疏水性聚倍半硅氧烷纳米杂化材料的合成及性能

Synthesis and property of hydrophobic Polysilsesquioxane Nano Hybrid Materials

摘要:

以甲基三乙氧基硅烷（MTES）和十二烷基三甲氧基硅烷（DTMS）为前驱体，以NaOH为催化剂，在乙醇-水体系中进行水解-缩合反应，制得了一种疏水性聚十二烷基/甲基倍半硅氧烷纳米杂化材料（PDMSQ NPs）。通过FTIR和XPS对PDMSQ NPs的化学结构进行了表征；用DLS、FE-SEM及 TGA等对PDMSQ NPs的平均粒径、微观形貌和耐热稳定性进行了考察，对其合成工艺条件进行了优化。结果表明，PDMSQ NPs表面C元素含量高达41.73 %，电子结合能103.04 eV处归属为聚倍半硅氧烷中Si 2p的特征峰，PDMSQ NPs为表面含十二烷基和甲基且以Si—O键为骨架的纳米球结构。PDMSQ NPs失重5 %时温度为351 ℃，表明PDMSQ NPs热稳定性优良。FE-SEM分析可知，当反应温度为60℃，n(MTES)∶n(DTMS)=10∶1.0~10∶1.4时，制得的PDMSQ NPs表面光滑、呈单分散性规整球形，水静态接触角最高达168°。提出了PDMSQ NPs的形成机理。

Abstract:

A sort of hydrophobic poly(dodecyl/methylsilsesquioxane) nanoparticles (PDMSQ NPs) were prepared by the hydrolysis-condensation reaction in ethanol/H2O mixed solutions. Methyltriethoxysilane (MTES) and dodecyltrimethoxysilane (DTMS) were used as precursors and sodium hydroxyl as the catalyst. FT-IR and XPS were utilized to characterize the structure of PDMSQ NPs. DLS, FE-SEM and TGA were applied to investigate its average particles size, micro-morphology and thermal stability. Results indicated that the carbon content was highly as 41.73% at the surface of PDMSQ NPs and signal at the binding energy of 103.04 eV was attributed to the characteristic signal of Si 2p from the PSQ. Hence, PDMSQ NPs had the nanosphere structure with Si-O bond as the skeleton and lots of dodecyl and methyl groups at its surface. While the weight loss of PDMSQ NPs was 5% and the corresponding temperature was 351 ℃, this demonstrate that thermal stability of the PDMSQ NPs was excellent. When the molar ratio of MTES to DTMS was amongst 10∶1.0~10∶1.4 and the reaction temperature was 60 ℃, the obtained PDMSQ NPs had the smooth surface with the regularly sperical and monodispersed patterns by the FE-SEM observation. Water contact angle on its surface attained 168° and finally the formation mechanism was also proposed.