纯钛表面制备复合纳米薄膜对钛瓷结合强度影响的研究
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摘要
近年来，纯钛金属凭借其优良的生物相容性、耐腐蚀性等优点已经被广泛的应用于口腔修复临床。随着低熔点、低热膨胀系数的钛瓷粉成功投放于市场，钛烤瓷技术也有了较大的发展，但是钛瓷结合强度仍明显低于镍铬合金与瓷的结合强度。其原因主要是由于高温环境下，钛表面极易形成疏松多孔且附着性差的氧化膜。纳米材料颗粒粒径小，表面张力大，表面结合能高，具有不饱和性，所以表现出极强的化学活性，易与瓷及金属表面的氧发生键合作用。本实验采用溶胶-凝胶技术，在钛金属表面均匀的涂附一层纳米薄膜，并对其进行相应的热处理，以期能限制在瓷烧结过程中钛表面的过度氧化，改善钛瓷结合性能，提高钛瓷结合强度；并模拟口腔环境，研究钛瓷结合强度在酸性含F-的人工唾液中的变化规律，探讨其腐蚀机理，为钛瓷修复体进一步的临床应用提供理论依据。
研究结果如下：
1．采用溶胶-凝胶技术均匀的在钛金属表面涂附TiO_2-SiO_2纳米薄膜，经750°C热处理后其钛瓷结合强度与对照组相比提高了21.77%，而300°C热处理后的钛瓷结合强度却降低了13.28%，两者均具有统计学差异；经750°C热处理不同时间后的钛瓷结合强度均显著增加，但是相互间无统计学差异；纳米薄膜各组成成分的摩尔比率对钛瓷结合强度也无显著的影响，但是随着Ti含量降低，Si含量增高，钛瓷结合强度呈现降低的趋势。
2.不同温度热处理的TiO_2-SiO2纳米薄膜X线衍射图谱(XRD)显示，尽管750°C组的XRD图明显不同于300°C和500°C组，但是所有试件均未发现金红石相TiO_2。这说明涂附在钛金属表面的TiO_2-SiO_2纳米薄膜可以作为氧隔离屏障，能够有效的防止钛在瓷熔附过程中继续氧化。改变热处理时间和各组成成分的摩尔比率，TiO_2-SiO2纳米薄膜的晶型无明显变化。
3.通过对表面涂附TiO_2-SiO2纳米薄膜的钛瓷界面进行扫描电镜(SEM)观察发现，300°C和500°C热处理后的纳米薄膜较为松散凌乱，薄膜开裂，且缝隙较大。而经750°C热处理的纳米薄膜相对较为致密，未见明显的裂缝存在。观察750°C热处理后的钛瓷试件在三点弯曲测试后其横切面的SEM图发现，钛瓷断裂的位置发生了变化，不再是钛表面氧化膜与钛基底之间，而是位于TiO_2-SiO_2纳米薄膜内部。
4.在上述研究的基础上，将Sn元素加入到TiO_2-SiO2纳米薄膜中，研究在不同处理条件下该复合型纳米薄膜对钛瓷结合强度的影响。实验结果显示，影响TiO_2-SiO_2-SnO_x纳米薄膜增强钛瓷结合强度的热处理温度与TiO_2-SiO_2纳米薄膜截然相反。其显著增强钛瓷结合强度的温度为300°C，约可提高21.32%。随着热处理时间的延长，钛瓷间的结合强度逐渐增大，但是无统计学意义。各组成成分的摩尔比率对钛瓷结合强度也有一定的影响作用，Ti:Si:Sn摩尔比率为5:4:1和2:2:1时的钛瓷结合强度显著提高，但是当三者比率为4:5.5:0.5时却无明显改变。
5.比较不同温度热处理的TiO_2-SiO_2-SnO_x纳米薄膜X线衍射图谱(XRD)发现，与300°C组和500°C组相比，750°C组的XRD相图中无SnO晶相，取而代之的是SnO_2晶相。表明随着温度的升高SnO可能被氧化为SnO_2。而所有试件中均未发现金红石相TiO_2的结果则说明涂附在钛金属表面的TiO_2-SiO_2-SnO_x纳米薄膜可以作为氧隔离屏障，有效的防止钛在瓷熔附过程中继续氧化。热处理时间和各组成成分的摩尔比率对TiO_2-SiO_2-SnO_x纳米薄膜的晶型变化无明显影响。6.通过观察比较不同处理条件下表面涂附TiO_2-SiO_2-SnO_x纳米薄膜的钛瓷界面SEM图发现，经300°C热处理的纳米薄膜较为致密，均匀一致，无明显的裂缝存在。而500°C和750°C热处理后的纳米薄膜则杂乱无序，且表面存在着明显的缝隙。对300°C热处理后的钛瓷试件在三点弯曲测试后其横切面进行SEM观察发现，钛瓷断裂的位置发生了变化，不再是钛表面氧化膜与钛基底之间，而是位于TiO_2-SiO_2-SnO_x纳米薄膜内部。7.分别采用划痕法对不同热处理温度下TiO_2-SiO_2和TiO_2-SiO_2-SnO_x纳米薄膜与钛基底间的膜基结合强度进行测试发现，当热处理温度为300°C、500°C和750°C时，TiO_2-SiO_2纳米薄膜与钛基底的膜基结合力分别为15.3N、22N和28.5N，说明随着温度的升高，TiO_2-SiO_2纳米薄膜与钛基底的膜基结合力也随之升高；而TiO_2-SiO_2-SnO_x纳米薄膜与钛基底的膜基结合力则分别为18.5N、24.5N和22.8N，说明随着温度的升高，TiO_2-SiO_2-SnO_x纳米薄膜与钛基底的膜基结合力先升高再降低。8.通过比较钛瓷试件在酸性含F-的人工唾液中浸泡不同时间后的钛瓷结合强度发现，浸泡1天钛瓷结合强度即可出现明显降低，且与对照组相比具有统计学差异。而后随着时间的延长，钛瓷结合强度逐渐减少，最后趋于稳定；酸的类型与钛瓷结合强度的减少无关；酸的pH值、F-浓度以及酸的类型均无法改变钛瓷断裂发生的位置和方式，断裂仍主要发生在钛表面氧化层和钛基底之间。
With the excellent biocompatibility, corrosion resistance and otheradvantages, titanium has been widely used in oral clinical. Due to the lowmelting point, low thermal expansion coefficient of titanium porcelain powderwas successfully placed on the market, titanium-ceramic technology has alsobeen considerable development. But the titanium-porcelain bond strength wasstill significantly lower than the bond strength of Ni-Cr alloy and porcelain. Thereasons was that the titanium surface can easily form a porous and nonadherentoxide under the high temperature environment. With small particle size, highsurface tension and surface binding energy, nano-materials displays a strongchemical activity and can take place chemical reaction with the oxygen of theporcelain and metal surfaces. In order to limit the excessive oxidation oftitanium in the porcelain sintering process and improve the bond strength oftitanium-porcelain, the surface of titanium was coated with nano-coatings by thesol-gel technology and then impose the appropriate heat treatment in this study. Otherwise, with the purpose of obtaining a theoretical basis for the furtherclinical applications of titanium porcelain restorations, we simulated the oralenvironment and studied the variational rule of titanium-porcelain bondstrength in acidic artificial saliva with the F-and the corrosion mechanism. Theresults are as follows:
1. Compared with the titanium-porcelain system without any intermediatecoatings, the bond strength of the same system coated with TiO_2-SiO_2nano-coatings, being produced by the sol-gel technology and fired at750°C wassignificantly increased by21.77%. While the titanium-porcelain bond strengthwas significantly reduced by13.28%under the heat treatment conditions of300°C; Little effect of heat treatment duration on the bond strength of titaniumporcelain was found; Though the effects of the molar ratio of nano-coatingscomposition to the titanium-porcelain bond strength was also not obvious, butthere was still the variational rule of the lower Ti content and the higher Sicontent, the lower bond strength of titanium-porcelain.
2. The X-ray diffraction patterns (XRD) patterns of the TiO_2-SiO_2nano-coatings fired at different temperatures was shown that although the XRDpattern of the specimen fired at750°C was significantly different from thespecimen fired at300°C and500°C, but the rutile phase was not found in allspecimens, which proved the TiO_2-SiO_2nano-coatings can be used as oxygenseparation barrier and effectively prevent oxidation of titanium in the process ofporcelain being fused to the titanium. With the different heat treatment durationand the molar ratio of the composition, no significant change of the crystal ofTiO_2-SiO_2nano-coatings was happened.
3. The scanning electron microscope (SEM) photomicrographs of titanium-porcelain interface morphology of the specimens before porcelain fused with different heat treatment temperature、heat treatment duration and the molar ratioof the composition were observed that the TiO_2-SiO_2nano-coatings fired at300°C or500°C was loose and messy with larger cracks while the same coatingfired at750°C was compact and homogeneous without any obvious cracksexisting. The cross-sectional SEM microphotograph of the specimen fired at750°C after three-point bending test revealed that the location of thetitanium-porcelain fracture had been changed, which not existed between theoxide film of the titanium surface and titanium substrate, but within theTiO_2-SiO_2nano-coatings.
4. With the basis of the above study, the Sn element was added into theTiO_2-SiO2nano-coatings to study the effects of the composite nano-coatings tothe bond strength of titanium-porcelain. The experimental results shown that thetemperature of the TiO_2-SiO_2-SnO_xnano-coatings fired which can significantlyincrease the bond strength of titanium-porcelain was opposite to the TiO_2-SiO_2nano-coatings. The bond strength of the titanium-porcelain system coated withTiO_2-SiO_2-SnO_xnano-coatings, being produced by the sol-gel technology andfired at300°C, was significantly increased by21.32%. With the more of heattreatment duration, the bond strength of titanium-porcelain was higher; Themolar ratio of nano-coatings composition can also effect the titanium-porcelainbond strength. When the molar ratio of Ti: Si: Sn was5:4:1and2:2:1, the bondstrength of titanium-porcelain was significantly increased, which was no notablychange under the three ratios for4:5.5:0.5.
5. The X-ray diffraction patterns (XRD) patterns of the TiO_2-SiO2-SnOxnano-coatings fired at different temperatures was shown that compared with theXRD patterns of the specimens fired at300°C and500°C, no SnO phase wasfound in the XRD pattern of the specimen fired at750°C, which was replaced by the SnO2phase. The results shown that SnO maybe oxidized to SnO2with thefiring temperature elevated. The rutile phase was not found in all specimens,which indicated the TiO_2-SiO_2-SnO_xnano-coatings can be used as oxygenseparation barrier and effectively prevent oxidation of titanium in the process ofporcelain being fused to the titanium. No significant change of the crystal wasobserved under different heat treatment duration and the molar ratio of thecomposition.6. The scanning electron microscope (SEM) photomicrographs of titanium-porcelain interface morphology of the specimens before porcelain fused underdifferent processing conditions shown that compared with the disorderly andloose surface morphology of the TiO_2-SiO_2-SnO_xnano-coatings fired at500°Cor750°C, the same nano-coatings fired at300°C was compact andhomogeneous without any obvious cracks existing. The cross-sectional SEMmicrophotograph of the specimen fired at300°C after three-point bending testrevealed that the location of the titanium-porcelain fracture had been changed,which not existed between the oxide film of the titanium surface and titaniumsubstrate, but within the TiO_2-SiO_2nano-coatings.7. The bond strength between the TiO_2-SiO_2or TiO_2-SiO_2-SnO_xnano-coatingsfired at different temperatures and titanium substrate was respectively tested bythe scarification. When the heat treatment temperature was300°C、500°C and750°C, the bond strength of the TiO_2-SiO_2nano-coatings to the titaniumsubstrate was15.3N、22N and28.5N respectively, which shown that with theincreasing heat treatment temperature the bond strength of the nano-coatings tothe titanium substrate was also increased; while the bond strength of theTiO_2-SiO_2-SnO_xnano-coatings to the titanium substrate was18.5N、24.5N and22.8N respectively, which shown that with the increasing heat treatment temperature the bond strength of the nano-coatings to the titanium substrate wasincreased and then gradually decreased.
8. The titanium-porcelain bond strength of the specimens immersed in the acidicartificial saliva containing F-was compared in this study, which wassignificantly decreased after1day. With the longer immersion time, the bondstrength of titanium-porcelain gradually reduced and finally stabilized. Therewas no obvious relationship between the bond strength of titanium-porcelainand the acid species. The location and manner of titanium-porcelain fracturecan’t changed with different pH values, F-concentration and acid species, thefracture still occurred mainly between the oxide film of the titanium surface andtitanium substrate.
研究结果如下：
1．采用溶胶-凝胶技术均匀的在钛金属表面涂附TiO_2-SiO_2纳米薄膜，经750°C热处理后其钛瓷结合强度与对照组相比提高了21.77%，而300°C热处理后的钛瓷结合强度却降低了13.28%，两者均具有统计学差异；经750°C热处理不同时间后的钛瓷结合强度均显著增加，但是相互间无统计学差异；纳米薄膜各组成成分的摩尔比率对钛瓷结合强度也无显著的影响，但是随着Ti含量降低，Si含量增高，钛瓷结合强度呈现降低的趋势。
2.不同温度热处理的TiO_2-SiO2纳米薄膜X线衍射图谱(XRD)显示，尽管750°C组的XRD图明显不同于300°C和500°C组，但是所有试件均未发现金红石相TiO_2。这说明涂附在钛金属表面的TiO_2-SiO_2纳米薄膜可以作为氧隔离屏障，能够有效的防止钛在瓷熔附过程中继续氧化。改变热处理时间和各组成成分的摩尔比率，TiO_2-SiO2纳米薄膜的晶型无明显变化。
3.通过对表面涂附TiO_2-SiO2纳米薄膜的钛瓷界面进行扫描电镜(SEM)观察发现，300°C和500°C热处理后的纳米薄膜较为松散凌乱，薄膜开裂，且缝隙较大。而经750°C热处理的纳米薄膜相对较为致密，未见明显的裂缝存在。观察750°C热处理后的钛瓷试件在三点弯曲测试后其横切面的SEM图发现，钛瓷断裂的位置发生了变化，不再是钛表面氧化膜与钛基底之间，而是位于TiO_2-SiO_2纳米薄膜内部。
4.在上述研究的基础上，将Sn元素加入到TiO_2-SiO2纳米薄膜中，研究在不同处理条件下该复合型纳米薄膜对钛瓷结合强度的影响。实验结果显示，影响TiO_2-SiO_2-SnO_x纳米薄膜增强钛瓷结合强度的热处理温度与TiO_2-SiO_2纳米薄膜截然相反。其显著增强钛瓷结合强度的温度为300°C，约可提高21.32%。随着热处理时间的延长，钛瓷间的结合强度逐渐增大，但是无统计学意义。各组成成分的摩尔比率对钛瓷结合强度也有一定的影响作用，Ti:Si:Sn摩尔比率为5:4:1和2:2:1时的钛瓷结合强度显著提高，但是当三者比率为4:5.5:0.5时却无明显改变。
5.比较不同温度热处理的TiO_2-SiO_2-SnO_x纳米薄膜X线衍射图谱(XRD)发现，与300°C组和500°C组相比，750°C组的XRD相图中无SnO晶相，取而代之的是SnO_2晶相。表明随着温度的升高SnO可能被氧化为SnO_2。而所有试件中均未发现金红石相TiO_2的结果则说明涂附在钛金属表面的TiO_2-SiO_2-SnO_x纳米薄膜可以作为氧隔离屏障，有效的防止钛在瓷熔附过程中继续氧化。热处理时间和各组成成分的摩尔比率对TiO_2-SiO_2-SnO_x纳米薄膜的晶型变化无明显影响。6.通过观察比较不同处理条件下表面涂附TiO_2-SiO_2-SnO_x纳米薄膜的钛瓷界面SEM图发现，经300°C热处理的纳米薄膜较为致密，均匀一致，无明显的裂缝存在。而500°C和750°C热处理后的纳米薄膜则杂乱无序，且表面存在着明显的缝隙。对300°C热处理后的钛瓷试件在三点弯曲测试后其横切面进行SEM观察发现，钛瓷断裂的位置发生了变化，不再是钛表面氧化膜与钛基底之间，而是位于TiO_2-SiO_2-SnO_x纳米薄膜内部。7.分别采用划痕法对不同热处理温度下TiO_2-SiO_2和TiO_2-SiO_2-SnO_x纳米薄膜与钛基底间的膜基结合强度进行测试发现，当热处理温度为300°C、500°C和750°C时，TiO_2-SiO_2纳米薄膜与钛基底的膜基结合力分别为15.3N、22N和28.5N，说明随着温度的升高，TiO_2-SiO_2纳米薄膜与钛基底的膜基结合力也随之升高；而TiO_2-SiO_2-SnO_x纳米薄膜与钛基底的膜基结合力则分别为18.5N、24.5N和22.8N，说明随着温度的升高，TiO_2-SiO_2-SnO_x纳米薄膜与钛基底的膜基结合力先升高再降低。8.通过比较钛瓷试件在酸性含F-的人工唾液中浸泡不同时间后的钛瓷结合强度发现，浸泡1天钛瓷结合强度即可出现明显降低，且与对照组相比具有统计学差异。而后随着时间的延长，钛瓷结合强度逐渐减少，最后趋于稳定；酸的类型与钛瓷结合强度的减少无关；酸的pH值、F-浓度以及酸的类型均无法改变钛瓷断裂发生的位置和方式，断裂仍主要发生在钛表面氧化层和钛基底之间。
With the excellent biocompatibility, corrosion resistance and otheradvantages, titanium has been widely used in oral clinical. Due to the lowmelting point, low thermal expansion coefficient of titanium porcelain powderwas successfully placed on the market, titanium-ceramic technology has alsobeen considerable development. But the titanium-porcelain bond strength wasstill significantly lower than the bond strength of Ni-Cr alloy and porcelain. Thereasons was that the titanium surface can easily form a porous and nonadherentoxide under the high temperature environment. With small particle size, highsurface tension and surface binding energy, nano-materials displays a strongchemical activity and can take place chemical reaction with the oxygen of theporcelain and metal surfaces. In order to limit the excessive oxidation oftitanium in the porcelain sintering process and improve the bond strength oftitanium-porcelain, the surface of titanium was coated with nano-coatings by thesol-gel technology and then impose the appropriate heat treatment in this study. Otherwise, with the purpose of obtaining a theoretical basis for the furtherclinical applications of titanium porcelain restorations, we simulated the oralenvironment and studied the variational rule of titanium-porcelain bondstrength in acidic artificial saliva with the F-and the corrosion mechanism. Theresults are as follows:
1. Compared with the titanium-porcelain system without any intermediatecoatings, the bond strength of the same system coated with TiO_2-SiO_2nano-coatings, being produced by the sol-gel technology and fired at750°C wassignificantly increased by21.77%. While the titanium-porcelain bond strengthwas significantly reduced by13.28%under the heat treatment conditions of300°C; Little effect of heat treatment duration on the bond strength of titaniumporcelain was found; Though the effects of the molar ratio of nano-coatingscomposition to the titanium-porcelain bond strength was also not obvious, butthere was still the variational rule of the lower Ti content and the higher Sicontent, the lower bond strength of titanium-porcelain.
2. The X-ray diffraction patterns (XRD) patterns of the TiO_2-SiO_2nano-coatings fired at different temperatures was shown that although the XRDpattern of the specimen fired at750°C was significantly different from thespecimen fired at300°C and500°C, but the rutile phase was not found in allspecimens, which proved the TiO_2-SiO_2nano-coatings can be used as oxygenseparation barrier and effectively prevent oxidation of titanium in the process ofporcelain being fused to the titanium. With the different heat treatment durationand the molar ratio of the composition, no significant change of the crystal ofTiO_2-SiO_2nano-coatings was happened.
3. The scanning electron microscope (SEM) photomicrographs of titanium-porcelain interface morphology of the specimens before porcelain fused with different heat treatment temperature、heat treatment duration and the molar ratioof the composition were observed that the TiO_2-SiO_2nano-coatings fired at300°C or500°C was loose and messy with larger cracks while the same coatingfired at750°C was compact and homogeneous without any obvious cracksexisting. The cross-sectional SEM microphotograph of the specimen fired at750°C after three-point bending test revealed that the location of thetitanium-porcelain fracture had been changed, which not existed between theoxide film of the titanium surface and titanium substrate, but within theTiO_2-SiO_2nano-coatings.
4. With the basis of the above study, the Sn element was added into theTiO_2-SiO2nano-coatings to study the effects of the composite nano-coatings tothe bond strength of titanium-porcelain. The experimental results shown that thetemperature of the TiO_2-SiO_2-SnO_xnano-coatings fired which can significantlyincrease the bond strength of titanium-porcelain was opposite to the TiO_2-SiO_2nano-coatings. The bond strength of the titanium-porcelain system coated withTiO_2-SiO_2-SnO_xnano-coatings, being produced by the sol-gel technology andfired at300°C, was significantly increased by21.32%. With the more of heattreatment duration, the bond strength of titanium-porcelain was higher; Themolar ratio of nano-coatings composition can also effect the titanium-porcelainbond strength. When the molar ratio of Ti: Si: Sn was5:4:1and2:2:1, the bondstrength of titanium-porcelain was significantly increased, which was no notablychange under the three ratios for4:5.5:0.5.
5. The X-ray diffraction patterns (XRD) patterns of the TiO_2-SiO2-SnOxnano-coatings fired at different temperatures was shown that compared with theXRD patterns of the specimens fired at300°C and500°C, no SnO phase wasfound in the XRD pattern of the specimen fired at750°C, which was replaced by the SnO2phase. The results shown that SnO maybe oxidized to SnO2with thefiring temperature elevated. The rutile phase was not found in all specimens,which indicated the TiO_2-SiO_2-SnO_xnano-coatings can be used as oxygenseparation barrier and effectively prevent oxidation of titanium in the process ofporcelain being fused to the titanium. No significant change of the crystal wasobserved under different heat treatment duration and the molar ratio of thecomposition.6. The scanning electron microscope (SEM) photomicrographs of titanium-porcelain interface morphology of the specimens before porcelain fused underdifferent processing conditions shown that compared with the disorderly andloose surface morphology of the TiO_2-SiO_2-SnO_xnano-coatings fired at500°Cor750°C, the same nano-coatings fired at300°C was compact andhomogeneous without any obvious cracks existing. The cross-sectional SEMmicrophotograph of the specimen fired at300°C after three-point bending testrevealed that the location of the titanium-porcelain fracture had been changed,which not existed between the oxide film of the titanium surface and titaniumsubstrate, but within the TiO_2-SiO_2nano-coatings.7. The bond strength between the TiO_2-SiO_2or TiO_2-SiO_2-SnO_xnano-coatingsfired at different temperatures and titanium substrate was respectively tested bythe scarification. When the heat treatment temperature was300°C、500°C and750°C, the bond strength of the TiO_2-SiO_2nano-coatings to the titaniumsubstrate was15.3N、22N and28.5N respectively, which shown that with theincreasing heat treatment temperature the bond strength of the nano-coatings tothe titanium substrate was also increased; while the bond strength of theTiO_2-SiO_2-SnO_xnano-coatings to the titanium substrate was18.5N、24.5N and22.8N respectively, which shown that with the increasing heat treatment temperature the bond strength of the nano-coatings to the titanium substrate wasincreased and then gradually decreased.
8. The titanium-porcelain bond strength of the specimens immersed in the acidicartificial saliva containing F-was compared in this study, which wassignificantly decreased after1day. With the longer immersion time, the bondstrength of titanium-porcelain gradually reduced and finally stabilized. Therewas no obvious relationship between the bond strength of titanium-porcelainand the acid species. The location and manner of titanium-porcelain fracturecan’t changed with different pH values, F-concentration and acid species, thefracture still occurred mainly between the oxide film of the titanium surface andtitanium substrate.
引文
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