齿科常用合金加工及其生物医学性能研究
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摘要
本文采用激光焊接、化学抛光及表面活性化处理等技术加工处理齿科常用CoCr、NiCr及Ti合金。利用XRD、SEM、EDS、AAS等分析手段研究了CoCr、NiCr、NiTi及Ti合金经激光焊接、活性化处理及化学抛光后组织结构、机械性能及耐腐蚀性变化规律,采用体内、体外生物学评价实验和临床应用对齿科常用合金经加工处理后生物相容性及生物活性进行了评价,结果表明:
1.在电压280V,脉冲时间10ms,光斑直径0.6mm焊接参数条件下,激光焊接CoCr-NiCr异种合金时,强度(565.42±60.02 MPa)与延伸率(6.24±0.38%)均可满足义齿正常功能要求。熔焊区显微组织致密、细小,熔焊区与两侧母材呈冶金结合。熔焊区NiCr合金侧发生晶间腐蚀倾向明显,热处理、烤瓷升温有助于降低熔焊区NiCr合金侧晶间腐蚀倾向。CoCr侧组元成分由于原子扩散分布比较均匀,和烤瓷升温相比,热处理后元素分布更加均匀。焊接付耐腐蚀能力较高,电化学腐蚀过程中,CoCr合金对NiCr合金具有阳极保护作用,有助于减少NiCr合金Ni~(2+)离子的释出。体内外实验表明激光焊接齿科CoCr-NiCr合金未见细胞毒性反应,病理组织学反应分级为0级,长期与口腔粘膜组织接触无刺激性,细胞相对增殖度(RGR)93.69%,反应分级为1级,急性全身毒性符合规定。临床应用及随访观察显示CoCr-NiCr合金激光焊接义齿就位顺利,固位良好,焊区未见断裂、开焊、变形及腐蚀变色现象,患者感觉义齿舒适、咀嚼效能高。
2.研制了适合口腔铸钛修复体化学抛光的抛光液,其组成是:体积比为1:1:3的氢氟酸、硝酸和乳酸。化学抛光1min铸钛表面的Ra值为0.092μm,失重率为2.768%,表面氧化膜厚度在5μm左右,使用该抛光液,在一定操作条件下进行化学抛光对钛的机械性能无影响,满足临床应用精度要求。临床应用表明钛修复体化学抛光操作简便、高效,抛光面光泽持久,义齿戴用后无明显变色及变暗现象。
3.利用化学法活性化处理可以在NiTi合金表面仿生生长磷灰石,其成分和结构近似于自然骨中的矿物质,晶粒为纳米尺度。长期(2年)植入兔股骨内种植体与受植骨间为完全性骨结合,较表面未处理组形成了更成熟的骨板层结构与骨改建的结合线,表明NiTi合金经过活性化处理后可以获得良好的生物活性及长期植入安全性。
In this study, the techniques of laser welding, chemical polishing and surface bioactivating treatment were adopted to process the commonly used dental alloys, including CoCr, NiCr, NiTi and pure titanium. The analyzing methods of XRD, SEM, EDS and AAS were used to investigate the microstructure, mechanical properties and corrosion resistance of the samples processed by above technologies. In vivo and in vitro tests, as well as clinical application, were chosen to evaluate biocompatibility and bioactivity of the processed samples. The results are as follows:
1. The suggested laser welding parameters is electric voltage 280 V, pulse time 10 ms, spot diameter 0.6 mm. Under this condition, the tensile strength (565.42±60.02 MPa) and elongation (6.24±0.38%) of laser-welded CoCr-NiCr alloys could meet common requirements of dental prostheses. The microstructures of the fusion zone were dense and fine. Metallurgical bonding between the fusion zone and both of the parent metals was observed. In the side of NiCr alloy close to the fusion zone, the presence of inter-grain corrosion was found. Heat treatment and heating in porcelain processing led to decreasing this tendency. The atoms of element beside the CoCr alloy in the fusion zone diffused evenly, and heat treatment resulted in more even element distribution, rather than heating in porcelain processing. After laser welding, the joint of dissimilar alloys showed good corrosion resistance. During electrochemical corrosion, CoCr alloy acted as anode and protected NiCr alloy from corrosion, which contributed to reducing the release of Ni~(2+) ion from NiCr alloy. Concerning laser welded CoCr-NiCr dissimilar alloys, both the in vivo and in vitro experiments indicated that, there was no cytotoxicity reaction, the pathohistological reaction was grading zero, there were no histomorphologic changes after long-term contact with oral mucosa, the RGR (relative growth rate) was 93.69%, the reaction degree was grade one, and the acute toxicity of whole body was conform to the regulations. Clinical application and follow-up visit observation demonstrated that there were no signs of crack, deformation, corrosion and discoloration in welding zone of laser welded CoCr-NiCr dissimilar alloys, the dental prostheses could be inserted and taken off smoothly. And the dentures were also felt comfortable with the excellent retention and masticatory efficiency.
2. The chemical polishing liquid for dental casting pure titanium was developed, which was consisted of hydrofluoric acid, nitric acid and lactic acid in volume ratio of 1:1:3. After 1min of chemical polishing, the Ra value of titanium casting samples was 0.092μm, the weight-lost rate was 2.768%, and the thickness of the superficial oxidized film was about 5μm. Under adequate condition, the chemical polishing technique merely affected the mechanical properties of the alloys, and the size of the polished samples met the clinical precision requirement of the dental prostheses. Clinical application verified that chemical polishing of dental titanium prostheses was simple and convenient, excellent polishing effect could be achieved, the polished surface maintained a lasting luster after a long-term use, and there was no apparent discoloration or getting darkness.
3. The chemical bioactivating treatment was used to coat the surface of NiTi alloy with biomimetic HA. The composition and structure of NiTi alloy coated with HA were similar to the mineral material within natural bone. The measurement of the crystal grains was at nano level. After long-term (2 years) use of the implant embedded in the thighbone of rabbit, the result showed the complete osseointegration between the implant and the bone. Compared with matched control group without any treatment on the surface, the NiTi alloy coated with biomimetic HA developed more mature bone structures including osseous lamellas and cement line at the bone reconstruction zone, which manifested that good biocompatibility and long term biological safety of NiTi alloy implant could be realized by means of the technique of chemical activating treatment.
1.在电压280V,脉冲时间10ms,光斑直径0.6mm焊接参数条件下,激光焊接CoCr-NiCr异种合金时,强度(565.42±60.02 MPa)与延伸率(6.24±0.38%)均可满足义齿正常功能要求。熔焊区显微组织致密、细小,熔焊区与两侧母材呈冶金结合。熔焊区NiCr合金侧发生晶间腐蚀倾向明显,热处理、烤瓷升温有助于降低熔焊区NiCr合金侧晶间腐蚀倾向。CoCr侧组元成分由于原子扩散分布比较均匀,和烤瓷升温相比,热处理后元素分布更加均匀。焊接付耐腐蚀能力较高,电化学腐蚀过程中,CoCr合金对NiCr合金具有阳极保护作用,有助于减少NiCr合金Ni~(2+)离子的释出。体内外实验表明激光焊接齿科CoCr-NiCr合金未见细胞毒性反应,病理组织学反应分级为0级,长期与口腔粘膜组织接触无刺激性,细胞相对增殖度(RGR)93.69%,反应分级为1级,急性全身毒性符合规定。临床应用及随访观察显示CoCr-NiCr合金激光焊接义齿就位顺利,固位良好,焊区未见断裂、开焊、变形及腐蚀变色现象,患者感觉义齿舒适、咀嚼效能高。
2.研制了适合口腔铸钛修复体化学抛光的抛光液,其组成是:体积比为1:1:3的氢氟酸、硝酸和乳酸。化学抛光1min铸钛表面的Ra值为0.092μm,失重率为2.768%,表面氧化膜厚度在5μm左右,使用该抛光液,在一定操作条件下进行化学抛光对钛的机械性能无影响,满足临床应用精度要求。临床应用表明钛修复体化学抛光操作简便、高效,抛光面光泽持久,义齿戴用后无明显变色及变暗现象。
3.利用化学法活性化处理可以在NiTi合金表面仿生生长磷灰石,其成分和结构近似于自然骨中的矿物质,晶粒为纳米尺度。长期(2年)植入兔股骨内种植体与受植骨间为完全性骨结合,较表面未处理组形成了更成熟的骨板层结构与骨改建的结合线,表明NiTi合金经过活性化处理后可以获得良好的生物活性及长期植入安全性。
In this study, the techniques of laser welding, chemical polishing and surface bioactivating treatment were adopted to process the commonly used dental alloys, including CoCr, NiCr, NiTi and pure titanium. The analyzing methods of XRD, SEM, EDS and AAS were used to investigate the microstructure, mechanical properties and corrosion resistance of the samples processed by above technologies. In vivo and in vitro tests, as well as clinical application, were chosen to evaluate biocompatibility and bioactivity of the processed samples. The results are as follows:
1. The suggested laser welding parameters is electric voltage 280 V, pulse time 10 ms, spot diameter 0.6 mm. Under this condition, the tensile strength (565.42±60.02 MPa) and elongation (6.24±0.38%) of laser-welded CoCr-NiCr alloys could meet common requirements of dental prostheses. The microstructures of the fusion zone were dense and fine. Metallurgical bonding between the fusion zone and both of the parent metals was observed. In the side of NiCr alloy close to the fusion zone, the presence of inter-grain corrosion was found. Heat treatment and heating in porcelain processing led to decreasing this tendency. The atoms of element beside the CoCr alloy in the fusion zone diffused evenly, and heat treatment resulted in more even element distribution, rather than heating in porcelain processing. After laser welding, the joint of dissimilar alloys showed good corrosion resistance. During electrochemical corrosion, CoCr alloy acted as anode and protected NiCr alloy from corrosion, which contributed to reducing the release of Ni~(2+) ion from NiCr alloy. Concerning laser welded CoCr-NiCr dissimilar alloys, both the in vivo and in vitro experiments indicated that, there was no cytotoxicity reaction, the pathohistological reaction was grading zero, there were no histomorphologic changes after long-term contact with oral mucosa, the RGR (relative growth rate) was 93.69%, the reaction degree was grade one, and the acute toxicity of whole body was conform to the regulations. Clinical application and follow-up visit observation demonstrated that there were no signs of crack, deformation, corrosion and discoloration in welding zone of laser welded CoCr-NiCr dissimilar alloys, the dental prostheses could be inserted and taken off smoothly. And the dentures were also felt comfortable with the excellent retention and masticatory efficiency.
2. The chemical polishing liquid for dental casting pure titanium was developed, which was consisted of hydrofluoric acid, nitric acid and lactic acid in volume ratio of 1:1:3. After 1min of chemical polishing, the Ra value of titanium casting samples was 0.092μm, the weight-lost rate was 2.768%, and the thickness of the superficial oxidized film was about 5μm. Under adequate condition, the chemical polishing technique merely affected the mechanical properties of the alloys, and the size of the polished samples met the clinical precision requirement of the dental prostheses. Clinical application verified that chemical polishing of dental titanium prostheses was simple and convenient, excellent polishing effect could be achieved, the polished surface maintained a lasting luster after a long-term use, and there was no apparent discoloration or getting darkness.
3. The chemical bioactivating treatment was used to coat the surface of NiTi alloy with biomimetic HA. The composition and structure of NiTi alloy coated with HA were similar to the mineral material within natural bone. The measurement of the crystal grains was at nano level. After long-term (2 years) use of the implant embedded in the thighbone of rabbit, the result showed the complete osseointegration between the implant and the bone. Compared with matched control group without any treatment on the surface, the NiTi alloy coated with biomimetic HA developed more mature bone structures including osseous lamellas and cement line at the bone reconstruction zone, which manifested that good biocompatibility and long term biological safety of NiTi alloy implant could be realized by means of the technique of chemical activating treatment.
引文
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