群聚奈米碳管的氧氣吸附與電漿誘發異質接面性質

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研究生：	蔡欣蓉 Tsai, Hsin Jung
論文名稱：	群聚奈米碳管的氧氣吸附與電漿誘發異質接面性質 Oxygen adsorption and plasma-induced heter-junction of aggregated carbon nanotubes
指導教授：	徐文光 Hsu, Wen Kuang
口試委員:	林樹均 Lin, Su Jien 郭信甫 Kuo, Hsin Fu 許景棟 Hsu, Ching Tung 呂昇益 Lu, Sheng Yi
學位類別：	博士 Doctor
系所名稱：	工學院 - 材料科學工程學系 Materials Science and Engineering
論文出版年：	2015
畢業學年度：	104
語文別：	英文
論文頁數：	72
中文關鍵詞：	奈米碳管、氧氣吸附、二極體
外文關鍵詞：	carbon nanotube, oxygen adsorption, diode
相關次數：	點閱：1 下載：0
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奈米碳管是廣泛被應用的一維奈米材料，氣體吸附、表面修飾與異質參雜都對奈米碳管的物理與化學性質有很大的影響。過去的文獻都著重於’’單根奈米碳管’’研究，但實際應用上卻鮮少只使用單根奈米碳管，例如：以奈米碳管塗佈的透明導電薄膜或是奈米碳管強化的複合材料。本論文以多根奈米碳管（奈米碳管薄膜、陣列奈米碳管束）製作氣敏元件，討論奈米碳管間的電子傳遞行為，並以第一原理模擬計算討論其理論機制。此外，藉由局部的表面改質讓奈米碳管兩端具有不同的電子結構，利用此特性製作出有整流效果的奈米碳管元件。
第一章首先簡介奈米碳管的基本性質與奈米碳管的表面改質。且簡述理論模擬之發展與原理。
第二章在進入主題前，本章節先介紹實驗設置以及所使用的儀器、實驗步驟與模擬結構設置與方法。
第三章此章節以陣列的奈米碳管製作氣敏元件，藉由改變有序排列的奈米碳管與金屬電極的接觸方向探討氧氣對奈米碳管間電子傳遞的影響。並利用氮氣電漿改質奈米碳管結構，進一步的提高元件的氣敏性。
第四章在本章節利用陣列奈米碳管有序方向的特性，使用氮氣電漿將奈米碳管的一端參雜氮原子，讓成束的奈米碳管兩端具有不同的電子結構，且利用此結構製作出有整流效果的奈米碳管元件。
第五章總結以上各章節的結果。

Carbon nanotubes, known as one-dimensional (1D) nanostructures, have drawn much attention in recent years and their electron structure can be changed by gas adsorption, surface modification and heteroatom injection. The current applications however often focus on bundled carbon nanotubes, such as flexible, transparent and conducting films are made by coatings of carbon nanotubes onto plastic substrates. Carbon nanotubes can also be used as reinforcing fillers to improve electrical and thermal properties of polymer composites. In this thesis, gas sensors are fabricated by aggregated nanotubes to probe charge transfer between tubes and sensing mechanism is verified by ab-initio calculations. Furthermore, we synthesize nitrogen-doped carbon nanotube to create on-tube Schottky junction devices.
Chapter 1 introduces the background and property of carbon nanotubes, surface modification for carbon nanotube and the simulation system.
Chapter 2 describes experimental setups、characterization techniques and simulation methods.
Chapter 3 discusses the oxygen sensing mechanism of carbon nanotubes. In this work, devices are fabricated by carbon nanotubes arranged in different fashions with respect to electrodes. Electrical measurements reveal intercalated molecules acting as charge carriers between tubes. Ab-initio calculation supports dynamic intercalation and charge transfer through bouncing of O2 between tubes.
Chapter 4 aligned multi-walled CNTs are built to exhibit diode behavior by N2 plasma treatments. Surface modification for carbon nanotubes is studied by material analysis and ab-initio calculation. The simple fabrication of device without lift-off process is provided, and the parallel combination of a bundle of CNTs can promote output current.
Chapter 5 concludes the experimental results.

Contents
Abstract………………………..……………………………………………………. I
Contents……………………..………………………………………………………Ⅳ
Figure Captions……………………………………………………………….……Ⅶ
Table list……………………………………………………………………………..Ⅹ

Chapter 1 Introduction    
1-1 Structure of carbon nanotubes…………………………………………………….    1
1-2 Electronic properties of carbon nanotubes………………………………………..    5
1-3 Absorption on carbon nanotubes………………………………………………….    9
1-3-1 Description to interactions of molecules and carbon nanotubes…………..    9
1-3-2 Adsorption of Oxygen Molecules on Carbon Nanotubes………………...11
1-4 Chemical properties of CNTs……………………………………………….........14
1-4-1 Electrical properties of doped carbon nanotubes………………………....14
1-4-2 Oxygen Plasma Functionalization    ………………………………………..15
1-4-3 Nitrogen Plasma Functionalization……………………………………….17
1-5 Syntheses of carbon nanotubes    …………………………………………………..19
1-6 Density Functional Theory and molecular dynamic simulations………………...24
Chapter 2 Experimental Section    
2-1 Instrumental characterization…………………………………………………….26
2-1-1 Pyrolysis System………………………………………………………….26
2-1-2 Low Temperature Vacuum System……………………………………….26
2-1-3 Low Pressure DC Glow Discharge N2 Plasma…………………………..26
2-1-4 Electrical General Source Meter - Keithley 2400………………………..27
2-1-5 Multi-Probe Nano-Electronics Measurement System……………………27
2-1-6 Field Emission Scanning Electron Microscope (Joel, JSM-6500F)……...27
2-1-7 Raman Spectrometer (HORIBA, HR800)………………………………..28
2-1-8 Electron Spectroscopy for Chemical Analysis (ULVAC-PHI PHI 5000)    …………………………………………………………………………………..28
2-1-9 Simulation Software - Materials Studio 4.2……………………………...31
2-2 Sample preparations………………………………………………………...31
2-2-1 Production of aligned MWCNTs…………………………………………31
2-2-2 N2 plasma treatment……………………………………………………...31
2-3 Computer Simulation Setups…………………………………………………….32
2-3-1 Computer Simulation Setups for chapter 3………………………………32
2-3-2 Computer Simulation Setups for chapter 4……………………………….33
Chapter 3 Extraction of intercalated O2 from aligned carbon nanotubes: the breaking of intertube paths and exponential change in resistance    
3-1 Introduction………………………………………………………………………35
3-2 Devices fabrication………………………………………………………………36
3-3 Results and Discussion…………………………………………………………..39
3-3-1 Oxygen sensing measurement of D1, D2, D3, DA and DB……………...39
3-3-2 Sensing mechanism of carbon nanotubes………………………………...41
3-3-3 Sensing mechanism of defective carbon nanotubes……………………47
Chapter 4 Fabrication of on-tube diodes by N2 plasma treatments    
4-1 Introduction………………………………………………………………………50
4-2 Results and Discussion…………………………………………………………..51
4-2-1 Surface analyses (Raman and XPS)……………………………………...51
4-2-2 The electron structure simulation for the N-doped CNTs………………...53
4-2-3 CNT-base diode…………………………………………………………..58
Chapter 5 Conclusion……………………………………………………………….63
References…………………………………………………………………………...64
































Figure Captions
Fig. 1.1 Structures of (a) C60, (b) C70, (c) CNT, (d) graphene, (e) graphite and (f) diamond………………………………………………………………………………..1
Fig. 1.2 Schematic representation of 2D honeycomb lattices. The figure is constructed for  tube. The OA and OB lines define chiral vector  and the translational vector T of carbon nanotubes. A CNT is formed as O and A and, B and B' are connected individually…………………………………………………………………………….3
Fig. 1.3 (a) Armchair CNT with , (b) zigzag CNT with , and (c) helix CNT with ……………………………………………………..4
Fig. 1.4 Structures of (a) SWCNT, (b) DWCNT, and (c) MWCNT…………………..5
Fig. 1.5 (a) A zigzag tube with tubule axis orientation, (b) wave vector incidents into nanotube with n=6 in the first BZ, (c) band structure for n = 3k and (d) n ≠ 3k………6
Fig. 1.6 (a) Armchair tube with tubule axis orientation. (b) wave vector incidents into nanotube with n=4 at the first BZ (c) band structure…………………………………7
Fig. 1.7 Band structure and DOS of SWCNT……………………………………….8
Fig. 1.8 Band structure and DOS of SWCNT………………………………………9
Fig 1.9 schematic diagrams of small molecules exohedrally (blue) and endohedrally (red) adsorbed on nanotubes of different diameters (dmolecule is van der waals diameter of molecule, and dNT is internal van der waals diameter of nanotube): (a) dNT<dmolecule, (b) dNT~dmolecule, (c) dNT>dmolecule, (d) dNT>>dmolecule, (e) dNT~∞………...11
Fig. 1.10 Three steps of R increase for O2 desorption from aggregated tubes………13
Fig. 1.11 O2 adsorption sites in a carbon nanotube bundle…………………………..13
Fig. 1.12 XPS spectra of untreated MWCNTs (a) and MWCNTs treated with H2O plasma at 140 W and 135 Pa (b). Percentage area of different carbon–carbon and carbon–oxygen bonds as a function of plasma power at a constant pressure of 50 Pa (c)……………………………………………………………………………………16
Fig. 1.13 (a, b) N1s spectra of untreated and nitrogen-plasma treated MWCNTs, respectively. (c) Nitrogen concentrations at a constant power of 75 W against nitrogen pressure, (d) structural disorder with respect to the nitrogen concentration. The solid lines are drawn to guide the naked eyes……………………………………………...19
Fig. 1.14 Schematic representation of arc discharge equipment……………………..21
Fig. 1.15 Scheme of laser ablation equipment. A laser is aimed at a block of graphite and a Cu-made cooled is placed at the rear of furnace to collect SWCNTs…………22
Fig. 1.16 Scheme of pyrolysis equipment……………………………………………22
Fig. 1-17 Low-magnification SEM image of a film composed of aligned MWCNTs……………………………………………………………………………23
Fig. 1.18 Growth of aligned MWCNTs on Co-coated Si wafer……………………...23
Fig. 2.1 Scheme of pyrolysis system…………………………………………………28
Fig. 2.2 Picture of pyrolysis system…………………………………………………28
Fig. 2.3 Picture of low temperature vacuum system…………………………………29
Fig. 2.4 Scheme of low temperature vacuum system………………………………...24
Fig. 3.1 (a) Arrays of aligned MWCNTs. (b) Device fabrications…………………...36
Fig. 3.1 Tube orientations in (c) D1 and (d) D2. Grey regions in D1 and D2 denote silver painted tubes which lie on metal electrodes. Tubes between dashlines are silver-free and act as gas sensors……………………………………………………37
Fig. 3.2 (a) Fabrications of DA, (b) DB (lower left) and (c) ACNT controlled DA…37
Fig. 3.3 The time-evolved R profiles of (a) D1, (b) D2  and (c) D3  in vacuum and O2 atmosphere and corresponding R/Ro plots (d-f)…………………………………38
Fig. 3.4 (a) The time-evolved R change profiles of DA and DB in O2 evacuation, and (b) the R-ACNT plots of DA…………………………………………………………39
Fig. 3.5 (a) Mulliken charge density at O2 adsorbed and desorbed C-C bonds.(b) highlighted electron density difference at C atoms with and without O adsorption…………………………………………………………………………….41
Fig. 3.6 (a) The C profiles of D3 in O2 (red) and vacuum (dark). (b) The R/Ro-T profiles of D3 in O2 (blue) and vacuum (dark). Insert: the ln(R/Ro) vs.1/T×1000 plots fit with linear function………………………………………………………………42
Fig. 3.7 (a). Three (10,0) tubes in an amorphous cell with an O2 at tube groove. (b). Geometrically optimized tubes-O2 complex at 300K, (b) at 200 K, (c) at 90 K …...44
Fig. 3.8 Geometrically optimized tubes-(O2)50 complexes at 90 K (left), 200 K (middle) and 300 K (right)………………………………………………………...45
Fig. 3.9 R-P(O2) plots of D3 at 300, 400 and 500 K. Insert, magnified profile from circles………………………………………………………………………………...46
Fig. 3.10 XPS spectra of (a) untreated and (b) treated tubes.    ……………………….47
Fig. 3.11 time-evovled R/Ro recording of untreated (dark) and treated tubes (blue) upon O2 introduction………………………………………………………………..48
Fig. 4.1 Raman spectroscopy of pristine and treated CNTs…………………………51
Fig. 4.2 XPS analysis of pristine and treated CNTs: (a) wide-scan, (b) C1s………...53
Fig. 4.2 XPS analysis of pristine and treated CNTs: (c) N1s, (d) O1s……………….54
Fig. 4.3 Electron density simulation of pristine and treated (8,0) CNTs……….........55
Fig. 4.4 Band structure simulation of pristine and treated (8,0) CNTs………………56
Fig. 4.5 Current-Voltage characteristic curve of p-type and diode-like CNTs……….58
Fig. 4.6 The schematic of Schottky and intratube junction…………………………..58
Fig. 4.7 carbon nanotube slab with 30 Å vacuum layer for work function simulaton……………………………………………………………………………..60
Fig. 4.8 (a) IV curve (insert, band diagram) and (b) XPS spectrum with different plasma treatment time………………………………………………………………..61
Table list
Table 1. The deq between CNT centroid and O2 at 90-300 K………………………43

                                

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