Tribology International 153 (2021) 106646

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Tribology International
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Nano friction and adhesion properties on Ti3C2 and Nb2C MXene studied
by AFM
Xuanli Zhou a, Yanbao Guo a, *, Deguo Wang a, Quan Xu b, **
a
College of Mechanical and Transportation Engineering, China University of Petroleum, Beijing, 102249, China
b
State Key Laboratory of Heavy Oil Processing, China University of Petroleum, Beijing, 102249, China

A R T I C L E I N F O A B S T R A C T

Keywords: MXene has been widely used in energy storage, photocatalysis and lubrication area due to its good mechanical,
Ti3C2 MXene electrical, and chemical properties. However, its friction and adhesion properties have not yet been fully grasped.
Nb2C MXene In this study, for the first time, atomic force microscopy (AFM) Nanoman technology was used to compare the
Friction
nano friction and adhesion of Ti3C2 and Nb2C MXene. The results indicated that the friction and adhesion of
AFM
Nb2C were less than Ti3C2 under the same conditions, which is related to the difference in surface dipole moment
density. In addition, adhesion and friction of both two MXenes decrease with the temperature increase. This
study provides a broader application prospect for these new materials.

1. Introduction
MXene is an emerging two-dimensional layered transition metal
carbide and nitride [1]. A lot of attention has been gained due to its
structure similar to graphene and its excellent mechanical [2–4], optical
[5–7], electrical [8,9], chemical [10,11], magnetic [12,13] and elec­
trochemical [14,15] characteristics. In addition, low friction and wear
characteristics provide MXene with a broad range of tribological ap­
plications, including as a liquid additive [16], an ultra-thin solid lubri­
cants [17] and nanofillers of composite materials [18]. Friction is very
common in almost every field, and often accompanied by huge energy
losses [19]. Therefore, MXene materials are catching a lot of attentions
because of their low friction and adhesion.
Ti3C2 and Nb2C MXene are very popular due to their layered struc­
ture and excellent physical and chemical properties [20]. Ti3C2 has low
shear strength, lubricating properties and high mechanical strength
[21]. Therefore, some scholars have studied the macroscopic and
microscopic friction properties of Ti3C2. Liu and Zhang et al. added Ti3C2
MXene as an additive to the base oil to greatly improve the anti-wear
ability of the oil [16,22]. Mai et al. used Ti3C2 MXenes as a lubri­
cating nanofiller to synthesize metal matrix composites to reduce the
friction and wear rate of the coating [23]. Zhang et al. calculated the
interlaminar sliding of Ti3C2 MXene with interlaminar friction co­
efficients between 0.24 and 0.27 [24]. Lian et al. evaluated Ti3C2 as a
solid lubricant for sliding friction. It is shown that the friction coefficient
of the Ti3C2 modified sample is much lower than that of the unmodified
sample [25]. All these studies have shown that Ti3C2 MXene nanosheets
have excellent friction properties and broad lubrication application
prospects, however, the investigation on the nanoscale is very lacking.
At the same time, Nb2C has shown promise in various applications such
as battery energy storage [26], adsorption [27], electrons [28], and
photocatalysis [29]. So far, as far as we know, there is no tribological
experimental study on Nb2C. Sha et al. studied the structure and me­
chanical properties of Nb2C. Nb2C is considered as a potential superhard
material [30]. Therefore, it is necessary to study the microscopic friction
of Nb2C.
In this study, the friction and adhesion behavior of these two mate­
rials on the nanoscale were studied and compared in this paper. First,
Ti3C2 and Nb2C MXene were either prepared or purchased, respectively,
and their morphology and chemical structure were characterized by
scanning electron microscope (SEM), X-ray photoelectron spectroscopy
(XPS) and Fourier transform infrared (FTIR). Then, we used an in-situ
atomic force microscope (AFM) to test the adhesion and friction force
of Ti3C2 and Nb2C MXene. The results show that under the same con­
ditions, the friction and adhesion of Ti3C2 are significantly greater than
Nb2C. This is due to the difference in polarity and dipole moment of the
materials. The adhesion and friction characteristics of the two MXenes
are similar. Both friction and adhesion increase with the pressure

* Corresponding author.
** Corresponding author.
E-mail addresses: gyb@cup.edu.cn (Y. Guo), xuquan@cup.edu.cn (Q. Xu).

https://doi.org/10.1016/j.triboint.2020.106646
Received 24 July 2020; Received in revised form 3 September 2020; Accepted 11 September 2020
Available online 14 September 2020
0301-679X/© 2020 Elsevier Ltd. All rights reserved.
X. Zhou et al.
Fig. 1. Schematic diagram of experimenting with 2D materials using AFM.
increase but decrease with the temperature increase. These findings will
greatly enhance the understanding of the nanoscale adhesion and fric­
tion characteristic of MXene materials.
2. Methods
2.1. Sample preparation
Ti3C2 was prepared by HF solution etching. TiC sample which ob­
tained from Johnson Matthey Electronic and Ti2AlC sample which
provided by 3-ONE-2 were mixed to synthesize Ti3AlC2 sample. The
molar ratio is 1:1. Then, the mixture was heated to 1350 ◦ C and argon
gas was introduced. After 2 h, the mixture was crushed in mortar. 5 g of
the mixture was evenly dispersed in 50 mL of HF (50%) solution and
stirred for 2 h. Then, the solution was washed 5 times with alcohol and
deionized water and then centrifuged. Finally, the powder was dried
using a freeze dryer to obtain Ti3C2.
The Ti3C2 and Nb2C (11 Technology Co., Ltd.) powders were sepa­
rately dispersed in deionized water. Then the dispersion was sonicated
for 30 min. The solution was dropped onto the mica plate and air dried.
2.2. Characterization
2.2.1. Scanning electron microscope
The microstructure of the material has a great influence on its per­
formance. The morphology of the two MXene samples, Ti3C2 and Nb2C
MXene, was collected by using a Scanning Electron Microscope
(SU8010, Hitachi). In order to observe the layered structure of the two
samples better, multi-layered areas were selected for observation. The
current used is 10 mA and the voltage is 5 kV. The working temperature
is 20 ◦ C, and the ambient humidity is 20%.
2.2.2. Transmission electron microscope
Transmission electron microscopy (TEM) uses electron beams as the
light source, greatly shortening the wavelength of the light, thereby
improving the resolution. Transmission electron microscopy (Tecnai G2
f20 200 kV, FEI) was used to characterize the nanostructures of the two
MXenes. The acceleration voltage is 200 kV, and the dot resolution is
0.24 nm 1 mg solid powder sample was sonicated in ethanol for 20 min
and then dropped into the copper mesh for testing.
2.2.3. X-ray diffraction
Two MXene samples were measured by Bruker D8 Advance X-ray
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Tribology International 153 (2021) 106646
Diffraction (D8 Advance, Bruker). The elemental composition of MXene
samples and the molecular structure are important factors influencing
friction and adhesion [31,32]. Therefore, the analysis of the phase and
the crystal was carried out by analyzing the diffraction pattern. The tube
voltage is 40 kV, tube current is 10 mA and the scan step length is 0.02◦ .
2.2.4. X-ray photoelectron spectroscopy
The different adhesion and friction characteristic of the two samples
are also attributed to differences in compound structure and element
category [33]. The X-ray Photoelectron Spectroscopy (K-Alpha+,
Thermo) was used to measure the difference between Ti3C2 and Nb2C
MXene samples under the same conditions. The test energy is 1486.8 eV
and spot area is 400 μm. The voltage of test tube is 15 kV and current is
10 mA. The background vacuum of the analysis chamber is 2 × 10− 9
mbar.
2.2.5. Fourier Transform Infrared Spectrometer
Ti3C2 and Nb2C MXene samples were measured using Fourier
Transform Infrared Spectrometer (VERTEX 70, Bruker). The resolution
can reach 4 cm− 1, and the scan time is 7 s. FTIR is based on dried po­
tassium bromide (KBr) as a background. 10 mg of KBr and 0.1 mg of
MXene sample were mixed and prepared into tablets, and then the
transmission infrared test was performed. FTIR determines the form of a
chemical bond by analyzing parameters such as the position and in­
tensity of the absorption peak.
2.3. Friction and adhesion measurements
AFM is a commonly used instrument for measuring the mechanical
properties of materials at the nanoscale [34–37]. Friction and adhesion
experiments were performed on Mica, Ti3C2 and Nb2C MXenes using a
situ Atomic Force Microscope (Dimension Icon, Bruker) including tem­
perature control modules as shown in Fig. 1. The parameters studied in
the experiment include pressure, sliding speed, temperature and delay
time. The difference in nanoscale adhesion and friction properties of the
two materials was compared. In order to reduce the influence of the
number of layers on the experimental results, more than 20 layers of
both materials were used for testing (S1). The probe model used in this
test was MESP-HM. The deflection sensitivity is 90.32 nm/V and the
spring constant is 4.332 N/m. The laboratory humidity is constantly
controlled at 20%. Each experiment was repeated 5 times.
X. Zhou et al.
Fig. 2. (a) SEM image of Ti3C2. (b) SEM image of Nb2C. (c, d) TEM images of Ti3C2. (e, f) TEM images of Nb2C.
3. Results and discussion
SEM images of Ti3C2 and Nb2C are shown in Fig. 2(a) and (b),
respectively. Both Ti3C2 and Nb2C are layered structures similar to ac­
cordion. Self-stacking occurs between the nanosheet layers, which is
caused by strong van der Waals forces [38]. Fig. 2(c) and (d) are TEM
images of Ti3C2, and Fig. 2(e) and (f) are TEM images of Nb2C. Ti3C2
MXene exhibits a multilayer crystal structure (Fig. 2(c)). Fig. 2(d) shows
that the typical lattice fringe spacing is about 0.98 nm (002) [39]. As
shown in Fig. 2(e), the Nb2C flakes are very thin. From Fig. 2(f), it can be
seen that the lattice fringe width is 0.26 nm and the crystal plane angle is
60◦ , indicating that the sample is high-quality Nb2C MXene [28]. A
diffraction pattern of pure Ti3C2 and Nb2C is shown in S2. On the 2θ
scale, the observed peak characteristics are very consistent within the
standard Ti3C2 and Nb2C. Thus, the results indicated that the two
experimental samples are pure and have a similar 2D layered structure.
The XPS results has been displayed in Fig. 3. S3 is XPS full spectrums
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of Ti3C2 and Nb2C. It can be observed from the figure that the Al element
is completely etched away during the preparation of Ti3C2. The spectra
for Ti 2p, C 1s, and O 1s of Ti3C2 are displayed in Fig. 3(a), (c) and (e)
while the spectra of Nb 3d, C 1s, O 1s of Nb2C are shown in Fig. 3(b), (d)
and (f), respectively. The elemental composition and chemical bond of
the two MXenes are observed at different binding energies. The three
chemical bonds of Ti–C, Ti–O and Ti-X are shown in the Ti 2p spectrum
in Fig. 3(a). The peaks at 460.4 eV (Ti–C 2p1/2) and 454.8 eV (Ti–C 2p3/
2) represent Ti–C bonds of Ti3C2. Peaks delegating Ti–O 2p1/2 and Ti–O
2p3/2 were found at 463.1 and 458 eV. Fig. 3(b) shows the presence of
Nb (V) and NbCxOy in addition to its own Nb–C bond. This indicates that
the sample is oxidized and Nb2C(OH) is present. The C 1s spectrum of
Ti3C2 in Fig. 3(c) can be deconvoluted into three peaks at 281.6, 284.3
and 285.5 eV, representing C–Ti, C–C, and C–O, respectively. In addi­
tion, 3 absorption peaks were observed in the O 1s of Ti3C2: 529.7, 531.4
and 533.2 eV (Fig. 3(e and f)). The 529.7 eV peak represents lattice
oxygen (O1). The 531.4 eV peak represents the oxygen defects (O2)
X. Zhou et al. Tribology International 153 (2021) 106646

Fig. 3. XPS spectra for Ti2p (a), C1s (c) and O1s (e) of Ti3C2. XPS spectra for Nb3d (b), C1s (d), O1s (f) of Nb2C.

[40]. The 533.2 eV peak corresponds to the surface-adsorbed oxygen

species (O3), and based on the result, the content of lattice oxygen (O1)
in Nb2C is much higher than that in Ti3C2, but the content of
surface-adsorbed oxygen species (O3) is less than Ti3C2.
Fig. 4 shows the FTIR spectra of Ti3C2 and Nb2C MXene and the
absorption peaks of the hydroxyl groups were located at 3428 cm− 1 and
1637 cm− 1, respectively. This is consistent with the Ref. [41]. In Ti3C2
sample, the peaks at 610 cm− 1 and 484 cm− 1 are caused by deformation
vibration of Ti–O bond and Ti–C bond [42,43]. And in Nb2C sample, the
peaks at 475 cm− 1 and 597 cm− 1 represent Nb–C bonds and Nb–O
bonds, respectively [44,45]. In addition, C–O (1060 cm− 1), C = C (1520
cm− 1) was also found in the spectrum. The C–O bond may cause by the
terminations O on the sample surface.
Since the test measures the voltage signal, the friction force is got by
multiplying the elastic coefficient by the voltage. Therefore, the elastic
coefficient K1 needs to be calculated by the following formula [46]:

Ewt3 2l
K1 = k 1 S 1 = S1 = kn Sn
6l2 (h + t/2) 3(h + t/2)

Fig. 4. FTIR spectra of Ti3C2 and Nb2C MXene samples. where w, t, l, h and E are the width, thickness, length, tip height and

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Fig. 5. (a) Friction curves of Ti3C2 and Nb2C at pressures of 4 μN at 30 ◦ C. (b) Friction of Ti3C2 and Nb2C at pressures of 2–8 μN at 30 ◦ C. (c) Friction of Mica, Ti3C2
and Nb2C at 4 μN at 25–40 ◦ C. (d) Adhesion curves of Mica, Ti3C2 and Nb2C MXene at the preloading force of 30 nN at 25 ◦ C. (e) Adhesion of Mica, Ti3C2 and Nb2C at
the preloading force of 10–60 nN at 25 ◦ C. (f) Adhesion force of Mica, Ti3C2 and Nb2C at the preloading force of 60 nN at 25–40 ◦ C.

Young’s modulus of the cantilever beam, respectively. Sn is the known
reflection sensitivity, and kn is spring constant of the cantilever beam
(obtained by thermal tuning before the experiment [47]).
Fig. 5(a) is a friction curve of Ti3C2 and Nb2C obtained by friction
tests at a pressure of 4 μN and a temperature of 30 ◦ C. Their frictional
forces reach maximum at 1 s and tend to stabilize as the probe continues
to slide. Fig. 5(b) shows a comparison of friction of Ti3C2, Nb2C and Mica
at a pressure of 2 μN–8 μN and a temperature of 30 ◦ C. The friction of
both materials increases proportionally with increasing pressure. This is
because the contact area of the probe and the sample increases as the
pressure increases. However, the friction of Nb2C is always smaller than
Ti3C2, and the gap increases with the increase of pressure. Fig. 5(c)
shows the change in friction of the materials at 25 ◦ C-40 ◦ C. The probe
speed was 0.2 μm/s and the experimental pressure was 4 μN. When the
temperature was raised from 25 ◦ C to 40 ◦ C, the friction of Ti3C2 and
Nb2C samples showed a downward trend, and decreased by about 61%
and 92%, respectively. At the same time, the friction of Nb2C is always
lower than the friction of Ti3C2 at any temperature. The main reason for
the decrease in the frictional force of Ti3C2 is that the degree of oxidation
of Ti3C2 increases with increasing temperature. When the O atom re­
places the C atom in the sample, the electron cloud is more evenly
distributed and the sample surface becomes denser. Therefore, the
degree of polarization of the sample is lowered. On the other hand, high
temperature causes the surface charge of the sample to move faster and
is less likely to accumulate. This all leads to a reduction in the friction
and adhesion of Ti3C2 [32]. Fig. 5(d) is a graph showing the adhesion
curve of Ti3C2 and Nb2C at adhesion force of 30 nN and 25 ◦ C. Fig. 5(e)
shows the change in adhesion force of Ti3C2 and Nb2C at a preloading
force of 10–60 nN. The adhesion force increases as the preloading force
increases. It clearly showed that Ti3C2 has an inflection point when the
force is 40 nN while Nb2C has an inflection point when the pressure is
50 nN. This is caused by the probe penetrating the single-layer nano­
sheet. The topography of the probe before and after unloading is shown
in S4. As can be seen from Fig. 5(f), the adhesion force of both Ti3C2 and
Nb2C decreases as the temperature increases. When the temperature was
raised from 25 ◦ C to 40 ◦ C, the adhesion of Ti3C2 decreased by 42%
while the adhesion of Nb2C decreased by 72%. From the results of the
temperature experiment, we can see that the friction and adhesion of the
two materials have the same trend. This is because the change trend of
adhesion and friction is consistent with the strength of molecular
interaction [48]. When the temperature increases, the adhesion of the
two MXene materials decreases, so the drag force that needs to be
overcome during friction also decreases. By comparing mica materials, it
is found that the friction and adhesion of the two MXene materials are

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X. Zhou et al.
Fig. 6. Schematic diagram of the structure and friction principle of (a) Ti3C2 and (b) Nb2C.
very small and easily affected by temperature. In addition, the sliding
speed of the probe and the residence time on the sample before the probe
slides have a negligible effect on the friction force of the Ti3C2 and Nb2C
MXene (S5 and S6). AFM was used to analyze the roughness of the test
area of the two MXene materials. The results show that the roughness of
the test area of the two materials is close, so the influence of roughness
on the results of friction and adhesion experiments is negligible (S7).
By consulting the references, it is found that the surface dipole
moment density is different due to the different molecular structures of
the Ti3C2 and Nb2C [49,50]. The molecular structure diagrams and
friction principle of Ti3C2 and Nb2C are shown in Fig. 6. When the
surface terminations is O or OH, the dipole moment and polarity of Ti3C2
are both greater than Nb2C. Therefore, the surface of Ti3C2 is more likely
to accumulate charge than Nb2C. When the surface terminations is O and
OH, the surface dipole moment density of Ti3C2 are 0.01976 e/Å and
− 0.0334 e/Å, respectively, and the surface dipole moments of Nb2C are
0.01121 e/Å and − 0.02609 e/Å, respectively [50]. Therefore, the sur­
face of Nb2C is denser than Ti3C2 and the electron cloud distribution is
more uniform. This is the root cause of the low friction and adhesion of
Nb2C.
Because MXene has excellent mechanical properties and has become
an important area of friction research, researchers have high hopes for
research on MXene. However, because of the wide variety of MXene and
the different chemical structures that lead to a variety of frictional
properties, the study of its friction properties is very challenging. In this
study, the results of XRD, XPS and FTIR analysis can be mutually verified
to better understand the chemical structure of Ti3C2 and Nb2C MXene.
The difference in chemical structure between the two MXene results in a
difference in dipole moment and polarity. The surface dipole moment
density of Ti3C2 obtained in the literature is greater than Nb2C [50],
which may be the cause of the friction and adhesion of Ti3C2 being
generally higher than Nb2C. The AFM experiment investigated the ef­
fects of pressure, temperature and probe slip speed on MXene materials
in order to gain a deeper understanding of the mechanical properties of
MXene. By comparing the nanoscale friction properties of the Ti3C2 and
Nb2C MXene materials not only link their frictional behavior to the
microstructure, but can also potentially provide insight into the mo­
lecular level required for their application to tribological behavior. Be­
sides, they are expected to be used in next-generation electronic devices
and nanoelectromechanical systems (NEMS) because of good nano
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mechanical properties.
4. Conclusion
In our experiments, the main chemical bonds contained in Ti3C2
were Ti–C, Ti–O, Ti-X, C–O, and C–C. Nb2C mainly includes Nb–C,
NbCxOy, and Nb(V). The results of atomic force microscopy experiments
show that the friction and adhesion of Ti3C2 are greater than Nb2C under
the same conditions. The nanomechanics of the two samples is similar.
The interface friction and adhesion between the MXene and the probe
increases with increasing pressure and decreases at high temperatures.
However, friction and adhesion force of samples are independent of the
movement speed and residence time of probe tip. The adhesion and
friction force of the sample are related to the dipole moment and po­
larity of the molecule. The greater the polarity and dipole moment, the
greater the friction and adhesion. This research is of great significance
for establishing the relationship between friction properties and
microstructure of different MXenes and expanding its application in the
micro-nano field.
Declaration of competing interest
The authors declare that they have no known competing financial
interests or personal relationships that could have appeared to influence
the work reported in this paper.
Acknowledgements
This research was supported by grants from the National Natural
Science Foundation of China (No. 51675534).
Appendix A. Supplementary data
Supplementary data to this article can be found online at https://doi.
org/10.1016/j.triboint.2020.106646.
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