本研究以電紡絲製備之奈米碳纖維作為基材，再以水熱法將鎳鈷前驅物沉積於碳纖維表面，經熱處理後形成鎳鈷氧化物/奈米碳纖維複合膜，作為鋰離子電池負極電極材料，我們對製程條件和物化性質進行分析，探討複合膜微結構對於電化學表現上之影響。透過改變鎳鈷前驅物濃度，以及添加乙醇改變水熱法之溶劑環境，並經過熱處理後，得到不同形貌的鎳鈷氧化物/奈米碳纖維複合膜。我們發現，針狀結構Ni(OH)2/Co(OH)2的形成是由於較快的反應速率，鎳鈷前驅物隨著反應進行，鎳鈷離子濃度下降，使得成長中的晶體沉積平面不斷限縮，最後形成針狀；片狀結構Ni(OH)2/Co(OH)2的形成，是因為乙醇的添加及較高鎳鈷離子濃度，使沉積反應速率下降，因為鎳鈷離子消耗速率較慢，沉積平面較不易受到限縮，最終生長成完整片狀結構。我們以針狀結構、片狀結構和不規則形狀的三種鎳鈷氧化物/奈米碳纖維為探討重點，組裝成鋰離子半電池，並進行變電流充放電及循環壽命測試。針狀結構之鎳鈷氧化物/奈米碳纖維複合膜在電流密度為150 mA/g時，具有539 mAh/g之放電比電容量。針狀結構之鎳鈷氧化物/奈米碳纖維複合膜也展現良好之循環表現，經過100圈充放電後，與第二次放電比電容量相比，其比電容殘留率仍達90.5%。由於針狀結構具有較大比表面積和中孔孔洞體積，在鋰離子電池充放電時，電極材料與電解液有更大接觸面積以及有利於鋰離子之儲存和傳遞，並有較多的體積膨脹彈性空間，較不易造成結構破壞，提升整體複合膜之穩定性。
 
我們亦合成氫氧化鎳/奈米碳纖維複合膜，作為超級電容器電極材料，透過改變碳化程序，得到不同碳化時間之奈米碳纖維，再進行氧電漿表面改質，並以水熱法沉積氫氧化鎳於碳纖維表面。碳化時間1小時之氫氧化鎳/奈米碳纖複合膜經由掃描速率2 mV/s之循環伏安測試，展現最佳比電容值1322 F/g。藉由交流阻抗測試，對不同碳化時間氫氧化鎳/奈米碳纖維複合膜進行分析，可以發現隨著碳化時間上升，電子轉移阻抗增加，因此電容表現下降。透過XPS分析複合膜C 1s軌域可以發現，碳化時間1小時的複合膜具有最高C-O-比例，其可視為氫氧化鎳與碳纖維之錨點，且C-O-能有效傳遞法拉第反應之電子，其比例越高，電子轉移阻抗越低，提升電化學反應之表現。

In this study, electrospun carbon nanofibers (CNF) served as a template. Subsequently, a hydrothermal approach was carried out to deposit the Ni/Co precursor on the fiber surface. We varied the processing conditions, and investigated how the different morphologies affected the electrochemical performance of the composites. We varied the concentration of precursors and manipulated the reaction environment through the addition of ethanol in water. After thermal treatment, NiCo2O4/CNF composites with different morphologies were obtained. We assembled the NiCo2O4/CNF composites with three types of morphologies as half-cells for lithium-ion battery. Galvanostatic charge-discharge tests revealed that the needle-like NiCo2O4/CNF composite delivered the specific capacity of 539 mAh/g at a current density of 150 mA/g. The composite also exhibited a capacity retention of 90.5% at the 100th cycle in relation to the second cycle, suggesting its favorable reversibility. This was attributed to the high specific surface area and rich mesopores in the needle-like NiCo2O4/CNF composite, thereby facilitating lithium-ion transport across the electrolyte/electrode interface and lithium-ion storage.
We also fabricated Ni(OH)2/CNF composites, which were used as supercapacitor electrodes. We treated CNF with different carbonization time, and the resulting CNF were surface modified with the oxygen plasma. Subsequently, a hydrothermal method was conducted to deposit Ni(OH)2 on the surface of fibers. The Ni(OH)2/CNF composite with the carbonization time of 1 h exhibited the highest specific capacitance of 1322 F/g at a scan rate of 2 mV/s. Electrochemical impedance spectroscopy revealed that the charge-transfer resistance of the Ni(OH)2/CNF composites increased with an increase in the carbonization time, causing a decrease in the specific capacitance.

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