首先利用紫外光在充滿氮氣環境中(手套箱)照射交聯,而中性層的產生則是在空氣下照射紫外光獲得,再利用紫外光於空氣中照光,製備具有中性表面之PS層,再利用旋轉塗佈法將dPS-b-PMMA薄膜旋鍍於以紫外光照射交聯及中性化改質之PS層上,接著在真空環境中進行210-280 oC恆溫熱回火。其結果發現在低於270 oC下熱回火,dPS-b-PMMA表面容易形成一層dPS潤濕層,這是由於在此溫度條件下,dPS鏈段及PMMA鏈段之自由表面能()並未相同(即dPSPMMA,非中性表面)。在270 oC恆溫回火,可抑制dPS潤濕層,顯示在此條件下dPSPMMA。此外我們發現在270 oC恆溫回火不同時間,短時間熱回火則形成垂直取向的層板狀結構,而隨著回火時間增加,垂直層板狀轉變為垂直奈米柱狀,最後形成穿孔層狀奈米結構,在此論文中,我們將針對相轉變之機制做深入探討及解釋。 ;In this study, the structural evolution of deuterated polystyrene-block-poly (methyl methacrylate) (dPS-b-PMMA) thin films with thermal annealing of various durations on a layer of UV-irradiated polystyrene were studied by means of atomic force microscopy (AFM), transmission electron microscopy (TEM), grazing incident small-angle X-ray scattering (GISAXS) and neutron reflectivity (NR). Upon exposure to UV light in a glove box and in air, the PS layer was cross-linked and neutralized. dPS-b-PMMA thin films supported on the cross-linked/neutralized PS layer were prepared by spin coating and then the specimens were isothermally annealed at 210280∘C under vacuum. We found that thermal annealing at a temperature below 270 oC would preferentially grew a wetting layer of dPS on top. The formation of the preferential wetting layer is due to the fact that the surface energy (dPS) of the dPS block was not equal to that (PMMA) of the PMMA block. In other words, below 270 oC, the free surface of the dPS-b-PMMA was not neutral. When annealed at 270 oC, dPS-b-PMMA would have a neutral free surface. Besides, we found that 270 oC-thermal annealing of a short period first led to the formation of perpendicular-oriented lamellae. Nevertheless, prolonged thermal annealing produced phase transitions from standing lamellae to vertical nanocylinders and finally to perforated-layer-like nanostructures. In this thesis, we would propose possible mechanisms about the morphology evolution.