金屬氧化物半導體因其物理特性如：能隙、光學反饋等而被廣泛應用於學術及工業領域。其奈米結構在近年更被大量使用於光電、感測之研究中。對奈米結構而言，電性以及表面形貌的量測可探測的物理現象相對光學量測較少，如結構變遷及化學態的轉換。故光學量測常為奈米結構物理化學性質之主要量測方法。然而當尺度縮小，體效應隨之降低，表面效應相對增大，使得光學量測也面臨瓶頸。奈米結構表面之物理特性如：位能障等皆與體內不同，導致表面與體的電子組態、原子結構經後處理後有所不同。因此，光學量測之結果隨表面效應增強而不易辨別表面貢獻及體貢獻，進而使物理模型含糊。再者，化學態之量測結果也因此而無法精確定位。綜上所述，光學量測之探測深度越顯重要。此研究引入多光學方法，藉由組合各工具所得資訊，考量其探測深度，以建立微觀動態模型。多光學方法對奈米結構具高度適應性，配合樣品需求選擇合適之光學量測，我們將研究其應用在氧化鋅、硼摻雜矽及硼摻雜矽鍺三種材料，並建立其熱處理的動態模型。氧化鋅奈米結構中，藉由溫度掃描退火處理，在多種深度製造多種表面狀態以驗證多光學方法對探測深度之精準度；同時以實驗方法探究缺陷之遷移能障並且建立退火造成的遷移模型；另一方面，利用高溫真空退火，完成自組成氧化鋅奈米柱之表面狀態規一化；並定義氧分子在退火處理中，不僅能修復氧空缺，同時亦在表面製造新的缺陷；氧氣在氧化鋅薄膜表面之物理、化學吸附亦為本研究的一大重點，我們發現藉由脈衝雷射及紫外光照射，可引發氧分子的物理及化學脫附。此發現更進一步使用臭氧–紫外光法對表面改質，以驗證表面品質與吸附比例之關係。在硼摻雜矽薄膜研究中，多光學方法因其探測深度的優勢而提供比傳統量測方式更精確之表面品質鑑定，並確立高能量離子佈植之最佳離子束電流；在硼摻雜矽鍺薄膜研究中，多光學方法提供良好的品質鑑定，並驗證硼除了提供載子，同時也參與矽鍺結構變遷；適量的硼可穩定結構，避免鍺聚集、硼堆疊等缺陷產生。我們相信，當電子元件的尺度持續縮小，除製程技術需求增加以外，檢測能力也須同步提升。本研究展現了多光學方法的高度適應性及實用性，尤其對於樣品表面探測深度的高解析能力更是其優勢，我們認為對於新一代奈米結構的物理化學特性探測，多光學方法可提供重要貢獻。

Metal oxide semiconductors are widely studied in the field of academy and the industry due to the variant physical properties such as the band gap and the optical response. Their nanostructures are widely applied on photonics and sensors in the recent years. Since the measurements of the electric properties and the TEM provide less information about the structural evolution and the variation of chemical states, the optical measurements are more suitable and often applied on physical and chemical properties of metal oxide semiconductors nanostructures. However, when the structure scales down, the surface effect is relatively enhanced so that the obstacles occur. For example, the migration energy barrier is different between the surface and bulk region. It becomes difficult to separate their contributions, which would lead to the confusion of the physical characteristics. Furthermore, the chemical interaction become not easy to distinguish between surface and bulk region. As the result, the depth–resolved optical measurements is the crucial and key approach. In this thesis, multi–optical methods, which combine the optical analyses with proper depth–resolution and described the dynamics, are proposed and demonstrated. The multi–optical methods show high adaptability by choosing suitable optical measurements for ZnO, B–doped Si (BS), and B–doped SiGe (BSG) nanostructures. In the ZnO nanorods (ZNRs), by scanning the annealing temperature and duration, the depth–dependent surface states were generated in different depth in order to demonstrate the resolution of optical probing depth. The migration energy barriers were approached by the experimental methods; on the other hand, by the high temperature annealing treatments in the vacuum, we accomplished the normalization of ZNR surface. The extrinsic oxygen molecules not only repaired the vacancies but also generated additional defects on ZNR surface; The physical and chemical oxygen adsorption are key issues to study in our research as well. By using the pulsed laser and UVA irradiation, the physical and chemical desorption can be induced. Namely, the physical and chemical adsorption could be identified and separated in the measured optical signals. Furthermore, the UVC–ozone method was applied to modify the ZnO surface so that the correlation between the surface composition and the oxide adsorption was verified. In the BS thin film, the multi–optical methods provided more surface sensitive analyses than the traditional measurements due to the limitation of optical penetration depth. The optima conditions of beam currents during the implantation processes were determined as well. In the BSG thin films, the multi–optical methods verified that the B atoms not only provided the carriers but also participated the structural evolution. When the semiconductor nanostructure scales down, not only the fabrication technology need to be improved, but also the technique of surface characterization shall also be promoted. In this thesis, the multi–optical methods demonstrate high adaptability, practicality, and the advantages of the depth–resolution. We believe that the multi–optical methods will play an important role in the development of next generation of semiconductor nanostructures.

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