本研究分別從質子交換膜燃料電池觸媒層之界面工程與結構工程兩大方向進行優化,以提升觸媒層之電化學耐久性與單電池輸出性能。 在界面工程方面,利用化學浴沉積與電沉積於多孔碳球殼表面導入 TiO2 保護層,並系統性調控熱處理順序與氣氛(Air、Ar、Ar/H2)。實驗結果顯示,適量的 TiO2 可提供良好的 Pt 錨定位點:採用乙醇輔助電沉積並結合 Ar 氣氛預熱處理,ECSA 保持率可達 57.8%;經 2.5 min CBD 改質後,再經由 Ar/H2 還原熱處理,推測誘發強金屬-載體交互作用,使 ECSA 保持率達到最高的 63%。 在結構工程方面,採用 PMMA與SiO2 雙模板法建立連通型多孔碳球殼載體。研究發現,當 SiO2 與 PMMA 之體積比為 7:3 時,可建立最佳化之開放性孔隙骨架,使 Pt 奈米顆粒均勻分散,平均粒徑維持於 3.06 nm。進一步針對Nafion功能層進行參數優化,最佳配方為:無退火、7.8 wt% 正丙醇前驅液及 2000 nm 等效厚度。在此條件,單電池於 60 °C、一大氣壓之常壓操作下,0.6 V 條件之電流密度達 1228 mA/cm2。 綜上所述,TiO2 界面改質可提升觸媒之電化學耐久性,而 PMMA 雙模板孔隙工程與 Nafion 於微結構分布調控則可提升單電池性能,本研究結果可作為後續開發 low-Pt 觸媒層之參考。;This study optimizes the PEMFC catalyst layer via interfacial and structural engineering to enhance Pt durability and single-cell performance. For interfacial engineering, a TiO2 layer was deposited onto porous carbon shells via chemical bath deposition (CBD) and electrodeposition, with thermal sequence and atmosphere (Air, Ar, Ar/H2 ) systematically controlled. Results show that TiO2 provides effective Pt anchoring sites: ethanol-assisted electrodeposition with Ar pre-thermal treatment achieved 57.8% ECSA retention, while 2.5 min CBD with Ar/H2 reduction reached 63% retention, likely induced by strong metal–support interactions (SMSI). For structural engineering, a PMMA/ SiO2 dual-template method constructed interconnected porous carbon shells. A SiO2/PMMA ratio of 7:3 yielded an optimal porous framework with an average Pt particle size of 3.06 nm. Optimizing Nafion (unannealed, 7.8 wt% n-propanol, 2000 nm thickness) achieved a single-cell current density of 1228 mA/cm² at 0.6 V (60 °C, 1 atm). In summary, TiO2 modification improves durability, whereas PMMA pore engineering and Nafion control enhance performance, offering a valuable reference for low-Pt catalyst layer design.