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標題: 鋅系列奈米光電薄膜機械性質研究
Zinc series nanometer electro-optic thin film mechanical property research
作者: 姚威宏
Yau, Wei-Hung
關鍵字: 氧化鋅;ZnO;奈米壓痕;奈米刮痕;機械性質;Nanoindentation;Nanoscratch;Mechanical Property
出版社: 機械工程學系所
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在寬能隙II-VI族半導體材料中,氧化鋅(ZnO)具有良好光電以及化學特性,使得氧化鋅可廣泛應用並具有相當發展性之半導體材料,欲使氧化鋅成功地導入半導體元件製作過程,需要徹底了解其機械與光學特性。而氧化鋅可藉由伴隨錳(Mn)等摻雜、硒(Se)化合物的合成,達到其調控光能階之特性,進而有效運用於光學元件等場合。本論文透過奈米壓痕、奈米刮痕探討其系列氧化鋅特性的影響,藉由深度感測技術(Depth Sensing Technique),可同時記錄量測過程中壓痕負載與壓痕深度的關係,藉由所得關係圖,來分析系列氧化鋅薄膜之硬度與楊氏模數機械性質。在奈米尺度結構下,系列氧化鋅化合物試片,實驗觀察到其產生之差排將對應楊氏模數與硬度值,進而評估機械可靠度特性,此有助於探討光學元件壽命與使用周期之評估,以下實驗將氧化鋅試片系統性分成幾個主題,討論如下:
(i)本研究使用物理氣相沉積法在藍賽克基材上成長氧化鋅薄膜,其成長功率由100到200瓦特過程,薄膜厚度由0.3增加到1.2微米,X光繞射分析當薄膜厚度增加造成其主要波峰為C軸面(002)主導,電子顯微鏡分析其結構主要為柱狀晶,氧化鋅會隨厚度增加而持續增加密度,此肇因於氧的化學性吸附與成長,實驗建議當高瓦特數的濺鍍過程會造成原子離子化轟擊,而有助於成核與成長,其中鋅與氧鍵結,可藉由高瓦特數的濺鍍過程獲得提升,實驗中使用奈米刮痕系統,對氧化鋅薄膜進行磨擦破壞實驗,探討氧化鋅薄膜所產生的晶格錯位與疊差對物理機械特性的影響,例如表面粗糙度 (11.3, 14.5, 16.5 奈米)與摩擦係數(0.1 ± 0.01, 0.175 ± 0.01, 0.183 ± 0.02)隨瓦特數(100, 150, 200 瓦特)增加而增加,其後,並使用X光電子能譜儀系統量測氧化鋅薄膜表面激發光特性的改變,其中濺鍍功率於100瓦特時:氧(O 1s)從529.4 eV波峰可歸因於氧鋅鍵結提升,而531.0 eV波峰可歸因於氧氫鍵結形成,功率於150瓦特時: 530.5 eV波峰可歸因於氧鋅鍵結整合與提升,從而讓氧鋅鍵結主導整個成長過程濺鍍功率的變化,此結果更進一步確認氧化鋅薄膜結構的鍵結轉換貢獻機制。
(ii) 本研究使用陰極光偵測系統探討單晶硒化鋅在受到奈米壓痕負載後之陰極發光特性,陰極光譜圖中得知單晶硒化鋅具有較偏(1.8–2.4 eV)與接近能帶之波峰(2.68 eV) ,而在陰極光譜圖中,能量降低是由於在奈米壓痕連續四次負載/卸負載過程中對硒化鋅造成晶格缺陷及衍生。這些缺陷與微裂痕藉由穿透式電子顯微鏡與陰極光譜圖轉換分析,最後得知壓痕連續四次負載/卸負載過程,將導致大量缺陷衍生進而造成壓痕曲線滯後的現象,從而了解硬度與楊氏模數對應光學特性的影響。硒化鋅不僅提供機械特性並且可以陰極光偵測之光學來分析,從而以陰極光譜圖證實薄膜受破壞後的非幅射發光中心機制,尤其是電子經由不同種類之缺陷產生的過渡能階,故而此技術可進而提供化學或物理特性判斷。

Zinc oxide (ZnO) has emerged as a well candidate because of its large band gap and large excitation binding energy. ZnO thin films are mainly used as transparent conductive films in solar cell windows. The successful fabrication of semiconductor devices incorporating ZnO-system (ZnO, ZnSe, ZnMnO) will require a better understanding of its mechanical characteristics and its optical and electrical properties. The thesis showed that hardness was depth-dependent and decreased with increasing indentation depth, measurements of surface with the ZnO-system material as a substrate underestimated the hardness by means of depth sensing technique. The effects of loading/unloading method were apparent in the load displacement results of ZnO-system. Young’ modulus and hardness values measured using the force modulation technique showed very depth dependence, even the relationship between the nano-scale and relative structures. In order to point out the mechanical reliability (Young’ modulus and hardness) of thin films, relative optical device, and lifetime cycle. We concluded the several parts of issues about ZnO-system as below:
(i) A radio frequency magnetron sputtering system was used to deposit ZnO thin films onto langasite substrates. The thickness of the ZnO film increased from 0.3 to 1.2 μm upon increasing the deposition power from 100 to 200 W. The predominant growth orientation was along the C-axis (002); the intensities of the signals in the X-ray diffraction spectrum increased significantly upon increasing the film thickness. Scanning electron microscopy images revealed columnar structures in the ZnO films and the morphology of ZnO grains is found to be continuous and dense. It is attributed that oxygen chemisorbs on the target and cases a surface layer of adsorbed oxygen. We suggest that the more neutral ion bombardment on the growing film which induces the higher sputtering rate of the growing film. From in situ imaging of scratched tracks, measurement of the coefficient of friction was an effective means of detecting the occurrence of structural defects in the microstructures. For example, the Rms (11.3, 14.5, 16.5 nm) and friction (0.1 ± 0.01, 0.175 ± 0.01, 0.183 ± 0.02) is increased depended on the increased sputtering power (100, 150, 200 watt). The O 1s state splits into two peaks: 529.4 eV can be attributed to the O–Zn bond formation, while the peak at 531.0 eV can be owing to the O–H bond formation. As the deposition power is increased at 150W. The O 1s peak shifted to lower binding energy and a main peak emerged at ca. 530.5 eV, which we attribute to Zn–O bond. Therefore, it appears that Zn–O bonds became dominant during the grain growth process when deposition power increased from 100 to 200W. We also found that the chemical compositions of ZnO films prepared under various deposition powers could be investigated using X-ray photoelectron spectroscopy.
(ii) We used cathodoluminescence (CL) spectroscopy to examine the CL emissions of zinc selenide (ZnSe) single crystals that had been subjected to Berkovich nanoindentation. The CL spectra of the ZnSe exhibited both impurity emission peaks (1.8–2.4 eV band) and near-bandgap emission peaks (2.68 eV). Although CL emissions were generated during four unloading/reloading cycles, the decreased intensity of the impurity emission can be explained in terms of extended dislocation nucleation and propagation during nanoindentation. The resultant dislocation and microcracks were visualized using CL mapping and transmission electron microscopy. We suspect that the formation of a hysteresis loop during the four unloading/reloading cycles was due, in part, to massive dislocation activities induced by the indenter. ZnSe not only have been evidenced in their mechanical properties, but also led to the reported on optical investigation of CL. The deformations act as non-radiative recombination centers that confirmed by CL emission and CL mapping images. CL may prove to be a useful technique for characterization of some of its chemical and physical properties. Particular, CL emissions result from several sources, including electronic transitions among energy levels caused by various types of structural defects.
(iii) We investigated the nanotribological properties of Zn1-xMnxO epilayers (0≤ x ≤0.16) grown by molecular beam epitaxy (MBE) on sapphire substrates. The surface roughness and friction coefficient (μ) were analyzed by means of atomic force microscopy (AFM) and hysitron triboscope nanoindenter techniques. The nanoscratch system gave the μ value of the films ranging from 0.17 to 0.07 and the penetration depth value ranging 294 to 200 nm when the Mn content was increased from x=0 to 0.16. The results strongly indicate that the scratch wear depth under constant load shows that higher Mn content leads to Zn1-xMnxO epilayers with higher shear resistance, which enhances the Mn-O bond. From the Zn1-xMnxO epilayers, the images are together with the corresponding cross-sectional height profiles. The observation of a compressive residual stress of moderate magnitude is beneficial to the film because it can suppress crack initiation. Strain energy can often be a dominant factor, which is usually plays a critical role at different film. Stick–slip motion was found, whereas the period and amplitude of stick–slip, which were averaged over each test, increased with the normal load. The profile of the pure ZnO sample shows serious wear of the components. These findings reveal that the role of Mn content on the growth of Zn1-xMnxO epilayers can be identified by their nanotribological behavior.
The interfacial area between both surface and inner films determines main physical and mechanical properties here. It has ever conducted them including contact resistance, electronic trapping and recombination, thermal conductance, and film adhesion and so on. The measurement methods: scratch and wear can be suggested that ease to aim the state of an interfacial science, such as fracture toughness or adhesion strength are taken into account from the continuous load-displacement profile by means of lateral indentation.
其他識別: U0005-1408201217102200
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