銅鍺合金奈米線的製備及其電性之研究｜國立臺灣科技大學博碩士論文系統

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研究生：	張庭翔 Ting-Hsiang Chang
論文名稱：	銅鍺合金奈米線的製備及其電性之研究 Fabrication and Electrical Properties of Cu-Ge Alloy Nanowires
指導教授：	王秋燕 Chiu-Yen Wang
口試委員:	周苡嘉 Yi-Chia Chou 蔡孟霖 Men-Lin Tsai 周賢鎧 Shian-Kai Jou 葉炳宏 Ping-Hung Yeh
學位類別：	碩士 Master
系所名稱：	工程學院 - 材料科學與工程系 Department of Materials Science and Engineering
論文出版年：	2023
畢業學年度：	111
語文別：	英文
論文頁數：	129
中文關鍵詞：	銅鍺合金奈米線、Cu3Ge/Ge異質奈米線、場效電晶體、金屬奈米線、異質結構、電性量測
外文關鍵詞：	Cu-Ge alloy nanowires, Cu3Ge/Ge heterostructure nanowires, Field effect transistors, Metal nanowires, Heterostructure, Electrical properties measurement
相關次數：	點閱：309 下載：2
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本研究主要為銅-鍺合金的奈米線材料的製程、材料微結構分析和電性量測表現。分為兩大主題，Cu3Ge和Cu3Ge/Ge材料系統。第一部分為金屬線的Cu3Ge，在Cu3Ge的系統中在熔點以下和熔點以上進行壓鑄，其中熔點以下（700 oC）進行壓鑄再細分為，有退火和沒有退火的部分，退火的條件為550 oC 持溫 12小時。再者，利用陽極氧化鋁(Anodic Aluminum Oxide, AAO)模板結合真空壓鑄系統來生成奈米線，再經由鉻酸溶液隔水加熱進行蝕刻取得奈米線。奈米線材料進行微結構分析，包含 X 光射線繞射分析、拉曼光譜分析和電子顯微鏡的能量散射光譜儀分析等。有無退火的奈米線進行 X 光射線繞射分析和拉曼光譜分析的比較，用來確定對奈米線退火是否有消除奈米線內部之缺陷之效果，來達到後續元件表現進步的依據。藉由進行電子束微影(E-Beam Lithography, EBL)製程製備元件、經由緩衝氧化物蝕刻(Buffer Oxide Etching)等處理。隨著設備的更新我們嘗試在熔點以上壓鑄（800 oC）Cu3Ge奈米線，其目的是希望塊材再高於熔點的溫度下更均勻，得到更純粹且更優取向的單晶奈米線，也希望在電性表現上有更加突破的展現。在電性量測中，獲取兩點探針和TLM量測數據，其電阻率最低至 6.01 μΩ• cm，更加證實了Cu3Ge奈米線具有良好的傳導特性和低電阻的優勢。
第二部分為Cu3Ge/Ge異質結構奈米線，由於鍺元素具有低的直接能隙能量Eg(~0.66 eV)和高的載流子遷移率µh、μe，對於異質結構的奈米線作為材料製備場效電晶體管(Field Effect Transistors, FETs)元件起到極大的作用。為了更好的達到異質結構(分段)的效果，根據相圖，配置過共晶相的成分，Cu0.55Ge0.45。製程方面，塊材以快速焠火的方式取得，透過陽極氧化鋁模板和真空壓鑄系統製備奈米線，壓鑄的過程中，塊材會進行固-液-固的熱力學相轉變，以陽極氧化鋁模板的緻密孔洞作為容器，達到分段之特殊的異質結構。經由接觸後之能帶圖顯示，Cu3Ge/Ge奈米線原件為p型金氧半場效應電晶體(MOSFETs)。但是，由於在壓鑄和蝕刻奈米線未找到最佳化的參數，導致在X光射線繞射分析和拉曼光譜分析甚至電性的量測數據上都有所欠缺，但進一步發現類似碗豆狀之異質結構的奈米線。對於此項研究起到極大的重要性。

This research mainly focuses on the manufacturing process, material microstructure analysis and electrical measurement performance of Cu-Ge alloy nanowires. Divided into two major themes, Cu3Ge and Cu3Ge/Ge material system. The first part is the Cu3Ge of the metal nanowires. In the Cu3Ge system, the die-casting is performed below the melting point and above the melting point. The die-casting is carried out below the melting point (700 oC) and subdivided into parts with and without annealing. The annealing condition is 550 oC and maintained for 12 hours. Furthermore, anodic aluminum oxide (AAO) templates are combined with a vacuum die-casting system to generate nanowires, and then etched by chromic-acid solution to obtain nanowires. Microstructure analysis of nanowires materials, including Xray diffraction analysis (XRD), Raman spectroscopy analysis and energy dispersive spectrometer analysis of scanning electron microscope (EDS), etc. The comparison of X-ray diffraction analysis and Raman spectrum analysis of nanowires with or without annealing is used to determine whether the annealing of nanowires has the effect of eliminating defects inside nanowires, so as to achieve the basis for the improvement of subsequent device performance. Components are prepared by performing electron beam lithography (EBL) process, and processed by buffer oxide etching (BOE). With the update of the equipment, Cu3Ge nanowires are prepared by die casting method above the melting point. The purpose is to hope that the bulk material will be more uniform at a temperature higher than the melting point. Better-oriented single crystal nanowires that there will be more breakthroughs in electrical performance. In the electrical measurement, the two-point probe and TLM measurement results were obtained, and the resistivity was as low as 6.01 μΩ• cm, which further confirmed that Cu3Ge nanowires have the advantages of good conductivity. The second part is Cu3Ge /Ge heterostructure nanowires. Since germanium has low direct energy gap energy Eg (~0.66 eV) and high carrier mobility µh, μe, the heterostructure nanowires as materials. The preparation of field effect transistors (FETs) elements plays a great role. In order to better achieve the effect of heterostructure (segmentation), according to the phase diagram, configure the composition of the hypereutectic phase, Cu0.55Ge0.45. In terms of manufacturing process, the block is obtained by rapid quenching, and the nanowires are prepared through an anodized aluminum template and a vacuum die-casting system. During the diecasting process, the block will undergo a solid-liquid-solid thermodynamic phase transition, and the anodized aluminum template the dense pores are used as containers to achieve a special heterogeneous structure of segments. The energy band diagram after contact shows that the Cu3Ge /Ge nanowire components are p-type metal oxide field effect transistors (MOSFETs). However, due to the lack of optimized parameters in die-casting and etching nanowires, there is a lack of X-ray diffraction analysis and Raman spectroscopy analysis and even electrical measurement data, but it is further found that similar peas heterostructure nanowires. is of great importance to this research.

摘要................................................................................I
Abstract..........................................................................III
致謝................................................................................V
List of Abbreviations and Acronyms.................................................IX
List of Figures and Tables..........................................................X
Chapter 1 Introduction .............................................................1
1 Nanostructure...................................................................1
1.1 One-dimensional (1D) nanostructure ...........................................1
2 Synthesis of one-dimensional nanostructures.....................................2
2.1 Vacuum hydraulic pressure injection process (die-casting).....................3
3 Crystal structure and characteristics of Cu3Ge .................................3
4 Ge element .....................................................................6
5 Heterostructure.................................................................8
6 Cu3Ge/Ge 1D materials...........................................................8
7 Selective etching ..............................................................9
8 Flow charts of research........................................................10
Chapter 2. Experimental Section ...................................................13
1 Fabrication of AAO templates...................................................13
2 Synthesis of Cu3Ge nanowires...................................................16
2.1 Preparation of Cu3Ge bulk....................................................16
2.2 Fabrication of Cu3Ge nanowires via die-casting method........................18
2.3 Etching Cu3Ge nanowire from AAO template ....................................20
2.4 Annealing process of Cu3Ge nanowires by die-casting below the melting point..20
2.5 Fabrication of Cu3Ge nanowires devices.......................................21
3 Synthesis of Cu3Ge/Ge nanowires................................................23
3.1 Preparation of Cu3Ge/Ge bulk.................................................23
3.2 Fabrication of Cu3Ge/Ge nanowires via die-casting method ....................25
3.3 Etching Cu3Ge/Ge nanowires from AAO template.................................25
3.4 Annealing process of Cu3Ge/Ge nanowires .....................................26
3.5 Fabrication of Cu3Ge/Ge nanowires devices....................................26
4 Characteristic analysis of microstructure .....................................29
4.1 X-ray diffractometer ........................................................29
4.2 Raman spectrum ..............................................................29
4.3 Scanning electron microscope (SEM)...........................................30
4.4 Energy dispersive X-ray spectrometry (EDS)...................................30
4.5 Electron beam lithography (EBL) .............................................31
4.6 Electron gun evaporation (E-gun) ............................................31
Chapter 3 Results and Discussions..................................................33
1 Research motivation of Cu3Ge and Cu3Ge/Ge nanowires devices ...................33
2 Characteristics of Cu3Ge nanowires.............................................34
2.1 Observation of the Cu3Ge bulk and nanowires from SEM ........................34
2.2 XRD spectrum of Cu3Ge bulk and nanowires.....................................37
2.3 Raman spectrum of Cu3Ge bulk and nanowires...................................40
2.5 Electrical properties of Cu3Ge nanowires die-casting below the
melting point (700 °C) by annealing in 550 oC for 12 hours ........................49
2.6 Electrical properties of Cu3Ge nanowires die-casting above the
melting point (800 °C).............................................................63
3 Characteristics of Cu3Ge/Ge nanowires .........................................72
3.1 Observation of the Cu3Ge/Ge bulk and nanowires from SEM......................72
3.2 XRD spectrum of Cu3Ge/Ge bulk ...............................................78
3.3 Raman spectrum of Cu3Ge/Ge bulk .............................................81
3.4 Electrical properties of Cu3Ge/Ge nanowires..................................84
Chapter 4 Summary and Conclusion...................................................90
1 Cu3Ge nanowires devices with different annealed/die-casting conditions.........90
2 Cu3Ge/Ge nanowires devices.....................................................90
Chapter 5 Future Works.............................................................92
1 The detailed structure analysis of Cu3Ge nanowires die-casting below
the melting point (700 °C).........................................................92
2 The detailed structure analysis of Cu3Ge nanowires die-casting above
the melting point (800 °C).........................................................92
3 The detailed structure analysis of Cu3Ge/Ge nanowires and the
electrical properties behavior.....................................................92
References.........................................................................94
Self-Introduction.................................................................106
Appendix..........................................................................107

                                

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