Li 2018

Review
2D Materials
www.advmatinterfaces.de
Mechanical Properties of 2D Materials Studied

by In Situ Microscopy Techniques
Xing Li, Mei Sun, Chongxin Shan, Qing Chen, and Xianlong Wei*
chemical and flow sensors,[8–11] flash

Two-dimensional (2D) materials have been demonstrated as promising memories,[12–14] analog electronics, etc.[15]
building blocks in future electronic and their mechanical properties are quite The emergence of transition metal dichal-
important for various applications. Due to their atomic thickness and planar cogenides (TMDs) with sizable bandgap
and intriguing optical phenomena,[16–18]
nature, the investigation of the mechanical properties and related atomic like strong quantum confinement,[19]
mechanism are quite challenging. This review focuses on the recently doping-dependent charge excitons, and
developed in situ techniques based on scanning electron microscopy (SEM), valley polarization,[20–25] further extends
transmission electron microscopy (TEM), and atomic force microscopy the application of 2D materials in field
(AFM) in characterization of the mechanical properties of 2D materials. effect transistors and novel optoelec-
tronics devices.[26] Different from three-
In situ methods used for studying their elastic properties, fracture behavior,
dimensional (3D) crystalline materials and
and surface/interface energy are introduced in detail. Specifically, the AFM one-dimensional (1D) nanowires, most 2D
indentation test and microelectromechanical systems (MEMS) device are materials have a layered structure, which
generally used to investigate the elastic properties; the manipulator based consists of covalent bonds in each layer
methods show their flexibility in studying the fracture, adhesion, cleavage, and is stacked together with van der Waals
and friction properties; atomic level fracture mechanism can be revealed interactions. This special crystal struc-
ture may endow these 2D materials with
with in situ high resolution TEM (HRTEM); the pressurized blister test and unique elastic, fracture, surface, and inter-
the buckle/wrinkle based methods are widely used to measure the surface/ facial properties.
interface properties. Moreover, the influence of sample preparation process, Investigation of their mechanical
defects and layer numbers to their mechanical properties are also discussed. properties and the underlying mecha-
Finally, the extensions of above methods to investigate the strain-modulated nisms can not only help us to know
better about 2D materials, but also acts as
physical properties of 2D materials are introduced.
a key procedure in developing new appli-
cations. First, because of their atomic
thickness and ultrahigh flexibility,[27–30]
1. Introduction 2D materials have been used as highly conducting and trans-
parent electrodes in flexible, stretchable, foldable electronics,
The successfully cleavage of graphene from graphite has pushed and their Young’s modulus and fracture behaviors are of vital
forward the development of two-dimensional (2D) materials. importance in these applications. Secondly, friction and wear
Until now, many other 2D materials like transition metal- are the main concerns which lead to unnecessary energy
dichalcogenides (TMDs), boron-nitride (BN), and black phos- loss and mechanical failures in industry and the hexagonal
phorous (BP), etc. have been discovered. Due to the high carrier molybdenum disulfide (MoS2) has long been used as solid
mobility,[1,2] high density of states, and unique physical proper- lubricant.[31] The emergence of other 2D materials with weak
ties originating from its low dimensionality planar atomic struc- interlayer interaction can provide us more choices in finding
ture and band structure, graphene has been widely explored ultrathin coatings and solid lubricants that can work reliably
in various applications, such as transistors,[3–6] amplifier,[7] and efficiently. Additionally, the covalent-bonded network
and their ability to integrate and adhere to various substrates
make them promising materials for microelectronics. There-
Dr. X. Li, Prof. C. Shan fore, the adhesion and interfacial properties of these 2D mate-
Department of Physics and Engineering rials are quite critical for the emerging technologies. Finally,
Zhengzhou University
Daxue Road 75, Zhengzhou 450052, China it has been proved theoretically and experimentally that the
M. Sun, Prof. Q. Chen, Dr. X. Wei band structure.[32–34] electronic, magnetic and optoelectronic
Key Laboratory for the Physics and Chemistry of Nanodevices properties of 2D materials can be modulated with strain engi-
and Department of Electronics neering.[35–40] Therefore, their mechanical properties measure-
Peking University ment is indispensable to evaluate related performance.
Beijing 100871, China
E-mail: weixl@pku.edu.cn
Theoretical calculations indicate that 2D materials usually
possess good elastic properties and their fracture properties
DOI: 10.1002/admi.201701246 are closely related with the crystal direction, grain boundaries,
Adv. Mater. Interfaces 2018, 1701246 1701246 (1 of 24) © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim
www.advancedsciencenews.com
and defects.[41] The negative Poisson’s ratio and the dependence

of surface/interlayer properties on the layer orientations have Xing Li obtained his
also been predicted. Hence, the experimental verification of Ph.D. in 2017 at Peking
these properties is quite necessary. However, the atomic thick- University (China) in physical
ness and planar nature of few-layered 2D materials have made electronics and was a visiting
their manipulation quite difficult and the mechanical properties scholar in Rice University in
measurements can hardly be realized with traditional methods. 2015. She now works in the
Therefore, new methods should be developed to realize easy department of physics and
manipulation of 2D materials, direct observation of the mechan- engineering in Zhengzhou
ical behavior at microscale/atomic level and revelation of the University. Her research focus
crystal-structure-dependent mechanical properties. is on the crystal structure
By introducing micromanipulators or multifunctional sample dependent physical properties
holders into material characterization systems like scanning of 1D and 2D nanomaterials,
electron microscope (SEM), transmission electron microscope including the mechanical, electromechanical, and electro-
(TEM), atomic force microscope (AFM), etc., the in situ micro chemical properties.
scopy techniques have been widely applied to study the physical
properties of various nanomaterials and reveal the underlying Qing Chen obtained her
mechanisms of related devices. As a versatile technique, the in Ph.D. in 1996 at University
situ microscopy technique has shown its advantages in exploring of Science and Technology
the mechanical properties of 2D materials from their basic Beijing (China) in Materials
behaviors to atomic level mechanisms. Science. After a COE
In this review, we will concentrate on the mechanical prop- researcher at the National
erty measurement of 2D materials through in situ microscopy Institute for Materials
techniques, which enable the property measurement of nano- Science (Japan) and a
material under the real time visualization of various micro postdoc at Arizona State
scopy techniques, e.g., SEM, TEM, and AFM. The advantages University (USA), she moved
and applications of in situ microscopy techniques in material back to Peking University
science and mechanical property measurement are intro- (China) in 2001. Since 2002,
duced in Section 2. The preparation processes of 2D mate- she was a full Professor in Department of Electronics,
rials are summarized in Section 3. The elastic and fracture Peking University. Her current research interests
properties measurement methods of 2D materials are intro- include nanodevices based on nanowires, nanotubes,
duced in Section 4. The experimental measurement results and nanosheets, and correlating properties and structures
of Young’s modulus and fracture properties are summarized of nanomaterials and nanodevices through in situ electron
in Sections 5 and 6. Measurements of the surface/interface microscopy study.
properties are introduced in Section 6. Besides, extension of
Xianlong Wei obtained his
the in situ mechanical measurement methods of 2D materials
Ph.D. in 2009 at Peking
in other fields is introduced in Section 7. Extensions of the in
University (China) in physical
situ mechanical methods of 2D materials are simply intro-
electronics, and then he
duced in Section 8. Finally, problems remained to be solved
worked in National Institute
in the mechanical property measurement of 2D materials are
for Materials Science (Japan)
discussed in Section 9.
for three years first as a post-
doctoral researcher and then
as an ICYS fellow. He currently
2. In Situ Microscopy Techniques works in Peking University as
an assistant professor from
Although nanomaterials possess small sizes, in situ micro
September 2012. His research
scopy techniques provide us powerful tools to investigate
areas include in situ electron microscopy of nanomaterials
their properties, establish property–structure relationships
and vacuum nanoelectronics.
of nanomaterials, reveal their difference with bulk materials
and verify the adaptation of the macroscopic physical law
in nanoscale. Generally, in situ microscopy techniques have
helped us to understand materials science in the following electrochemical properties under external stimulus can be
four aspects: investigated.[46,47] More importantly, novel physical phe-
First, as a relatively flexible technique, external stimulus nomena, like the brittle-to-ductile transition of silica glass
can be introduced through holders and various microelectro- nanofiber,[48] cold welding of Au nanowire, etc.,[49] can also be
mechanical systems (MEMS) chips. The manipulation of nano- revealed with in situ microscopy technique.
materials can be easily realized with nano/micromanipulators Second, the relationship between material properties and
and their corresponding physical properties like thermal,[42,43] microstructures can also be revealed with in situ microscopy
mechanical,[44] electrical,[45] optical, electromechanical, and techniques. The crystal structure, growth direction, and size
related electrical transport properties, mechanical and elec- AFM technique is widely used to measure the mechanical and
tromechanical properties of nanomaterials can be system- electromechanical properties of 2D nanomaterials because of
atically investigated with the help of in situ SEM and TEM the convenient force and displacement measurements with an
techniques.[45,50,51] AFM tip. The Young’s modulus, breaking strength and friction
Third, along with the resolution improvement of TEM, the coefficient of 2D materials can be directly measured with AFM,
synthesis,[52,53] diffusion,[54] and reconstruction process of mate- while the interfacial property measurements of 2D materials
rials can be directly observed at the atomic scale,[55,56] related usually require other sample preparation process like wrinkles/
thermodynamic and thermokinetic problems in materials blister formation. Though the above-mentioned mechanical
science can be easily understood and insights for the macro- parameters can be easily measured, the corresponding mechan-
scopic growth of nanomaterials can be provided. ical behaviors like crack formation and propagation process
Finally, by constructing various devices in situ in a TEM, the cannot be intuitively illustrated.
microscopic mechanism of macroscopic devices can be explored SEM provides a spatial resolution of about several nano
and the underlying mechanisms of various devices, like lithium- meters and various probes, like electrical measurement
ion battery,[57,58] resistive random access memory,[59] and cata- probes, optical fiber probes, and force sensing probes, etc.,
lytic behavior can also be intuitively revealed.[60–65] This is quite can be introduced into its large sample chamber for multiple
critical for the analysis of material structure change during the property measurements of nanomaterials (Figure 1a). By con-
device applications and instructions for device performance ducting suitable measurements methods in SEM, various
improvement can also be provided. mechanical properties, and related behaviors of 2D materials
To investigate the physicochemical properties of nanoma- can be successfully obtained. Specifically, the elastic proper-
terials, in situ techniques based on AFM, SEM, and TEM are ties of 2D layered materials can be measured with in-plane
generally utilized (Figure 1). AFM shows its advantage in thick- tensile test conducted with MEMS devices. The interfacial
ness and topography characterization of nanomaterials. In situ behaviors like friction, sliding, and peeling between layers
Figure 1. In situ microscopy techniques for investigating the physicochemical properties of nanomaterials. a) Schematic illustration of the in situ
SEM technique: various size-dependent physical properties of nanomaterials can be studied with different probes and platform introduced into the
SEM chamber. Reproduced with permission.[66] Copyright 2016, Inderscience Enterprises Ltd. b) Images showing the mechanical property measure-
ment sample holder and investigation of atomic level growth of ZnO nanopillar and microstructure evolution of electrode materials in lithium-ion
battery with in situ HRTEM. Left: Reproduced with permission.[67] Copyright 2015, American Chemical Society. Middle: Reproduced with permission.[68]
Copyright 2017, Nature Publishing Group. Right: Reproduced with permission. Reproduced with permission.[57] Copyright 2016, Elsevier. c) Schematic
illustration of the mechanical properties measurement setup with AFM.
Figure 2. Advantages of various in situ techniques in studying the mechanical properties of 2D materials. a) SEM and TEM images of the uniaxial tensile
tests realized with in situ SEM and TEM with MEMS devices. TOP: Reproduced with permission.[73] Bottom: Reproduced with permission.[74]
Copyright 2017, Nature Publishing Group. b) TEM images showing in situ investigation of the atomic level cleavage process and fracture mechanism.
Left: Reproduced with permission.[75] Copyright 2014, American Chemical Society. Right: Reproduced with permission.[76] Copyright 2016, Nature Publishing
Group. c Top: Reproduced with permission.[77] Copyright 2014, ACS Publications. Bottom: Reproduced with permission.[78] Copyright 2015, The American
Association for the Advancement of Science. Schematic illustrations showing the surface/interface energy and friction coefficient studied with in situ
SEM/AFM techniques. d) Images showing the nanoindentation test of suspended 2D films with AFM. Reproduced with permission.[79] Copyright 2008,
The American Association for the Advancement of Science.
can be realized with novel experimental design. During these and reveal the influence of crystal structure, defects, and
probe based measurements, the force and size can be meas- crystallographic direction on the mechanical parameters of
ured with the AFM cantilever and SEM images, thus corres materials.
ponding coefficients like friction coefficient, surface energy, The above-mentioned in situ AFM, SEM, and TEM tech-
etc., can be quantitatively obtained. However, limited by the niques (Figure 2) are complementary to each other and can
resolution of SEM, the underlying mechanisms at atomic help us to understand the mechanical properties and related
level and their relationship with crystal structure, crystallo- mechanisms of 2D materials comprehensively. Details for
graphic direction, and defects cannot be revealed. the mechanical property measurement of 2D materials will be
Along with the resolution improvement, in situ TEM tech- discussed in detailed in Sections 4–6.
nique shows its advantage in the atomic-level investigation
of materials. Although TEM chamber is relatively smaller
than SEM, various in situ TEM holders enabled heating,[69] 3. Sample Preparation Process
mechanical measurement,[70] chemical reactions, etc.,[71]
have been developed. Moreover, the introduction of optical The mechanical properties of various 1D nanomaterials have
fibers and gas into the TEM chamber further expands its been widely investigated with electric-field-induced resonance
applications.[72] Thus, in situ TEM technique is now a com- method,[70,80] bending and uniaxial tensile tests conducted
prehensive technique to study the physicochemical proper- in SEM or TEM,[51,81,82] which generally require effective
ties of materials at atomic level and has become an essential and controllable fixation of suspended nanomaterials with
tool to observe various mechanical processes at atomic level probes/stages. However, due to the planar nature and atomic
thickness, 2D materials tend to fold and break during their thus the materials supported by PMMA is floating on the
manipulations, making their in situ mechanical measure- solution. After cleaning with deionized water, the PMMA
ment more difficult than 1D nanomaterial. Therefore, novel supported 2D material is fished out with desired substrate
transfer and sample preparation process should be developed (Figure 3a). Finally, the PMMA is removed with acetone or
in order to precisely obtain mechanical parameters for single thermal annealing.
or few layered 2D materials. The in situ mechanical measurements usually require the
transfer of nanomaterials onto specific positions of stages,
while the mechanical exfoliation and PMMA assisted methods
3.1. Transfer Process can only transfer samples onto random positions of substrates.
To solve this problem, Yang et al. has developed a site-specific
To ensure their flatness and integrity, 2D materials should be transfer method for 2D materials.[73] Specifically, in the final
supported by substrates during their mechanical measure- step of the PMMA assisted transfer process, the PMMA sup-
ment and the transfer process of atomic layer 2D materials ported 2D material is fished out with a clean copper grid,
onto targeted substrate is the precondition. Different from which possesses a relatively larger surface roughness com-
1D nanomaterials, which can be easily transferred by the pared with Si substrate. Thus, the contact area between
mechanical scratch or solution-based method,[44] the transfer PMMA supported material and the copper substrate can be
of 2D materials are usually accomplished by mechanical reduced, preventing them from sticking to the substrate. With
exfoliation, poly(methyl methacrylate) (PMMA) assisted and the help of an optical microscope and a micromanipulator, a
manipulator assisted methods. certain piece of 2D material can be selected, cut and picked
Due to the weak van der Waals interaction between the up from the copper substrate and loaded onto a specific loca-
layers of 2D materials, atomic-thick layered materials can be tion (Figure 3b) of the substrates. Finally, the PMMA can be
obtained by repeated peeling small pieces of corresponding removed with suitable methods. Defined by the micromanipu-
bulk materials with adhesive tapes.[83] This mechanical exfo- lator, the transferred sample is generally in an irregular shape
liation method is widely used to transfer 2D materials from and further process like focused ion beam (FIB) etching is
their bulk materials onto rigid, stretchable, and prepatterned needed, during which thin layered 2D materials, especially the
substrates.[84] suspended ones, are easily broken. To solve this problem and
For the transfer process of single/few layered 2D materials increase the success rate in the mechanical measurement of
grown by chemical vapor deposition (CVD) method, a thin 2D materials, Liu et al. prepatterned PMMA coated graphene
layer of PMMA is usually used to facilitate their transfer. with electron beam lithography (EBL) before the manipulator
Specifically, 200–300 nm thick PMMA is firstly spin coated assisted transfer process.[85]
on the grown samples. Then the substrate where materials The PMMA assisted and site-specific transfer method is
are grown on is etched away by suitable chemical solutions, widely used in sample preparation process of MEMS chip-based
Figure 3. Transfer methods of 2D materials. Illustrations for a) the PMMA assisted transfer of 2D materials onto desired substrates; b) site-specific
transfer of MoSe2 sample onto the MEMS stage with micromanipulators. Reproduced with permission.[73]
tensile testing and in situ atomic-level fracture investigation. 4. Elastic and Fracture Property
Except for the mechanical measurement, the site-specific transfer Measurement Methods
method can also be used to construct 2D heterostructures.
Elastic and fracture properties are important factors in
the applications in flexible electronic devices and nano -
3.2. Shape Control of 2D Materials electromechanical systems of 2D materials. Many theoretical
and computational studies have been performed to investigate
Except for the transfer process, the shape control of 2D mate- the mechanical properties of various 2D materials. Though qual-
rials is also very important for the quantitative calculation itatively evaluation and observation of the superior mechanical
of their mechanical properties. FIB can be used to cut sus- flexibility of 2D materials, e.g., bending, rolling, and stretching
pended 2D materials into rectangular shape, thus uniform behavior, can be demonstrated simply with manipulator-based
tensile stress can be applied and their Young’s modulus and in situ in situ TEM,[88,89] novel and straightforward methods
breaking strength can be precisely obtained.[73] Similarly, are quite necessary for the quantitatively measurement of their
precracks in 2D thin films can also be introduced with FIB elastic and fracture properties. In this section, related in situ
for their fracture toughness measurement. In addition, the microscopy methods in measuring the elastic and fracture
shape control of 2D materials can also be realized by trans- properties of 2D materials are introduced in detail.
ferring them to substrates with certain patterns, which can
be fabricated by EBL and dry etching technique, etc.[86] These
techniques can also be used to fabricate mesas and rectan- 4.1. AFM Based Methods
gular plates of 2D materials for their interfacial property
measurement.[87] The adhesion energy of 2D materials can AFM based methods have been widely used to measure the
also be measured from their wrinkles, which can be formed mechanical properties of nanomaterials. According to the
by releasing the prestrained substrates where 2D materials geometry of the prepared samples, static AFM deflection and
are exfoliated. AFM indentation test can be utilized.
The above discussed transfer and shape control methods For the suspended 2D films fabricated by mechanically exfoli-
can help to realize the mechanical property measurements of ating bulk materials on the patterned trenches (Figure 4a), static
2D materials quantitatively and intuitively with in situ micro AFM deflection method is usually applied. The AFM deflection
scopy techniques. method is a simple, direct and nondestructive approach to obtain
Figure 4. Elastic properties of 2D materials with AFM-based methods. a) 2D materials on prepatterned trenches. b) Illustration for the deflection/
indentation test carried out on freely suspended 2D sheet with AFM tip. The tip deflection and the deformation of 2D material are shown. c) Plot of
the effective spring constant versus W(t/L)3 of eight graphene sheets measured with static AFM deflection method and the Young’s modulus and
pretension can be directly extracted. Graphene sheets with similar length L are selected and their width W and thickness t are variables here, the tension T
is assumed similar in these samples. Reproduced with permission.[90] Copyright 2007, AIP Publishing LLC. d) Plot of Eeff versus L2/W for different
reduced graphene oxide monolayers with the same thickness t and the pretension T can be extracted from the linear fit. Reproduced with permission.[91]
Copyright 2008, American Chemical Society. e) Schematic illustration of the 2D materials covered over circular wells. f) Plot of force verses the deflec-
tion of MoS2 flakes with different layers. Reproduced with permission.[86]
the elastic properties of atomically thin membranes. By pressing unloading process should be carried to verify that no plastic
suspended 2D sheets with calibrated AFM tips (Figure 4b), deformation or membrane detachment occurs during our
their Young’s modulus can be successfully extracted.[90,91] measurement and the material can be considered as elastic.
The width W, length L, and thickness t of 2D materials can be Multiple curves with increasing indentation depths can be
precisely measured with AFM and Raman spectroscopy. It should acquired for each well until mechanical failure of 2D films
be noted that the mechanically exfoliated 2D materials are was observed, and the corresponding force (F) versus δ curves
usually under tension (T). can be plotted.
After dimension measurement, the AFM tip is pushed down Generally, when the AFM tip radius rtip << well radius r, this
slowly in the center of the membrane. Meanwhile, the tip deflec- curve can be fitted by the following equation[79,92]
tion (ηtip) and the position of the piezoelectric tube (zpiezo) moving
the tip are recorded. Thus, with the spring constant (k) of the  4 π E  t 3   Etq 3 
F= ⋅  2  δ + σπδ +  2  δ 3 (4)
AFM tip, relation between the force (F = kηtip) applied by the tip  3 (1 − ν )  r 
2
 r 
and the displacement of 2D sheet (δ) can be obtained. The dis-
placement can be calculated through the following relationship where σ is the prestress in 2D films, δ is the deflection of 2D
films, t is the film thickness, q relates to the Poisson ratio (ν)
zpiezo = ηtip + δ (1) with q = 1/(1.05 − 0.15ν − 0.16ν2), E is Young’s Modulus.
The first term in Equation (4) corresponds to the mechanical
In the small displacements regime of the F–δ graph, the behavior of a plate with a certain bending rigidity. The second
effective spring constant (Keff) of tested 2D materials can be term indicates the mechanical behavior of a stretched mem-
obtained in the linear region with Hooke’s law. According to brane. The third term takes into account the stiffening of the
continuum mechanics, in the case of static deflection measure- layer during the force load cycle which makes F–δ curve non-
ments, for a doubly clamped beam in equilibrium with a static linear. Thus, for thin films, by fitting the acquired F–δ curve
force applied at the center of the beam and under axial tension, with Equation (4), the prestress σ and Young’s modulus E can
the Young’s modulus (E) can be related to Keff and dimension be obtained (Figure 4f). Moreover, when the sample is indented
parameters (W, L, t) by the expression to the breaking point, the breaking strength (σm) for the cir-
cular membrane under a spherical indenter can be derived
3
t T as σm = [FEt/(4πR)]1/2.[79,92] Here, F is the breaking force and
K eff = 16.23 EW   + 4.93 (2)
L  L R is the radius of indenter. Since this equation ignores nonlinear
elasticity, the fracture strength measured here is an overesti-
If the measured suspended 2D sheets have similar L, then mation of the intrinsic value.
W(t/L)3 is expected to vary much more than the T/L term.
By assuming that all the sheets have similar T, the T/L term can
be modeled as a constant offset in the linear fit of Keff and 4.2. MEMS Chip-Based Tensile Testing
W(t/L)3 and E can be extracted from the slope. Figure 4c shows
the plot of Keff versus W(t/L)3 for eight different graphene sam- Expect for the AFM based methods, various MEMS chips
ples with similar L, their thickness t and width W are both vari- have been developed to realize the accurately measurement
ables, and T is assumed to be similar for these samples. The of the elastic properties and simultaneously visualization of
linear nature of the calculated date indicates the rationality of the fracture behaviors of 2D materials. The in-plane tensile
above assumption. device shown in Figure 5a consists of a thermally actuated
However, if the corresponding plot of the experimental data shuttle, which is used to induce tensile strain in materials,
of Keff exhibits a pronounced scatter, sizable built-in tensions (T) and a load shuttle fixed to calibrate springs, which is used to
exists and can be extracted from Equation (3) rewritten from measure the pulling force. Thus the stress–strain curve can be
Equation (2)[91] directly measured. Moreover, Jun Lou’s group have developed
a nanomechanical device used in a SEM and have successfully
3
K eff  L  4.93 TL2 studied the fracture behavior of graphene and MoSe2.[73,93]
E =   − (3)
16.23W t 16.23 Wt 3 The key process of this method contains the following two
steps: (1) site specific transfer of suspended 2D materials
The first term in the right hand is obtained from the experi- onto the testing stages; (2) patterning the transferred film
3
K eff  L  into rectangular shape with FIB for further tests. By using
mental data: E eff =   and this effective modulus (Eeff)
16.23W t the “push-to-pull” mechanism (Figure 5b,c),[74] these devices
4.93 TL2 can transfer the force exerted on the beam by the indenter to
depends on the geometry of the sample: E eff = E + .
16.23 Wt 3 the tension of the stage, thus the in-plane tensile test of 2D
Thus, for samples with fixed thickness t, through the plot of materials can be realized.
Eeff versus L2/W (Figure 4d, where t is fixed, L and W are varia-
bles), we can finally obtain T existing in the sample and E can
also be calculated. 4.3. Manipulator-Based Methods
AFM indentation process is based on 2D materials cov-
ered circular wells (Figure 4e), which is indented by an AFM Combining with SEM and TEM, manipulators provide us
tip at the center position with a constant speed. Loading and more flexibility to investigate various mechanical properties
relationship with crystal structures. In order

to maintain the “double tilt” capabilities of
TEM, several microscopy mechanic devices
have been developed to obtain reliable defect
investigations in crystalline materials.[98] Via
the mechanical force created by the TEM
specimen-supporting grid under electron
beam irradiation, axial tensile experiments
can be conducted on individual nanowires
(NWs) and their deformation processes can
be recorded in situ at the atomic scale.[99–102]
To further control the strain rate and defor-
mation mode, Han et al. have developed a
novel in situ controllable tensile testing
device based on the thermal bimetallic tech-
nique.[103–105] While the fracture behavior
of 2D material is closely related with their
applications, investigation of their crack
propagation manner and mechanism will
help to enhance the mechanical properties
via material design. By tearing 2D mate-
rials with focused electron beam in a high
resolution TEM (HRTEM), the crystallog-
raphy-selective cracking, transgranular/
intragranular fracture, and the dislocation
movement can be in situ observed.[76,106]
Thus, the atomistic information and mecha-
nism about fracture can be presented intui-
tively with this in situ HRTEM method.
5. Young’s Modulus
Figure 5. MEMS chips for the mechanical properties measurement of 2D materials. a) Ther- Generally, 2D layered materials can be exfo-
mally actuated in-plane tensile testing stage and the strain measurement of graphene. SEM
liated from their bulk materials or synthe-
images for the “push-to-pull” devices for the in-plane tensile tests of b) graphene, and
c) MoSe2. a) Reproduced with permission.[94] Copyright 2014, American Chemical Society. sized with CVD method.[107,108] Compared
b) Reproduced with permission.[74] Copyright 2017, Nature Publishing Group. c) Reproduced with pristine samples, CVD grown samples
with permission.[73] usually contains vacancies and grain bound-
aries. Therefore, the comparison of the
of 2D materials (Figure 6). This method generally consists mechanical properties of 2D materials prepared with different
of a W probe to exert different mechanical deformations to methods and the revelation of the influence of various defects
nanomaterials and an AFM probe to sense the exerted force. is quite necessary.
With manipulator-based method conducted in TEM, fracture
toughness and the relationship with the crack geometrical
structure of multilayer 2D materials can be directly revealed. 5.1. Pristine 2D Materials
The bond-breaking manner can also be witnessed simultane-
ously.[67] Related mechanical processes like interlayer sliding, Investigated with the AFM deflection method, the Young’s
shearing, and exfoliation,[75,95] and interfacial properties like modulus along the basal plane of the mechanical exfoliated
surface energy, frictional coefficient, and cleavage energy graphene with thickness of 2–8 nm has been reported to
can be calculated with elaborate experimental design.[77,96,97] be 0.5 TPa.[90] Lee et al. measured the elastic properties and
The manipulator-based methods for surface related mechan- intrinsic breaking strength of monolayer free-standing gra-
ical properties measurement will be discussed in detail phene with the AFM indentation and revealed 1 TPa Young’s
in Section 6. modulus and 130 GPa fracture strength, which agrees well with
the density functional theory (DFT) calculations (1050 GPa)
and established graphene as the strongest material ever meas-
4.4. Atomic-Level Investigation ured.[79,109] Compared with pristine graphene, the monolayer
graphene oxide was found to have a lower effective Young’s
The high spatial resolution of TEM has enabled the modulus (207.6 ± 23.4 GPa).[110] More importantly, it has been
atomic level investigation of mechanical behaviors and their theoretically predicted that the elastic properties of graphene
Figure 6. Flexibility of the manipulator based method. a) TEM images showing the elastic flexibility of MoS2 flakes evaluated with a scanning tun-
neling microscope tip. Reproduced with permission.[89] Copyright 2014, American Chemical Society. b) Fracture toughness of graphene measured with
a nanomanipulator controlled W tip and AFM cantilever. Reproduced with permission.[67] Copyright 2015, American Chemical Society. c) Schematic
and TEM image showing the nanomechanical cleavage process of MoS2 realized with W tip. Reproduced with permission.[95] Copyright 2014, Nature
Publishing Group. d) SEM image showing the surface energy measurement process between graphene and nanotube with a manipulator controlled
W tip. Reproduced with permission.[77] Copyright 2013, American Chemical Society. e) SEM and optical images showing the cleavage energy measure-
ment of graphite with a manipulator. Reproduced with permission.[97] Copyright 2015, Nature Publishing Group.
are strongly dependent on their size/chirality, but there still thickness of 14.3–34 nm and found that the elastic modulus
lacks experimental investigations.[111,112] of BP declines with thickness and ranging from 276 ± 32.4 to
The Young’s modulus of bulk MoS2 and single walled MoS2 89.7 ± 26.4 GPa.[119] The maximum breaking strength of BP
nanotube has been measured to be 0.25 TPa and >130 GPa, nanosheets reaches 25 GPa. However, Moreno-Moreno et al.
respectively.[113] For the exfoliated monolayer MoS2, Betolazzi found that the elastic modulus and breaking strength of BP
et al. studied its in-plane stiffness and breaking strength with nanosheets in high vacuum are measured to be 46 ± 10 and
the AFM indentation tests and found that the Young’s modulus 2.4 ± 1 GPa respectively and is independent of thickness. Addi-
reaches 270 ± 100 GPa, which is comparable with the Young’s tionally, due to the self-passivation process of BP in atmosphere,
modulus of steel. Besides, the breaking stress reaches 11% of a clear decreasing tendency of elastic modulus is observed for
Young’s modulus (23 GPa) at effective strains of 6–11% and is very thin BP nanosheet.[120]
exceeded only by carbon nanotubes (11–63 GPa) and graphene
(130 GPa).[92] These results agree well with the first-principles
DFT calculations reported by Cooper et al., where the Young’s 5.2. CVD Grown 2D Materials
modulus and intrinsic strength of MoS2 are 210 and 26.8 GPa,
respectively.[114] Mechanical properties of materials are usually related with
For mechanical exfoliated MoS2 nanosheets with thickness their microstructures, which can be greatly influenced by the
from 25 down to 5 layers, the measured Young’s modulus is in growth methods. For graphene synthesized by the chemical
the range of 0.21–0.37 TPa with a mean Young’s modulus of reduction of graphene oxide, the elastic modulus was meas-
0.33 ± 0.07 TPa.[86] Zhang et al. studied the mechanical prop- ured to be 0.25 TPa.[91] CVD grown 2D materials usually con-
erties of exfoliated WSe2 with 5, 6, 12, and 14 layers and sist of defects and grain boundaries and their influence to the
showed that the Young’s modulus is statistically independent of mechanical properties quite matters for their applications. Ruiz-
the thickness of the membranes (167.3 ± 6.7 GPa) and is about Vargas et al. reported that grain boundaries could significantly
two thirds of those of MoS2 and WS2.[115] For the question of decrease the breaking strength of CVD grown graphene mem-
size-dependent properties, the surface effect contributes to the branes. The measured upper bound for the in-plane breaking
diameter-dependent Young’s modulus of 1D materials,[51] while stress was ≈35 GPa and the elastic modulus was measured to
stacking faults dominate in layered 2D materials. The thickness be ≈164 GPa.[121] Since the sample transfer technique can signi
of few-layer 2D materials is smaller than the average distance ficantly influence the measurement results of 2D materials,
between stacking faults, thus thickness-independent Young’s Lee et al. reexamined the mechanical properties of CVD grown
modulus was measured. graphene with grain boundaries using improved material pro-
Due to the puckered structure, both the Young’s modulus cessing technique. And they found that the obtained Young’s
and ultimate strain of monolayer black phosphorus (BP) have modulus was quite similar (≈1 TPa) for single-layer graphene
been calculated to be highly anisotropic: the in-plane Young’s with small grains (1–5 µm) and the isolated single-crystals with
modulus along the direction perpendicular (armchair direc- large grains (50–200 µm). Due to the randomly distributed
tion) and parallel (zigzag direction) to the Pucker is 41.3 and defects and grain boundaries, graphene with small grains
106.4 GPa; and the ultimate strength along the two directions show relatively smaller breaking strength compared with the
is 8 and 18 GPa, respectively.[116–118] Wang et al. experimen- pristine and large grain graphene (98.5 GPa vs 103 GPa).[122]
tally measured the elastic properties of BP nanosheets with The uniaxial strains of graphene has reached >10% as tested
Figure 7. Comparison of the Young’s modulus and fracture strength of various 2D materials.
with a tensile-MEMS device.[94] For CVD grown monolayer strain fields in 2D materials and factors like indenter radius,
MoS2, the 2D elastic modulus was measured to be ≈276 GPa, indentation location and prestress in tested samples could
which is very close to that of the above mechanical exfoliated lead to uncertainties and possible errors. Thus, it is difficult to
MoS2 monolayer.[123] extract intrinsic mechanical properties.
Except for the widely investigated graphene and MoS2, In contrast to AFM based methods, the MEMS chip-based
AFM indentation method has been used to explore the elastic tensile testing methods can realize the uniform in-plane
properties of WS2, WSe2, and BN. The CVD grown mon- loading on a freestanding membrane of 2D materials. There-
olayer WS2 was measured to have almost the same Young’s fore, the Young’s modulus and fracture stress can be directly
modulus with monolayer MoS2.[123] The Young’s modulus of calculated from the stress-strain curves. Most importantly,
CVD grown h-BN was 220–255 GPa and the breaking strength the dynamic breaking processes of 2D materials can also be
was 8.8 GPa. Moreover, vacancy concentration can lead to observed during the tensile test. To transfer 2D materials
the decrease of 2D elastic modulus and breaking strength onto stages of these MEMS devices, PMMA-assisted method
of BN layers.[124] To give a clear comparison between these is usually adopted and it should be noted that defects or
2D materials, the Young’s modulus E and fracture strength of polymer residue may be introduced during the sample prepa-
various tested 2D materials is concluded in Figure 7. Impor- ration process and should be considered during the data
tantly, with the AFM indentation test, Liu et al. also tested the processing process.
2D modulus of MoS2/WS2 and MoS2/graphene bilayers and
found that the calculated value were lower than the sum of
each 2D layers and comparable to the corresponding bilayer 6. Fracture Toughness and Mechanism
homostructures.[123]
The calculations of Young’s modulus in the AFM deflection In the application of 2D flexible devices, the stress induced
and indentation methods (see Section 4.1) are based on the crack formation serves as a main failure mechanism. However,
beam bending behavior for doubly clamped beams[91,125–127] compared with the widely studied Young’s modulus, the experi-
and the mechanical response of circular elastic film under mental demonstration of the fracture behavior of 2D materials
point load,[128,129] respectively. Theoretically, these two and the influence of preexisting defects has been seldomly
methods can obtain similar results for the same samples. reported.
Except for the sample thickness t, the AFM deflection method Theoretical calculations have been frequently conducted to
also requires a rectangular sample shape and the measure- study fracture behaviors of 2D materials. It has been predicted
ment of sample length and width. Generally, the pretension that the crack growth behaviors of graphene are closely related
obtained with this method is a mean value of all the tested with the initial crack length, strain rate, and chiral angles.[130–132]
samples. Therefore, for samples with sizable pretensions, the The ultimate strength of graphene is revealed to increase
calculated Young’s modulus may have a small deviation from with grain boundary angle and can be severely deteriorated by
its real value. hydrogen functionalization.[133,134] Apart from the defect den-
Compared with the AFM deflection method, samples in sity, the detailed arrangements of pentagon–heptagon defects
AFM indentation tests can be obtained by the same 2D flake can also greatly influence the ultimate strength of graphene.[135]
with the same thickness and pretension, their size can be For the nanocrystalline graphene, it is theoretically proved that
easily controlled by the circular wells on substrate. The Young’s the tensile fracture behavior is insensitive to the existing flaws
modulus and pretension can be directly obtained by fitting the and microcracks can nucleate randomly at intrinsic defects
F–δ curve with Equation (4). Therefore, the AFM indentation along their grain boundaries. The predicated uniaxial tensile
method has been widely used to measure the Young’s modulus strength and fracture surface energy is 96.2 ± 4.2 GPa (≈25 nm
of 2D materials. grain size) and 8 J m−2 for nanocrystalline graphene.[136,137]
However, the local probing by an AFM tip in the AFM With the development of in situ microscopy techniques,
based methods can introduce highly non-uniform stress and observation of the crack initiation and propagation process,
determination of the fracture toughness and atomic level film on Cu foil and reported the selectively propagation of
fracture mechanism can be comprehensively investigated crack with smooth edges along zigzag orientation.[138] Zhang
and insights can be provided for their mechanical stabili- et al. developed a quantitative in situ nanomechanical testing
ties. This section will concentrate on the in situ mechanical method to study the fracture toughness of CVD grown gra-
measurement results for the fracture properties of various phene.[93] Suspended graphene with rectangular shape and
2D materials. a central precrack can be successfully obtained across the
stage with a dry transfer method and FIB patterning. Then
the tensile test was conducted with a push-to-pull MEMS
6.1. Fracture Toughness device in situ in a SEM (Figure 5c). The initial crack length
2a0 and the fracture stress σc can be directly measured from
Fracture toughness is another important mechanical property SEM images and the displacement–force curves. Hence,
and describes the ability of a material containing a crack to the stress intensity factor of fracture Kc was calculated to be
resist fracture. For the brittle fracture of material with a central 4.0 MPa m , the critical strain energy release rate of fracture
crack length 2a0, the critical stress σc of the onset of fast frac- Gc was measured to be 15.9 J m−2, the edge energy γ of gra-
ture can be expressed with the Griffith criterion phene is estimated to be 8.0 J m−2. Similarly, with in situ SEM
tensile testing, Jang et al. observed the fracture behavior of a
2γE freestanding pristine graphene with a zigzag direction crack
σc = (5)
and found that the crack propagate along with a straight path
π a0
perpendicular to the loading direction though local crack
where E is the Young’s modulus, γ is the surface energy branching and meandering occurs.[139] The measured plane
(edge energy for 2D materials). Thus, with measured σc and stress fracture toughness reaches 21.25 MPa m and this
2a0, the effectiveness of classic Griffith theory in atomic-layered much higher value is caused by the geometrical nonlinearity
2D materials can be verified, the critical stress intensity factor and the nonlinear elasticity in the stress–strain relationship
of fracture K c = σ c π a0 , the critical strain energy release rate and of graphene.[140,141]
The fracture properties of ultrathin 2D materials depend
of fracture Gc = σ c2π a0 /E , and the edge surface energy
strongly on the quality of the individual single crystal.
γ = σ c2π a0 /(2E ) can be obtained. With the help of the improved dry transfer process intro-
Though AFM indentation method has been widely used to duced in Section 3, Yang et al. investigated the fracture
obtain the elastic properties of various 2D materials, straight- behavior of monolayer and bilayer MoSe2 with an in-plane
forward in-plane tensile tests are quite necessary to observe nanomechanical testing system (Figure 5c). Importantly,
their fracture behavior and explore the deformation mecha- the initiation and propagation of cracks and final fracture
nism. Fujihara et al. has realized the uniaxial tensile on gra- were directly observed (Figure 8).[73] Specifically, when the
phene films by immediately cooling the CVD grown graphene critical stress was reached, a major crack with length of
Figure 8. Brittle fracture of 2D MoSe2 investigated with in situ SEM. a) SEM image of the MoSe2 sample before tensile testing. b–e) SEM images
showing the crack initiation, propagation, and fracture process of MoSe2. f) The stress–strain curve for the measured sample, from where the elastic
properties can be extracted. Reproduced with permission.[73]
≈200 nm appeared, and then fast propagation of this be induced by the sparse S vacancies and the fracture mecha-
crack occurs, leading to the catastrophic brittle fracture of nism can be shifted from brittle to ductile by the migration of
MoSe2. The Young’s modulus and fracture strength of MoSe2 vacancies in the strain fields into networks with increasing
is measured to be 177.2 ± 9.3 and 4.8 ± 2.9 GPa, respectively defect density. Controlled defect creation is an effective approach
and the variation of preexisting flaws/cracks size can lead to to avoid catastrophic failure in 2D materials. Due to the inter-
the scattering of fracture strength. With the measured action between the atomically sharp crack tip and the vacancy
Young’s modulus and fracture strength, the size of a domi- clusters, the crack tips become blunt and the propagation speed
nant fracture-producing crack/flaw can be estimated by reduces dramatically during the crack propagation process,
a0 = 2γ E/(πσ c2 ). leading to the increased fracture toughness of defective MoS2.[106]
Except for the above center-cracked in situ tensile tests, Lopez-Polin et al. have performed nanoindentation experiments
Wei et al. studied the effect of crack blunting on the meas- on suspended graphene membranes with a known density of
ured fracture toughness with nanomanipulator-based in situ randomly distributed carbon single defects created by argon ion
HRTEM method.[67] The V/U shaped single-edge notches irradiation. Similarly, they found that though the presence of
were fabricated by a 300 keV focused electron probe. By ana- atomic scale defects can lower the breaking strength, the crack
lyzing the notch tip stresses just before fracture and taking propagation can be effectively limited.[143] Therefore, the intro-
into account the local notch tip structures using finite ele- duction of random distribution of atomic scale defects can be
ment method, the apparent stress intensity factor for the exploited to avoid catastrophic failure of 2D materials.
V/U-notched samples was calculated and the fracture tough-
ness of the multilayer graphene and boronitrene was deter-
mined to be 12.0 ± 3.9 and 5.5 ± 0.7 MPa m , which are 7. Surface/Interface Properties
larger than the theoretical estimations of the fracture tough-
ness of their monolayer counterparts (3.08 and 2.48 MPa m MoS2 has long been used as an additive in lubricant and
for the fracture along armchair edges; 3.33 and 3.17 MPa m a promising candidate in the field where low friction is
for the zigzag edges). This larger fracture toughness may required. Due to the atomic level flat surface without defect
result from the crack meandering caused by disordered layer and dangling bond, the surface and interlayer properties of 2D
stacking, crack branching caused by edge loading[142] and materials have attracted much attention in studying their
structural defects introduced by synthesis process and high friction/sliding behaviors, surface/adhesion energy, and
energy electron beam. cleavage behaviors. Moreover, the performance and reliability
The center-cracked in situ tensile tests based on MEMS of 2D flexible devices is often limited by their interfacial
devices can provide uniform in-plane loading on suspended properties between various substrates. Hence, a clear under-
2D films during the fracture toughness measurement. How- standing of their cleavage process and tribological properties
ever, due to the existing prestress, samples can easily break is quite necessary. Conventional experimental methods, like
during the FIB process, which is used to shape and make tribometers, can hardly be applied to the atomic layered 2D
center cracks in 2D films. Thus, the successful sample prep- materials. Therefore, novel methods combined with in situ
aration is quite challenging in this method. Additionally, microscopy techniques have shown their advantages in this
the influence of polymer residue to the measured fracture field, which will be introduced in detail in this section.
toughness and observed fracture behavior should also be con-
sidered. Compared with the MEMS devices-based methods,
uniform tensile load can hardly be obtained in the nano 7.1. Frictional Properties
manipulator-based in situ method.
Given the planar nature and atomic thickness, the friction prop-
erties of 2D materials and their relationship with thickness,
6.2. Atomic Level Fracture Mechanisms substrate, surface decoration and relative rotation angles can
be measured through the friction force microscope method and
In engineering applications, the atomic level investigation manipulator based sliding process.
of the dynamic fracture behavior can provide instructions for
small structure design. The improvement of the fracture tough-
ness and the avoidance of the mechanical failure both require 7.1.1. Friction Force Microscopy (FFM)
the elucidation of the fracture mechanism at the atomic level,
which can be realized with in situ HRTEM technique. The FFM method has been used as a powerful tool to
The atomically sharp crack tips play important role in mate- study the frictional properties between a sharp tip and atomi-
rial fracture. Focused electron beam is generally used to ini- cally thin sheets of lamellar materials including graphene and
tiate cracks in a TEM sample in order to dynamically observe MoS2. In the FFM measurement, a normal load is generally
the atomic structure and dislocation movement in the crack tip applied with an AFM tip (with specified tip radius and force
zone of a propagating crack in 2D materials (Figure 9). Straight constant) in contact mode. The topography images, fric-
cracking surfaces along the zigzag edge and dislocation propa- tion images, and corresponding friction force can be meas-
gation around the crack tip are observed in the intragranular ured.[144] The friction properties of the exfoliated thin flakes
cracking of MoS2.[76] Fracture behavior of 2D materials is closely of graphene, MoS2, NbSe2, and BN on SiO2 are measured
related with defect density. It is found that crack deflection can to increase with the thickness decrease, which arises from
Figure 9. HRTEM images showing the fracture mechanisms of 2D materials. a) Focused electron beam is used to generate crack on MoS2 membrane
covered on the TEM grid. The crack edge with zigzag termination can be clearly observed. Reproduced with permission.[106] Copyright 2016, American
Chemical Society. b) In situ dynamics of crack deflection of MoS2 through a region with low S vacancy concentration. Reproduced with permission.[106]
Copyright 2016, American Chemical Society. c) In situ TEM images showing the crack propagation and dislocation climb of MoS2. Reproduced with
permission.[76] Copyright 2016, Nature Publishing Group.
increased susceptibility to out-of-plane elastic deformation 7.1.2. Manipulator Based Sliding Process
of the thinner sheets.[145] Kwon et al. have measured the fric-
tion properties of CVD grown graphene with FFM in ultra- The interlayer sliding and friction behavior of 1D nanotubes
high vacuum and found that the friction was greatly enhanced have been carefully studied with micromanipulator-based in
in fluorinated graphene.[146] With this method, the rough- situ SEM technique because of their flexibility in manipula-
ness and sliding friction of MoS2 monolayers is revealed to tion.[149,150] Due to the low resistance to shear between neigh-
be strongly influenced by the substrate.[147] Fang et al. inves- boring atomic layers, graphite, and other 2D materials are also
tigated the thickness dependent friction on few-layer MoS2, known as good solid lubricants and self-retracting motion can
WS2, and WSe2 with AFM.[148] According to the morphology be observed in layered materials.[87,151] Motohisa Hirano first
of AFM tips, different behaviors were observed: when sharp proposed the concept of superlubricity, which can occur when
tip was used, the friction decreases with increasing thickness; structural incommensuration between two crystalline solid sur-
when a preworn and flat-ended tip was used, the friction of face exists and the friction coefficient is smaller than 10−3.[151,152]
WS2 and WSe2 increased monotonically with thickness, while It has been theoretically predicated that the dynamic friction of
for MoS2, friction decreased from monolayer to bilayer and MoS2 and graphene are both strongly dependent on their rela-
then subsequently increased with thickness. tive orientations (commensurate/incommensurate state).[153–156]
Though the FFM method can help to measure the friction Though the sliding properties of graphene and MoS2 have been
properties of 2D materials, an overestimation of friction can widely studied with theoretical calculations,[154,155,157] the quan-
usually be caused due to the out-of-plane elastic deformation titatively demonstration and intuitively observation of the
induced by the sharp tip. Additionally, the sliding between two sliding behavior of 2D materials still rely on the development of
atomic layers can also hardly be realized with FFM method. various in situ techniques.
Figure 10. Friction and lubrication property measurement of graphite. a) Schematic demonstration, SEM and optical images showing the graphite
mesa sheared with micromanipulator and the self-retraction of sheared flake after manipulator release. Reproduced with permission.[158] Copyright
2012, American Physical Society. b) STM images showing the sliding and rotation behavior of graphene nanoflakes on the graphene surface. Reproduced
with permission.[160] Copyright 2013, American Chemical Society.
With the help of a micromanipulator, the lithographi- observed and this transition is likely caused by the thermal
cally defined square mesas of highly oriented pyrolytic fluctuations (Figure 10b).[160]
graphite were successfully sheared in a SEM and the super- Recently, our group has developed a versatile method to study
lubric motion was observed after releasing the sheared the frictional properties between atomic-layered 2D materials
graphite flake (Figure 10a).[158,159] When shearing a square by combining the in situ SEM technique with a Si nanowire
2D mesa with length L to a distance x, the excess surface free cantilever.[96] The basic idea of this method is to slide a single
energy, U = 2γLx is produced, where γ is the surface energy layer MoS2 flake on another incommensurate single-layer MoS2
of their basal plane. Then, the self-retraction force and the nanosheet by a micromanipulator (Figure 11). First, a single
friction resistance force can be expressed as Fretract = 2γL layer MoS2 is peeled off with Si nanowire connected with
and Ff = τfL(L − x), where τf denotes shear strength. Then W probe controlled by the micromanipulator. Then, the peeled
the upper limit of the estimated friction stress can be calcu- layer is placed onto another single layer MoS2 for sliding.
lated through Si nanowire is used as a cantilever force sensor to measure the
friction force F = kδ during sliding, where k and δ are spring
2γ constant and deflection of the Si nanowire cantilever, respec-
τ fupper = (6)
(L − x max ) tively. Meanwhile, the cohesive force N = σS/c contribute to the
normal load, where σ is the interface energy of MoS2, c is the
where xmax is the maximum sheared distance of the graphite interaction length between MoS2 atomic layers, S is the contact
flake. The calculated shear strength between graphite layers area. Hence, the friction coefficient can be obtained through
is 0.02–0.04 MPa and closely related with grain boundaries in F/N. This method can be applied to investigate the friction
graphite and the orientation between the upper and bottom properties of various 2D materials. With this method, the fric-
flakes. With the scanning probe microscopy, the effective friction coefficient of MoS2 was measured to be ≈10−4 and showed
tion coefficient between graphite basal planes is estimated to be no dependence on the thickness of MoS2 substrate. The super-
7 × 10−5.[78] The results obtained with this method have lubricity between incommensurate atomic-layered materials
much larger precisions compared with the traditional FFM can preserve even for two monolayers.
method.[151] The lithographically defined square mesas can be used
To understand the relative motion of contacting surfaces at to measure the friction properties of mechanical exfoliation
the atomic level and better control the friction and lubrication 2D materials and the nanowire cantilever method can be used
process, Feng et al. observed the translational and rotational to investigate that of other CVD grown 2D materials. It should
motions of graphene flakes between commensurate states be noted that when the manipulator based methods are con-
at low temperature with the scanning tunneling microscopy. ducted in SEM, the electron beam induced deposition of amor-
Facile sliding behavior of graphene flakes from super phous carbon should be avoided in order to get an accurate
lubric states to a stable commensurate ground state is clearly value on the friction coefficients of 2D materials.
microcavity is formed by transferring

2D membrane onto the predefined micro-
cavities on the SiO2/Si substrate. During
this process, 2D membrane is clamped
on all sides of the chamber by the van der
Waals force and creates a volume of con-
fined gas. In order to create a pressure
difference, the substrate with 2D mem-
brane-sealed microcavities is placed into a
chamber with pressure p0 (p0 > pext) for sev-
eral days to allow pint = p0. When removed
from the pressure chamber, a significant
pressure difference Δp will be created,
resulting in the stretch and upward deflec-
tion of 2D film (Figure 12a). This process is
actually a “constant N blister test,” because
the number of molecules in the microcavity
is constant during the blister delamination.
According to the ideal gas law, pint will grad-
ually decrease during the expansion of the
gas volume. When pint = pext, the stable state
is reached and the maximum deflection of
the membrane can be obtained. AFM is
then used to measure the deflection δ and
radius a under different p0. The pressure
difference Δp = K(ν)(Etδ3)/a4 and blister
volume Vb(a) = C(ν)πa2δ, here K(ν) and
Figure 11. In situ SEM measurement of the friction coefficient of MoS2 with manipulator. C(ν) are coefficients depend only on the
a) SEM images showing the peeling of a monolayer MoS2 nanoflake form substrate with a Si
Poisson’s ratio ν.
nanowire cantilever. b,c) The experimental process and schematic illustration of the sliding
of the peeled MoS2 flake on the surface of another MoS2 substrate. d) The friction coefficient Before delamination, through the graph
measured from the sliding of a single-layer MoS2 flake on both monolayer and thick MoS2 of K(ν)δ3/a4 versus Δp, the Young’s modulus
substrate. Reproduced with permission.[96] of 2D films can also be measured. At certain
value of p0, stable delamination will happen.
Thus the adhesion energy can be determined
7.2. Adhesion and Surface Energy from the free energy F[162,164]
Adhesion energy of 2D materials is quite important in their ( pint − pext )Vb  V0 + Vb 

F= + Γπ ( a 2 − a02 ) − p0V0 ln  + pextVb
 V0 
transfer and device fabrication process, especially for the (7)
4
mechanical loading process of flexible 2D devices. Because
2D materials are difficult to handle, their adhesion and Here, V0 is the initial volume of the microcavity, Γ is the
surface energy measurement is quite challenging. With modi- adhesion energy, a0 is the initial radius before delamination.[165]
fied surface force balance, surface energies of CVD-grown Then relationship between Γ, δ, and a can be got after mini-
monolayer graphene in dry nitrogen (0.115 ± 0.004 J m−2), mize the free energy with respect to a
water (0.083 ± 0.007 J m−2), and sodium chlorate (0.029 ±
0.006 J m−2) are directly measured.[161] Recently, the pres- 5C  V0 
Γ=  p0 − pext  δ (8)
surized blister test, in situ peeling test and the buckle/ 4  V0 + Vb (a ) 
wrinkle-based methods have been developed to measure the
surface/interface properties between 2D materials and various With the pressurized blister test, the adhesion energy of
substrates. graphene layers with SiO2 substrate has been measured to be
0.45 ± 0.02 and 0.31 ± 0.03 J m−2 for monolayer and multilayer
graphene, respectively.[164]
7.2.1. Pressurized Blister Test
Combined with AFM characterization, the pressurized blister 7.2.2. In Situ Peeling Test
test can be used to measure the interface adhesion and friction
energy.[162,163] The pressurized blister test is generally based The adhesion and surface energy is quite important for the
on a 2D membrane-sealed microcavity and a pressure differ- understanding of its bonding mechanism and control of the
ence between the internal pressure in the microcavity (pint) mechanical release of the 2D materials from their bulk mate-
and the atmospheric pressure (pext). The 2D material-sealed rials or substrates.[166] To directly measure the surface energy
applied force and the elastic energy caused

by the extension of the film gives
F2
F (1 − cos θ ) = 2γ w − (9)
2Ebd
where γ is the interface surface energy. The
average surface energy is calculated to be
0.20 ± 0.09 and 0.36 ± 0.16 J m−2 for fully
collapsed and flattened contact widths of
MWCNT, respectively.
7.2.3. Buckle/Wrinkle Based Method
Except for the adhesion energy between

2D materials and rigid substrate, the adhe-
sion energy between 2D materials and elas-
tomers has been widely investigated with the
aid of AFM. To accurately obtain the adhe-
sion energy between 2D materials and elasto-
mers, Brennan et al. adopted a buckling-based
method.[168] As shown in Figure 13, by firmly
press down MoS2 on the polydimethylsiloxane
(PDMS) substrate, buckles and wrinkles of
MoS2 thin layers will appear after this mechan-
ical exfoliation process. The adhesion energy
can be obtained from the buckling profile with
the following equation[169]
π 4 h 3δ 2 E
Γ = (10)
6 λ 4 (1 − ν 2 )
where Γ is the adhesion energy, δ is the delami-

nation height, λ is the delamination width, h is
the film thickness, E and ν are the Young’s
modulus and Poisson’s ratio of the film, respec-
tively. Then the adhesion energy between MoS2
and PDMS is obtained to be 0.018 ± 0.002 J m−2
Figure 12. Surface/interface energy measurements. a) Schematic illustration of the pressured with accurate measurement of δ, λ, and h.
blister test and morphology of the 2D membrane characterized with AFM after remove from the The above method can be applied to measure
pressure chamber. Reproduced with permission.[164] Copyright 2011, Nature Publishing Group. the adhesion energy between 2D materials and
b) Schematic illustration and SEM image of peeling a CNT from the graphene substrate by moving various substrates. Deng et al. have obtained
the stage. Reproduced with permission.[77] Copyright 2013, American Chemical Society.
the interfacial energy between 2D materials
and substrate simply by measuring their
between CNT and graphene, Roenbeck et al. conducted the wrinkle morphology on rigid substrate (Figure 13b), which is
in situ peeling test in a SEM.[77] As shown in Figure 12b, caused by the interplay between the adhesion and bending ener-
a multiwalled carbon nanotube (MWCNT) was connected gies. The adhesion energy between MoS2 on SiO2 and Si3N4 were
with an AFM cantilever and attached to the graphene sub- then measured to be 0.170 ± 0.033 and 0.252 ± 0.041 J m−2, respec-
strate in line contact. The MWCNT is then peeled from gra- tively.[170] Scharfenberg et al. examined the competition between
phene surface by pulling the substrate away. The geometrical adhesive and bending energies for few-layer graphene exfoliated
configuration during the peeling process can be recorded on microscale-corrugated metallic substrates and revealed the
and peeling force can be calculated through the deflection layer thickness-dependent transitions between conforming to the
of the AFM cantilever. Then the surface energy between substrate and lying flat on top of the substrate. The graphene-
MWCNT and graphene can be calculated with Kendall Pd/Au surface adhesion energy (1.1 eV nm−2) is then extracted
Analysis. [167]
When an elastic film with thickness d, width b with the critical transition thickness in an elasticity model for
and Young’s modulus E peeling at an angle θ from a rigid graphene bending.[171] Similarly, by probing the conformability
substrate under a constant force F, the energy balance of the of the exfoliated graphene on a precorrugated PDMS surface, the
surface energy change caused by the creation of new sur- adhesion energy between exfoliated graphene and PDMS elas-
faces, the potential energy caused by the movement of the tomer was estimated to be larger than 0.007 J m−2.[172]
Figure 13. Adhesion energy of 2D materials measured with buckle/wrinkle based method. a) Buckle formation process of MoS2 on PDMS and the
corresponding AFM characterization. Reproduced with permission.[168] (b) Wrinkled MoS2 on silicon based substrate. Schematic illustration of the
morphology and energy distribution and the calculated adhesion energy between MoS2 and SiO2/Si3N4 substrate are also shown. Reproduced with
permission.[170] Copyright 2017, American Chemical Society.
7.3. Cleavage of 2D materials interfacial energy, the unique layer-dependent bending behav-
iors like spontaneous rippling (<5 atomic layers), homogeneous
Due to the weak van der Waals interaction between layers, curving (≈10 layers), and kinking (20 or more layers) have been
2D layered materials can be mechanically exfoliated from their revealed (Figure 14a).[95]
bulk materials and used as good lubricant. With statistical To understand the interlayer sliding process of MoS2 at the
analysis under optical microscopy, Guo et al. revealed that nanoscale, Oviedo et al. tore and slide a freestanding MoS2 flake
2D layered materials tend to cleave along specific in-plane pre- with electrostatic probe-assisted manipulation.[75] A tungsten
ferred crystallography orientations:[173] Graphene and BN show probe with a native oxide layer is mounted on a piezo-driven
moderate tendency to cleave along 〈1010 〉 and 〈1120 〉 direction; manipulator inside the TEM. Then, bulk MoS2 is attached to
the 2H phase MoS2 and 1T phase PtS2 show a strong tendency to this tungsten probe at a high DC electrostatic bias. By varying
cleave along 〈1120 〉 direction; FePS3 shows a strong tendency the probe bias, MoS2 nanoflakes can be tear from their bulk
to cleave along 〈010〉 and 〈110〉 directions; and BP shows a weak materials and aligned in cross section view. As shown in
tendency to cleave along 〈100〉 direction. In addition, they also Figure 14b, the shear-induced interlayer sliding process is real-
developed a fast and noninvasive method to identify the crystal ized and observed by moving the tip. Moreover, FIB prepared
direction of mechanical exfoliated layered materials. However, MoS2 cross section samples are sheared with a nanoindenter
the interlayer sliding and cleavage process can hardly be visu- force sensor (Figure 14c), thus the observation and force meas-
alized due to the incapability of simultaneously mechanical urement of the interlayer dynamics during the shear-induced
manipulation and imaging. The in situ TEM technique has pro- sliding is realized. With the measured force F and sheared
vided us straightforward solutions to clearly understand these area A, the shear strength can be calculated by F/A and the
processes. zero normal load shear strength of MoS2 is measured to be
The nanomechanical cleavage of MoS2 atomic layers has 25.3 ± 0.6 MPa. The above-mentioned methods can be widely
been investigated by a straightforward in situ TEM technique. used to directly measure the shear strength of other 2D layered
Atomically thin flakes ranging from single to more than materials, providing atomic level mechanisms for their lubri-
20 layers can be peeled off and the mechanical behaviors can be cating and failure mechanisms for related applications.
in situ investigated by manipulating an ultrasharp metal probe. Similar with the self-retraction phenomenon observed by
Layer number selective cleavage of MoS2 from single layer to the setup in Figure 10a, Wang et al. accurately measured the
double layer and up to 23 atomic layers has been demonstrated. cleavage energy of graphite with a force sensor probe, which
Importantly, depending on the competition of strain energy and was used to push the upper graphite flake. The cleavage energy
Figure 14. Cleavage of 2D materials investigated with in situ TEM technique. a) TEM images showing the layer dependent bending behavior of
MoS2 during the nanomechanical cleavage process. Reproduced with permission.[95] Copyright 2014, Nature Publishing Group. b) TEM images of
the sliding process of a nine-layer MoS2. Reproduced with permission.[75] Copyright 2014, American Chemical Society. c) TEM images of the in situ
mechanical shearing test of a MoS2 flake cross section sample. Reproduced with permission.[75] Copyright 2014, American Chemical Society.
is then calculated to be 0.39 ± 0.02 J m−2 for ideal ABAB 8. Extension of the In Situ Mechanical
stacking graphite and 0.37 ± 0.01 J m−2 for the incommensu- Measurement Methods of 2D Materials
rate state of bicrystal graphite through Fapp/W, where Fapp is the
applied sheared force and W is the sample width.[97] The excellent mechanical properties of 2D materials indicate
With the above-mentioned in situ methods, surface/interface that they are promising building blocks for various flexible
properties like friction, sliding, cleavage, and adhesive prop- devices.[174] Mechanical deformation can be used to control their
erties of 2D layered materials can be directly measured. electronic, optical and magnetic properties.[35,36,175–178] Various
Generally, the pressurized blister test requires the micro- theoretical works have proven that the reduction of bandgap,
cavity fabrication process and this method is frequently direct-to-indirect bandgap and semiconductor-to-metal transi-
used to measure the adhesion energy of 2D materials with tions of TMDs can be induced by mechanical strains.[33,37,179–181]
silicon-based substrates. The above mentioned in situ peeling When combined suitable property measurement equipment
test conducted in SEM can also be used to measure the with the aforementioned various in situ mechanical measure-
surface energy between other 1D nanomaterials and 2D ment methods, strain-induced physical property change can be
materials. Buckle/wrinkle based method is generally applied investigated experimentally.
to measure the adhesion energy between 2D materials and The controlled delamination and wrinkle formation on sub-
elastomers. Since the adhesion energy is greatly related with strate has also been widely used to study strain induced Raman
the geometric configuration (h3δ2/λ4, see Section 7.2.3) of the and photoluminescence (PL) spectra change of 2D materials
formed buckles and wrinkles, precise measurement of these (Figure 15a). Strain induced direct bandgap reduction and
parameters is quite critical for the accurate measurement of funneling of photogenerated excitons toward higher strain
the adhesion energy. regions is observed with PL imaging.[182] Red shift of PL peak,
Figure 15. Electromechanical properties of 2D materials. a) SEM image of MoS2 wrinkle formed on elastomer substrate. Photoluminescence spectra
measured on the flat region (unstrained) and on top of the wrinkle (strained) in the same MoS2 flake. Reproduced with permission.[182] Copyright
2013, American Chemical Society. b) Schematic illustration of the electromechanical characterization of suspended channel MoS2 devices under strain.
The relationship between resistance and MoS2 deflection is also shown, indicating the piezoresistive effect in MoS2. Reproduced with permission.[187]
Copyright 2015, American Chemical Society. c) Schematic illustration of the suspended graphene and the nanoindentation measurement setup.
The charge gradient caused by AFM indentation in graphene is expressed by a color change. The mechanical deformation of the suspended graphene
under different negative back-gate voltages is also shown. Reproduced with permission.[39] Copyright 2015, Nature Publishing Group.
light emission enhancement, degenerate and split of Eg-like the piezoelectric coefficient is 6.3 × 10−3 Cm−2, much larger
Raman peak, and magnetism appearance of ReSe2 nanosheet than bulk piezoelectric materials.[39]
are induced by local strain produced by wrinkles.[183] The Our group has recently developed a SEM compatible multi-
bending test can also be applied to flexible substrates where property study platform for nanomaterial, which can introduce
2D materials were transferred.[184,185] With this method, the mechanical strain and enables three terminal electrical meas-
G and 2D bands of graphene were found to show significant urements.[188] This platform consists of a sample holder with
red shifts accompanied by the split of G band. Additionally, an extremely narrow slit which can hold suspended nanoma-
strain induced phonon softening, optical bandgap decrease terials and predefined metallic electrodes (Figure 16). Driven
(≈45 and ≈120 meV %−1 for monolayer and bilayer MoS2, by the piezoelectric ceramic, in-plane strain can be applied on
respectively) and PL intensity reduction is observed with tensile the sample through the sample holder and the influence to the
strain in MoS2.[34] With a highly strained graphene nanobubble electrical properties of nanomaterials can be simultaneously
formed during the growth process, Levy et al. experimentally evaluated.[189] Combined with appropriate transfer process, the
demonstrated the giant strain-induced pseudomagnetic field, study of electromechanical properties of 2D materials may also
which is higher than 300 Tesla.[186] be realized with similar methods.
Recently, with the development in manipulating 2D mate-
rials, the piezoresistivity and piezoelectricity has been investi-
gated experimentally with in situ technique: the combination 9. Future Perspectives
of nanoindentation and electrical measurement. AFM probe is
used to exert mechanical strain on suspended MoS2 devices, Though basic mechanical parameters and corresponding
and the bandgap of monolayer (Figure 15b), bilayer, and trilayer behaviors of 2D materials have been successfully investigated
MoS2 is modulated by strain at rates of −77.3 ± 10, −116.7 ± 10, with above-mentioned in situ microscopy techniques, there is
and −22.7 ± 6 meV %−1, respectively. The comparable piezore- plenty of room in understanding the mechanical properties of
sistive gauge factor with Si implies that MoS2 thin layers are 2D materials and efforts are still needed.
also promising materials for strain sensors.[187] Similarly, the Except for the reported atomic level fracture mechanism of
piezoelectric coefficient of a freestanding monolayer MoS2 2D materials, the relationship between crystal structure and
is measured to be 0.5 C m−2.[40] Backgate voltage has also other mechanical properties and the dynamic response of
been used to induce bending and biaxial strain of suspended atomic structure under various mechanical strains require the
2D materials (Figure 15c). Due to strain modified band struc- simultaneous mechanical property measurement and crystal
ture, the band-piezoelectric effect on a biaxial-strained structure characterization.[190,191] Therefore, careful experi-
suspended graphene has been observed with this method and mental design with in situ HRTEM technique is quite essential.
large on/off ratio, ultrasensitive photode-

tector,[199] room temperature light-emitting
diode,[200] and strong light–matter interac-
tion with high quantum efficiency have been
successfully demonstrated.[201] During the
design of 2D heterostructures, the interfa-
cial interactions quite matters in the perfor-
mance of final devices and understanding
the interface–interface interaction would pro-
vide us more direct knowledge to design new
materials at the fundamental atomic levels.
Therefore, measurement of the elastic, frac-
ture, friction, and adhesion properties of
2D heterostructures is another developing
direction of the mechanical properties of
2D materials.
10. Concluding Remarks

In this review, we comprehensively intro-
duced advantages of in situ microscopy
technique in materials science and con-
Figure 16. Illustration and application of the SEM compatible multi-property study platform.
a) Schematic side-view of the platform installed on a SEM sample stage. b) Schematic top view cluded the material preparation process
of a sample holder. c) 3D schematic diagram showing the construction of a CNT resonator with and in situ microscopy techniques based
the multi-property platform. d) The change of the resonance frequency as a function of gate on AFM, SEM, and TEM in measuring the
voltage and the axial strain introduced by pulling the CNT with the platform. Reproduced with mechanical properties of 2D layered mate-
permission.[189] Copyright 2014, American Chemical Society. rials, including Young’s modulus, breaking
strength, friction coefficient, adhesive and
In addition, the time-dependent mechanical characterization cleavage energy. The in situ AFM technique is generally used
of materials is critical to evaluate their long-term reliability in to measure the elastic properties with nanoindentation test
various applications.[192] It is also of great importance to study and the friction coefficient with FFM. Combined with its
the mechanics of 2D materials under time-dependent loading morphology characterization, the adhesion energy between
conditions, like stress-relaxation and fatigue, and to reveal their various substrates can be measured with pressurized blister
microstructure evolution during these processes. test and buckle/wrinkle based method. Uniaxial in-plane ten-
The Poisson’s ratio is a mechanical parameter denoting the sile test of 2D materials is usually accomplished with MEMS
ratio of transverse strain to axial strain and is generally positive devices conduced in SEM or TEM, from which the elasticity
for most materials. Except for the bulk auxetic material, it has and fracture behavior can be simultaneously observed. With
been theoretically shown that single-layer black phosphorus also HRTEM, the atomic level investigation of the fracture mecha
possesses negative Poisson’s ratio in the out-of-plane direction, nisms can be revealed. Combined with SEM, TEM, and
which originates from its puckered structure.[193] Dominated by optical microscopy, the manipulator-based method can help
electronic effects, 1T-type crystalline 2D TMDs are calculated to conduct the sliding, peeling and cleavage process on 2D
to exhibit intrinsic in-plane negative Poisson’s ratio as well.[194] layered materials, thus the friction coefficient, surface, and
Through introduction of vacancy defects, creation of periodic cleavage energy can be directly obtained. The influence of syn-
porous structure, warping of the free edges, and introduction thesis methods, defects, and layer numbers to their mecha
of rippling curvature by entropic effect at high temperature, nical properties has also been discussed in this review. Finally,
graphene could be modified to exhibit a negative Poisson’s ratio extension of aforementioned in situ microscopy methods in
with MD simulations.[193,195–197] Jiang et al. revealed recently that studying the strain induced band structure, optical, magnetic,
negative Poisson’s ratio is an intrinsic property of graphene and and electrical property change is also simply introduced.
is independent of size and temperature.[198] However, since the Therefore, with the above-mentioned in situ techniques, the
transverse strain measurement of 2D materials in the out-of- mechanical properties of 2D materials can be comprehen-
plane direction is hard to realize during the uniaxial tension pro- sively investigated and their mechanical performances in
cess, there still lacks the experimental demonstration of these various device applications can be clearly evaluated.
properties.
2D layered material also show their advantages in forming
different kinds of vertical heterostructures, which do not exist Acknowledgements
in nature, by stacking monolayers of different chemical compo- This work was supported by the General Financial Grant from
sitions together, realizing material design at the atomic level. China Postdoctoral Science Foundation (No. 2017M622371),
With 2D heterostructures, tunneling field-effect transistor with National Key Research and Development Program of China grants
(Nos. 2017YFA0205003, 2016YFA0200802), the National Basic Research [22] D. Xiao, G. B. Liu, W. Feng, X. Xu, W. Yao, Phys. Rev. Lett. 2012,
Program of China grant 2013CB933604, and the National Science 108, 196802.
Foundation of China grants (61371001, 61775006, 11528407, U1604263, [23] H. Zeng, J. Dai, W. Yao, D. Xiao, X. Cui, Nat. Nanotechnol. 2012,
and 61621061). 7, 490.
[24] K. F. Mak, K. L. McGill, J. Park, P. L. McEuen, Science 2014,
344, 1489.
[25] A. M. Jones, H. Yu, N. J. Ghimire, S. Wu, G. Aivazian, J. S. Ross,
Conflict of Interest B. Zhao, J. Yan, D. G. Mandrus, D. Xiao, W. Yao, X. Xu, Nat. Nano-
The authors declare no conflict of interest. technol. 2013, 8, 634.
[26] Q. H. Wang, K. Kalantar-Zadeh, A. Kis, J. N. Coleman,
M. S. Strano, Nat. Nanotechnol. 2012, 7, 699.
[27] J. A. Rogers, T. Someya, Y. Huang, Science 2010, 327, 1603.
Keywords [28] K. S. Kim, Y. Zhao, H. Jang, S. Y. Lee, J. M. Kim, K. S. Kim,
2D materials, in situ microscopy, mechanical property J. H. Ahn, P. Kim, J. Y. Choi, B. H. Hong, Nature 2009, 457, 706.
[29] W. Zhang, J. K. Huang, C. H. Chen, Y. H. Chang, Y. J. Cheng,
Received: September 27, 2017 L. J. Li, Adv. Mater. 2013, 25, 3456.
Revised: November 23, 2017 [30] O. Lopez-Sanchez, D. Lembke, M. Kayci, A. Radenovic, A. Kis,
Published online: Nat. Nanotechnol. 2013, 8, 497.
[31] H. Xie, B. Jiang, J. He, X. Xia, F. Pan, Tribol. Int. 2016, 93, 63.
[32] A. P. Nayak, T. Pandey, D. Voiry, J. Liu, S. T. Moran, A. Sharma,
C. Tan, C. H. Chen, L. J. Li, M. Chhowalla, J. F. Lin, A. K. Singh,
[1] K. I. Bolotin, K. J. Sikes, Z. Jiang, M. Klima, G. Fudenberg, J. Hone, D. Akinwande, Nano Lett. 2015, 15, 346.
P. Kim, H. L. Stormer, Solid State Commun. 2008, 146, 351. [33] P. Johari, V. B. Shenoy, ACS Nano 2012, 6, 5449.
[2] C. R. Dean, A. F. Young, I. Meric, C. Lee, L. Wang, S. Sorgenfrei, [34] H. J. Conley, B. Wang, J. I. Ziegler, R. F. Haglund Jr., S. T. Pantelides,
K. Watanabe, T. Taniguchi, P. Kim, K. L. Shepard, J. Hone, Nat. K. I. Bolotin, Nano Lett. 2013, 13, 3626.
Nanotechnol. 2010, 5, 722. [35] Y. Ma, Y. Dai, M. Guo, C. Niu, Y. Zhu, B. Huang, ACS Nano 2012,
[3] F. Schwierz, Nat. Nanotechnol. 2010, 5, 487. 6, 1695.
[4] F. Xia, D. B. Farmer, Y. M. Lin, P. Avouris, Nano Lett. 2010, 10, 715. [36] Y. Zhou, Z. Wang, P. Yang, X. Zu, L. Yang, X. Sun, F. Gao, ACS
[5] Y. M. Lin, C. Dimitrakopoulos, K. A. Jenkins, D. B. Farmer, Nano 2012, 6, 9727.
H. Y. Chiu, A. Grill, P. Avouris, Science 2010, 327, 662. [37] P. Lu, X. Wu, W. Guo, X. C. Zeng, Phys. Chem. Chem. Phys. 2012,
[6] S. J. Jeong, S. Jo, J. Lee, K. Yang, H. Lee, C.-S. Lee, H. Park, S. Park, 14, 13035.
Nano Lett. 2016, 16, 5378. [38] L. Huang, Y. Li, Z. Wei, J. Li, Sci. Rep. 2015, 5, 16448.
[7] X. Yang, G. Liu, A. A. Balandin, K. Mohanram, ACS Nano 2010, [39] X. Wang, H. Tian, W. Xie, Y. Shu, W.-T. Mi, M. Ali Mohammad,
4, 5532. Q.-Y. Xie, Y. Yang, J.-B. Xu, T.-L. Ren, NPG Asia Mater. 2015,
[8] P. K. Ang, A. Li, M. Jaiswal, Y. Wang, H. W. Hou, J. T. L. Thong, 7, e154.
C. T. Lim, K. P. Loh, Nano Lett. 2011, 11, 5240. [40] H. Zhu, Y. Wang, J. Xiao, M. Liu, S. Xiong, Z. J. Wong, Z. Ye, Y. Ye,
[9] A. K. M. Newaz, D. A. Markov, D. Parasai, K. I. Bolotin, Nano Lett. X. Yin, X. Zhang, Nat. Nanotechnol. 2015, 10, 151.
2012, 12, 2931. [41] W. Zhou, X. Zou, S. Najmaei, Z. Liu, Y. Shi, J. Kong, J. Lou,
[10] S. J. Park, O. S. Kwon, S. H. Lee, H. S. Song, T. H. Park, J. Jang, P. M. Ajayan, B. I. Yakobson, J. C. Idrobo, Nano Lett. 2013,
Nano Lett. 2012, 12, 5082. 13, 2615.
[11] S. Rumyantsev, G. Liu, M. S. Shur, R. A. Potyrailo, A. A. Balandin, [42] W. Yuan, Y. Wang, H. Li, H. Wu, Z. Zhang, A. Selloni, C. Sun, Nano
Nano Lett. 2012, 12, 2294. Lett. 2016, 16, 132.
[12] J. K. Park, S. M. Song, J. H. Mun, B. J. Cho, Nano Lett. 2011, [43] T. T. Xu, X. L. Wei, J. P. Shu, Q. Chen, Appl. Phys. Lett. 2013,
11, 5383. 103, 193112.
[13] N. Zhan, M. Olmedo, G. Wang, J. Liu, Appl. Phys. Lett. 2011, [44] X. Li, X. L. Wei, T. T. Xu, Z. Y. Ning, J. P. Shu, X. Y. Wang, D. Pan,
99, 113112. J. H. Zhao, T. Yang, Q. Chen, Appl. Phys. Lett. 2014, 104, 103110.
[14] A. J. Hong, E. B. Song, H. S. Yu, M. J. Allen, J. Kim, J. D. Fowler, [45] X. Li, X. Wei, T. Xu, D. Pan, J. H. Zhao, Q. Chen, Adv. Mater. 2015,
J. K. Wassei, Y. Park, Y. Wang, J. Zou, R. B. Kaner, B. H. Weiller, 27, 2852.
K. L. Wang, ACS Nano 2011, 5, 7812. [46] R. A. Bernal, T. Filleter, J. G. Connell, K. Sohn, J. Huang,
[15] S. K. Hong, C. S. Kim, W. S. Hwang, B. J. Cho, ACS Nano 2016, L. J. Lauhon, H. D. Espinosa, Small 2014, 10, 725.
10, 7142. [47] A. Lugstein, M. Steinmair, A. Steiger, H. Kosina, E. Bertagnolli,
[16] K. F. Mak, C. Lee, J. Hone, J. Shan, T. F. Heinz, Phys. Rev. Lett. Nano Lett. 2010, 10, 3204.
2010, 105, 136805. [48] J. Luo, J. Wang, E. Bitzek, J. Y. Huang, H. Zheng, L. Tong, Q. Yang,
[17] T. Chu, H. Ilatikhameneh, G. Klimeck, R. Rahman, Z. Chen, Nano J. Li, S. X. Mao, Nano Lett. 2016, 16, 105.
Lett. 2015, 15, 8000. [49] Y. Lu, J. Y. Huang, C. Wang, S. Sun, J. Lou, Nat. Nanotechnol. 2010,
[18] Y. Zhang, T. R. Chang, B. Zhou, Y. T. Cui, H. Yan, Z. Liu, F. Schmitt, 5, 218.
J. Lee, R. Moore, Y. Chen, H. Lin, H. T. Jeng, S. K. Mo, Z. Hussain, [50] M. Fu, Z. Tang, X. Li, Z. Ning, D. Pan, J. Zhao, X. Wei, Q. Chen,
A. Bansil, Z. X. Shen, Nat. Nanotechnol. 2014, 9, 111. Nano Lett. 2016, 16, 2478.
[19] A. Splendiani, L. Sun, Y. Zhang, T. Li, J. Kim, C. Y. Chim, G. Galli, [51] M.-R. He, Y. Shi, W. Zhou, J. W. Chen, Y. J. Yan, J. Zhu, Appl. Phys.
F. Wang, Nano Lett. 2010, 10, 1271. Lett. 2009, 95, 091912.
[20] K. F. Mak, K. He, C. Lee, G. H. Lee, J. Hone, T. F. Heinz, J. Shan, [52] L. Fei, S. Lei, W. B. Zhang, W. Lu, Z. Lin, C. H. Lam, Y. Chai,
Nat. Mater. 2013, 12, 207. Y. Wang, Nat. Commun. 2016, 7, 12206.
[21] J. S. Ross, P. Klement, A. M. Jones, N. J. Ghimire, J. Yan, [53] S. Rackauskas, H. Jiang, J. B. Wagner, S. D. Shandakov,
D. G. Mandrus, T. Taniguchi, K. Watanabe, K. Kitamura, W. Yao, T. W. Hansen, E. I. Kauppinen, A. G. Nasibulin, Nano Lett. 2014,
D. H. Cobden, X. Xu, Nat. Nanotechnol. 2014, 9, 268. 14, 5810.
[54] S. C. Wang, M. Y. Lu, A. Manekkathodi, P. H. Liu, H. C. Lin, [85] S. Liu, Q. Zhao, J. Xu, K. Yan, H. Peng, F. Yang, L. You, D. Yu,
W. S. Li, T. C. Hou, S. Gwo, L. J. Chen, Nano Lett. 2014, 14, 3241. Nanotechnology 2012, 23, 085301.
[55] M. R. He, R. Yu, J. Zhu, Angew. Chem., Int. Ed. 2012, 51, 7744. [86] A. Castellanos-Gomez, M. Poot, G. A. Steele, H. S. J. Zant,
[56] Z. Aabdin, J. Lu, X. Zhu, U. Anand, N. D. Loh, H. Su, U. Mirsaidov, N. Agrait, G. Rubio-Bollinger, Adv. Mater. 2012, 24, 772.
Nano Lett. 2014, 14, 6639. [87] Q. Zheng, B. Jiang, S. Liu, Y. Weng, L. Lu, Q. Xue, J. Zhu, Q. Jiang,
[57] X. Li, D. Xiao, H. Zheng, X. Wei, X. Wang, L. Gu, Y.-S. Hu, T. Yang, S. Wang, L. Peng, Phys. Rev. Lett. 2008, 100, 067205.
Q. Chen, Nano Energy 2016, 20, 194. [88] F. Xu, H. Ma, S. Lei, J. Sun, J. Chen, B. Ge, Y. Zhu, L. Sun,
[58] H. Zheng, D. Xiao, X. Li, Y. Liu, Y. Wu, J. Wang, K. Jiang, Nanoscale 2016, 8, 13603.
C. Chen, L. Gu, X. Wei, Y. S. Hu, Q. Chen, H. Li, Nano Lett. [89] G. Casillas, U. Santiago, H. Barron, D. Alducin, A. Ponce,
2014, 14, 4245. M. Jose-Yacaman, J. Phys. Chem. C 2015, 119, 710.
[59] C. Li, B. Gao, Y. Yao, X. Guan, X. Shen, Y. Wang, P. Huang, L. Liu, [90] I. W. Frank, D. M. Tanenbaum, A. M. van der Zande, P. L. McEuen,
X. Liu, J. Li, C. Gu, J. Kang, R. Yu, Adv. Mater. 2017, 29, 1602976. J. Vac. Sci. Technol. B 2007, 25, 2558.
[60] Y. Kuwauchi, S. Takeda, H. Yoshida, K. Sun, M. Haruta, H. Kohno, [91] C. Gomez-Navarro, M. Burghard, K. Kern, Nano Lett. 2008,
Nano Lett. 2013, 13, 3073. 8, 2045.
[61] S. Zhang, P. N. Plessow, J. J. Willis, S. Dai, M. Xu, [92] S. Bertolazzi, J. Brivio, A. Kis, ACS Nano 2011, 5, 9703.
G. W. Graham, M. Cargnello, F. Abild-Pedersen, X. Pan, Nano [93] P. Zhang, L. Ma, F. Fan, Z. Zeng, C. Peng, P. E. Loya, Z. Liu,
Lett. 2016, 16, 4528. Y. Gong, J. Zhang, X. Zhang, P. M. Ajayan, T. Zhu, J. Lou, Nat.
[62] P. L. Hansen, J. B. Wagner, S. Helvveg, J. R. Rostrup-Nielsen, Commun. 2014, 5, 3782.
B. S. Clausen, H. Topsoe, Science 2002, 295, 2053. [94] H. H. Perez Garza, E. W. Kievit, G. F. Schneider, U. Staufer, Nano
[63] Y. Jiang, H. Li, Z. Wu, W. Ye, H. Zhang, Y. Wang, C. Sun, Z. Zhang, Lett. 2014, 14, 4107.
Angew. Chem., Int. Ed. 2016, 55, 12427. [95] D. M. Tang, D. G. Kvashnin, S. Najmaei, Y. Bando, K. Kimoto,
[64] Y. Jiang, Z. Zhang, W. Yuan, X. Zhang, Y. Wang, Z. Zhang, Nano P. Koskinen, P. M. Ajayan, B. I. Yakobson, P. B. Sorokin, J. Lou,
Res. 2017, https://doi.org/10.1007/s12274-017-1645-9. D. Golberg, Nat. Commun. 2014, 5, 3631.
[65] W. Yuan, Y. Jiang, Y. Wang, S. Kattel, Z. Zhang, L.-Y. Chou, [96] H. Li, J. Wang, S. Gao, Q. Chen, L. Peng, K. Liu, X. Wei, Adv. Mater.
C.-K. Tsung, X. Wei, J. Li, X. Zhang, G. Wang, S. X. Mao, Z. Zhang, 2017, 29, 1701474.
Chem. Commun. 2015, 51, 350. [97] W. Wang, S. Dai, X. Li, J. Yang, D. J. Srolovitz, Q. Zheng, Nat.
[66] X. Li, X. Wei, Q. Chen, Int. J. Nanomanuf. 2016, 12, 264. Commun. 2015, 6, 7853.
[67] X. Wei, S. Xiao, F. Li, D. M. Tang, Q. Chen, Y. Bando, D. Golberg, [98] L. Wang, Z. Zhang, X. D. Han, NPG Asia Mater. 2013, 5, e40.
Nano Lett. 2015, 15, 689. [99] X. D. Han, Y. F. Zhang, K. Zheng, X. N. Zhang, Z. Zhang, Y. J. Hao,
[68] X. Li, S. Cheng, S. Deng, X. Wei, J. Zhu, Q. Chen, Sci. Rep. 2017, X. Y. Guo, J. Yuan, Z. L. Wang, Nano Lett. 2007, 7, 452.
7, 40911. [100] K. Zheng, X. D. Han, L. Wang, Y. Zhang, Y. Yue, Y. Qin, X. Zhang,
[69] Z. Zhang, Y. Wang, H. Li, W. Yuan, X. Zhang, C. Sun, Z. Zhang, Z. Zheng, Nano Lett. 2009, 9, 2471.
ACS Nano 2016, 10, 763. [101] X. D. Han, K. Zheng, Y. F. Zhang, X. Zhang, Z. Zhang, Z. L. Wang,
[70] P. Poncharal, Z. L. Wang, D. Ugarte, W. A. d. Heer, Science 1999, Adv. Mater. 2007, 19, 2112.
283, 1513. [102] K. Zheng, C. Wang, Y.-Q. Cheng, Y. Yue, X. Han, Z. Zhang, Z. Shan,
[71] J. Wu, W. Gao, J. Wen, D. J. Miller, P. Lu, J. M. Zuo, H. Yang, Nano S. X. Mao, M. Ye, Y. Yin, E. Ma, Nat. Commun. 2010, 1, 24.
Lett. 2015, 15, 2711. [103] L. Wang, X. D. Han, P. Liu, Y. Yue, Z. Zhang, E. Ma, Phy. Rev. Lett.
[72] T. Fujita, T. Tokunaga, L. Zhang, D. Li, L. Chen, S. Arai, 2010, 105, 135501.
Y. Yamamoto, A. Hirata, N. Tanaka, Y. Ding, M. Chen, Nano Lett. [104] P. Liu, S. C. Mao, L. H. Wang, X. D. Han, Z. Zhang, Scr. Mater.
2014, 14, 1172. 2011, 64, 343.
[73] Y. Yang, X. Li, M. Wen, E. Hacopian, W. Chen, Y. Gong, J. Zhang, [105] Y. Zhang, X. D. Han, K. Zheng, Z. Zhang, X. Zhang, J. Fu, Y. Ji,
B. Li, W. Zhou, P. M. Ajayan, Q. Chen, T. Zhu, J. Lou, Adv. Mater. Y. Hao, X. Guo, Z. Wang, Adv. Funct. Mater. 2007, 17, 3435.
2017, 29, 1604201. [106] S. Wang, Z. Qin, G. S. Jung, F. J. Martin-Martinez, K. Zhang,
[74] Z. Liao, L. Medrano Sandonas, T. Zhang, M. Gall, A. Dianat, M. J. Buehler, J. H. Warner, ACS Nano 2016, 10, 9831.
R. Gutierrez, U. Muhle, J. Gluch, R. Jordan, G. Cuniberti, [107] X. Wang, Y. Gong, G. Shi, W. L. Chow, K. Keyshar, G. Ye, R. Vajtai,
E. Zschech, Sci. Rep. 2017, 7, 211. J. Lou, Z. Liu, E. Ringe, B. K. Tay, P. Ajayan, ACS Nano 2014,
[75] J. P. Oviedo, S. KC, N. Lu, J. Wang, K. Cho, R. M. Wallace, 8, 5125.
M. J. Kim, ACS Nano 2015, 9, 1543. [108] Y. Gong, J. Lin, X. Wang, G. Shi, S. Lei, Z. Lin, X. Zou, G. Ye,
[76] T. H. Ly, J. Zhao, M. O. Cichocka, L.-J. Li, Y. H. Lee, Nat. Commun. R. Vajtai, B. I. Yakobson, H. Terrones, M. Terrones, B. K. Tay,
2016, 8, 14116. J. Lou, S. T. Pantelides, Z. Liu, W. Zhou, P. M. Ajayan, Nat. Mater.
[77] M. R. Roenbeck, X. Wei, A. M. Beese, M. Naraghi, A. Furmanchuk, 2014, 13, 1135.
J. T. Paci, G. C. Schatz, H. D. Espinosa, ACS Nano 2014, 8, 124. [109] F. Liu, P. Ming, J. Li, Phys. Rev. B 2007, 76, 064120.
[78] E. Koren, E. Lortscher, C. Rawlings, A. W. Knoll, U. Duerig, Science [110] J. W. Suk, R. D. Piner, J. An, R. S. Ruoff, ACS Nano 2010, 4, 6557.
2015, 348, 679. [111] H. Zhao, K. Min, N. R. Aluru, Nano Lett. 2009, 9, 3012.
[79] C. Lee, X. Wei, J. W. Kysar, J. Hone, Science 2008, 321, 385. [112] Q. Lu, W. Gao, R. Huang, Model. Simul. Mater. Sci. Eng. 2011,
[80] Z. L. Wang, P. Poncharal, W. A. Heer, Pure Appl. Chem. 2000, 19, 054006.
72, 209. [113] A. Kis, D. Mihailovic, M. Remskar, A. Mrzel, A. Jesih, I. Piwonski,
[81] M.-F. Yu, O. Lourie, M. J. Dyer, K. Moloni, T. F. Kelly, R. S. Ruoff, A. J. Kulik, W. Benoît, L. Forró, Adv. Mater. 2003, 15, 733.
Science 2000, 287, 637. [114] R. C. Cooper, C. Lee, C. A. Marianetti, X. Wei, J. Hone, J. W. Kysar,
[82] R. Agrawal, B. Peng, E. E. Gdoutos, H. D. Espinosa, Nano Lett. Phys. Rev. B 2013, 87, 035423.
2008, 8, 3668. [115] R. Zhang, V. Koutsos, R. Cheung, Appl. Phys. Lett. 2016,
[83] K. S. Novoselov, A. K. Geim, S. V. Morozov, D. Jiang, Y. Zhang, 108, 042104.
S. V. Dubonos, I. V. Grigorieva, A. A. Firsov, Science 2004, 306, 666. [116] J.-W. Jiang, H. S. Park, J. Phys. D: Appl. Phys. 2014, 47, 385304.
[84] S. Wu, J. S. Ross, G.-B. Liu, G. Aivazian, A. Jones, Z. Fei, W. Zhu, [117] Z. Zhang, Y. Yang, E. S. Penev, B. I. Yakobson, Adv. Funct. Mater.
D. Xiao, W. Yao, D. Cobden, X. Xu, Nat. Phys. 2013, 9, 149. 2017, 27, 1605059.
[118] Q. Wei, X. Peng, Appl. Phys. Lett. 2014, 104, 251915. [152] M. Hirano, K. Shinjo, Phys. Rev. B 1990, 41, 11837.
[119] J.-Y. Wang, Y. Li, Z.-Y. Zhan, T. Li, L. Zhen, C.-Y. Xu, Appl. Phys. Lett. [153] T. Onodera, Y. Morita, R. Nagumo, R. Miura, A. Suzuki, H. Tsuboi,
2016, 108, 013104. N. Hatakeyama, A. Endou, H. Takaba, F. Dassenoy, C. Minfray,
[120] M. Moreno-Moreno, G. Lopez-Polin, A. Castellanos-Gomez, L. Joly-Pottuz, M. Kubo, J. M. Martin, A. Miyamoto, J. Phys. Chem.
C. Gomez-Navarro, J. Gomez-Herrero, 2D Mater. 2016, 3, 031007. B 2010, 114, 15832.
[121] C. S. Ruiz-Vargas, H. L. Zhuang, P. Y. Huang, A. M. van der Zande, [154] A. S. Wijn, C. Fusco, A. Fasolino, Phys. Rev. E 2010, 81, 1046105.
S. Garg, P. L. McEuen, D. A. Muller, R. G. Hennig, J. Park, Nano [155] G. Levita, A. Cavaleiro, E. Molinari, T. Polcar, M. C. Righi, J. Phys.
Lett. 2011, 11, 2259. Chem. C 2014, 118, 13809.
[122] G.-H. Lee, R. C. Cooper, S. J. An, S. Lee, A. Zande, N. Petrone, [156] I. V. Lebedeva, A. A. Knizhnik, A. M. Popov, O. V. Ershova,
A. G. Hammerberg, C. Lee, B. Crawford, W. Oliver, J. W. Kysar, Y. E. Lozovik, B. V. Potapkin, Phys. Rev. B 2010, 82, 155460.
J. Hone, Science 2013, 340, 1073. [157] Y. Shibuta, J. A. Elliott, Chem. Phys. Lett. 2011, 512, 146.
[123] K. Liu, Q. Yan, M. Chen, W. Fan, Y. Sun, J. Suh, D. Fu, S. Lee, [158] Z. Liu, J. Yang, F. Grey, J. Z. Liu, Y. Liu, Y. Wang, Y. Yang, Y. Cheng,
J. Zhou, S. Tongay, J. Ji, J. B. Neaton, J. Wu, Nano Lett. 2014, Q. Zheng, Phys. Rev. Lett. 2012, 108, 205503.
14, 5097. [159] J. Yang, Z. Liu, F. Grey, Z. Xu, X. Li, Y. Liu, M. Urbakh, Y. Cheng,
[124] L. Song, L. Ci, H. Lu, P. B. Sorokin, C. Jin, J. Ni, A. G. Kvashnin, Q. Zheng, Phys. Rev. Lett. 2013, 110, 255504.
D. G. Kvashnin, J. Lou, B. I. Yakobson, P. M. Ajayan, Nano Lett. [160] X. Feng, S. Kwon, J. Y. Park, M. Salmeron, ACS Nano 2013, 7, 1718.
2010, 10, 3209. [161] C. D. Engers, N. E. A. Cousens, V. Babenko, J. Britton, B. Zappone,
[125] M. W. Pruessner, T. T. King, D. P. Kelly, R. Grover, L. C. Calhoun, N. Grobert, S. Perkin, Nano Lett. 2017, 17, 3815.
R. Ghodssi, Sens. Actuators A 2003, 105, 190. [162] J. S. Bunch, S. S. Verbridge, J. S. Alden, A. M. Zande, J. M. Parpia,
[126] V. R. Stamenkovic, B. Fowler, B. S. Mun, G. Wang, P. N. Ross, H. G. Craighead, P. L. McEuen, Nano Lett. 2008, 8, 2458.
C. A. Lucas, N. M. Markovic, Science 2007, 315, 439. [163] J. S. Bunch, M. L. Dunn, Solid State Commun. 2012, 152, 1359.
[127] D. Garcia-Sanchez, A. M. van der Zande, A. S. Paulo, B. Lassagne, [164] S. P. Koenig, N. G. Boddeti, M. L. Dunn, J. S. Bunch, Nat. Nano-
P. L. McEuen, A. Bachtold, Nano Lett. 2008, 8, 1399. technol. 2011, 6, 543.
[128] U. Komaragiri, M. R. Begley, J. G. Simmonds, J. Appl. Mech. 2005, [165] K.-T. Wan, Y.-W. Mai, Acta Metall. Mater. 1995, 43, 4109.
72, 203. [166] T. Yoon, W. C. Shin, T. Y. Kim, J. H. Mun, T. S. Kim, B. J. Cho, Nano
[129] K.-T. Wan, S. Guo, D. A. Dillard, Thin Solid Films 2003, 425, 150. Lett. 2012, 12, 1448.
[130] Z. Jiang, R. Lin, P. Yu, Y. Liu, N. Wei, J. Zhao, J. Appl. Phys. 2017, [167] K. Kendall, J. Phys. D: Appl. Phys. 1975, 8, 1449.
122, 025110. [168] C. J. Brennan, J. Nguyen, E. T. Yu, N. Lu, Adv. Mater. Interfaces
[131] M. J. B. Moura, M. Marder, Phys. Rev. B 2013, 88, 032405. 2015, 2, 1500176.
[132] M.-Q. Le, R. C. Batra, Comput. Mater. Sci. 2013, 69, 381. [169] D. Vella, J. Bico, A. Boudaoud, B. Roman, P. M. Reis, Proc. Natl.
[133] R. Grantab, V. B. Shenoy, R. S. Ruoff, Science 2010, 330, 946. Acad. Sci. USA 2009, 106, 10901.
[134] Q. X. Pei, Y. W. Zhang, V. B. Shenoy, Carbon 2010, 48, 898. [170] S. Deng, E. Gao, Z. Xu, V. Berry, ACS Appl. Mater. Interfaces 2017,
[135] Y. Wei, J. Wu, H. Yin, X. Shi, R. Yang, M. Dresselhaus, Nat. Mater. 9, 7812.
2012, 11, 759. [171] S. Scharfenberg, N. Mansukhani, C. Chialvo, R. L. Weaver,
[136] T. Zhang, X. Li, S. Kadkhodaei, H. Gao, Nano Lett. 2012, 12, 4605. N. Mason, Appl. Phys. Lett. 2012, 100, 021910.
[137] A. Cao, J. Qu, Appl. Phys. Lett. 2013, 102, 071902. [172] S. Scharfenberg, D. Z. Rocklin, C. Chialvo, R. L. Weaver,
[138] M. Fujihara, R. Inoue, R. Kurita, T. Taniuchi, Y. Motoyui, S. Shin, P. M. Goldbart, N. Mason, Appl. Phys. Lett. 2011, 98, 091908.
F. Komori, Y. Maniwa, H. Shinohara, Y. Miyata, ACS Nano 2015, [173] Y. Guo, C. Liu, Q. Yin, C. Wei, S. Lin, T. B. Hoffman, Y. Zhao,
9, 9027. J. H. Edgar, Q. Chen, S. P. Lau, J. Dai, H. Yao, H. S. Wong, Y. Chai,
[139] B. Jang, A. E. Mag-isa, J.-H. Kim, B. Kim, H.-J. Lee, C.-S. Oh, ACS Nano 2016, 10, 8980.
T. Sumigawa, T. Kitamura, Extreme Mech. Lett. 2017, 14, 10. [174] Y. Wang, R. Yang, Z. Shi, L. Zhang, D. Shi, E. Wang, G. Zhang, ACS
[140] S. Singh, B. P. Patel, Compos. Struct. 2015, 119, 412. Nano 2011, 5, 3645.
[141] E. Cadelano, P. L. Palla, S. Giordano, L. Colombo, Phys. Rev. Lett. [175] H. Pan, Y.-W. Zhang, J. Phys. Chem. C 2012, 116, 11752.
2009, 102, 235502. [176] W. S. Yun, S. W. Han, S. C. Hong, I. G. Kim, J. D. Lee, Phys. Rev. B
[142] K. Kim, V. I. Artyukhov, W. Regan, Y. Liu, M. F. Crommie, 2012, 85, 033305.
B. I. Yakobson, A. Zettl, Nano Lett. 2012, 12, 293. [177] W. S. Yun, J. D. Lee, J. Phys. Chem. C 2015, 119, 2822.
[143] G. Lopez-Polin, J. Gomez-Herrero, C. Gomez-Navarro, Nano Lett. [178] Y. Y. Hui, X. Liu, W. Jie, N. Y. Chan, J. Hao, Y.-T. Hsu, L.-J. Li,
2015, 15, 2050. W. Guo, S. P. Lau, ACS Nano 2013, 7, 7126.
[144] T. Filleter, J. L. McChesney, A. Bostwick, E. Rotenberg, K. V. Emtsev, [179] L. Kou, C. Tang, Y. Zhang, T. Heine, C. Chen, T. Frauenheim,
T. Seyller, K. Horn, R. Bennewitz, Phys. Rev. Lett. 2009, 102, 086102. J. Phys. Chem. Lett. 2012, 3, 2934.
[145] C. Lee, Q. Li, W. Kalb, X.-Z. Liu, H. Berger, R. W. Carpick, J. Hone, [180] N. Lu, H. Guo, L. Li, J. Dai, L. Wang, W. N. Mei, X. Wu, X. C. Zeng,
Science 2010, 328, 76. Nanoscale 2014, 6, 2879.
[146] S. Kwon, J. H. Ko, K. J. Jeon, Y. H. Kim, J. Y. Park, Nano Lett. 2012, [181] A. M. van der Zande, J. Kunstmann, A. Chernikov, D. A. Chenet,
12, 6043. Y. You, X. Zhang, P. Y. Huang, T. C. Berkelbach, L. Wang, F. Zhang,
[147] J. Quereda, A. Castellanos-Gomez, N. Agraït, G. Rubio-Bollinger, M. S. Hybertsen, D. A. Muller, D. R. Reichman, T. F. Heinz,
Appl. Phys. Lett. 2014, 105, 053111. J. C. Hone, Nano Lett. 2014, 14, 3869.
[148] L. Fang, D. M. Liu, Y. Guo, Z. M. Liao, J. B. Luo, S. Z. Wen, Nano- [182] A. Castellanos-Gomez, R. Roldan, E. Cappelluti, M. Buscema,
technology 2017, 28, 245703. F. Guinea, H. S. van der Zant, G. A. Steele, Nano Lett. 2013,
[149] R. Zhang, Z. Ning, Z. Xu, Y. Zhang, H. Xie, F. Ding, Q. Chen, 13, 5361.
Q. Zhang, W. Qian, Y. Cui, F. Wei, Nano Lett. 2016, 16, 1367. [183] S. Yang, C. Wang, H. Sahin, H. Chen, Y. Li, S. S. Li, A. Suslu,
[150] A. Nigues, A. Siria, P. Vincent, P. Poncharal, L. Bocquet, Nat. F. M. Peeters, Q. Liu, J. Li, S. Tongay, Nano Lett. 2015,
Mater. 2014, 13, 688. 15, 1660.
[151] M. Dienwiebel, G. S. Verhoeven, N. Pradeep, J. W. Frenken, [184] M. Huang, H. Yan, C. Chen, D. Song, T. F. Heinz, J. Hone, Proc.
J. A. Heimberg, H. W. Zandbergen, Phys. Rev. Lett. 2004, Natl. Acad. Sci. USA 2009, 106, 7304.
92, 126101. [185] K. He, C. Poole, K. F. Mak, J. Shan, Nano Lett. 2013, 13, 2931.
[186] N. Levy, S. A. Burke, K. L. Meaker, M. Panlasigui, A. Zettl, F. Guinea, [196] V. H. Ho, D. T. Ho, S.-Y. Kwon, S. Y. Kim, Phys. Status Solidi B 2016,
A. H. Castro Neto, M. F. Crommie, Science 2010, 329, 544. 253, 1303.
[187] S. Manzeli, A. Allain, A. Ghadimi, A. Kis, Nano Lett. 2015, [197] K. V. Zakharchenko, M. I. Katsnelson, A. Fasolino, Phys. Rev. Lett.
15, 5330. 2009, 102, 046808.
[188] Z. Y. Ning, M. Q. Fu, T. W. Shi, Y. Guo, X. L. Wei, S. Gao, Q. Chen, [198] J. W. Jiang, T. Chang, X. Guo, H. S. Park, Nano Lett. 2016,
Nanotechnology 2014, 25, 275703. 16, 5286.
[189] Z. Y. Ning, T. W. Shi, M. Q. Fu, Y. Guo, X. L. Wei, S. Gao, Q. Chen, [199] Y. Deng, Z. Luo, N. J. Conrad, H. Liu, Y. Gong, S. Najmaei,
Nano Lett. 2014, 14, 1221. P. Ajayan, J. Lou, X. Xu, P. D. Ye, ACS Nano 2014, 8, 8292.
[190] J.-W. Jiang, H. S. Park, T. Rabczuk, J. Appl. Phys. 2013, 114, 064307. [200] C. Palacios-Berraquero, M. Barbone, D. M. Kara, X. Chen,
[191] Q. Peng, S. De, Phys. Chem. Chem. Phys. 2013, 15, 19427. I. Goykhman, D. Yoon, A. K. Ott, J. Beitner, K. Watanabe,
[192] R. Ramachandramoorthy, Y. Wang, A. Aghaei, G. Richter, W. Cai, T. Taniguchi, A. C. Ferrari, M. Atature, Nat. Commun. 2016,
H. D. Espinosa, ACS Nano 2017, 11, 4768. 7, 12978.
[193] J. W. Jiang, H. S. Park, Nano Lett. 2016, 16, 2657. [201] L. Britnell, R. M. Ribeiro, A. Eckmann, R. Jalil,
[194] L. Yu, Q. Yan, A. Ruzsinszky, Nat. Commun. 2017, 8, 15224. B. D. Belle, A. Mishchenko, Y.-J. Kim, R. V. Gorbachev,
[195] J. N. Grima, S. Winczewski, L. Mizzi, M. C. Grech, R. Cauchi, T. Georgiou, S. V. Morozov, A. N. Grigorenko, A. K. Geim,
R. Gatt, D. Attard, K. W. Wojciechowski, J. Rybicki, Adv. Mater. C. Casiraghi, A. H. Castro Neto, K. S. Novoselov, Science
2015, 27, 1455. 2013, 340, 1311.

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Review

Mechanical Properties of 2D Materials Studied

chemical and flow sensors,[8–11] flash

and defects.[41] The negative Poisson’s ratio and the dependence

relationship with crystal structures. In order

microcavity is formed by transferring

Adhesion energy of 2D materials is quite important in their ( pint − pext )Vb  V0 + Vb 

applied force and the elastic energy caused

7.2.3. Buckle/Wrinkle Based Method

Except for the adhesion energy between

where Γ is the adhesion energy, δ is the delami-

large on/off ratio, ultrasensitive photode-

10. Concluding Remarks

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