改質奈米二氧化鋯/高分子抗靜電鍍膜之製備與性質研究

Preparation and Characterization of modified nano-zirconia/polymer anti-static coatings

謝致遠(Chin-Yuan Hsieh)

指導教授 ： 鄭廖平

淡江大學/工學院/化學工程與材料工程學系碩士班/碩士(2008年)

https://doi.org/10.6846/TKU.2008.00660

摘要

本研究利用溶膠-凝膠法製備奈米級的改質二氧化鋯粒子，我們將四丙氧基鋯烷(ZNP)與螯合劑甲基丙烯酸(MA)反應後，再加入硝酸水溶液反應三小時後，製備成奈米級的二氧化鋯微粒，接著加入偶合劑三異丙基矽基丙烯酸酯(MSMA)對二氧化鋯微粒進行表面修飾，最後再補入硝酸水溶液反應三小時，使系統反應更趨完整；其後我們將製作完成之溶膠加入DPHA以及光起始劑1173製作成具有抗靜電性的有機-無機奈米混成塗料。
製程中反應時間的選擇以及化學結構的檢測，我們利用FTIR、動態光散射粒徑分析儀、固態29SiNMR進行分析。在複合材料方面我們利用SEM觀測薄膜是否在製作過程中有聚集的現象，熱性質方面利用TGA檢測溶膠的添加對於高分子薄膜的熱性質影響。
最後我們利用三成份ZNP、MA以及MSMA之間不同比例的調配，製作成三成份圖，測試各比例成膜後之機械性質(密著、硬度)以及表面電阻，在其間找出使複合薄膜展現出最好之機械性質以及最佳抗靜電性的比例。
實驗結果顯示，經過修飾之二氧化鋯微粒，能使其在溶膠狀態中分散良好，製作塗料的過程中也不會產生物理性的聚集，藉由三成份圖的選擇，我們找出了具有良好機械性質之塗料比例，而製成之塗料也達到了市售靜電消散材料的標準。

關鍵字

奈米二氧化鋯 ； 溶膠凝膠程序 ； 抗靜電 ； 有機無機混成複合材料

並列摘要

This study demonstrated the production of modified nano-zirconia by utilizing the Sol-Gel Process. The nano-zirconia was formed by reaction of zirconium-n-propoxide (ZNP) with chelating agent methacrylic acid (MA) first, followed by addition of nitric acid and reaction for three hours. The formed nano-zirconia was then modified by using coupling agent 3-(trimethoxysilyl) propyl methacrylate (MSMA). Additional nitric acid was finally added and the reaction was allowed to proceed for another 3 hours to assure the completeness of the reaction. The anti-static organic-inorganic nano hybrid coatings were produced from the formed sol by adding DPHA and photoinitator darocure 1173.

In this research, we used FTIR, dynamic light scattering particle size analyzer and solid-state 29SiNMR to determine the appropriate reaction time and to analyze the chemical bonds; SEM to observe whether aggregation has occurred in the hybrid material ;TGA to examine the effect of inorganic component on the thermal property of the hybrid material.

In addition, we used the mixture of ZNP, MA and MSMA in different ratios to create a ternary composition diagram. Based on this diagram,we checked the physical properties (adhesion and hardness test) and surface resistivity hybrid materials with various ratios ZNP,MA, and MSMA to find out the most appropriate ratio to produce a hybrid membrane having the best mechanical and anti-static properties.

The experimental results indicated that modification of nano-zirconia by MSMA has made it possible to distribute properly in the sol and also avoid the physical aggregation during the proportion of nano-hybrid coatings. We have found out the proper ratios from the ternary composition diagram for preparing hybrid materials with good physical properties. The produced coating material has also reached the market standard for static dissipative materials.

並列關鍵字

nano-zirconia ； sol-gel process ； anti-static ； organic-inorganic hybrid

參考文獻

22. 陳建銘，溶膠凝膠法製備紫外光硬化型抗眩鍍膜，淡江大學化學 工程與材料工程學系碩士論文 (2007)。

39. 歐陽岱岳，改奈米二氧化矽/高分子複合材料之製備與物性分析， 淡江大學化學工程與材料工程學系碩士論文 (2006)。

56. S. A. Halperin, “Guidelines for Static Control Management,” Eurostat., (1990).

41. Michael Mager. Markus Mechtel. Stephan Kirchmeyer silicones in coatingsⅡ. New Polyfunctional Silanols in Sol-Gel synthesis。

31. Yen Wei, Wei Wang, Jui Ming Yeh, et al. Polym. Mater. Sci.Eng.(1994).