ll91* ~± 1=1 tm ~~m 1rrd~! li E01WM 22
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~f~ . LL.I;;/ )(.. . ____ _ ll91* ~± 1=1 tm 1rrd~! li E01WM 22: m R:P-~m~ili:'tiMWFJL 1~~~Yfn : ~P:-%i~ ~Jc ± ------~~~~------ 9 ~f4¥rSJE4m:f:11iJf1Efofr ~{,'1.~~lj : ------- ~~=-- - ~--'- ' --'--'-' t:W'-=-± =--- ----- 2017 11 J=j
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Transcript of ll91* ~± 1=1 tm ~~m 1rrd~! li E01WM 22
~f~ . LL.I;;/)(.. . ____ _
ll91* ~± 1=1 tm ~~m 1rrd~! li E01WM 22: m R:P-~m~ili:'tiMWFJL
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2017 ~ 11 J=j
Upgrade of a Four-probe Scanning Tunneling Microscopy
System and Electrical Transport Properties of Graphene
By
Ruisong Ma
A Dissertation/Thesis Submitted to
The University of Chinese Academy of Sciences
In partial fulfillment of the requirement
For the degree of
Doctor/Master of Science
Institute of Physics
Chinese Academy of Sciences
Nov, 2017
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Abstract
Abstract
Graphene, a two-dimensional (2D) crystal with a honeycomb structure, has novel
mechanical, electrical, optical properties and potential applications, such as field-effect
transistors, solar cells and flexible transparent electrodes, etc. Due to its unique
properties, it is of great importance both in fundamental science and industrial
applications. In the past decades, researchers have developed a variety of ways to
synthesize high-quality and large-area graphene. However, an obstacle in practical
electronic applications of large-area graphene is its polycrystalline nature and the
presence of defects such as grain boundaries (GBs) would strongly scatter charge
carriers. Therefore, the conductivity and mobility are reduced, which impact its large
scale technological applications in electronics. To study the transport properties of
graphene, the synthesized graphene should be transferred to the insulating substrate and
lithographically defined electrodes are fabricated in order to connect with the
macroscopic measuring instrument. The microfabrication process would inevitably
contaminate graphene surface and thus changes its intrinsic transport properties. The
four-probe scanning tunneling microscope (STM) is ideal for utilizing the ultra-high
spatial resolution of STM in standard four-point transport characterization and can
effectively characterize the morphology and transport properties of graphene and other
2D crystals in situ.
This PhD thesis is focused on the upgrade of a commercial ultra-high vacuum
(UHV) four-probe STM system, morphology and transport properties of single-crystal
and polycrystalline graphene grown by chemical vapor deposition (CVD).
The first part of the thesis is the upgrade of a commercial UHV four-probe STM
system. The first generation of commercial UHV four-probe STM system was
manufactured by OMICRON company. As the world's earliest commercial multi-probe
system (model: UHV Nanoprobe), it cannot effectively characterize the morphology
and transport propertie of nano systems in situ as proposed. In views of the problems
in large noise, obvious thermal drift and low resolution, the upgrade is mainly focused
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on several aspects, including vibration isolation and damping, scanning structure,
thermal links and thermal shielding, time-shared control unit, and replacement of the
scanning electron microscope by an optical microscope. Meanwhile, modifications in
sample pretreatment and wire shielding are also introduced. After the upgrade, the
performance of the four-probe STM system has been fundamentally improved in signal
to noise ratio, mechanical and temperature stabi lity, imaging resolution, cooling, etc.
The second part of the thesis is direct four-probe measurements of conductivity and
mobility in millimeter-sized single-crystalline graphene. The STM characterization
verifies the continuity of CVD-grown graphene on Cu foil. Direct four-probe
measurements of millimeter-sized single-crystalline graphene on Si02/Si are performed
by the upgraded system. The extracted conductivity and mobility of the overall
graphene flake from three setups via van der Pauw geometry confirm homogenous
nature of the whole graphene flake. However, the local transport properties measured
via square and collinear configurations show great deviations from the overall
properties. These differences are due to the local distributions of graphene wrinkles,
residues, and multilayered graphene islands on the monocrystalline graphene sheet,
affecting the local transport properties of graphene, but the presence of these factors
does not destroy uniform nature of the whole graphene flake.
The third part is direct four-probe measurement of grain-boundary resistivity and
mobility in millimeter-sized graphene. The work was focused on graphene bicrystals
transferred onto Si02/Si substrate, ensuring s ingle GBs in the measurements. Non
destructive four-probe measurements of intra-grain and inter-grain sheet resistances are
performed on graphene bicrystals. To extract GB resistivity, an extending model based
on Ohm's law is proposed, and accordingly, GB resistivities under different carrier
densities can be obtained. In addition, this model can be applied to the measurements
of graphene wrinkles. Based on the Drude transport model, the carrier mobility of
graphene GBs or wrinkles can be extracted. The results show that the mobility of GBs
is three to four orders of magnitude lower than that of intrinsic graphene, and the
mobility at the wrinkles is about 1/6 to 1/5 of intrinsic graphene. This work extends the
IV
Abstract
understanding of the intrinsic electron transport properties of graphene GBs/wrinkles,
and shows the unique advantages of four-probe STM systems in studying the effects of
microstructures such as defects on the transport properties of materials. Moreover, it
provides a feasible method to characterize the transport properties of GBs on other 2D
materials.
KEY WORDS: [four-probe STM, upgrade, grain boundary, resistivity, mobility]
V
AFM
ASNOM
BEEM
BNC
CCD
CPLD
cu CVD
DOS
EFM
FET
GB
HOPG
Atomic Force Microscopy
Apertureless Scanning Near-field Optical Microscope
Ballistic Electron Emission Microscopy
Bayonet Nut Connector
Charge Coupled Device
Complex Programmable Logic Device
Control Unit
Chemical Vapor Deposition
Density of States
Electric Force Microscopy
Field-effect Transistor
Grain Boundary
Highly Oriented Pyrolytic Graphite
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57
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Material Properties EBL #2
d31AN@293 K -1.73
d33A/V@293 K 3.8
d31A/[email protected] K -0.3 I
d33A/[email protected] K 0.69
Dielectric constant KT3 1725
AC depoling field kV/cm rms 7
Young's modulus 1010 Nini 6.3
Curie Temperature ·c 350
Thermal Conductivity W /m • ·c 1.5
Thermal expansion coefficient ppm/°C ---Density g/cm3 7.5
Mechanical Q 100
Poisson's ratio 0.31
Industry Type PZT-5A
61
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106
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A 2D'
2D
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G
A 20'
1000 1500 2000 2500 3000 3500 Raman shift (cm·')
1fil~7 Grain-I CMB, Ri o ) , Grain-2 CttB, R 20 ) ;fD~~W (~B, R inter-grain
o ) Er-J = ~tit~Jl Ra o ..tJ£= ~tit1m Ro.!:§~W· i:g~Jl R1 1v23 Er-1*-*Y~:
(4.5)
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ffit B'-JIK~o
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107
R - 2TCRI IV23
o - ln((s 2+(s+J)2)/s2) o
(a) 60oo~======~
5000
4000
£ 3000
0:.0 2000
1000
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(c) eooo~------~
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~ 4000
D 3000 .s ~ 2000 .; 11 1000
0:.
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(b)
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s+A.
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5 (1012cm·2)
2TC R inter-grainD = --R /IV23 °
In 2
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(4.7)
(4.8)
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7.0 kQ•µmo
(a)
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0 5000
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;2000 s
rr.i= 1000
101,1m
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5000
- 4,000
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109
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r 2000 E
er 1000
(b)
G
G
1000 1500
- ExperlmenI • F tt g
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~ 0 1 2 3 4 5 6 n,(10'~cm" )
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20
20'
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)
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- = -~ms<J~~ffi. ft~~a~~tt~~ o
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110
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111
(4.14)
( 4.16)
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(4.17)
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~~ s to s+l '.5tJJU79fr" Ji.JB~%~:ill* ( 00 4.10 (b) ) o 4 Rm= R20= Ro , !i!U0
~( 4.20)r.iJ ~ WH-tn0~(4.9):
Ra s2+(s+1)2 ~nter-grainD = f(Ra,s,A)= ln
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112
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µm o EB J..=p00/R20, "i:iJi-1-~>1<1~ GB-Sl ;flJ GB-S2 Wlt~.EI.$ C 00 4.9 (c);flJ(f)) o
xt r GB-S1, ;!( P GB W'.3t1tffill~ EB 5.9 ~ 26.4 k.Q•µm, imxtr GB-S2, P GB 1¥1
~1t1i11E~ 1.7 ~ 9.5 k.Q•µm o
(a) 1500 -g,-::! (c)1ao -GS-S3r..-st,-"lt'j ~
6000
0 £ 4500
rr::° 3000
150 .. . . . .
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V "'""' (e) 7500
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(d) 7500
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60 !\ 6000
£ 4500 0
a: 3000
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3'¥-1~~ rt~.§.$ 1¥]~,f,tffi~ 133-fLl-a g; kQ•µm ( 00 4.12 (a)) o
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J '' I i :U I O _,,.,
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1E·3 ,_,__._.._.__,___,__,__._..__.__,___,__,__._.,_,
Reference
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Katsnelson, Yu. N. Gornostyrev, K.Watanabe, T. Taniguchi, C. Casiraghi, H-J. Gao,
A. K. Geim and K. S. Novoselov
"Commensurate-incommensurate transition in graphene on hexagonal boron
nitride"
Nature Phys., 10,451 (2014)
[5] Guocai Wang, L ihong Bao, Ruisong Ma, Tengfei Pei, Yu-Yang Zhang, Liangmei
Wu, Zhang Zhou, Haifang Yang, Junjie L i, Changzhi Gu, Shixuan Du, Sokrates T
Pantelides, Hong-Jun Gao
"From bidirectional rectifier to polarity-controllable transistor in black
phosphorus by dual gate modulation"
2D Mater., 4, 025056 (2017)
[6] Guocai Wang, Lihong Bao, Tengfei Pei, Ruisong Ma, Yu-Yang Zhang, Liling Sun,
Guangyu Zhang, Haifang Yang, Junjie Li, Changzhi Gu, Shixuan Du, Sokrates T.
Pantelides, Ronald D. Schrimpf, and Hong-Jun Gao
"Introduction of Interfaciaf Charges to Black Phosphorus for a Family of Planar
Devices"
Nano Lett., 16, 6870 (2016)
[7] Tengfei Pei, Lihong Bao, Ruisong Ma, Shim Song, Binghui Ge, Liangmei Wu,
Zhang Zhou, Guocai Wang, Haifang Yang, Junjie Li, Changzhi Gu, Chengmin
Shen, Shixuan Du, and Hong-Jun Gao
"Epitaxy of Uftrathin SnSe Single Crystals on Polydimethylsiloxane: In-Plane
EL ectrical Anisotropy and Gate - Tunable Thermopower"
138
Adv. Electron. Mater., 2, 1600292 (2016)
[8] Jun Li, Jianing Zhuang, Chengmin Shen, Yuan Tian, Yande Que, Ruisong Ma,
Jinbo Pan, Yanfang Zhang, Yeliang Wang, Shixuan Du, Feng Ding, Hong-Jun Gao
"Impurity-induced formation of bilayered graphene on copper by chemical vapor
deposition"
Nano research, 9, 2803 (2016)
[9] Tengfei Pei, Lihong Bao, Guocai Wang, Ruisong Ma, Haifang Yang, Junjie Li,
Changzhi Gu, Sokrates Pantelides, Shixuan Du, and Hong-Jun Gao
"Few-layer SnSe2 transistors with high on/off ratios"
Appl. Phys. Lett., 108, 053506 (2016)
[10] X. M. Zhang, R. S. Ma, X. C. Liu, G. Z. Xu, E. K. Liu, G.D. Liu, Z. Y. Liu, W.
H. Wang and G. H. Wu
"Topological insulators with unexpectedly HgTe-like band inversion in hexagonal
wurtzite-type binary compounds"
EPL., 103, 57012 (2013)
[11] Zhao-Ming Wang, Roi-Song Ma, C. Allen Bishop, and Yong-Jian Gu
"Quantum state transfer through a spin chain in a multiexcitation subspace"
Phys. Rev. A, 86, 022330 (2012)
[12] Su-Na Fan, Ren-Wei Liu, Roi-Song Ma, Shan-Sheng Yu, Ming Li, Wei-Tao
Zheng, Shu-Xin Hu
"Two-dimensionalpolyaniline nanosheets via liquid-phase exfoliation"
Chin. Phys. B, 26, 048102 (2017)
139
[ 1] Ruisong Ma, Qing Huan, Liangmei Wu, Jiahao Yan, Yu-Yang Zhang, Lihong Bao,
Shixuan Du, Sokrates T Pantelides, and Hong-Jun Gao
Direct Four-Probe Measurement of Grain-Bounda,y Resistivity and Mobility in
Millimeter-Sized Graphene (poster)
Chinese Physical Society 2017 fall meeting, Sep. 2017, Chengdu, Sichuan, China
[2] Ruisong Ma, Qing Huan, Liangmei Wu, Jiahao Yan, Qiang Zou, Aiwei Wang,
Christian A. Bobisch, Lihong Bao, and Hong-Jun Gao
Upgrade of a Commercial Four-probe Scanning Tunneling Microscopy System
Improvement of STM Resolution, Cooling Capability and Stability (poster)
20th International Conference on Non-Contact AFM, Sep. 2017, Suzhou, Jiangsu,
China
[3] Ruisong Ma, Jiahao Yan, Qing Huan, Lihong Bao, Shixuan Du, and Hong-jun Gao
Upgradation of a commercial four-probe STM system-Improvement of STM
Resolution, Cooling Efficiency and Stability (poster)
2016 annual academic forum of CVS, Aug. 2016, Kunming, Yunnan, China
[4] Ruisong Ma, Guocai Wang, Qing Huan, Lihong Bao, Xiao Lin, Hongliang Lu, and
Hong-jun Gao
The Upgrading of Four-probe STM- lmprovement of STM Resolution and Cooling
Efficiency (poster)
2014 annual academic forum of CVS, Nov. 2014, Guangzhou, Guangdong, China
140
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