistance and could prevent harmful metal ions being released into the SBF solution more effectively than single HA coatings. Furthermore, active Ca²⁺ ions can be rapidly released from the coating surface during initial immersion in the SBF solution, and facilitated the formation of bone-like apatite.