本研究針對對稱型超高分子量雙嵌段共聚物薄膜進行熱退火處理,並透過原子力顯微鏡(atomic force microscopy)觀察其缺陷隨退火時間演化行為。實驗結果顯示,受限於高分子高度鏈糾纏性與旋轉塗佈過程中溶劑的快速揮發,僅透過熱退火或使用選擇性溶劑退火難以有效形成層狀結構,最終形成限於動力學控制之相形態與缺陷。相較之下,慢速揮發所形成之塊材(bulk)樣品,經超薄切片處理後可獲得具有缺陷的層板結構,作為後續熱退火觀察之起始態。進一步應用自動化圖像分析技術,輔助一維缺陷辨識,藉由像素連接性將缺陷分為三種基本幾何特徵,分別為點狀(dots)、端點(terminal points)與交會點(junction points),並根據特定的標記組合判定差排(dislocation)與向錯(disclination)。結果顯示,在熱退火過程中,缺陷密度隨時間遞減。此研究成果有助於了解超高分子量系統於熱退火下的缺陷演化機制,並為高分子薄膜中缺陷控制與動力學研究提供重要的基礎。 ;In this study, we conducted thermal annealing on symmetric ultrahigh molecular weight block copolymer thin films and investigated the evolution of structural defects over time using atomic force microscopy. The experimental results revealed that, due to the high degree of chain entanglement and the rapid evaporation of solvent during the spin-coating process, it is challenging to achieve well-ordered lamellar structures through either thermal annealing or selective solvent vapor annealing. Consequently, the morphology becomes kinetically trapped in non-equilibrium states characterized by persistent defects. In contrast, bulk samples prepared through slow solvent evaporation and subsequently sectioned into ultrathin slices can obtain lamellar structures with defects. This method offers a suitable initial state for further thermal annealing analysis. Automated image analysis techniques were employed to detect one-dimensional defects (dislocations and disclinations). By analyzing pixel connectivity, the defects were classified into three fundamental geometric categories: dots, terminal points, and junction points. Specific combinations of these labeled features were then used to identify the presence of dislocations and disclinations. The findings indicated a gradual reduction in defect density throughout the thermal annealing process. This study enhances the understanding of defect evolution mechanisms in ultrahigh molecular weight block copolymers subjected to thermal treatment and provides a foundational framework for the control and management of defects in polymer thin films.