本研究旨在進行高溫質子交換膜燃料電池觸媒層之系統性製程最佳 化。研究重點探討氣體擴散層碳基材類型(碳纖維基碳紙與碳纖維編織 布)、白金(Pt)與聚苯並咪唑(PBI)滴塗順序(Pt Before PBI 與 Pt After PBI)、 PBI 包覆厚度、溶劑烘乾溫度及熱處理條件之協同影響,並 結合交流阻抗譜與弛豫時間分佈進行阻抗分量解耦與傳輸機制分析。 研究結果表明,在基材選擇上,具備良好柔韌特性之碳纖維編織布能 有效改善界面接觸,將歐姆阻抗下降 40%,帶動電流密度提升 52%。在 滴塗順序方面,採行 Pt Before PBI 順序可確保白金與碳基材建構直接電 子傳導路徑,使其電荷轉移阻抗較 Pt After PBI 降低 44.5%。此外,經過 熱處理後,能促使高分子充分弛豫並均勻鋪展,有效避免觸媒活性位點遭 封閉與劇烈熱收縮現象。歸納本研究所確立之最佳化製程(採用碳纖維編 織布、Pt Before PBI 滴塗、25 nm PBI 厚度、85 °C 烘乾及 270 °C 與 30 分鐘熱處理、總鉑用量0.2 mg/cm2),於140 °C、0.60 V條件下其電流密度 可達 60.6 mA/cm²。;This study presents a systematic process optimization for the catalyst layers in HT-PEMFCs. We investigate the impacts of gas diffusion layer substrates (carbon paper vs. woven carbon cloth), platinum (Pt) and polybenzimidazole (PBI) deposition order (Pt Before PBI vs. Pt After PBI), PBI coating thickness, solvent drying temperature, and heat treatment parameters. Electrochemical impedance spectroscopy (EIS) coupled with the distribution of relaxation times (DRT) was employed for impedance deconvolution and transport mechanism analysis. Results demonstrate that the high flexibility of woven carbon cloth enhances interfacial contact, yielding a 40% reduction in ohmic resistance and a 52% enhancement in current density. Implementing the Pt Before PBI deposition sequence establishes a direct electron transport pathway between Pt nanoparticles and the carbon matrix, lowering charge transfer resistance by 44.5% relative to the Pt After PBI configuration. Additionally, thermal post-treatment induces polymer chain relaxation and uniform coverage, suppressing both active site blockage and severe thermal contraction. Under the optimized conditions (woven carbon cloth, Pt Before PBI deposition, 25 nm PBI thickness, drying at 85 °C, heat treatment at 270 °C for 30 min, and a total Pt loading of 0.2 mg/cm2), the cell achieves a current density of 60.6 mA/cm2 at 140 °C and 0.60 V.