激光快速成形制备钛表面HA涂层及其成骨相关性能研究
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摘要
纯钛等金属材料具有良好的机械性能和生物相容性,但其不具有生物活性,无法与植入区骨组织形成化学结合,其固位只能依靠机械嵌合;以羟基磷灰石为代表的磷酸钙陶瓷具有较好的生物活性,能够与植入区骨组织形成稳定的化学结合,然而其机械性能差,无法承受生理载荷。表面涂层技术可以将二者的优势结合在一起,目前在纯钛等金属表面制备磷酸钙涂层的技术较多,然而均存在结合强度低、物相活性差等问题。激光熔覆技术能够使涂层与基材之间发生冶金结合,提高涂层的结合强度,但是其涂层内部物相的生物活性及稳定性较差。本课题将激光快速成形技术应用于纯钛表面磷酸钙生物活性陶瓷涂层的制备研究,以CaHPO_4·2H_2O和CaCO_3混合粉末为原料,探讨了原料粉末钙磷比、激光功率、扫描速度和热处理条件对涂层生成物相的影响规律;在优化的工艺条件下,在纯钛表面制备出了HA涂层;并对该涂层材料的机械、理化和生物学性能进行了评价,探索出了一种纯钛表面HA涂层制备的新方法,为HA涂层材料的进一步制备研究及应用奠定实验基础。
研究方法:
1.通过分组设计,进行涂层的成形制备,利用X射线衍射和能谱分析技术,分析原料粉末钙磷比值、激光功率、扫描速度和热处理条件对涂层内部物相的影响规律。
2.在优化的条件下制备出纯钛表面HA涂层,利用X射线衍射、能谱分析、扫描电镜等技术及力学实验对其微观组织结构、元素分布、物相组成和机械性能进行表征。
3.采用静态浸泡实验方法,以经表面处理后的纯钛为对照组,对涂层材料在模拟体液中的溶解和沉积行为进行研究。
4.采用成骨细胞与材料共培养技术和动物骨内植入实验,研究涂层材料与成骨相关的生物学性能。
研究结果
1. CaHPO_4·2H_2O和CaCO_3混合原料粉末的钙磷比对激光快速成形技术制备的涂层物相具有显著的影响,其中钙磷比为2.0时可以在纯钛表面生成含HA、α-TCP和TTCP生物活性物相的涂层。
2.在激光的低功率区,即450 w～550 w的范围内,涂层中的HA成分分解较少,同时所含的生物活性物相保持了较高的水平;而激光的扫描速度对涂层生成物相无显著性影响。
3.获得了制备磷酸钙涂层的优化工艺参数,即原料粉末钙磷比为2.0、激光功率450 w、扫描速度200 mm/min、搭接率35 %、送粉速率2.0 g/min、光斑直径3.0 mm;在上述优化参数下,在纯钛表面制备出了含HA、α-TCP和TTCP生物活性物相的涂层;该涂层的微观表面凹凸不平,内部含有微孔,涂层与基材之间形成了冶金结合;从基材到涂层表面存在渗P的基材层(Ti_3P层)、CaTiO_3层和陶瓷层等三层结构;其中,Ti_3P层硬度最高,达到了1263.0±35.3 HV_(0.1),而陶瓷层硬度最低,达到了482.2±20.3HV0.1。
4.随着涂层热处理条件的不同,涂层内部的物相也发生变化,当热处理温度为800℃、保温时间6 h时,涂层内部的物相全部转变为HA;热处理后,涂层与基材之间的结合强度达到了24.50±0.72 MPa。
5. HA/Ti涂层在模拟体液中会释放出一定量的Ca、P离子,但对模拟体液的pH值没有显著影响,同时可以诱导HA颗粒在涂层的表面发生沉积。
6. HA/Ti涂层能够促进成骨细胞的早期黏附、增殖和ALP活性,成骨细胞在涂层表面呈立体、多向性伸展。
7. HA/Ti涂层能够促进植入区的骨再生和骨改建,并能够与再生骨形成紧密的结合。
结论
在优化的工艺条件下,激光快速成形技术结合热处理技术可以在纯钛表面制备出HA涂层,该涂层与基材间形成了良好的结合,并具有较好的生物活性,能够促进成骨细胞的早期黏附和增殖,进而促进了骨组织的早期形成和改建,而且能与再生骨组织形成紧密的骨结合。
Pure titanium and titanium alloys possess excellent mechanical properties and biocompatibility, but no bioactivity. As the implant material, they cannot induce the chemical integration with the host bone tissue, and their fixation only relys on the mechnical interlocking. The Ca-P ceramic possess excellent bioactivity, therefore they can induce the steady chemical integration with the host bone tissue. However, the Ca-P ceramics is not strong to bare the physical load. Coatings technology has the ability to take advantage of both Ti and Ca-P ceramic. Until now, many methods have been applied in preparation of Ca-P coatings on titanium and titanium alloys, but there are some problem need to resolve, such as low bonding strength and poor-bioactive phase. Laser cladding series technology can produce a sound metallurgical bonding between Ca-P coatings and metallic substrate, however the bioactive phase is less and poor stability. In this study, the Laser Rapid Forming (LRF) technology was applied to fabricate the Ca-P coatings on the pure titanium with mixed powder of CaHPO_4·2H_2O and CaCO_3 as raw material. The effect of technological parameter, such as the ratio of Ca to P in raw material, the laser power, the scanning velocity and the heat-treat condition, on the phase composition of coatings were studied. Under the optimized process, the HA coatings on the pure titanium was obtained. The mechanical properties, the physical and chemical properties and the biological properties of the HA coatings were evaluated. At the end, a new method was formed to fabricate the HA coatings on pure titanium and the experimental basis was built for the further research and application of this fabricating methods.
Methods:
1. The coatings were fabricated by the different parameters and the phase compositions of coatings were analyzed by the means of XRD and EDS. The effects of the ratio of Ca to P in raw material, the laser power, the scanning velocity and the heat-treatment condition on the phase composition of the coatings were revealed.
2. Under the optimized parameter, the HA coatings on pure titanium were fabricated and the microstructure, the distribution of elements, the phase composition and the mechanical properties were characterized by the means of XRD, EDS, SEM and mechanical tests.
3. The static immersing test was performed to analyze the behaviors of the HA coatings in simulated body fluid (SBF). At the same time, the pure titanium was tested as control group, which were subjected to sand-blast and acid pickling beforehand.
4. The osteoblasts were cultured on the surface of the HA coatings. The adherence and proliferation of the osteoblasts were investigated using MTT assay and the spreading was observed by the means of SEM. In addition, the titanium coated with the HA by LRF were implanted into the femur of the experimental rabbits. After the healing period of 4, 8 and 12 weeks, the interfaces between the host bone tissue and the surface of implants were observed and evaluated by histomorphometric methods. In the above tests, the surface-treated titanium was tested as control group.
Results:
1. The ratio of Ca to P in the mixed powder of CaHPO_4·2H_2O and CaCO_3 can affect remarkably the phase composition of the coatings fabricated by LRF. When the ratio was 2.0, the phase composition of the fabricated coatings was made up of HA,α-TCP and TTCP, which all possess bioactivity.
2. In the lower range of laser power, from 450 w to 550 w, the less HA in the fabricated coatings was decomposed and the content of bioactive ingredient was high. On the other hand, the effect of the scanning velocity on the phase composition of coating was not remarkable.
3. The optimized parameters were obtained as follow: the ratio of Ca/P was 2.0, the laser power was 450 w, the scanning velocity was 200 mm/min, the overlap rate was 35 %, the speed of powder feeding was 2.0 g/min, and the diameter of laser was 3.0 mm. The coatings fabricated by these parameters contained HA,α-TCP and TTCP. The surface of the coating was uneven and contained many micro pores. The metallurgical bonding between the coatings and the Titanium substrate was clearly observed. From the substrate to the surface of the coatings, there were three layers which were Titanium substrate penetrated by P (Ti_3P), CaTiO_3 layer (transitional layer) and ceramic layer. The hardness in the Ti3P layer was the highest at 1263.0±35.3 HV_(0.1), the hardness in ceramic layer was the lowest at 482.2±20.3HV0.1.
4. Theα-TCP and TTCP in the coatings fabricated by the optimized LRF parameters can be transformed to HA under the condition of heating to 800℃and keeping for 6 h. After heat-treatment, the bonding strength between the coatings and the substrate was 24.50±0.72 MPa.
5. After immersing in SBF, the coatings on the Titanium released some Ca and P ion and induced HA particles to deposit on the coatings surface.
6. The coatings on the pure titanium improved the adherence, the proliferation and the ALP activity of osteoblast at the early stage. The osteoblast spread well on the coatings surface.
7. The titanium implant with the coatings improved the regeneration and the reconstruction of the host bone tissue. At the same time, the coatings combined with the new bone tightly.
Coclusion:
Under the optimized process, LRF combined with heat-treatment, the HA coatings on pure titanium can be obtained. The coatings bond to the substrate well, and possess the excellent bioactivity which can improve the adherence and the proliferation of osteoblast, improve the regeneration and the reconstruction of the host bone tissue and can combine with the new bone tightly.
研究方法:
1.通过分组设计,进行涂层的成形制备,利用X射线衍射和能谱分析技术,分析原料粉末钙磷比值、激光功率、扫描速度和热处理条件对涂层内部物相的影响规律。
2.在优化的条件下制备出纯钛表面HA涂层,利用X射线衍射、能谱分析、扫描电镜等技术及力学实验对其微观组织结构、元素分布、物相组成和机械性能进行表征。
3.采用静态浸泡实验方法,以经表面处理后的纯钛为对照组,对涂层材料在模拟体液中的溶解和沉积行为进行研究。
4.采用成骨细胞与材料共培养技术和动物骨内植入实验,研究涂层材料与成骨相关的生物学性能。
研究结果
1. CaHPO_4·2H_2O和CaCO_3混合原料粉末的钙磷比对激光快速成形技术制备的涂层物相具有显著的影响,其中钙磷比为2.0时可以在纯钛表面生成含HA、α-TCP和TTCP生物活性物相的涂层。
2.在激光的低功率区,即450 w～550 w的范围内,涂层中的HA成分分解较少,同时所含的生物活性物相保持了较高的水平;而激光的扫描速度对涂层生成物相无显著性影响。
3.获得了制备磷酸钙涂层的优化工艺参数,即原料粉末钙磷比为2.0、激光功率450 w、扫描速度200 mm/min、搭接率35 %、送粉速率2.0 g/min、光斑直径3.0 mm;在上述优化参数下,在纯钛表面制备出了含HA、α-TCP和TTCP生物活性物相的涂层;该涂层的微观表面凹凸不平,内部含有微孔,涂层与基材之间形成了冶金结合;从基材到涂层表面存在渗P的基材层(Ti_3P层)、CaTiO_3层和陶瓷层等三层结构;其中,Ti_3P层硬度最高,达到了1263.0±35.3 HV_(0.1),而陶瓷层硬度最低,达到了482.2±20.3HV0.1。
4.随着涂层热处理条件的不同,涂层内部的物相也发生变化,当热处理温度为800℃、保温时间6 h时,涂层内部的物相全部转变为HA;热处理后,涂层与基材之间的结合强度达到了24.50±0.72 MPa。
5. HA/Ti涂层在模拟体液中会释放出一定量的Ca、P离子,但对模拟体液的pH值没有显著影响,同时可以诱导HA颗粒在涂层的表面发生沉积。
6. HA/Ti涂层能够促进成骨细胞的早期黏附、增殖和ALP活性,成骨细胞在涂层表面呈立体、多向性伸展。
7. HA/Ti涂层能够促进植入区的骨再生和骨改建,并能够与再生骨形成紧密的结合。
结论
在优化的工艺条件下,激光快速成形技术结合热处理技术可以在纯钛表面制备出HA涂层,该涂层与基材间形成了良好的结合,并具有较好的生物活性,能够促进成骨细胞的早期黏附和增殖,进而促进了骨组织的早期形成和改建,而且能与再生骨组织形成紧密的骨结合。
Pure titanium and titanium alloys possess excellent mechanical properties and biocompatibility, but no bioactivity. As the implant material, they cannot induce the chemical integration with the host bone tissue, and their fixation only relys on the mechnical interlocking. The Ca-P ceramic possess excellent bioactivity, therefore they can induce the steady chemical integration with the host bone tissue. However, the Ca-P ceramics is not strong to bare the physical load. Coatings technology has the ability to take advantage of both Ti and Ca-P ceramic. Until now, many methods have been applied in preparation of Ca-P coatings on titanium and titanium alloys, but there are some problem need to resolve, such as low bonding strength and poor-bioactive phase. Laser cladding series technology can produce a sound metallurgical bonding between Ca-P coatings and metallic substrate, however the bioactive phase is less and poor stability. In this study, the Laser Rapid Forming (LRF) technology was applied to fabricate the Ca-P coatings on the pure titanium with mixed powder of CaHPO_4·2H_2O and CaCO_3 as raw material. The effect of technological parameter, such as the ratio of Ca to P in raw material, the laser power, the scanning velocity and the heat-treat condition, on the phase composition of coatings were studied. Under the optimized process, the HA coatings on the pure titanium was obtained. The mechanical properties, the physical and chemical properties and the biological properties of the HA coatings were evaluated. At the end, a new method was formed to fabricate the HA coatings on pure titanium and the experimental basis was built for the further research and application of this fabricating methods.
Methods:
1. The coatings were fabricated by the different parameters and the phase compositions of coatings were analyzed by the means of XRD and EDS. The effects of the ratio of Ca to P in raw material, the laser power, the scanning velocity and the heat-treatment condition on the phase composition of the coatings were revealed.
2. Under the optimized parameter, the HA coatings on pure titanium were fabricated and the microstructure, the distribution of elements, the phase composition and the mechanical properties were characterized by the means of XRD, EDS, SEM and mechanical tests.
3. The static immersing test was performed to analyze the behaviors of the HA coatings in simulated body fluid (SBF). At the same time, the pure titanium was tested as control group, which were subjected to sand-blast and acid pickling beforehand.
4. The osteoblasts were cultured on the surface of the HA coatings. The adherence and proliferation of the osteoblasts were investigated using MTT assay and the spreading was observed by the means of SEM. In addition, the titanium coated with the HA by LRF were implanted into the femur of the experimental rabbits. After the healing period of 4, 8 and 12 weeks, the interfaces between the host bone tissue and the surface of implants were observed and evaluated by histomorphometric methods. In the above tests, the surface-treated titanium was tested as control group.
Results:
1. The ratio of Ca to P in the mixed powder of CaHPO_4·2H_2O and CaCO_3 can affect remarkably the phase composition of the coatings fabricated by LRF. When the ratio was 2.0, the phase composition of the fabricated coatings was made up of HA,α-TCP and TTCP, which all possess bioactivity.
2. In the lower range of laser power, from 450 w to 550 w, the less HA in the fabricated coatings was decomposed and the content of bioactive ingredient was high. On the other hand, the effect of the scanning velocity on the phase composition of coating was not remarkable.
3. The optimized parameters were obtained as follow: the ratio of Ca/P was 2.0, the laser power was 450 w, the scanning velocity was 200 mm/min, the overlap rate was 35 %, the speed of powder feeding was 2.0 g/min, and the diameter of laser was 3.0 mm. The coatings fabricated by these parameters contained HA,α-TCP and TTCP. The surface of the coating was uneven and contained many micro pores. The metallurgical bonding between the coatings and the Titanium substrate was clearly observed. From the substrate to the surface of the coatings, there were three layers which were Titanium substrate penetrated by P (Ti_3P), CaTiO_3 layer (transitional layer) and ceramic layer. The hardness in the Ti3P layer was the highest at 1263.0±35.3 HV_(0.1), the hardness in ceramic layer was the lowest at 482.2±20.3HV0.1.
4. Theα-TCP and TTCP in the coatings fabricated by the optimized LRF parameters can be transformed to HA under the condition of heating to 800℃and keeping for 6 h. After heat-treatment, the bonding strength between the coatings and the substrate was 24.50±0.72 MPa.
5. After immersing in SBF, the coatings on the Titanium released some Ca and P ion and induced HA particles to deposit on the coatings surface.
6. The coatings on the pure titanium improved the adherence, the proliferation and the ALP activity of osteoblast at the early stage. The osteoblast spread well on the coatings surface.
7. The titanium implant with the coatings improved the regeneration and the reconstruction of the host bone tissue. At the same time, the coatings combined with the new bone tightly.
Coclusion:
Under the optimized process, LRF combined with heat-treatment, the HA coatings on pure titanium can be obtained. The coatings bond to the substrate well, and possess the excellent bioactivity which can improve the adherence and the proliferation of osteoblast, improve the regeneration and the reconstruction of the host bone tissue and can combine with the new bone tightly.
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