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适合紫外/可见光反应的全聚合物微流体反应器制备金纳米粒子的研究

Preparation of Gold Nanoparticles in a Complete Polymeric Microfluidic Reactor under UV Irradiation

【作者】 商运生

【导师】 杨万泰;

【作者基本信息】 北京化工大学 , 材料科学与工程, 2010, 硕士

【摘要】 以PMMA为基体,通过对SU-8 2075光刻工艺中旋涂、前烘、曝光、后烘、显影等参数的优化,制备出厚度达500μm的全聚合物微流体反应器。同时提出了一种新型光刻工艺,即根据光刻胶固化收缩率,取定量光刻胶,用特氟龙刮刀铺展开,绕开旋涂,直接进行前烘、曝光、后烘、显影,制成具有特定厚度的全聚合物微流体反应器。然后使用旋涂了UV快速固化胶(SE-1)的BOPP膜对其进行封盖。实现了流道内无阻塞,且显著地改善了微反应器顶部的透光性,特别适合进行紫外/可见光反应。利用该微反应器,在紫外光照射下制备了金纳米粒子。采用紫外-可见吸收光谱、激光粒度分析仪、透射电镜等对柠檬酸钠-氯金酸微流体光化学反应体系进行了表征。考察了注射泵的流速、柠檬酸钠/氯金酸的浓度比和紫外光辐射强度对金纳米粒子紫外-可见光吸收峰强度和粒径大小的影响。结果表明,金纳米粒子的紫外-可见光吸收峰强度随注射泵流速的增大而增强,但是随柠檬酸钠/氯金酸浓度比的增大和紫外辐射强度的增强而减弱。金纳米粒子的粒径随注射泵流速的增大和紫外辐射强度的增强而减小;但是金纳米粒子的粒径在柠檬酸钠/氯金酸浓度比小于16时,变化不大;当柠檬酸钠/氯金酸浓度比大于16时,其迅速增大。

【Abstract】 A complete polymeric microfluidic reactor with 500μm depth was fabricated by optimization of SU-8 2075 photolithography parameters such as spin coating, soft baking, exposure, post exposure baking, and development. A new photolithography technology was developed. According to curing shrinkage rate of SU-8 2050, a fixed amount of SU-8 2050 was taken out and spread around to the edge of PMMA substrate by a Teflon scraper. A microfluidic reactor with fixed channel depth was fabricated through soft baking, exposure, post exposure baking, and development without spin coating. Then a piece of hydroxylated BOPP film, on which SE-1 was coated, was used to seal the microfluidic structure. There was no blockage in the microchannel and the top transparency which was very useful and critical for photoreaction was significantly improved.Gold nanoparticles were synthesised in the complete polymeric microfluidic reactor under UV irradiation. The gold nanoparticle dispersions prepared by photoreaction of sodium citrate with chloroauric acid in aqueous solution were characterised by UV-vis adsorption spectrum, laser particle size analyzer and transmission electron microscope (TEM). The effects of process factors, such as flow rates of reactants, [sodium citrate]/[HAuCl4] and UV light intensity, on UV-vis adsorption intensity and diameters of gold nanoparticles were investigated. The results showed that the UV-vis absorption intensity of gold nanoparticles increased as flow rates increased, but decreased as [sodium citrate]/[HAuCl4] increased and UV light intensity increased. The diameter of gold nanoparticles decreased as flow rates increased and UV light intensity increased. At low [sodium citrate]/[HAuCl4] (<16), with its increasement the size of nanoparticles changed a little. However, at higher [sodium citrate]/[HAuCl4] (>16), the diameters of the obtained gold nanoparticles increased with the increasement of [sodium citrate]/ [HAuCl4].

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