臺灣博碩士論文加值系統

靜電紡絲技術係以高分子聚合物材料為導向，配合相應有機溶劑調配出適當紡絲溶液進行奈微米纖維成型的加工技術，其具有低加工成本與材料多樣化等特性；現今研究應用於微生物燃料電池已有跡可循，然僅針對質傳反應的交換膜與極板進行改良，目前研究極少與電芬頓反應相結合進行相關探討。
本研究以聚乙烯醇(polyvinylalcohol, PVA)作為複合極板的高分子聚合物材料，藉由添加石墨烯作為薄膜複合極板的觸媒並以銦錫氧化物(Indium Tin Oxide, ITO)導電玻璃作為複合纖維載台，應用於生物-電-芬頓微生物燃料電池(Bio-Electreo-Fenton Microbial Fuel Cell, BEFMFC)陰極極板，過程進行未添加、2wt%、4wt%、6wt%與8wt%石墨烯添加量，製備複合薄膜纖維極板應用於生物-電-芬頓微生物燃料電池陰極環境當中進行性能探討。
實驗以(1)纖維形貌與狀態，藉由接觸角量測儀對複合纖維親水性進行量測，並透過傅立葉紅外光譜(Fourier Transform Infrared Spectroscopy, FT-IR)對石墨烯與PVA靜電紡絲纖維結合官能基狀態分析；而後以掃描式電子顯微鏡(Scanning Electron Microscope, SEM)與穿透式電子顯微鏡(Transmission Electron Microscopy, TEM)確認靜電紡絲纖維狀態與石墨烯的結合情形。(2)石墨烯複合PVA靜電紡絲層積ITO電極的電化學能力、電阻率與電導度，以四點探針進行石墨烯複合PVA電極電導度量測；由電化學量測儀使用循環伏安法(Cyclic Voltammogram, CV)分析不同電極個別電化學能力。(3)最後測量本研究所製備之複合極板於生物-電-芬頓微生物燃料電池之產電能力；生物-電-芬頓反應效率則藉由偶氮染料(Reactive Black 5, RB5)脫色度分析。
結果顯示，經接觸角親水性量測結果，接觸角隨著石墨烯添加量增加逐漸減小，於8wt%添加量時可達到10.71°，透過傅立葉紅外光譜分析確認石墨烯能成功與PVA結合，且石墨烯添加量其官能基特徵在4wt%時較為明顯。在SEM觀察部分，可發現纖維線徑隨著添加石墨烯含量提升而逐漸減小，當添加8wt%時纖維線徑縮減至103.74nm。電阻率與電導度量測顯示，於8wt%石墨烯添加量具最佳電導度1.46× 10-6(S/m)；於循環伏安法掃描電化學活性分析部分，顯示於4wt%時石墨烯添加量具最佳電化學活性，綜上實驗分析，石墨烯添加量漸增，對於物理層面效果亦有逐漸提升之成效。
在生物-電-芬頓微生物燃料電池中進行系列化電池性能量測；結果顯示，石墨烯添加量為4wt%時之複合ITO極板具有最佳功率密度74.1mW/m2與開路電壓0.42V，循環伏安法分析亦為4wt%石墨烯添加量時具有最佳的氧化還原效果。而在RB5偶氮染料脫色度量測部分，4wt%石墨烯添加量時，系統具有最大脫色率為60.25%；顯示此時生物-電-芬頓反應效率最佳，亦即當石墨烯添加量為4wt%時與PVA具有最佳電化學反應效果。

Electrospinning was based on high polymer material oriented. It is the processing technology to coordinated with the organic solvent and modulate electrospinning solution to make micro fiber even nanofiber, have low processing costs and material characteristics diversification. Nowadays, electrospinning used in Microbial Fuel Cell (MFC) has been tracked in current study. But almost research only modified on proton exchange membrane and electrode plates. Only a few research combined with electro-Fenton-reaction to discuss.
In this study, polyvinyl alcohol (PVA) polymer as a composite plate material by adding grapheme film composite plate as a catalyst and Indium Tin Oxide (ITO) as a composite fiber stage. Used in Bio-Electro-Fenton Microbial Fuel Cell (BEFMFC) system cathode plates by adding 0wt%, 2wt%, 4wt%, 6wt% and 8wt% of graphene to composite with PVA and prepare the electrospinning nanofiber. Discuss with the BEFMFC’s power performance and efficiency of Fenton system.
Experimented with (1)composited fibers morphology and state by contact angle measurement instrument hydrophilic composite fibers were measured. Fourier transform infrared spectroscopy (FT-IR) to analysis the graphene and PVA electrospun fibers functional group binding state, and then to a scanning electron microscope (SEM) and a transmission electron microscope (TEM) to confirm the status of binding with the case of electrospinning PVA composited fibers with graphene. (2) To analysis the graphene/PVA electrospinning laminated ITO composited electrode’s electrochemical capacity, electrical resistivity and electrical conductivity, use the four-point probe measured the electrical conductivity of graphene/PVA composite electrode. Use electrochemical measuring instrument to measuring Cyclic voltammetry (CV) in different individual electrode electrochemical capacity. (3) Finally, a composite measure of the plate prepared in this study on BEFMFC’s Power performance and efficiency of azo dyes(Reactive Black5, RB5) decolorization by bio-electro-fenton system.
The results showed that by measuring the contact angle of the hydrophilic contact angle with increasing graphene additive amount is gradually reduced, at the time 8wt% added amount can be reduced to 10.71 °. Using fourier transform infrared spectroscopy confirmed that graphene can be successfully combined with the PVA and the added amount of graphene characterized its functional group was obvious at 4wt% of graphene. SEM can be observed with the addition of fiber diameter graphene content to enhance and gradually decreased when adding 8wt% fiber diameter can reduced to 103.74nm. Resistivity and the electrical conductivity measured with the 8wt% graphene contents has the best electrical conductance 1.46 × 10-6 (S/m).The CV in electrochemical activity scanning at 4wt% graphene contents have the best electrochemical activity.
BEFMFC in a series of energy measurement showed the composite ITO plate graphene addition amount of 4wt% has the best power density 74.1mW/m2 and the open circuit voltage (OCV) of 0.42V.Cyclic voltammetry analysis has the best effect of also 4wt% amount of graphene. The RB5 decolorization at 4wt% graphene additive amount has the highest rate of 60.25%, showing that bio-electro-Fenton reaction efficiency is best at 4wt% amount of graphene/PVA composited electrode. Also, the graphene addition amount of 4wt% with PVA to produce the composited electrode should has the best electrochemical reaction.

中文摘要............I
Abstract............II
謝誌............IV
目錄............V
圖目錄............VII
表目錄............XI
壹、前言............1
貳、文獻回顧............3
2.1 微生物燃料電池............3
2.1.1微生物燃料電池原理............4
2.1.2微生物燃料電池系統結構............5
2.2電-芬頓系統............6
2.3生物-電-芬頓微生物燃料電池............9
2.4生物-電-芬頓微生物燃料電池影響因素............11
2.4.1微生物燃料電池極板特性............12
2.4.2銦錫氧化物(Indium Tin Oxide, ITO) 導電薄膜............13
2.4.3石墨烯複合電極............14
2.5靜電紡絲(Electrospinnig)............16
參、實驗材料與方法............20
3.1實驗架構............20
3.2實驗材料............21
3.2.1石墨烯複合聚乙烯醇電紡纖維............21
3.2.2微生物燃料電池系統............25
3.3靜電紡絲溶液調配與製程參數............25
3.3.1高分子聚合物溶液調配............25
3.3.2靜電紡絲設備參數............27
3.4微生物-電-芬頓微生物燃料電池實驗前處理與場域建立............29
3.5實驗相關儀器設備............30
3.6.1層積形貌觀察............ 30
3.6.2接觸角............31
3.6.3官能基鍵結............31
3.6.4電極阻抗量測............ 32
3.6.5電化學特性分析............33
3.6.6極化曲線與功率密度............34
3.6.7脫色率............36
3.6.8誤差值(Error Bar)............37
肆、結果與討論............38
4.1不同含量石墨烯複合聚乙烯醇電紡纖維形貌分析............38
4.1.1石墨烯/PVA複合纖維親水性比較............38
4.1.2複合纖維官能基與鍵結............41
4.1.3 PVA複合纖維織構形貌SEM觀察............45
4.2石墨烯複合聚乙烯醇靜電紡絲層積於ITO之電極性能分析............49
4.2.1電阻率與電導度............49
4.2.2循環伏安法............51
4.3石墨烯複合聚乙烯醇靜電紡絲層積ITO電極於生物-電-芬頓系統微生物燃料電池電性分析 ............54
4.3.1功率密度與極化曲線分析............54
4.3.2定電阻放電分析............57
4.3.3脫色率量測............58
伍、結論............60
陸、未來研究方向............61
柒、參考文獻............62

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