以靜電場輔助電鍍具微米構形普魯士藍薄膜之研究

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Title:	以靜電場輔助電鍍具微米構形普魯士藍薄膜之研究
Other Titles:	Study on the electrostatic field-assisted electrodeposition of micropatterned prussian blue thin films
Authors:	丁坤億;Ding, Kuen-Yi
Contributors:	淡江大學化學工程與材料工程學系碩士班林正嵐;Lin, Cheng-Lan
Keywords:	普魯士藍;微米構形;電鍍;靜電場;Prussian blue;micropattern;Electroplating;electrostatic field
Date:	2013
Issue Date:	2014-01-23 14:29:33 (UTC+8)
Abstract:	微米構形 (micropattern) 技術已在各領域的研究與應用上受到廣泛的使用。如在太陽能電池、感測器、發光元件等….而常被用來製作微米構形的方法大致上可分為光微影蝕刻法 (photolithography) 、軟式微影法 (soft lithography) 、反應濕式轉印法 (reactive wet stamping) 、模板法 (templating) 、水相化學成長法 (aqueous chemical growth) 等…由於這些製程往往須經過多個步驟使得製程變得相當繁雜。本研究提出了一項新的技術，於塑膠導電基材上成長微米構形。我們將具有微米構形之靜電膜貼於 ITO/PET 導電基材之導電側，經過接觸後靜電場間接誘發下方 PET 之電性，在 ITO 表面產生分佈不均的微米構形靜電場，而靜電膜移除後因靜電累積在 ITO 表面造成電位的差異。此電位的差異造成在電鍍普魯士藍 (Prussian Blue, PB) 電鍍時沉積速率的不同，因而表面形成普魯士藍之微米構形。此方法應用於導電基材上製作微米構形之相關應用是相當的有前瞻性的。為了解微米構形/聚乙烯之靜電膜 (Micropatterned polyacrylate/polyethylene, MPA/PE) 與 ITO/PET 工作電極接觸所產生相應的電性，Polyacrylic resin / PE靜電膜表面官能基團是一個影響的因素。以顯微拉曼 (Microscopes Raman Spectrometer) 進行選擇區域之官能基測量。並以傅立葉轉換紅外線光譜-衰減式全反射 (FTIR-ATR, Fourier transform infrared spectroscopy-Attenuated Total Reflectance) 進行接觸面之官能基測量。實驗結果發現靜電膜接觸面具有含氧官能基。此屬於在接觸時偏向正電荷之材料。以定電位電鍍法製備普魯士藍微米構形，比較經過接觸起電程序與未經過接觸起電程序之工作電極在電鍍過程中所反應的 i-t 曲線。實驗選擇在不同電位參數下電鍍相同時間。藉由 i-t 曲線之觀察結果判斷每個操作電位在何電鍍時間下可得到較好選擇性之普魯士藍微米構形。以脈衝電鍍法製備普魯士藍微米構形，經由兩種工作電極定電位實驗，以電鍍初始電流密度差值來判斷脈衝電鍍法之最佳 Ed 電位。在此電位下可能得到選擇性較高的普魯士藍微米構形。經由實驗後將 Ed 電位縮小範圍至最適化。將所製作出微米構形之工作電極以光學顯微鏡（Optical microscope, OM）、電子顯微鏡 (Scanning Electron Microscope, SEM) 與表面輪廓儀 ( Surfcorder ) 進行表面的初步觀察與實際的高低差測量。將普魯士藍總膜厚定義為 Tt ( Thickness ) 、微米構形表面之高低差為 ∆T ，將 ∆T/Tt×100% 定義為薄膜之選擇性。藉由比較此值來判斷薄膜之選擇性好壞。在定電位電鍍系統所得到的普魯士藍微米構形，其選擇性隨著電鍍時間的增加而下降。這是因為普魯士藍薄膜的成長由動力控制階段轉變為擴散控制階段造成靜電場的影響力下降，因此欲得到選擇性較高的普魯士藍微米構形必須將電鍍時間控制在短時間內。在0.65V 定電位電鍍下將電鍍時間控制在 15 秒，可以得到94.14%選擇性之普魯士藍微米構形。在脈衝系統上以 Er=0.90V 、 Ed=0.05V 、 tr 與 td 為 0.01s ， 15000 次循環電鍍後，可以得到膜厚達 2 μm 、選擇性高達 92.66% 之普魯士藍微米構形，這成功的克服定電位長時間電鍍下無法得到高選擇性之微米構形。 Micropatterns have been extensively used in many research and application aspects, such as solar cells, sensors, and light emitting devices, etc.. Methods of photoresist lithography, soft lithography, reactive wet stamping, templating, or aqueous chemical growth are commonly employed to prepare micropatterns. These procedures usually consist of multiple steps and are relatively complicate. In this study, a new approach to create micropatterns on conducting plastic substrate is proposed. An electrostatic film with micropatterns (Micropatterned polyacrylate/polyethylene, MPA/PE) is firstly attached onto the conductive side of an ITO/PET conducting substrate. The electrostatic field exhibited between the micropatterned electrostatic film and PET will induced an uneven surface potential distribution on the ITO surface. After the electrostatic film is removed, the remaining surface potential difference might alter the electrodeposition rate of Prussian Blue (PB) at different location on the ITO surface, and thus leading to the formation of a micropatterned PB thin film. This method might find its potential appliactions in preparing micropatterns on conducting substrates. In order to understand the corresponding polarity of charge between Micropatterned polyacrylate/polyethylene and ITO/PET during contact, the functional group of polyacrylic resin / PE of surface is an effective factor. The functional group of selective area is measured by Microscopes Raman Spectrometer. And the functional group of contact surfacre is measured by Fourier transform infrared spectroscopy-Attenuated Total Reflectance. The result of spectrum found that the electrostatic film of contact side possess oxygen-containing functional group. This material tends toward postive charge when it contacts with other substance. The misropattern of Prussian Blue thin film is prepared by potentiostatic method. In comparison, two types of working electrodes show different i-t curve during electrodepostion. One of these working electrodes is attached by electrostatic film, and the other one is not. Experiment is executed by constant potential for same time. Observed that i-t curves response, and determined how long of deposition time can obtain more better selectiveness of micropattern of Prussian blue . The misropattern of Prussian Blue thin film prepare by pulse plating method. Observed the initial current density of i-t curves of two types of working electrodes under potentiostatic experiment, and determined what range of Ed can obtain the best micropattern of Prussian Blue. The resultant micropattern of Prussian Blue have been characterized by means of Optical microscope (OM), Scanning Electron Microscope (SEM) and Surfcorder analysis. The selectivity of micropattern defined formula as ∆T/Tt×100%, where Tt is thickness of Prussian Blue film, ∆T is concave micropattern of height. For the potentiostatic deposition condition, the selectivity of micropattern decreased with the deposition time increaseing. Because the growing process of PB film, from dynamic comtrol change to diffuse control. It caused the effect of electrostatic field decrease when electrodeposition executed. Therefore if the selectiveness want to achieve more better, plating time must be controled in a short time. For example, plated under 0.65V and controled deposition time below 15s, then it can obtain micropattern with selectivity as high as 94.14%. Under the pluse plating system, Electrodeposition cyclig 15000 times with Er=0.90V、Ed=0.05V 、tr and td which are both 0.01s obtain film reaching 2 μm and selectiveness reaching to 92.66%. This resultant sucessfully overcome that long time Electrodeposition can not obtain micropattern of great selectiveness by potentiostatic.
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