Kaizer M R, Almeida J R, Gonçalves A P R, Zhang Y, Cava S S, Moraes R R
1 Graduate Program in Dentistry, Federal University of Pelotas, Pelotas, Brazil.
2 College of Dentistry, New York University, New York, NY, USA.
J Dent Res. 2016 Nov;95(12):1394-1400. doi: 10.1177/0022034516662022. Epub 2016 Jul 29.
This study was designed to develop and characterize a silica-coating method for crystalline nonsilicate ceramic nanoparticles (AlO, TiO, and ZrO). The hypothesis was that the coated nonsilicate nanoparticles would stably reinforce a polymeric matrix due to effective silanation. Silica coating was applied via a sol-gel method, with tetraethyl orthosilicate as a silica precursor, followed by heat treatment. The chemical and microstructural characteristics of the nanopowders were evaluated before and after silica coating through x-ray diffraction, BET (Brunauer-Emmett-Teller), energy-dispersive x-ray spectroscopy, field emission scanning electron microscopy, and transmission electron microscopy analyses. Coated and noncoated nanoparticles were silanated before preparation of hybrid composites, which contained glass microparticles in addition to the nanoparticles. The composites were mechanically tested in 4-point bending mode after aging (10,000 thermal cycles). Results of all chemical and microstructural analyses confirmed the successful obtaining of silica-coated nanoparticles. Two distinct aspects were observed depending on the type of nanoparticle tested: 1) formation of a silica shell on the surface of the particles and 2) nanoparticle clusters embedded into a silica matrix. The aged hybrid composites formulated with the coated nanoparticles showed improved flexural strength (10% to 30% higher) and work of fracture (35% to 40% higher) as compared with composites formulated with noncoated nanoparticles. The tested hypothesis was confirmed: silanated silica-coated nonsilicate nanoparticles yielded stable reinforcement of dimethacrylate polymeric matrix due to effective silanation. The silica-coating method presented here is a versatile and promising novel strategy for the use of crystalline nonsilicate ceramics as a reinforcing phase of polymeric composite biomaterials.
本研究旨在开发并表征一种用于结晶非硅酸盐陶瓷纳米颗粒(AlO、TiO和ZrO)的二氧化硅涂层方法。假设是由于有效的硅烷化作用,涂覆的非硅酸盐纳米颗粒将稳定地增强聚合物基体。通过溶胶-凝胶法,以正硅酸四乙酯作为二氧化硅前驱体进行二氧化硅涂层,随后进行热处理。通过X射线衍射、BET(布鲁诺尔-埃米特-泰勒)、能量色散X射线光谱、场发射扫描电子显微镜和透射电子显微镜分析,在二氧化硅涂层前后评估纳米粉末的化学和微观结构特征。在制备除纳米颗粒外还包含玻璃微粒的混合复合材料之前,对涂覆和未涂覆的纳米颗粒进行硅烷化处理。在老化(10000次热循环)后,以四点弯曲模式对复合材料进行力学测试。所有化学和微观结构分析的结果均证实成功获得了二氧化硅涂层纳米颗粒。根据所测试的纳米颗粒类型观察到两个不同的方面:1)颗粒表面形成二氧化硅壳层;2)纳米颗粒簇嵌入二氧化硅基体中。与由未涂覆纳米颗粒配制的复合材料相比,由涂覆纳米颗粒配制的老化混合复合材料表现出更高的弯曲强度(高10%至30%)和断裂功(高35%至40%)。所测试的假设得到证实:由于有效的硅烷化作用,硅烷化的二氧化硅涂层非硅酸盐纳米颗粒对二甲基丙烯酸酯聚合物基体产生了稳定的增强作用。本文提出的二氧化硅涂层方法是一种通用且有前景的新策略,可用于将结晶非硅酸盐陶瓷用作聚合物复合生物材料的增强相。