School of Dentistry and Institute of Oral Medicine, College of Medicine, National Cheng Kung University, Tainan, Taiwan.
School of Dentistry and Institute of Oral Medicine, College of Medicine, National Cheng Kung University, Tainan, Taiwan; Department of Stomatology, National Cheng Kung University Hospital, Tainan, Taiwan.
Dent Mater. 2022 Apr;38(4):715-724. doi: 10.1016/j.dental.2022.02.014. Epub 2022 Mar 3.
To investigate the effect of silane contents on their chemical interaction with 10-methacryloyloxydecyl-dihydrogen phosphate (MDP), and affecting the bonding of MDP to zirconia by time-of-flight secondary ion mass spectrometry (TOF-SIMS) and solid-state nuclear magnetic resonance (SSNMR) spectroscopy.
Zirconia (Cercon ht, Dentsply) slabs were prepared and fully sintered. Experimental primers SE-5 and SE-10 were formulated by adding 5 wt% and 10 wt% γ-methacryloxypropyltrimethoxysilane to an MDP-based primer SE BOND (SE), respectively. SE, SE-5, and SE-10 were applied on the assigned zirconia slabs. The chemical compositions on the surface and adhesive interfaces were examined by TOF-SIMS in a depth-profiling mode. Hydrophilicity and resin affinity of treated zirconia were analyzed. The bond strengths to resin cylinder were examined either after 24-h storage or thermocycles. In addition, zirconia powders treated with three primers were assessed by SSNMR spectrometry for the adsorption of MDP.
TOF-SIMS analysis showed that SE treatment generated the greatest amount of P-O-Zr related ions, which reduced in SE-5 and SE-10 groups. The 3D ion-images illustrated the generation of ZrO(OH) ions with silane contents. The SSNMR analysis revealed that the chemical bonding was mainly P-O-Zr ionic bonds in SE but shifted to P-OH-Zr hydrogen bonds in SE-5 and SE-10. SE-5 and SE-10 treated zirconia presented higher hydrophilicity and affinity to resin compared to Zr did. SE showed the highest initial bond strength which significantly decreased after thermocycling.
MDP adsorption onto zirconia via P-O-Zr ionic bond promotes bonding with resin. The silane enhances the hydroxylation of zirconia and impairs the adsorption of MDP, but does not adversely affect the bond durability.
通过飞行时间二次离子质谱（TOF-SIMS）和固态核磁共振（SSNMR）光谱研究硅烷含量对其与 10-甲氧基丙烯酰氧癸基二氢磷酸酯（MDP）的化学相互作用的影响，并影响 MDP 与氧化锆的键合。
制备并完全烧结氧化锆（Cercon ht，登士柏）平板。实验性底漆 SE-5 和 SE-10 通过向基于 MDP 的底漆 SE BOND（SE）中分别添加 5wt%和 10wt%γ-甲基丙烯酰氧基丙基三甲氧基硅烷来配制。SE、SE-5 和 SE-10 应用于指定的氧化锆平板上。通过深度剖析模式的 TOF-SIMS 检查表面和粘合界面上的化学成分。分析处理后的氧化锆的亲水性和树脂亲和力。检查树脂圆柱的结合强度，无论是在 24 小时储存后还是热循环后。此外，通过 SSNMR 光谱评估用三种底漆处理的氧化锆粉末对 MDP 的吸附。
TOF-SIMS 分析表明，SE 处理产生了最多的与 P-O-Zr 相关的离子，而在 SE-5 和 SE-10 组中则减少了。3D 离子图像说明了随硅烷含量的产生的 ZrO(OH)离子。SSNMR 分析表明，化学键合主要是 SE 中的 P-O-Zr 离子键，但在 SE-5 和 SE-10 中转变为 P-OH-Zr 氢键。与 Zr 相比，SE-5 和 SE-10 处理的氧化锆具有更高的亲水性和对树脂的亲和力。SE 表现出最高的初始结合强度，在热循环后显著降低。
通过 P-O-Zr 离子键将 MDP 吸附到氧化锆上促进与树脂的键合。硅烷增强了氧化锆的羟基化作用，并削弱了 MDP 的吸附，但不会对键合耐久性产生不利影响。
