人工股骨头表面硅碳氮薄膜生长特性及其摩擦学性能研究
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摘要
人工关节置换可以达到矫正畸形，重塑关节功能，使原来病损即结构失效的关节能够恢复正常的目的。无菌松动是限制人工关节在体内服役寿命和安全使用的主要障碍，关节失效后患者二次手术的代价不是仅仅可以用金钱来衡量的，更是给患者带来巨大的痛苦。目前在临床应用中人工关节股骨头的使用仍是以金属材质为主，通过物理或化学的手段对金属股骨头进行各种改性，提高其表面硬度和耐磨损性能是解决人工关节无菌松动与远期失效的有效手段之一。
针对关节置换术后，由磨屑引起的无菌松动和骨吸收导致的人工关节失效问题，利用表面工程理论，在人工股骨头表面设计被覆一层超薄硅碳氮薄膜，控制和降低人工股骨头及对偶缓冲材料的磨损；硅碳氮薄膜质硬耐磨且具有自润滑性能，化学性能稳定，可以改善股骨头的抗腐蚀性能，从源头上降低或消除磨屑和腐蚀的发生，能够到达延长人工关节使用寿命的目的。
本研究利用红外光谱（FT–IR）、X–Ray光电子能谱（XPS）、摩擦磨损试验机、纳米压痕等技术和其它现代分析测试手段对硅碳氮硬质薄膜的表面形貌、元素组成和薄膜厚度、粗糙度和表面能态以及机械性能等一系列材料学特征进行检测和分析。研究表明，硅碳氮薄膜被覆的人工关节配伍摩擦系数低至0.017，摩擦学评价过后硅碳氮薄膜表面没有对偶材料的粘附，表明能有效地改善了人工股骨头材料的摩擦学性能，是一类有潜质的人工股骨头保护膜层。
在人工股骨头表面被覆化学性能稳定的硅碳氮薄膜，研究薄膜对其表面能态、力学性能、摩擦学性能的影响。硅碳氮的双性表面能态特性，使人工关节股骨头对植入环境胎牛血清稀释液有良好的浸润性，且具有清洁作用，推测这有利于关节的转动灵活性；薄膜硬度在16Gpa左右，弹性模量约为180GPa，能够有效抵抗外力的刻划摩擦，且力学性能与对偶材料匹配，加之良好的润滑，降低了UHMWPE的磨损。
氮气流量和离子轰击能量显著的调整了硅氮薄膜的化学结合状态，氮气流量的提高显著地加强了薄膜中Si-N键的含量；调整沉积过程中的基体负偏压，适当的轰击偏压可以促进薄膜生长，改善薄膜性能。其中，硅含量随偏压变化明显，随着基体偏压的增大（–50V~–200V），薄膜中的硅含量最大达到40.5%；离子轰击能量的变化显著影响薄膜的化学组成和结构，高能粒子轰击薄膜生长表面，本征态的Si–Si键不断被破坏，薄膜中Si–N键含量随基体偏压的提高而增加，原子排列更加紧密，键长缩小，薄膜的结构更加紧凑致密，显微硬度逐渐提高。薄膜表面光滑平整，膜基结合紧密，硬度均在12GPa以上。薄膜为非晶结构，显微硬度在–200V基体负偏压下达到最大值，通过控制基体负偏压可以调节薄膜的显微硬度和弹性模量，据此调整薄膜生长过程中的氮气分压和离子轰击能量对薄膜的性能进行“裁剪”，以满足不同领域不同材质的应用需求。
在空间等离子体中Si原子/离子产额不变的情况下，真空系统中N和C等离子体活性基团的密度，是影响F:Si–C–N薄膜化学结构、性能的主要因素；CF4本身催化和活化性能以及刻蚀效用并存，CF4的引入有效地调整了非晶硅氮薄膜的生长体系。随着CF4流量的增加，薄膜的氟化程度逐渐加强，薄膜从硅氮为主导的结构逐渐转化为氟化硅碳氮薄膜；随着四氟化碳流量的增加，薄膜的硬度逐渐增加，从11.3GPa迅速提高到16.3GPa，这有助于提高薄膜自身抵抗外力刻划和擦伤的能力，对基体材料的保护作用加强。
薄膜表面由尺寸在20nm左右的突起密密麻麻的排列生长而成，薄膜表面形成了一层极薄的厚度在纳米级别的空气层。液体或者是尺寸上大于该厚度的固体颗粒接触时，液体在自身表面张力的作用下形成球状，只能与薄膜表面的凸起形成点接触，这种独特的结构是薄膜材料在介质环境中具备独特的自清洁功能。
本文所研制的硅碳氮薄膜是在亲疏水环境均能良好润湿的双性特性功能薄膜，不同离子轰击能量下沉积的非晶硅氮薄膜，是一种高色散的薄膜，在表面能的色散分量和极性分量中，色散分量占很大的比例；随着四氟化碳流量的增加，薄膜表面能的极性分量逐渐超过色散分量，极性分量与色散分量的比值迅速上升到1.5。硅碳氮薄膜的具有亲疏水双性特征的功能材料，在FBS中表面得到良好的浸润，其润滑特性是一种流体力学润滑；摩擦化学反应产物溶于水，并吸附在摩擦副的界面，形成超平坦接触膜，起到良好的润滑效果；氮气分压和氟碳掺杂过程，显著的调整了薄膜化学结合状态，薄膜中的化学键组成不断变化，硅碳氮薄膜的表面能态也随之改变，表面能的极性分量和色散分量比值在0.55–0.77之间时，薄膜表面能够显著抑制血小板的粘附激活反应。
Biomedical implants such as artificial heart valves or interventional devices and artificialhip and knee joints have been gaining widespread use with development of medicalengineering. The knee and hip joints are complicatedly loaded parts, implantation materialsbear the comprehensive action of tension–compression, torsion, interface shear andreciprocating fatigue, wear in weight bearing conditions. The implants should withstanddynamical mechanical contact pressures and avoid formation of debris over a desiredlong–term biological interaction with the surrounding biological tissue. With time, mechanicalwear and stress, corrosion and tissue reactions lead either to a mechanical failure or to asepticloosening of the implant, the lifetime of the artificial joint implant is limited. The highlycorrosive environment and the low tolerance of the body to some dissolution productsstrongly restrict the materials available for implants.
Some of protective functional film materials being considered for joint applications mayprevent or alleviate production of wear debris. Coating for biomedical materials is thephysical deposition of a ceramic and inert surface onto a medical implant device to improveits performance. In this paper, the F:Si–C–N films coating on Co alloy as bio–mechanicalcoating was put forward. The thickness, phase, composition, morphology andbiocompatibility of the coating were characterized by X–ray diffraction (XRD), atomic forcemicroscope (AFM), scanning electron microscopy (SEM) and Platelet adhesion tests. Thechemical bonding configurations and mechanical properties were characterized by means ofX–ray photoelectron spectroscopy (XPS), and nano–indentation technique and CSMpin–on–disk tribometer. Static contact angle measurements were performed by sessile–dropmethod to determine the wettability and surface free energy of the Si–N–O and F:Si–C–Nfilms.
The results are summarized as follow: N2flow rate was the key parameters. On thecondition of keeping other parameter constant, the ratio of N/Si increased with the increasingof the N2flow rate. The Si–N bond gradually became dominant chemical binding state withthe increase of the partial pressure ratio of N2to Ar, the RPN2:PAr=0.3is a critical value to obtain high content of the Si–N bond and high hardness/elastic modulus. With the increase ofsputtering power, the films became smoother and with finer particle growth. The hardnessvaried between6GPa and11.23GPa depending on deposition condition (RPN2:PAr). Duringthe process of film deposition, the increasing N2flow made the bombardment of Ar+decreasewhile the silicon target was poisoned, causing the film to have insufficient density. Asystematic study on the preparation and properties of fluorinated silicon–nitride (Si–N) filmsunder varying different substrate bias voltage was carried out on the matrix of Co–Cr–Moalloy by direct current unbalanced magnetron sputtering techniques. It was found that thedeposition rate decreased linearly when the substrate bias voltage increased. When the biasvoltage exceeded to150V, the deposition rate increased again. It was easily detached by ionbombardment for Si–Si bond during high bias voltage that is less stable than Si–C bond. Theoptimum conditions were observed at substrate negative bias voltage of100–150V. The filmsshowed high hardness and elastic modulus at100V, while the state of samples betweensputtering and the control for Si, C, and N plasma reached to equilibrium at150V to growslow and dense.
Significant role of fluorine and carbon–doped on growth characteristics and mechanicalproperties in the film was observed. It was found that CF4flows has a little effect on thecoefficient friction of the films, but large variations took place these films’ deposition rate,composition, microstructure and mechanical properties when CF4flows varied from0to9sccm. At9sccm CF4gas flow, the F:Si–C–N coatings demonstrated a fluorine content of5.95at.%and a maximum nano–hardness of15.3GPa, and a moderate friction coefficient of0.03. It is obvious from the hardness results that the F:Si–C–N coating enhances the hardnessof the Co–Cr–Mo alloy to approximately one time on a smoother surface.
Behaviors of silicon nitride films and their relation to blood compatibility andbiomechanical properties have been interesting subjects to researchers. The results of theplatelet adhesion tests shown here have significant difference for the behavior of plateletadhesion between the silicon nitride films with various the ratio of polar component anddispersion component deposited on different N2and CF4flows. Si–N–O coating can be agreat candidate for developing antithrombogenic surfaces in blood contacting materials. Thechemical bonding state made an adjustment in microstructured surfaces, once in the totally wettable configuration, may improve the initial contact between platelet and biomedicalmaterial, due to the appropriate the ratio of and.
The tribological characterisation of Co–Cr–Mo alloy with Si–(C)–N coating slidingagainst UHMWPE counter–surface in fetal bovine serum, shows that the wear resistance ofthe Si–(C)–N coated Co–Cr–Mo alloy/UHMWPE sliding pair show much obviouslyimprovement over that of uncoated Co–Cr–Mo alloy/UHMWPE sliding pair. The F:Si–C–Nand Si–N films have potential properties for joint surface modification applications.
针对关节置换术后，由磨屑引起的无菌松动和骨吸收导致的人工关节失效问题，利用表面工程理论，在人工股骨头表面设计被覆一层超薄硅碳氮薄膜，控制和降低人工股骨头及对偶缓冲材料的磨损；硅碳氮薄膜质硬耐磨且具有自润滑性能，化学性能稳定，可以改善股骨头的抗腐蚀性能，从源头上降低或消除磨屑和腐蚀的发生，能够到达延长人工关节使用寿命的目的。
本研究利用红外光谱（FT–IR）、X–Ray光电子能谱（XPS）、摩擦磨损试验机、纳米压痕等技术和其它现代分析测试手段对硅碳氮硬质薄膜的表面形貌、元素组成和薄膜厚度、粗糙度和表面能态以及机械性能等一系列材料学特征进行检测和分析。研究表明，硅碳氮薄膜被覆的人工关节配伍摩擦系数低至0.017，摩擦学评价过后硅碳氮薄膜表面没有对偶材料的粘附，表明能有效地改善了人工股骨头材料的摩擦学性能，是一类有潜质的人工股骨头保护膜层。
在人工股骨头表面被覆化学性能稳定的硅碳氮薄膜，研究薄膜对其表面能态、力学性能、摩擦学性能的影响。硅碳氮的双性表面能态特性，使人工关节股骨头对植入环境胎牛血清稀释液有良好的浸润性，且具有清洁作用，推测这有利于关节的转动灵活性；薄膜硬度在16Gpa左右，弹性模量约为180GPa，能够有效抵抗外力的刻划摩擦，且力学性能与对偶材料匹配，加之良好的润滑，降低了UHMWPE的磨损。
氮气流量和离子轰击能量显著的调整了硅氮薄膜的化学结合状态，氮气流量的提高显著地加强了薄膜中Si-N键的含量；调整沉积过程中的基体负偏压，适当的轰击偏压可以促进薄膜生长，改善薄膜性能。其中，硅含量随偏压变化明显，随着基体偏压的增大（–50V~–200V），薄膜中的硅含量最大达到40.5%；离子轰击能量的变化显著影响薄膜的化学组成和结构，高能粒子轰击薄膜生长表面，本征态的Si–Si键不断被破坏，薄膜中Si–N键含量随基体偏压的提高而增加，原子排列更加紧密，键长缩小，薄膜的结构更加紧凑致密，显微硬度逐渐提高。薄膜表面光滑平整，膜基结合紧密，硬度均在12GPa以上。薄膜为非晶结构，显微硬度在–200V基体负偏压下达到最大值，通过控制基体负偏压可以调节薄膜的显微硬度和弹性模量，据此调整薄膜生长过程中的氮气分压和离子轰击能量对薄膜的性能进行“裁剪”，以满足不同领域不同材质的应用需求。
在空间等离子体中Si原子/离子产额不变的情况下，真空系统中N和C等离子体活性基团的密度，是影响F:Si–C–N薄膜化学结构、性能的主要因素；CF4本身催化和活化性能以及刻蚀效用并存，CF4的引入有效地调整了非晶硅氮薄膜的生长体系。随着CF4流量的增加，薄膜的氟化程度逐渐加强，薄膜从硅氮为主导的结构逐渐转化为氟化硅碳氮薄膜；随着四氟化碳流量的增加，薄膜的硬度逐渐增加，从11.3GPa迅速提高到16.3GPa，这有助于提高薄膜自身抵抗外力刻划和擦伤的能力，对基体材料的保护作用加强。
薄膜表面由尺寸在20nm左右的突起密密麻麻的排列生长而成，薄膜表面形成了一层极薄的厚度在纳米级别的空气层。液体或者是尺寸上大于该厚度的固体颗粒接触时，液体在自身表面张力的作用下形成球状，只能与薄膜表面的凸起形成点接触，这种独特的结构是薄膜材料在介质环境中具备独特的自清洁功能。
本文所研制的硅碳氮薄膜是在亲疏水环境均能良好润湿的双性特性功能薄膜，不同离子轰击能量下沉积的非晶硅氮薄膜，是一种高色散的薄膜，在表面能的色散分量和极性分量中，色散分量占很大的比例；随着四氟化碳流量的增加，薄膜表面能的极性分量逐渐超过色散分量，极性分量与色散分量的比值迅速上升到1.5。硅碳氮薄膜的具有亲疏水双性特征的功能材料，在FBS中表面得到良好的浸润，其润滑特性是一种流体力学润滑；摩擦化学反应产物溶于水，并吸附在摩擦副的界面，形成超平坦接触膜，起到良好的润滑效果；氮气分压和氟碳掺杂过程，显著的调整了薄膜化学结合状态，薄膜中的化学键组成不断变化，硅碳氮薄膜的表面能态也随之改变，表面能的极性分量和色散分量比值在0.55–0.77之间时，薄膜表面能够显著抑制血小板的粘附激活反应。
Biomedical implants such as artificial heart valves or interventional devices and artificialhip and knee joints have been gaining widespread use with development of medicalengineering. The knee and hip joints are complicatedly loaded parts, implantation materialsbear the comprehensive action of tension–compression, torsion, interface shear andreciprocating fatigue, wear in weight bearing conditions. The implants should withstanddynamical mechanical contact pressures and avoid formation of debris over a desiredlong–term biological interaction with the surrounding biological tissue. With time, mechanicalwear and stress, corrosion and tissue reactions lead either to a mechanical failure or to asepticloosening of the implant, the lifetime of the artificial joint implant is limited. The highlycorrosive environment and the low tolerance of the body to some dissolution productsstrongly restrict the materials available for implants.
Some of protective functional film materials being considered for joint applications mayprevent or alleviate production of wear debris. Coating for biomedical materials is thephysical deposition of a ceramic and inert surface onto a medical implant device to improveits performance. In this paper, the F:Si–C–N films coating on Co alloy as bio–mechanicalcoating was put forward. The thickness, phase, composition, morphology andbiocompatibility of the coating were characterized by X–ray diffraction (XRD), atomic forcemicroscope (AFM), scanning electron microscopy (SEM) and Platelet adhesion tests. Thechemical bonding configurations and mechanical properties were characterized by means ofX–ray photoelectron spectroscopy (XPS), and nano–indentation technique and CSMpin–on–disk tribometer. Static contact angle measurements were performed by sessile–dropmethod to determine the wettability and surface free energy of the Si–N–O and F:Si–C–Nfilms.
The results are summarized as follow: N2flow rate was the key parameters. On thecondition of keeping other parameter constant, the ratio of N/Si increased with the increasingof the N2flow rate. The Si–N bond gradually became dominant chemical binding state withthe increase of the partial pressure ratio of N2to Ar, the RPN2:PAr=0.3is a critical value to obtain high content of the Si–N bond and high hardness/elastic modulus. With the increase ofsputtering power, the films became smoother and with finer particle growth. The hardnessvaried between6GPa and11.23GPa depending on deposition condition (RPN2:PAr). Duringthe process of film deposition, the increasing N2flow made the bombardment of Ar+decreasewhile the silicon target was poisoned, causing the film to have insufficient density. Asystematic study on the preparation and properties of fluorinated silicon–nitride (Si–N) filmsunder varying different substrate bias voltage was carried out on the matrix of Co–Cr–Moalloy by direct current unbalanced magnetron sputtering techniques. It was found that thedeposition rate decreased linearly when the substrate bias voltage increased. When the biasvoltage exceeded to150V, the deposition rate increased again. It was easily detached by ionbombardment for Si–Si bond during high bias voltage that is less stable than Si–C bond. Theoptimum conditions were observed at substrate negative bias voltage of100–150V. The filmsshowed high hardness and elastic modulus at100V, while the state of samples betweensputtering and the control for Si, C, and N plasma reached to equilibrium at150V to growslow and dense.
Significant role of fluorine and carbon–doped on growth characteristics and mechanicalproperties in the film was observed. It was found that CF4flows has a little effect on thecoefficient friction of the films, but large variations took place these films’ deposition rate,composition, microstructure and mechanical properties when CF4flows varied from0to9sccm. At9sccm CF4gas flow, the F:Si–C–N coatings demonstrated a fluorine content of5.95at.%and a maximum nano–hardness of15.3GPa, and a moderate friction coefficient of0.03. It is obvious from the hardness results that the F:Si–C–N coating enhances the hardnessof the Co–Cr–Mo alloy to approximately one time on a smoother surface.
Behaviors of silicon nitride films and their relation to blood compatibility andbiomechanical properties have been interesting subjects to researchers. The results of theplatelet adhesion tests shown here have significant difference for the behavior of plateletadhesion between the silicon nitride films with various the ratio of polar component anddispersion component deposited on different N2and CF4flows. Si–N–O coating can be agreat candidate for developing antithrombogenic surfaces in blood contacting materials. Thechemical bonding state made an adjustment in microstructured surfaces, once in the totally wettable configuration, may improve the initial contact between platelet and biomedicalmaterial, due to the appropriate the ratio of and.
The tribological characterisation of Co–Cr–Mo alloy with Si–(C)–N coating slidingagainst UHMWPE counter–surface in fetal bovine serum, shows that the wear resistance ofthe Si–(C)–N coated Co–Cr–Mo alloy/UHMWPE sliding pair show much obviouslyimprovement over that of uncoated Co–Cr–Mo alloy/UHMWPE sliding pair. The F:Si–C–Nand Si–N films have potential properties for joint surface modification applications.
引文
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