复合纳米金膜技术增强牙科钛瓷结合的基础研究

A basic study on improving dental titanium-ceramic bonding by Au nanoparticle film deposition technique

目的利用离子多层自组装技术在纯钛表面沉积复合纳米金膜并烧结专用钛瓷粉,探讨该技术对钛瓷之间结合强度的影响。方法根据ISO 9693要求制备预成纯钛试件20个,沉积纳米金膜为实验组(AuS);非沉积纳米金膜为对照组(S),每组10个钛瓷标准试件。运用场发射扫描电镜(FE-SEM)观察钛试件沉积纳米金膜后的表面形态以及钛瓷结合界面的微观形貌。三点弯曲法测定钛瓷结合强度,并进行统计学分析。体视显微镜观察钛瓷界面的断裂模式。电子探针(EMP)检测结合界面上Au元素的分布情况。结果 AuS组的钛瓷结合强度(36.24±3.64)MPa明显高于S组的钛瓷结合强度(30.78±3.83)MPa,P<0.05。FE-SEM观察显示:钛表面沉积纳米金颗粒后形成了均匀、致密的复合纳米金膜。电镜观察结合界面显示,AuS组钛瓷结合界面连续而紧密,体视显微镜观察断裂模式以混合断裂为主;对照组钛瓷结合界面可见明显的裂隙,偶有气泡,断裂模式以界面断裂为主。EMP检测结果显示:结合界面上可见Au元素分布,纳米金颗粒在烧结过程中团聚成簇后沿钛瓷结合界面呈带形分布,在粘接瓷底部呈点状弥散。结论在本研究条件下,纯钛表面沉积复合纳米金膜可显著提高Super porcelain Ti-22专用钛瓷粉与预成纯钛试件之间的结合强度。

Objective Depositing nano-gold films on the pure titanium substrate by ionic self-assembled mutilayers technique （ISAM） and sintering a special titanium porcelain powder, the study was aim to investigate the effect of the deposited nanogold composite films on the adhesion of porcelain to titanium. Methods Twenty pure titanium specimens were prepared according to ISO 9693 requirement. Grouped according to whether or not depositing composite nano-gold film, nano-gold film deposited pure titanium specimens as the experimental group （AuS）; non-nanogold gold film deposited specimens as the control group （S）, each group has 10 standard specimens. Field emission scanning electron microscope（FE-SEM） was used to observe the surface morphology of titanium specimen after depositing composite nano-gold films, and further observe the microstructure of the interface between titanium and porcelain after sintered. The titanium-porcelain bonding strength was assessed by three point bending method and statistical analysis. The titanium - porcelain fracture mode of the specimens was determined by Stereoscopic microscope. The distribution of the Au element on the interface of titanium-porcelain was detected by electron microprobe （EMP）. Results The titanium-porcelain bonding strength of nano-gold film deposited group was significantly higher than those of the undeposited group [（36.24±3.64） MPa and （30.78 ± 3.83） MPa, P 〈 0.05 ] . FE-SEM illustrated that the surface of the nano-gold deposited group formed a uniform, dense composite nano-gold film. Stereomicroscope and SEM images showed that the titanium-porcerlain interface of AuS group was continuous and closely, the fracture mode was given priority to mixed mode fracture; while the interface of S group had an obviously crack and occasional bubble, the fracture mode was given priority to interfacial fracture. Small, white spots of gold particles could be detected along the titanium-porcelain bonding interface by electron microprobe （EMP）. Conclusions Under the conditions of the present study, composite nano-gold films deposited on the pure titanium surface can significantly improve the bonding strength between the Super porcelain Ti-22 special titanium porcelain powder and the preformed titanium specimens.