预处理对纯钛表面微弧氧化膜物相结构与性能的影响
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摘要
本文采用JEOL JEM-2100型高分辨透射电子显微镜、HITACHI SU-70型热场发射扫描电镜、MicroNano多模式扫描探针显微镜. Rigaku D/max-rc型X射线衍射仪、FTIR-8400型傅立叶变换红外光谱仪. EG&G(Princeton)PAR2273电化学工作站等先进研究手段,试验研究了纯钛试样微弧氧化工艺过程和氧化膜生长规律,分析了纯钛基体微弧氧化的反应机理,建立了微弧氧化膜生长模型和工艺模型；运用“复合制备工艺+工艺条件设计”的研究方法,系统研究了喷砂、酸蚀、“喷砂+酸蚀”(喷蚀)表面处理方法对纯钛试样的预处理,并对预处理后的试样进行了微弧氧化制备加工,深入分析了喷砂、酸蚀、喷蚀纯钛试样及其微弧氧化膜的表面微观结构、物相组成、结合强度、表面力学性能、润湿性、耐蚀性等内容,探讨了不同预处理方式对纯钛牙种植体试样微弧氧化复合制备工艺的影响；用超声、低温方法辅助了复合制备工艺,对比了制备的样品对羟基磷灰石(HA)沉积的引导能力及其动物体内、体外试验结果,得出以下研究结论：
纯钛微弧氧化膜表面的微观形貌、粗糙度、显微硬度、膜重、膜厚、物相结构、元素组成等随着氧化时间不同呈现出相应的改变,当氧化20min时纯钛基体微弧氧化膜即生长完成。纯钛微弧氧化工艺模型分析表明其氧化膜微观结构、物相组成等与工艺参数之间存在必然的联系。其中,微弧氧化工艺时间t是最主要的工艺参数,膜层结构及其他各参数都受工艺时间t的影响,工艺参数t决定了微弧氧化的加工时间。另外,纯钛微弧氧化膜还具有电容效应。
喷砂纯钛基体表面在45s的喷砂时间呈现出一定微观粗糙度与显微硬度的较好组合.HF+HCI混合溶液与基体Ti及其氧化层能够发生酸蚀化学反应,影响了纯钛基体的微观形貌及力学性能,酸蚀纯钛基体表面在90s的酸蚀时间组合了明显的α+β复相组织结构。纯钛基体经过喷砂、酸蚀预处理后复合微弧氧化制备加工时,喷砂纯钛基体微弧氧化膜经过25min生长完成,而酸蚀纯钛基体微弧氧化膜经过15min即可生长完成。不同方式预处理的纯钛基体微弧氧化膜表现出不同的表面微观结构、力学性能、膜层厚度及重量,也表现出不同的物相结构和元素组成,尤其是微弧氧化膜的结合强度、润湿性、耐蚀性等性能不同,说明预处理方式对纯钛试样具有重要的影响。
喷蚀对纯钛试样主要产生了喷砂和腐蚀的综合作用,纯钛基体经过45s时间喷砂及120s的酸蚀预处理,试样表面具有喷砂和酸蚀综合作用效果,并去除了喷砂作用的残留物。从不同环境条件辅助微弧氧化制备喷蚀纯钛试样表面的特征和特性试验结果研究发现,超声条件辅助制备的喷蚀纯钛微弧氧化试样具有较均匀的表面微孔结构、微孔平均尺寸较大、膜层含有较高的磷酸钙Ca3(PO4)2及Ca,P含量,其结合强度与润湿性也较高,因此制备的试样适合牙种植体与骨组织接触部分的处理；而低温辅助微弧氧化制备的喷蚀纯钛试样具有较低的表面微观粗糙度、表面微孔尺寸较小,尤其是其膜层耐蚀性得到大幅提高的同时,结合强度与润湿性无明显降低,因此适合牙种植体与软组织接触部分的处理。
用不同预处理工艺及不同环境辅助条件下微弧氧化制备的纯钛试样,经过模拟体液(SBF)浸泡及仿生矿化后,试样表面出现了不同微观形貌和沉积重量的HA晶体,其中喷蚀纯钛基体微弧氧化膜对HA的引导能力最强。通过对复合工艺制备的纯钛试样表面L929成纤维细胞黏附、伪足形态和增殖,以及对种植体试样在大鼠皮下种植的外观表现和软组织切片研究发现,制备的牙种植体试样生物活性和生物相容性良好。
This paper studies titanium micro-arc oxidation process and growth rules of its oxide coatings, analyzes reaction mechanisms of micro-arc oxidation on titanium matrix and establish the models of coating growth and treatment process using JEOL JEM-2100High Resolution Transmission Electron Microscope (HRTEM), HITACHI SU-70Field Emission Scanning Electron Microscopy (FE-SEM), MicroNano Multi-mode Scanning Probe Microscopy (MSPM), Rigaku D/max-rc X-ray diffraction (XRD), FTIR-8400Fourier Transform Infrared Spectrometer (FTIR), EG&G Princeton PAR2273Electrochemical Workstation and etc. advanced research tools;to discuss the effects of different pretreatments on the complex preparations in micro-arc oxidation, the paper also systematically studies sandblasting, etching, sandblast-etching (blast-etching) surface pretreatments on titanium samples and their micro-arc oxidation coatings through the "Design-of-complex-preparation-optimization-of-process-condition" methods, deeply analyzes the surface microstructures, phase compositions, bonding strength, mechanical properties, wettability and corrosion resistance of the sandblasted, etched, blast-etched titanium specimen surfaces and their micro-arc oxidation coatings as well as the samples prepared by assistant conditions of ultrasound and low temperature, comparing the hydroxyapatite (HA)-inducing ability and the animal in vivo/vitro test. The achieved conclusions include:
The titanium micro-arc oxidation coating surfaces'morphology, microroughness, hardness, weigh, thickness, phase and element composition vary with different oxidation time correspondingly, and the micro-arc oxidation coatings finish growing on pure titanium at20min. The models of titanium micro-arc oxidation process indicate certain links between the microstructures or phase compositions of oxide coatings and the process parameters, in which the treatment time t is the most necessary one, and it determines the intensity of oxidation process, affecting the coatings' microstructures and the other parameters. In addition, titanium micro-arc oxidation coating also exhibits a capacitive effect.
The surface of sandblasted titanium substrate performs a better combination of microroughness and hardness at the blasting intensity of45s. The titanium substrate and its oxide film are etched in the mixed HF-HCI-solution, being influenced on its microstructure and mechanical properties, and the surface of etched titanium substrate shows a distinct combination of α-β-phase structure at the etching intensity of90s. Afer titanium substrates are pretreated with complex preparations, the micro-arc oxidation coating on sandblasted substrate completes in25min, while it on acid-etched substrate completes in15min. The micro-arc oxidation coatings on differently pretreated titanium substrates perform varied surface microstructures, mechanical properties, coating thicknesses and weights as well as varied phase structures and elemental compositions, and especially perform bonding strength, wettability, corrosion resistance or other properties describing that the pretreatments has a significant influence on the titanium samples.
Blast-etching mainly produces a compound function on the titanium samples. When the substrate is sandblasted for45s and etched for120s, its so-prepared surface synthesizes a complex effect of the combined sandblasting and acid-etching, being got rid of the sandblasting residuals. The test results of characterization and properties of the coatings prepared in different assistant conditions show that the micro-arc oxidation coating on blast-etched titanium substrate in ultrasonic assistant condition has a more uniform surface microstructure, bigger micropore size, higher contents of Ca3(PO4)2and Ca, P elements together with a higher wettability and bonding strength, indicating it suitable for the contact with bone tissues; while the micro-arc oxidation coating on blast-etched titanium substrate in low-temperature assistant condition has a smaller surface microroughness and micropore size, improving corrosion resistance without reduced wettability and bonding strength, therefore indicating it suitable for the contact with soft tissues.
When the titanium micro-arc oxidation samples which are prepared by different pretreatments and assistant conditions soak in simulated body fluid (SBF) and are mineralized biomimetically, they deposit varied morphologies and weights of HA layers, in which the blast-etched titanium substrate exhibits the best HA-inducing ability. It is found favourable bioacivities and biocompatibilities that L929fibroblast adhesion, morphology of filopodia and its proliferation on prepared titanium samples, as well as the appearance of their subcutaneous implantation and soft tissue biopsies in rats.
纯钛微弧氧化膜表面的微观形貌、粗糙度、显微硬度、膜重、膜厚、物相结构、元素组成等随着氧化时间不同呈现出相应的改变,当氧化20min时纯钛基体微弧氧化膜即生长完成。纯钛微弧氧化工艺模型分析表明其氧化膜微观结构、物相组成等与工艺参数之间存在必然的联系。其中,微弧氧化工艺时间t是最主要的工艺参数,膜层结构及其他各参数都受工艺时间t的影响,工艺参数t决定了微弧氧化的加工时间。另外,纯钛微弧氧化膜还具有电容效应。
喷砂纯钛基体表面在45s的喷砂时间呈现出一定微观粗糙度与显微硬度的较好组合.HF+HCI混合溶液与基体Ti及其氧化层能够发生酸蚀化学反应,影响了纯钛基体的微观形貌及力学性能,酸蚀纯钛基体表面在90s的酸蚀时间组合了明显的α+β复相组织结构。纯钛基体经过喷砂、酸蚀预处理后复合微弧氧化制备加工时,喷砂纯钛基体微弧氧化膜经过25min生长完成,而酸蚀纯钛基体微弧氧化膜经过15min即可生长完成。不同方式预处理的纯钛基体微弧氧化膜表现出不同的表面微观结构、力学性能、膜层厚度及重量,也表现出不同的物相结构和元素组成,尤其是微弧氧化膜的结合强度、润湿性、耐蚀性等性能不同,说明预处理方式对纯钛试样具有重要的影响。
喷蚀对纯钛试样主要产生了喷砂和腐蚀的综合作用,纯钛基体经过45s时间喷砂及120s的酸蚀预处理,试样表面具有喷砂和酸蚀综合作用效果,并去除了喷砂作用的残留物。从不同环境条件辅助微弧氧化制备喷蚀纯钛试样表面的特征和特性试验结果研究发现,超声条件辅助制备的喷蚀纯钛微弧氧化试样具有较均匀的表面微孔结构、微孔平均尺寸较大、膜层含有较高的磷酸钙Ca3(PO4)2及Ca,P含量,其结合强度与润湿性也较高,因此制备的试样适合牙种植体与骨组织接触部分的处理；而低温辅助微弧氧化制备的喷蚀纯钛试样具有较低的表面微观粗糙度、表面微孔尺寸较小,尤其是其膜层耐蚀性得到大幅提高的同时,结合强度与润湿性无明显降低,因此适合牙种植体与软组织接触部分的处理。
用不同预处理工艺及不同环境辅助条件下微弧氧化制备的纯钛试样,经过模拟体液(SBF)浸泡及仿生矿化后,试样表面出现了不同微观形貌和沉积重量的HA晶体,其中喷蚀纯钛基体微弧氧化膜对HA的引导能力最强。通过对复合工艺制备的纯钛试样表面L929成纤维细胞黏附、伪足形态和增殖,以及对种植体试样在大鼠皮下种植的外观表现和软组织切片研究发现,制备的牙种植体试样生物活性和生物相容性良好。
This paper studies titanium micro-arc oxidation process and growth rules of its oxide coatings, analyzes reaction mechanisms of micro-arc oxidation on titanium matrix and establish the models of coating growth and treatment process using JEOL JEM-2100High Resolution Transmission Electron Microscope (HRTEM), HITACHI SU-70Field Emission Scanning Electron Microscopy (FE-SEM), MicroNano Multi-mode Scanning Probe Microscopy (MSPM), Rigaku D/max-rc X-ray diffraction (XRD), FTIR-8400Fourier Transform Infrared Spectrometer (FTIR), EG&G Princeton PAR2273Electrochemical Workstation and etc. advanced research tools;to discuss the effects of different pretreatments on the complex preparations in micro-arc oxidation, the paper also systematically studies sandblasting, etching, sandblast-etching (blast-etching) surface pretreatments on titanium samples and their micro-arc oxidation coatings through the "Design-of-complex-preparation-optimization-of-process-condition" methods, deeply analyzes the surface microstructures, phase compositions, bonding strength, mechanical properties, wettability and corrosion resistance of the sandblasted, etched, blast-etched titanium specimen surfaces and their micro-arc oxidation coatings as well as the samples prepared by assistant conditions of ultrasound and low temperature, comparing the hydroxyapatite (HA)-inducing ability and the animal in vivo/vitro test. The achieved conclusions include:
The titanium micro-arc oxidation coating surfaces'morphology, microroughness, hardness, weigh, thickness, phase and element composition vary with different oxidation time correspondingly, and the micro-arc oxidation coatings finish growing on pure titanium at20min. The models of titanium micro-arc oxidation process indicate certain links between the microstructures or phase compositions of oxide coatings and the process parameters, in which the treatment time t is the most necessary one, and it determines the intensity of oxidation process, affecting the coatings' microstructures and the other parameters. In addition, titanium micro-arc oxidation coating also exhibits a capacitive effect.
The surface of sandblasted titanium substrate performs a better combination of microroughness and hardness at the blasting intensity of45s. The titanium substrate and its oxide film are etched in the mixed HF-HCI-solution, being influenced on its microstructure and mechanical properties, and the surface of etched titanium substrate shows a distinct combination of α-β-phase structure at the etching intensity of90s. Afer titanium substrates are pretreated with complex preparations, the micro-arc oxidation coating on sandblasted substrate completes in25min, while it on acid-etched substrate completes in15min. The micro-arc oxidation coatings on differently pretreated titanium substrates perform varied surface microstructures, mechanical properties, coating thicknesses and weights as well as varied phase structures and elemental compositions, and especially perform bonding strength, wettability, corrosion resistance or other properties describing that the pretreatments has a significant influence on the titanium samples.
Blast-etching mainly produces a compound function on the titanium samples. When the substrate is sandblasted for45s and etched for120s, its so-prepared surface synthesizes a complex effect of the combined sandblasting and acid-etching, being got rid of the sandblasting residuals. The test results of characterization and properties of the coatings prepared in different assistant conditions show that the micro-arc oxidation coating on blast-etched titanium substrate in ultrasonic assistant condition has a more uniform surface microstructure, bigger micropore size, higher contents of Ca3(PO4)2and Ca, P elements together with a higher wettability and bonding strength, indicating it suitable for the contact with bone tissues; while the micro-arc oxidation coating on blast-etched titanium substrate in low-temperature assistant condition has a smaller surface microroughness and micropore size, improving corrosion resistance without reduced wettability and bonding strength, therefore indicating it suitable for the contact with soft tissues.
When the titanium micro-arc oxidation samples which are prepared by different pretreatments and assistant conditions soak in simulated body fluid (SBF) and are mineralized biomimetically, they deposit varied morphologies and weights of HA layers, in which the blast-etched titanium substrate exhibits the best HA-inducing ability. It is found favourable bioacivities and biocompatibilities that L929fibroblast adhesion, morphology of filopodia and its proliferation on prepared titanium samples, as well as the appearance of their subcutaneous implantation and soft tissue biopsies in rats.
引文
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