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Electronic Transport in Single-Walled Carbon Nanotubes, and Their Application As Scanning Probe Microscopy Tips

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Electronic Transport in Single-Walled Carbon Nanotubes, and Their Application As Scanning Probe Microscopy Tips Electronic Transport in Single-Walled Carbon Nanotubes, and their Application as Scanning Probe Microscopy tips by Neil Richard Wilson Thesis Submitted to the University of Warwick for the degree of Doctor of Philosophy Physics April 2004 ii Contents List of Tables vii List of Figures viii Acknowledgments xiv Declarations xvi Abstract xviii Abbreviations xix Chapter 1 Introduction 1 1.1 Introduction to Single-Walled Carbon Nanotubes ........... 3 History .............................. 4 Structure and mechanical properties .............. 6 Electronic properties of SWNT ................. 9 Why study SWNT devices: the Physics and the Funding . 17 1.2 Introduction to Atomic Force Microscopy . 20 Dynamic or 'Tapping' mode AFM . 24 Dynamic lateral force mode or 'Torsional Resonance' mode . 30 Electric Force Microscopy .................... 33 iii Tips and Cantilevers ....................... 36 Multimode and Dimension AFM's . 39 1.3 Outline of thesis ............................. 41 Chapter 2 SWNT growth and devices 42 2.1 SWNT growth .............................. 42 2.1.1 Experimental setup and results . 44 2.1.2 Characterisation ......................... 53 AFM and SCM .......................... 53 Electron Microscopy ....................... 55 micro-Raman spectroscopy ................... 59 2.2 SWNT devices .............................. 62 Lithography ............................ 63 Device Fabrication ........................ 66 2.2.1 Room Temperature Electronic Transport Characteristics . 68 2.3 Conclusions and future work ...................... 75 Chapter 3 EFM and SGM of carbon nanotube devices 77 3.1 Experimental setup for EFM and SGM . 79 3.2 Manipulation of SWNT devices, and characterisation by SGM . 82 3.3 SSPM of SWNT devices ......................... 89 3.3.1 Current saturation in mSWNT devices . 90 3.3.2 Hysteresis in the transconductance of SWNT devices . 97 3.4 Conclusions and future work . 101 Chapter 4 SWNT as AFM probes 103 4.1 Fabrication of SWNT-AFM tips . 105 The 'pick-up' technique . 107 iv Electrical Pulse Shortening . 110 4.1.1 Characterisation . 114 Force curve analysis . 114 Electron microscopy . 116 4.2 Imaging with SWNT-AFM tips . 120 4.3 Electrical transport through nt tips . 127 4.3.1 Fabrication of electrically connected nt tips. 128 4.3.2 Transport through nt tips and a liquid (Hg) electrode . 129 Length dependence of resistance . 134 4.3.3 Transport through nt tips and a solid electrode . 136 4.4 SWNTs as templates for nanowire conducting probes . 139 4.5 Conclusions and future work . 148 Chapter 5 Increased Resolution EFM and SGM 150 5.1 Increased Resolution EFM . 151 5.1.1 Theoretical background to force gradient EFM . 151 Tip cone and cantilever contributions to the electrostatic force 155 Real oscillation amplitudes . 158 Conclusions ............................ 160 5.1.2 Force gradient EFM with nt tips . 161 SWNT arrays for EFM spatial resolution calibration . 163 Comparison of the resolution of Si tips and nt tips. 168 High resolution EFM imaging with nt tips . 169 z dependence of the frequency shift . 172 Conclusions ............................ 174 5.2 Torsional Resonance Mode EFM . 175 5.3 Increased Resolution SGM . 178 v 5.3.1 ac-SGM of SWNT device . 180 5.3.2 Conclusions ............................ 186 Chapter 6 Conclusions and future work 188 Appendix A Mechanical properties of SWNT and nanowire AFM tips 191 A.1 Flexural rigidity ............................. 193 Appendix B Force exerted by a Hg surface 194 Appendix C Toy model for the lorentzian dependence of the EFM linescan 196 vi List of Tables 1.1 Dependence of chiral angle and diameter on (n; m) indices . 8 1.2 Typical properties of tips used ..................... 37 2.1 Typical growth conditions, with flow rates of Ar = 600 sccm, H2 = 400 sccm, and C2H4 = 2 sccm. ..................... 47 4.1 Properties of the nt tips shown in Figure 4.11. 119 vii List of Figures 1.1 Representation of (a) a SWNT and (b) a MWNT ........... 3 1.2 Number of papers with 'nanotube' in their title or abstract from a Web of Science search. .......................... 4 1.3 Timeline .................................. 5 1.4 Lattice structure of graphite sheet ................... 6 1.5 Schematic of the formation of SWNTs by rolling a sheet of graphite 7 1.6 Band structure of graphite ........................ 10 1.7 Quanitisation conditions for SWNTs . 12 1.8 SWNT schematics ............................ 13 1.9 STM and STS of SWNTs ........................ 14 1.10 SPM introductory ¯gure ......................... 20 1.11 Force transduction in AFM ....................... 21 1.12 Schematic of c-AFM ........................... 22 1.13 Schematic of a force curve in contact mode. 23 1.14 Schematic of (a) free oscillation, and (b) intermittent contact . 25 1.15 Theoretical frequency response of a tapping mode cantilever . 27 1.16 Experimental frequency response of a tapping mode cantilever . 28 1.17 Tapping mode force curves ....................... 29 1.18 Comparison of the di®erent topogrqaphical imaging modes . 32 viii 1.19 Schematic of a tip operating in lift mode. 33 1.20 Schematic of Scanned Conductance Microscopy. 35 1.21 The AFM tip and cantilever ....................... 36 1.22 Topography of 30% Al on Al In Sb. ................... 37 1.23 Thermal tune spectrum ......................... 38 2.1 Upper Photographs, and lower schematic of the cCVD setup. 45 2.2 Height images of SWNT grown with (a) C2H4, and (b) CH4. 48 2.3 Nanotube growth on SiO2, Si, and Si on sapphire substrates. 49 2.4 Height images of low and high density cCVD growth. 52 2.5 Histogram of SWNT diameters from Figure 2.2 (a) . 53 2.6 (a) topography, and (b) SCM image of a SWNT growth sample. 54 2.7 FESEM images of a SWNT growth substrate . 57 2.8 TEM images of a bundle of SWNTs on an AFM tip . 58 2.9 Raman spectrum of SWNTs ....................... 61 2.10 Metal electrodes under resist in the LSM. 64 2.11 SEM images of a SWNT device pattern. 66 2.12 Schematic of the lift-o® process ..................... 67 2.13 Optical and AFM images of SWNT device pattern. 68 2.14 AFM topography image / schematic of a SWNT device. 69 2.15 Electrical characteristics of a sSWNT device. 72 2.16 Gate response of a metallic SWNT device. 73 2.17 Gate response of a mSWNT device displaying weak VG dependence. 74 2.18 i ¡ Vsd response of a mSWNT device at VG = 0 V. 74 3.1 Experimental setup for multiple contact experiments on the Dimen- sion AFM. ................................. 79 3.2 SEM images of a bonded sample on a PCB. 81 ix 3.3 Optical images of a bonded sample on a PCB. 81 3.4 Experimental setup for multiple contact experiments on the Multi- mode AFM. ................................ 81 3.5 Schematic of the setup for SGM. .................... 82 3.6 SGM image of a sSWNT device in the depletion regime. 83 3.7 SGM image revealing the active SWNT. 83 3.8 Intentional cutting of SWNTs ...................... 84 3.9 Accidental cutting of SWNTs revealed by EFM . 84 3.10 A SWNT device with a kink. ...................... 86 3.11 i ¡ Vsd response of the device after insertion of kink. 86 3.12 SGM and EFM images of the response of the kinked device . 87 3.13 1.3 ¹m topography and SGM images at di®erent Vtip, Vsd = ¡1 V. 88 3.14 left; Vtip response of the device after insertion of kink. right; Current as a function of distance of the tip from the kink, Vtip = 5 V. 88 3.15 i ¡ Vsd response of a mSWNT device showing current saturation. 91 3.16 SSPM and SGM images of a mSWNT device . 91 3.17 Simpli¯ed schematic demonstrating the variation in potential along the SWNT in a device for ballistic, and di®usive transport. 92 3.18 SSPM images of the mSWNT device at low and high bias voltages. 93 3.19 Fitted SSPM images comparing the behaviour at low and high bias . 95 3.20 left; Gate response of the device taken at 1 V bias. right; i ¡ Vsd response at VG = 0 V. .......................... 97 3.21 Current at 1 V bias through the device as a function of time, with pulses of VG = §10 V. .......................... 98 3.22 Schematic of the charge injection process . 99 3.23 SSPM images of the device showing charge injection. 100 x 4.1 TEM image of a SWNT-AFM tip fabricated by direct cCVD growth. 106 4.2 Schematic of the pick-up process. 107 4.3 Amplitude and height images whilst scanning a pick-up sample. 108 4.4 TEM image of an nt tip fabricated by the pick-up technique . 110 4.5 Length of nt tip giving Ath = 0:5 nm (solid line), and Fb = 10 nN (dashed line), plotted as a function of nt tip radius. 111 4.6 Height and amplitude images taken during shortening of an nt tip. 113 4.7 Schematic of the buckling of an nt tip. 114 4.8 Force curve response of an nt tip . 115 4.9 Amplitude response showing 4 buckling events, implying the presence of several SWNTs of di®erent lengths. 116 4.10 FESEM image of an nt tip. 117 4.11 TEM images of nt tips . 119 4.12 Examples of high resolution imaging with nt tips . 121 4.13 Images of DNA taken with nt tip. 123 4.14 Images of a silica ¯lm demonstrating the longevity of nt tips. 124 ¡1 4.15 Length of nt tip giving kl = 10 N m (solid line), and Fb = 1000 nN (dashed line), plotted as a function of nt tip radius. 125 4.16 Contact mode image of Au ¯lm taken with an nt tip . 126 4.17 Experimental setup of Hg electrode experiment, and example current and deflection responses. 130 4.18 Schematic of immersion of an nt tip into a Hg microelectrode. 130 4.19 i ¡ V responses of nt tips taken with a Hg electrode .
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