磁控溅射氮化铌对钛-瓷结合强度的影响

Effect of niobium nitride on the bonding strength of titanium porcelain by magnetron sputtering

目的 探讨磁控溅射氮化铌（niobium nitride，NbN）对钛-瓷（Vita钛瓷粉系统）结合强度的影响，以期为钛-瓷修复体的临床应用提供参考。方法根据随机数字表将60个钛试件随机分为T1、T2、T3和T4四个实验组。T1和T2组试件表面均先行120μmAl2O3喷砂，T2组试件表面再行磁控溅射氮化铌涂层。T3和T4组试件表面均先行磁控溅射氮化铌涂层，T4组试件表面再行120μmAl2O3喷砂。X射线衍射分析仪（X—ray diffraction，XRD）分析各组涂层物相。试件烤瓷后用万能实验机测试钛-瓷结合强度。扫描电子显微镜-X射线能谱仪（scanning electron microscopy with energy depressive spectrum，SEM—EDS）观察和分析钛-瓷结合界面。结果XRD观察到T2、T3和T4组均存在立方晶型的氮化铌新相。三点弯曲实验测得T1～T4组试件的钛-瓷结合强度分别为（27．2±0．8）、（43．1±0．6）、（31．4±1．0）和（44．9±0．6）MPa，4组间差异有统计学意义（P〈0．05）。两两比较显示，任意两组间差异均有统计学意义（P〈0．05）。SEM观察T1和T3组钛-瓷结合界面可见明显孔隙和裂纹，T2和T4组钛-瓷结合较好，EDS线扫描显示，T1组钛基底氧化明显，T2组和T3组界面处存在钛氧化行为，T4组界面处钛基底的氧化得到抑制。结论磁控溅射氮化铌可抑制烤瓷侧钛基底的氧化，提高钛-瓷结合强度，同时表明Al2O3喷砂处理也能提高钛-瓷结合强度。

Objectives To investigate the effect of magnetron sputtered niobium nitride （NbN） on the bonding strength of commercially pure cast titanium（Ti） and low-fusing porcelain （Ti/Vita titankeramik system）. Methods Sixty Ti specimens were randomly divided into four groups, group T1, T2, T3 and T4. All specimens of group T1 and T2 were first treated with 120μm blasted Al2O3 particles, and then only specimens of group T2 were treated with magnetron sputtered NbN film. All specimens of group T3 and T4 were first treated with magnetron sputtered NbN film and then only specimens of group T4 were treated with 120μm blasted Al2O3 particles. The composition of the deposits were analyzed by X-ray diffraction（XRD）. A universal testing machine was used to perform the three-point bending test to evaluate the bonding strength of Ti and porcelain. The microstructure of NbN, the interface of Ti-porcelain and the fractured Ti surface were observed with scanning electron microscopy （SEM） and energy depressive spectrum （EDS） , and the results were compared. Results The XRD results showed that the NbN deposits were cubic crystalline phases. The bonding strength of Ti and porcelain in T1 to T4 group were （27.2 ±0. 8 ）, （43.1 ±0. 6 ）, （31.4± 1.0） and （44. 9 ±0. 6） MPa. These results were analyzed by one-way analysis of variance and differences between groups were compared using least significant difference test. Significant inter-group differences were found among all groups（ P 〈 0. 05 ）. The results of SEM showed that with treatment of A12 03 or NbN, alone, pre-cracks were found in the interface of Ti-porcelain, while samples treated with both Al2O3 and NbN had better bond. EDS of Ti-porcelain interface showed oxidation occurred in T1, T2 and T3, but was well controlled in T4. Conclusions Magnetron sputtered NbN can prevent Ti from being oxidized, and can improve the bonding strength of Ti/Vita titankeramik system. Al2O3 blast can also improve the bonding strength of Ti/Vita titankeramik system.