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研究生：	林宛嫺 Lin, Wan-Hsien
論文名稱：	有機金屬化學氣相沉積氧化鋅鎂磊晶薄膜之鑑定及其表面化學之研究 Characterizations and Surface Chemistry of Metalorganic Chemical Vapor Deposited Zn1-xMgxO Epitaxial Films
指導教授：	吳季珍 Wu, Jih-Jen
學位類別：	博士 Doctor
系所名稱：	工學院 - 化學工程學系 Department of Chemical Engineering
論文出版年：	2013
畢業學年度：	101
語文別：	英文
論文頁數：	191
中文關鍵詞：	化學氣相沉積、氧化鋅鎂、極性、能隙調控、蝕刻、光觸媒反應
外文關鍵詞：	MOCVD, ZnMgO, polarity, band gap engineering, etching, photocatalytic reaction
相關次數：	點閱：82 下載：6
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本論文的研究主軸主要區分為兩部分。第一部份，乃利用有機金屬氣相沉積法，藉由不同鎂濃度的合金化方式，成功於鋁酸鋰及鎵酸鋰基板上製備出可調控能隙的非極性(10-10)與鋅極性面之氧化鋅鎂磊晶薄膜，研究其結晶結構與光學特性。第二部份，則利用“光輔助掃描探針顯微鏡”探討氧化鋅磊晶薄膜之表面化學行為，包含氧化鋅分別與酸性或鹼性溶液反應的溶蝕機制，以及金奈米粒子優化之氧化鋅磊晶薄膜光觸媒反應中，金奈米粒子所扮演的角色。
本研究嘗試於鋁酸鋰(100)與氧化鋁(10-10)基板沉積不同鎂濃度之非極性氧化鋅鎂磊晶薄膜。晶體結構鑑定結果顯示，於本實驗室化學氣相沉積系統的最佳反應條件下，唯有鋁酸鋰(100)基板能成功製備出單晶(10-10)氧化鋅鎂薄膜，且鎂濃度可控制於0到0.113之間。反觀氧化鋁(10-10)基板所製備出之氧化鋅鎂薄膜同時存在(10-10)和(101-3)晶面。此外，在(10-10)氧化鋅鎂薄膜之陰極發光圖譜觀察到，隨鎂濃度增加，氧化鋅鎂薄膜之近能隙邊緣發光能量位置有明顯藍位移現象。此結果證實於鋁酸鋰(100)基板成長之非極性(10-10)氧化鋅鎂磊晶薄膜具有能隙可調控性。
本研究亦利用具備高空間解析度的陰極發光系統探討非極性(10-10)氧化鋅磊晶薄膜內基面疊差之發光行為。利用實驗過程參數的調控證實基面疊差內延氧化鋅c軸方向存在一極化電場。本研究更確定了基面疊差於低溫與常溫之發光行為。另一方面，藉由氧化鋅鎂磊晶薄膜內之基面疊差陰極發光實驗結果，推測不同鎂濃度改變對基面疊差發光的影響，唯此部分討論仍須理論計算或數據統計分析相輔方可證實。再者，我們觀察到於鎵酸鋰(100)基板上成長之非極性(10-10)氧化鋅磊晶薄膜，其陰極發光圖譜由基面疊差發光所主導，且由發光點推測之基面疊差密度較與鋁酸裡(100)基板所成長之氧化鋅薄膜高，此結果可歸因為氧化鋅薄膜於兩基板上不同的成長行為所致。
本研究於鎵酸鋰(001)基板上成長極性之氧化鋅鎂磊晶薄膜。結構鑑定結果顯示氧化鋅鎂薄膜內並無氧化鎂或鎂金屬的存在。由掃描式穿遂電子顯微鏡之收斂束電子繞射結果與酸蝕的結果證實氧化鋅鎂磊晶薄膜的表面為鋅極性。此外，氧化鋅鎂磊晶薄膜之近能隙邊緣發光能量位置隨鎂濃度增加呈現藍位移現象，證明於鎵酸鋰(001)基板成長鋅極性之氧化鋅鎂薄膜同樣具備能隙可調控性。
本研究利用氧化鋅的半導體特性發展“光輔助掃描穿遂顯微鏡”，於常溫常壓環境下探究(0001)氧化鋅磊晶薄膜於氫氧化鈉處理後之原子級表面幾何結構。未經過氫氧化鈉處理之氧化鋅磊晶薄膜表面具備兩種不同形貌，分別為層狀堆疊六角錐與六角形平面。光輔助掃描穿遂顯微鏡之圖像顯示，此兩種不同形貌之氧化鋅晶體存在非等向性蝕刻行為。規則層狀晶面的六角錐隨氫氧化鈉處理的時間增加，逐漸變得不規則且表面呈現圓形狀；反觀六角形平面在未經氫氧化鈉處理前，即存在小六角形凹洞，且凹洞隨氫氧化鈉處理時間增加而擴大，同時在表面上發展出平坦的三角形階梯狀排列，以穩定化氧化鋅之極性表面。
本研究利用光降解甲基橙溶液鑑定金奈米粒子優化之非極性(10-10)氧化鋅磊晶薄膜的光觸媒活性。使用“光輔助表面電位顯微鏡”量測未濺鍍金奈米粒子的氧化鋅和不同濺鍍條件之金-氧化鋅複合物於黑暗中與紫外光照射下的功函數值。金-氧化鋅複合物光降解甲基橙的反應系統內共具備三個界面，分別為金奈米粒子與氧化鋅，氧化鋅與甲基橙溶液，以及金奈米粒子與甲基橙溶液的界面。藉由表面電位顯微鏡於黑暗中與照光下量測到各樣品的功函數結果，針對此三種界面提出個別的能階圖，並加以探討光激發載子於各界面的傳輸行為。研究結果顯示，金奈米粒子與氧化鋅為歐姆界面，促進氧化鋅的光載子分離效率。而由量測結果所推算出各個金-氧化鋅複合物的表面光電壓值，與該複合物的光觸媒活性具有高關聯性。顯示金奈米粒子的密度影響氧化鋅中光電洞濃度，對於甲基橙溶液界面的自由基形成與光觸媒活性有決定性的影響。

The subjects of this thesis are classified into two parts. First, growth and band gap engineering of nonpolar (10-10) and Zn-polar (0001) Zn1-xMgxO epitaxial films on LAO and LGO substrates were conducted using metalorganic vapor deposition (MOCVD). Crystal and optical properties of as-grown Zn1-xMgxO epilayers are studied. In the second part, the surface chemistry of ZnO, including the etching behaviors of Zn-polar ZnO in the acidic/alkaline solutions as well as the photoactivity of (10-10) ZnO epitaxial films were investigated using photo-assisted scanning probe microscopy techniques.
In the first part, we demonstrate the growth and crystal characterization of (10-10) Zn1-xMgxO films with various Mg contents (0 ≤ x ≤ 0.113) on two well-known substrates for preparation of nonpolar ZnO films, i.e., gamma-LiAlO2 (100) and sapphire (10-10). Epitaxial (10-10) Zn1-xMgxO films are attainable when gamma-LiAlO2 (100) substrates are used while those with both (10-10) and (101-3) orientations are obtained on sapphire (10-10) substrates. Obvious blue shifts of the near-band-edge (NBE) emissions with increasing Mg composition are observed in the cathodoluminescence (CL) spectra of the (10-10) Zn1-xMgxO films, confirming a feasible band gap engineering in the (10-10) Zn1-xMgxO films on the gamma-LiAlO2 (100) substrates.
The luminescence of basal plane stacking faults (BSFs) in (10-10) Zn1-xMgxO epilayers grown on gamma-LiAlO2 (100) substrate is analyzed using spatially resolved CL spectroscopy. A polarization field in the SFs along the c-axis of the (10-10) ZnO epilayer is experimentally demonstrated. Moreover, we clearly identify the BSF-related transition from low temperatures to room temperature. Based on our CL observations, we temporarily deduce the transition of the BSF-related emissions as a function of Mg compositions in the (10-10) ZnxMg1-xO epilayers. A dominant BSF-associated emission is observed in a (10-10) ZnO epilayer grown on a β-LiGaO2 (100) substrate compared with that on a gamma-LiAlO2 (100) substrate, which can be ascribed to the different growth behavior.
In addition to m-plane ZnO epitaxial films, growth and characterization of Zn-polar (0001) Zn1-xMgxO epilayers on the small lattice-mismatched β-LiGaO2 (001) substrates were also performed using MOCVD. Structure characterizations by employing X-ray diffraction (XRD) and transmission electron microscope (TEM) demonstrate that no MgO or Mg cluster exists throughout the Zn1-xMgxO films. Together with an apparent blue shift of the NBE emission with increasing Mg content observed in the CL spectra of the Zn-polar (0001) Zn1-xMgxO films, a successful band gap engineering in the epitaxial (0001) Zn1-xMgxO films on the (001) LiGaO2 substrates has been achieved.
In the second part, a photo-assisted scanning tunneling microscopy (STM) were developed to investigate the surface geometric structures of epitaxial (0001) ZnO films treated by NaOH(aq) in ambient condition. Two types of topographic features, i.e. hexagonal pyramid and flat plane, are observed in the as-grown epitaxial (0001) ZnO film. Photo-assisted STM images reveal the anisotropic etching behaviors of these two topographic features. The faceted and symmetrically layered hexagonal-pyramid feature is getting asymmetrical and rounded while few small hexagonal pits on the as-grown flat ZnO(0001)-Zn surface are developed to asymmetrically hexagonal cavities with flat terraces and steps after different period of NaOH treatments.
Au nanoparticles (NPs) enhanced photocatalytic activity of the (10-10) ZnO epilayer by means of photodegradation of methyl orange (MO) solution was demonstrated in this thesis. Work functions of pristine ZnO and Au-ZnO composites are investigated in the dark and under UV illumination utilizing Kelvin probe force microscopy (KPFM). Based on KPFM results, we propose the band diagrams of three fundamental interfaces, including Au NP/ZnO, ZnO/MO(aq) and Au NP/MO(aq). An Ohmic contact is formed at the Au NP/ZnO interface, which facilitates photoelectrons transfer from ZnO to Au NP for efficient charge separation. On the other hand, hole transfer at the Schottky interface of ZnO/MO(aq) is responsible for the degradation of MO molecules. The surface photovoltages (SPV) values of the pristine ZnO and the Au-ZnO composites show a systematic correlation with their photocatalytic activities. It suggests that the density of Au NPs influences the excess hole concentration and therefore the photocatalytic activity of ZnO.

Abstract...............................................I
Acknowledgement........................................VII
Table of contents......................................IX
List of tables.........................................XIII
List of figures........................................XIV
List of abbreviations..................................XXV
List of symbols........................................XXVII

Chapter 1 Introduction and Motivation....................1
      1.1. Preface.......................................2
      1.2 Overview of ZnO................................4
         1.2.1 Crystal structures and polarity of ZnO....4
         1.2.2 Determination and stabilization of polar ZnO	.................................................5
         1.2.3 Spontaneous polarization of ZnO...........7
         1.2.4 Nonpolar planes of ZnO....................8
      1.3 Introduction of sapphire, γ-LiAlO2, and β-LiGaO2 substrates...............................................11
         1.3.1 Introduction of sapphire substrates.......11
         1.3.2 Introduction of γ-LiAlO2 substrates.......12
         1.3.3 Introduction of β-LiGaO2 substrates.......13
      1.4. Motivation....................................17
      1.5. Organization of the dissertation..............19

Chapter 2 Literatures review.............................21
      2.1. Zn1-xMgxO alloy...............................22
         2.1.1 Lattice constants of Zn1-xMgxO............23
         2.1.2 Excitonic transition of Zn1-xMgxO.........24
      2.2 Basal plane stacking faults of ZnO.............26
         2.2.1 Types and band structure of basal plane stacking faults in ZnO...................................27
         2.2.2 Basal plane stacking fault-related luminescence of ZnO......................................30
      2.3 Surface chemistry of ZnO.......................32
         2.3.1 Acidic and alkaline etching of ZnO........32
         2.3.2 Photodegradation of methyl orange using ZnO as photocatalyst.........................................35
         2.3.3 The role of Au in enhancing the photocatalytic activity of ZnO under UV irradiation......36

Chapter 3 Experimental methods...........................39
      3.1 Growth of ZnO/Zn1-xMgxO epilayers utilizing metalorganic chemical vapor deposition...................40
         3.1.1 Fundamentals of chemical vapor deposition	.................................................40
         3.1.2 Growth of ZnO/Zn1-xMgxO epilayers.........41
      3.2 Experimental details of surface chemical reactions	.................................................43
         3.2.1 Acidic and alkaline treatments of c-plane Zn1-xMgxO epilayers......................................43
         3.2.2 Photocatalysis of m-plane ZnO films.......44
      3.3 Characterization of Zn1-xMgxO epilayers........45
         3.3.1 X-ray diffraction.........................45
            3.3.1.1 ω-2θ scan............................45
            3.3.1.2 ω scan (rocking curve)...............46
         3.3.2 X-ray photoelectron spectroscopy..........47
         3.3.3 Scanning electron microscopy and cathodoluminescence......................................49
            3.3.3.1 Scanning electron microscopy.........49
            3.3.3.2 Cathodoluminescence..................51
         3.3.4 Transmission electron microscopy..........53
            3.3.4.1 Preparation of TEM specimen..........53
            3.3.4.2 Bright field and dark field images...56
            3.3.4.3 Selective area electron diffraction..57
            3.3.4.4 Convergent-beam electron diffraction.58
            3.3.4.5 High-angle annular dark-field........59
         3.3.5 Scanning probe microscopy.................60
            3.3.5.1 Atomic force microscopy..............61
            3.3.5.2 Scanning Kelvin probe force microscopy	.................................................63
            3.3.5.3 Photo-assisted scanning tunneling microscopy...............................................66

Chapter 4 Growth of (10-10) Zn1-xMgxO epilayers on LiAlO2 (100) and sapphire (10-10) substrates....................69
      4.1 Determination of the Mg composition in the (10-10) Zn1-xMgxO films..................................70
      4.2 (10-10) Zn1-xMgxO films grown on sapphire (10-10) substrates...............................................72
         4.2.1 SEM images of (10-10) Zn1-xMgxO films/sapphire...........................................72
         4.2.2 XRD Investigation of (10-10) Zn1-xMgxO films/sapphire...........................................72
      4.3 (10-10) Zn1-xMgxO films grown on LiAlO2 (100) substrates...............................................77
         4.3.1 SEM images of (10-10) Zn1-xMgxO films/LiAlO2	.................................................77
         4.3.2 XRD investigation of (10-10) Zn1-xMgxO films/LiAlO2.............................................77
         4.3.3 TEM Characterization of (10-10) Zn1-xMgxO films/LiAlO2.............................................81
         4.3.4 Optical property of (10-10) Zn1-xMgxO films/LiAlO2.............................................82
      4.4 Summary........................................85

Chapter 5 Basal plane stacking fault-related cathodoluminescence of m-plane Zn1-xMgxO films...........87
      5.1 Basal plane stacking fauls in 850-nm-thick ZnO epilayer grown on LiAlO2 substrate.......................88
         5.1.1 Cathodoluminescence of ZnO Film ― Spectrum and Images measured at Low Temperature...................88
         5.1.2 BSF-related cathodoluminescence at low temperature ― investigations of spectral line scan.......91
         5.1.3 Transition of the basal plane stacking fault-related luminescence ― 7 K to 300 K......................95
         5.1.4 Temperature-dependence of basal plane stacking fault-related luminescence......................96
      5.2 Basal plane stacking fault-related cathodoluminescence in 180-nm-thick Zn1-xMgxO epilayers grown on LiAlO2 substrates...............................100
         5.2.1 Basal plane stacking fault-related cathodoluminescence in 180-nm-thick ZnO epilayer.........100
         5.2.2 Basal plane stacking fault-related cathodoluminescence in 180-nm-thick Zn0.988Mg0.012O epilayer	.................................................102
         5.2.3 Basal plane stacking fault-related cathodoluminescence in 180-nm-thick Zn0.960Mg0.040O epilayer	.................................................104
         5.2.4 Transition of plane stacking fault-related cathodoluminescence in of ZnO after alloying Mg..........104
      5.3 Basal plane stacking fault-related cathodoluminescence in the 65-nm-thick ZnO epilayer grown on LiGaO2 substrates.....................................109
5.4 Summary..............................................112

Chapter 6 (0001) Zn1-xMgxO epilayer grown on β-LiGaO2 (001) substrates...............................................113
      6.1 Determination of Mg content in (0001) Zn1-xMgxO films....................................................114
      6.2 XRD investigation of (0001) Zn1-xMgxO films....114
      6.3 TEM characterization of (0001) Zn1-xMgxO films	.................................................116
      6.4 Polarity determination of (0001) Zn1-xMgxO films	.................................................118
         6.4.1 BF and DF TEM Analysis of the Zn1-xMgxO film	.................................................118
         6.4.2 CBED Investigations of theZn1-xMgxO films	.................................................119
         6.4.3 Acidic etching of the Zn1-xMgxO films.....121
      6.5 Optical properties of (0001) Zn1-xMgxO films...122
      6.6 Summary........................................124

Chapter 7 NaOH(aq) treated ZnO (0001)-Zn surface.........127
      7.1 TEM characterization of (0001) ZnO films (650 °C) grown on LiGaO2 (001) substrates.........................128
      7.2 SEM images of as-grown (0001) ZnO films (650 °C)	.................................................129
      7.3 AFM Topography of NaOH(aq) Treated (0001) ZnO Films (650 °C)...........................................131
      7.4 Surface polarity determination (0001) ZnO films (650 °C).................................................133
      7.5 Photo-assisted STM Analysis of NaOH(aq) Treated ZnO (0001)-Zn Surface....................................135
         7.5.1 Working principle of the photo-assisted STM investigations on ZnO....................................135
         7.5.2 Evolutions of ZnO (0001)-Zn surface after NaOH(aq) treatment.......................................137
      7.6 Summary........................................142

Chapter 8 Au-Enhanced photoactivity of (10-10) ZnO epilayer grown on LiGaO2 (100) Substrates.........................145
      8.1 TEM investigations on the interfaces of ZnO/LiGaO2 and Au/ZnO....................................146
      8.2 Photodegradation of methyl orange using (Au)-ZnO photocatalysts...........................................148
      8.3 Size estimation of Au nanoparticles and their distribution/coverage on m-plane ZnO surface.............150
      8.4 Discussions of the interfaces in the photocatalytic reaction system ― KPFM analyses of (Au)-ZnO composites in the dark and under UV irradiation..........153
         8.4.1 Interface of Au nanoparticle/ZnO..........153
         8.4.2 Interface of ZnO/methyl orange solution...157
         8.4.3 Interface of Au nanoparticle/methyl orange solution.................................................159
      8.5 Minor factors that affect the photoactivity of (Au)-ZnO photocatalysts..................................161
      8.6 Summary........................................163

Chapter 9 Conclusions and Future Prospects...............165
      9.1 Conclusions....................................165
      9.2 Future Prospects...............................169

References...............................................171

Lists of Publications and Honors.........................189
                                    

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