口腔医学研究

口腔医学研究 ›› 2020, Vol. 36 ›› Issue (6): 585-590.DOI: 10.13701/j.cnki.kqyxyj.2020.06.019

• 口腔材料学研究 • 上一篇    下一篇

釉质表面超疏水凝胶纳米涂层的制备及其性能研究

金小婷1, 史诗1, 陈欢欢1, 薛冬1, 麻健丰1,2*   

  1. 1.温州医科大学口腔医学研究所 浙江 温州 325027;
    2.温州医科大学口腔医学院附属口腔医院 浙江 温州 325027
  • 收稿日期:2019-03-06 出版日期:2020-07-03 发布日期:2020-07-06
  • 通讯作者: *麻健丰,E-mail:dentistmacn@aliyun.com
  • 作者简介:金小婷(1993~ ),女,浙江人,硕士,研究方向:口腔修复学。
  • 基金资助:
    国家自然科学基金(编号:81870813)

Preparation and Performance of Superhydrophobic Gel Nano-coating on Enamel Surface

JIN Xiaoting1, SHI Shi1, CHEN Huanhuan1, XUE Dong1, MA Jianfeng1,2*   

  1. 1. Institute of Stomatology, Wenzhou Medical University,Wenzhou 325027,China;
    2. School and Hospital of Stomatology, Wenzhou Medical University, Wenzhou 325027,China
  • Received:2019-03-06 Online:2020-07-03 Published:2020-07-06

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摘要： 目的: 牙釉质表面超疏水凝胶纳米涂层的制备及其性能研究。方法: 采用溶胶凝胶法制备三甲基硅基改性的多巴胺-硅凝胶(DSTM)超疏水涂层。制备4 mm×4 mm×2 mm牛牙釉质块若干,随机分为两组:实验组涂布DSTM,对照组采用去离子水处理。通过测量接触角对涂层的超疏水性能进行评价。使用扫描电子显微镜(SEM)观察涂层表面微观结构,傅立叶变换红外光谱(FT-IR)和X射线光电子能谱(XPS)对釉质表面涂层的成分进行分析,CCK-8比色法进行细胞毒性实验,检测其生物安全性。为了评价该涂层在口腔环境中的疏水稳定性,将涂层处理过的釉质块分别放入37 ℃人工唾液中浸泡2 h、4 h、6 h、10 h、12 h,观察其表面接触角和微观结构的变化。结果: 接触角测量结果显示,对照组牙片表面接触角为(60.20±4.56)°,实验组表面接触角达(153.88±2.81)°,明显高于对照组,差异有统计学意义(P<0.05);SEM结果显示涂层表面由相互连接的纳米孔组成三维纳米网状结构;XPS与FT-IR结果均显示釉质表面DSTM涂层的成功制备;CCK-8细胞毒性实验表明在24、48和72 h的检测结果中,实验组与对照组的CCK-8吸光度值均与空白组相当;涂层稳定性实验结果显示,在人工唾液浸泡12 h后,涂层接触角为(149.40±2.43)°,仍然具备超疏水性能,同时唾液处理后的牙面SEM结果显示涂层的纳米结构等微观形貌未发生明显变化。结论: 本试验通过溶胶凝胶法成功制备了具有良好疏水性、生物安全性及稳定性的DSTM凝胶涂层,为探索抑制细菌粘附的新型防龋材料提供了依据。

关键词: 超疏水涂层, 牙釉质表面, 多巴胺, 溶胶凝胶

Abstract: Objective: To investigate the preparation and performance of superhydrophobic gel nano-coating on enamel surface. Methods: A sol-gel method was used to prepare a trimethylsilyl-modified dopamine-silicone gel (DSTM) superhydrophobic coating. Several 4 mm × 4 mm × 2 mm enamel blocks of bovine tooth were randomly divided into two groups: the experimental group and the control group, which were treated separately by DSTM and deionized water. The effect of coating superhydrophobicity was evaluated by the contact angle. Scanning electron microscope (SEM), Fourier transform infrared spectroscopy (FT-IR), and X-ray photoelectron spectroscopy (XPS) were used to assess the microstructure of the coating surface and analyze the composition of the tooth surface coating. The cell toxicity and biological safety were tested by CCK-8 colorimetry. In order to evaluate the stability of the hydrophobic coating in the oral environment, the coated enamel mass was immersed in artificial saliva at 37 ℃ for 2 h, 4 h, 6 h, 10 h, and 12 h and then observed the contact angle and surface microstructure changes. Results: The contact angle of dental tablets was (60.20±4.56)°, while that of the experimental group was (153.88±2.81)° (P<0.05). Under the SEM observation, the coating surface was composed of interconnected micrometers and nanopores that form a three-dimensional nano-network structure. The XPS and FT-IR showed that the DSTM coating on the tooth surface was successfully prepared. Among the detection values at 24 h, 48 h, and 72 h, the OD values of all groups were comparable to the blank group values. The results of the coating stability experiment showed that the sample still had superhydrophobic properties with a contact angle value of (149.40±2.43)° after being soaked in artificial saliva for 12 h. However, there was no significant changes in the micro-morphology of the micropores and micro-nano structures from the SEM of the saliva-treated coating. Conclusion: In this experiment, a DSTM gel coating was successfully prepared by the sol-gel method. The coating with good biological safety and hydrophobicity has certain stability in a 37 ℃ artificial saliva environment, which provided a basis for the new anti-caries materials.

Key words: super-hydrophobic coating, enamel surface, dopamine, sol-gel