磺酸化氧化石墨烯接枝鹼金屬離子薄膜應用於質子傳導

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研究生：	楊若綺 Jo-Chi Yang
論文名稱：	磺酸化氧化石墨烯接枝鹼金屬離子薄膜應用於質子傳導 Sulfonated Graphene Oxide Grafted with Alkali Metal Ions Membranes in Proton Conductivity
指導教授：	洪維松 Wei-Song Hung
口試委員:	胡蒨傑 Chien-Chieh Hu 林嘉和 Chia-Her Lin
學位類別：	碩士 Master
系所名稱：	應用科技學院 - 應用科技研究所 Graduate Institute of Applied Science and Technology
論文出版年：	2023
畢業學年度：	111
語文別：	中文
論文頁數：	68
中文關鍵詞：	磺化氧化石墨烯、質子交換膜、鉀離子傳導膜、高電導率傳導膜、電解水產氫氣
外文關鍵詞：	sulfonated graphene oxide, proton exchange membrane, potassium ion-conductive membrane, high conductivity membrane, electrolytic hydrogen production
相關次數：	點閱：327 下載：0
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隨著科技不斷地創新進步，能源的需求也日益增加，為了減緩地球能源之耗竭，並改善日漸嚴重地環境汙染問題，各國開始提倡綠色能源，以潔淨能源產氫氣，以實現永續發展之目的，而產氫方式中又以水電解法最為出眾。本研究將碘化物氧化反應（Iodide oxidation reaction, IOR）來取代並優化傳統水電解之析氧反應（Oxygen evolution reaction, OER），此種方法為一種高值化產氫系統，在系統中之陽極使用碘化鉀溶液來進行碘離子氧化反應（IOR），同時結合陰極進行水的電解產氫氣。相對於傳統的電解水產氫氣方法，優化水電解法在相對較低的電位差（1.07伏特）下進行反應，這一優勢可以提高能量轉換效率，同時，除了產生氫氣作為潔淨能源，還能產生具有高附加價值的碘，從而提高整個系統的經濟效益和能源利用率。
目前最常見被使用於水電解法產氫氣之薄膜：Nafion系列作為代表，由於此類薄膜為一種相對昂貴的材料，其生產成本較高，且在製造過程可能涉及氟化物等一些環境不友好的化學物質和工藝，因此，本研究製作一種應用於氫能源之親水磺化氧化石墨烯薄膜，以具有高鉀離子傳導能力、尺寸安定性以及於電化學系統穩定性的鉀離子傳導膜為目標。實驗步驟首先先將氧化石墨烯以硫酸和甲醇改質成磺化氧化石墨烯，此外，也將磺化氧化石墨烯分別以氫氧化鋰、氫氧化鈉、氫氧化鉀改質接枝上鋰、鈉、鉀離子，以不鏽鋼壓力輔助自組裝裝置（Pressure-assisted self-assembly technique）製作成薄膜並將其分別命名為GO、GO-SO3H、GO-SO3Li、GO-SO3Na、GO-SO3K。本研究先利用ATR-FTIR以及EDS來確認磺酸根官能基以及正一價金屬離子的接枝情形，再以SEM和AFM來觀察薄膜表面型態與物理結構鑑定；以XRD了解接枝磺酸根官能基、不同正一價金屬離子對於GO奈米片層間距之影響；使用WCA來確認薄膜之親疏水性，同時測量了薄膜之膨潤度與吸水率。在效能的部分，以EIS 進行薄膜電性分析，發現GO-SO3K具有最佳的質子傳導率119.16 mS；於鉀離子傳導度方面，GO-SO3K之效能也以43 mg/L最為突出。而於穩定性方面，在電化學系統中，GO系列之薄膜皆具有良好之穩定性。
結合各種效能結果與各項不同鑑定，GO-SO3K薄膜將有做為鉀離子傳導膜之潛力。

With the continuous innovation and progress of technology, the demand for energy also increases. In order to mitigate the depletion of earth's energy and address the increasingly severe environmental pollution problems, countries are advocating for green energy. Hydrogen production through clean energy source is being promoted to achieve sustainable development, with water electrolysis being the most prominent method. In this study, the iodide oxidation reaction (IOR) is proposed as a replacement and improvement on the traditional oxygen evolution reaction (OER) in water electrolysis. This method is a high-value hydrogen production system, where the anode utilizes a potassium iodide solution for iodide ion oxidation reaction (IOR), while hydrogen gas is simultaneously produced at the cathode through water electrolysis. Compared to the conventional electrolytic hydrogen production method, the optimized water electrolysis operates at a relatively low potential difference (1.07 V), resulting in higher energy conversion efficiency. Aside from besides generating hydrogen gas as a clean energy source, the process also produces valuable iodine. This enhances the economic benefits and energy utilization efficiency of the entire system.
Currently, the most commonly used membrane in water electrolysis for hydrogen production is the Nafion series, which has a relatively high production cost. Additionally, the manufacturing process may involve harmful chemicals such as fluoride. Therefore, this study aims to develop a hydrophilic sulfonated graphene oxide (GO-SO3H) membrane for hydrogen energy applications, targeting a potassium ion-conductive membrane with high potassium ion conductivity, dimensional stability, and electrochemical system stability. The experimental procedure involves modifying graphene oxide with sulfuric acid and methanol to obtain sulfonated graphene oxide. Furthermore, sulfonated graphene oxide is separately modified and grafted with lithium hydroxide (LiOH), sodium hydroxide (NaOH), and potassium hydroxide (KOH) to introduce lithium, sodium, and potassium ions, respectively. Using a stainless-steel pressure-assisted self-assembly technique, thin membranes are prepared from the modified sulfonated graphene oxide and named GO, GO-SO3H, GO-SO3Li, GO-SO3Na, and GO-SO3K, respectively. The study confirms the grafting of sulfonic acid groups and monovalent metal ions using attenuated total reflectance Fourier-transform infrared spectroscopy (ATR-FTIR), while scanning electron microscope (SEM) and atomic force microscopy (AFM) are used to observe the surface morphology and physical structure of the membranes. X-ray diffractometer (XRD) is employed to understand the effects of grafted sulfonic acid groups and different monovalent metal ions on the interlayer spacing of GO nanosheets. The water contact angle (WCA) is measured to determine the hydrophilicity of the membranes, and the swelling degree and water uptake are also evaluated. In terms of performance, electrochemical impedance spectroscopy (EIS) is conducted to analyze the electrical properties of the membranes. The results show that GO-SO3K exhibits the highest proton conductivity of 119.16 mS, and in terms of potassium ion conductivity, GO-SO3K performs the best with a concentration of 43 mg/L. Regarding stability, all GO series membranes exhibit good stability in the electrochemical system.
Combining the various performance results and different characterizations, the GO-SO3K membrane shows potential as a potassium ion-conductive membrane.

摘要     I
Abstract III
致謝     V
目錄     VI
圖目錄     IX
表目錄     XI
第一章    緒論    1
第二章    文獻回顧    3
1    潔淨能源    3
2    產氫方式    4
2.1    化石燃料熱分解（Thermal decomposition of fossil fuels）    4
2.1.1    烴類重整法（Hydrocarbon reforming）    4
2.1.2    烴類熱裂解法（Pyrolysis）    5
2.2    水電解（Water Electrolysis）    6
2.2.1    水電解法    6
2.2.2    優化水電解法    7
2.3    生物分解（Biohydrogen）    7
2.3.1    發酵產氫（Photofermentation）    7
2.3.2    光合產氫（Biophotolysis）    7
2.4    太陽能光解（Solar Photolysis）    8
2.4.1    光熱水分解（Thermochemical Water Splitting）    8
2.4.2    光電化學水分解（Photoelectrochemical Water Splitting）    8
3    離子交換膜    10
3.1    理想離子交換膜    10
3.2    常見離子交換膜    11
3.2.1    由氟系高分子組成    11
3.2.2 由碳氫系高分子組成    13
3.3    離子交換膜機制    14
3.3.1    吉布斯-唐南效應（Gibbs–Donnan effect）    14
3.3.2    擴散效應（Diffusion effect）    14
3.3.3    吸附/脫附（Adsorption/desorption）    15
3.4    磺化氧化石墨烯作為離子傳導膜    16
第三章    實驗材料與方法    17
1    實驗藥品    17
2    實驗儀器與設備    18
3    實驗步驟    19
3.1   氧化石墨烯之製備    19
3.2    磺酸化氧化石墨烯之製備    20
3.3    磺酸化氧化石墨烯接枝一價離子之合成    21
3.4    氧化石墨烯系列之薄膜製備    22
4    薄膜之鑑定    23
4.1    衰減全反射式傅立葉紅外光譜儀（ATR-FTIR）    23
4.2    X射線能量散布分析儀（EDS）    23
4.3    場發射掃描電子顯微鏡（FESEM）    24
4.4    原子力顯微鏡（AFM）    25
4.5    X光繞射儀（XRD）    26
4.6    水接觸角（WCA）    27
4.7    薄膜之膨潤度與吸水率之量測    28
4.8    電化學交流阻抗    29
4.9    離子滲透裝置    30
4.10    電化學系統及測試    31
第四章    結果與討論    32
1    磺酸化氧化石墨烯薄膜之鑑定與分析    32
1.1    氧化石墨烯磺酸化之薄膜鑑定    32
1.2    接枝一價離子磺酸化氧化石墨烯薄膜之鑑定    33
1.3    薄膜之表面型態與粗糙度分析    35
1.4    薄膜層間距之變化    39
1.5    薄膜之表面親疏水性分析    40
1.6    薄膜之尺寸安定性與吸水率    42
2    磺酸化氧化石墨烯之效能檢測    43
2.1    薄膜之質子傳導度    43
2.2    鉀離子傳導度    45
2.3    電化學以及穩定性測試    46
第五章    結論    47
參考文獻    48
                                

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全文公開日期 2028/08/17 (校內網路)
全文公開日期 2028/08/17 (校外網路)
全文公開日期 2028/08/17 (國家圖書館：臺灣博碩士論文系統)

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