Synthesis and characterization of PMMA-grafted-ZrO2 hybrid nanoparticles

Linh Nguyen Thi Dieu, Dung Nguyen Thi Kim, Thang Dam Xuan, Tham Do Quang
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Abstract

In this study, we reported a facile synthesis and the characterization of PMMA-grafted ZrO2 hybrid nanoparticles from original ZrO2 (oZrO2) nanoparticles. The synthesis process included of three steps: (i) modification of nano ZrO2 with a vinyl silane agent, (ii) graft copolymerization of methyl methacrylate (MMA) monomers and modified ZrO2 (mZrO2) nanoparticles, and (iii) extraction of homo PMMA to obtain the final product of PMMA-g-ZrO2 (gZrO2) nanoparticles. Fourier transform infrared (FTIR) spectra and thermogravimetric analysis (TGA) of mZrO2, oZrO2, and gZrO2 indicated that the silane coupling agent was grafted onto oZrO2 nanoparticles. FTIR spectra of gZrO2 indicated PMMA had been successfully grafted onto the surface of ZrO2 nanoparticles. Using TGA method, the PMMA grafting content onto ZrO2 nanoparticles was evaluated as 9.03 wt.%. The electron microscopy (SEM) images of gZrO2, mZrO2, and oZrO2 indicated that their primary particle size and shape were almost unchanged after modification processes, their particle size was in the range from 50 nm to 140  nm. XRD analysis showed the monoclinic crystalline structure of three kinds of ZrO2 nanoparticles (nanocrystals). The organic gZrO2 nanoparticles can be a better candidate as an opacifier additive for polymer nanocomposites or acrylic bone cement.
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PMMA 接枝-ZrO2 混合纳米粒子的合成与表征
在这项研究中,我们报道了一种从原始 ZrO2(oZrO2)纳米粒子中简便合成 PMMA 接枝 ZrO2 混合纳米粒子的方法及其特性。合成过程包括三个步骤:(i) 用乙烯基硅烷剂改性纳米 ZrO2;(ii) 甲基丙烯酸甲酯(MMA)单体与改性 ZrO2(mZrO2)纳米粒子接枝共聚;(iii) 萃取均质 PMMA,得到最终产品 PMMA-g-ZrO2(gZrO2)纳米粒子。mZrO2、oZrO2 和 gZrO2 的傅立叶变换红外光谱(FTIR)和热重分析(TGA)表明,硅烷偶联剂接枝到了 oZrO2 纳米粒子上。gZrO2 的傅立叶变换红外光谱表明 PMMA 已成功接枝到 ZrO2 纳米粒子表面。使用 TGA 方法评估了接枝到 ZrO2 纳米粒子上的 PMMA 含量为 9.03 wt.%。gZrO2、mZrO2 和 oZrO2 的电子显微镜(SEM)图像表明,改性后它们的原始粒径和形状几乎没有变化,粒径范围在 50 纳米到 140 纳米之间。XRD 分析表明,三种 ZrO2 纳米粒子(纳米晶体)均为单斜晶系结构。有机 gZrO2 纳米粒子可以更好地用作聚合物纳米复合材料或丙烯酸骨水泥的不透明添加剂。
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