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Communications
MXene
Stabilizing MXene by Hydration Chemistry in Aqueous Solution
Xingyu Wang, Zhiyu Wang,* and Jieshan Qiu
Abstract: MXenes attract interest in diverse fields but suffer
from fast structural degradation by attacking of dissolved
oxygen and water molecules in aqueous solution. This draw-
back hinders the long-term storage, applications and under-
standing of the chemical nature of MXenes. Herein, we report
a cost-effective and environmentally sustainable way for long-
term storage of MXenes in aqueous solution by hydration
chemistry of nontoxic inorganic salts. The attacking of MXene
by free water and dissolved oxygen molecules is inhibited by
decreasing the water activity, which simultaneously lowers the
dissolved oxygen concentration, of saline solution. As a result,
the storage life of MXene can be prolonged to up to 400 days at
ambient conditions without loss of intrinsic surface chemistry
and bulk carrier properties. Over 90 % of salt protectant can be
recycled by simply evaporating the final waste liquor after fully
extracting the MXene to minimize the waste discharge and
processing cost. This work offers a commercializable approach
with high cost-effectiveness, processing sustainability and
environmental benefit for extending the shelf life of MXenes.
Transition metal carbide/nitrides named as MXenes have
emerged as a new type of two-dimensional (2D) materials
with a quickly expanding family and applications.[1] They
share a general chemical formula of Mn+1XnTx (n = 1–3),
where Mn+1Xn stands for transition metal carbide/nitride
backbone and T is chemical groups (e.g., -OH, -O, -F, -Cl)
grafted on it.[1a] One of the most remarkable features of
MXenes is the metallic character enabled by intrinsic high
carrier density (e.g., 8  3  1021 cm 3 for Ti3C2Tx).[2] This
favorable characteristic can be further tuned across a wide
spectrum by the strong interaction of plasmonic MXenes with
broadband electromagnetic waves.[1c, 3] Moreover, the pres-
ence of abundant chemical groups on MXene surface brings
the extra benefit of rich surface chemistry.[4] Their interplay
with Mn+1Xn backbones also allows one to readily tailor the
electronic band structure and surface properties of MXenes in
a wide range (e.g., from semiconductive to metallic, hydro-
philic to hydrophobic).[1a] A good combination of these
fascinating merits renders high promise of MXenes in vast
[*] X. Y. Wang, Prof. Dr. Z. Y. Wang
State Key Lab of Fine Chemicals, Liaoning Key Lab for Energy
Materials and Chemical Engineering, School of Chemical Engineer-
ing, Dalian University of Technology
Dalian 116024 (China)
E-mail: zywang@dlut.edu.cn
Prof. Dr. J. S. Qiu
College of Chemical Engineering, Beijing University of Chemical
Technology
Beijing 100029 (China)
Supporting information and the ORCID identification number(s) for
the author(s) of this article can be found under:
https://doi.org/10.1002/anie.202113981.
Angew. Chem. Int. Ed. 2021, 60, 26587 –26591
Chemie
How to cite: Angew. Chem. Int. Ed. 2021, 60, 26587 – 26591
International Edition: doi.org/10.1002/anie.202113981
German Edition: doi.org/10.1002/ange.202113981
applications such as energy, catalysis, superconductor, elec-
tromagnetic shielding, biotherapy and edge-cutting smart
technologies, etc.[5]
However, the MXenes generally suffer fast structural
degradation by oxidation in aqueous solution, which greatly
shortens their storage life and makes practical use difficult.[6]
The reaction of MXenes with dissolved oxygen can be limited
in short days by protecting them in the solution saturated with
inert gas.[7] Freezing at ultralow temperature (e.g., 20 8C)
can also restrict the oxidation kinetics of MXenes to extend
the shelf life to two years at a high cost.[8] Usually, the
oxidation is initiated at the defect and edge sites of MXenes.
It can be reduced by exfoliating them to large nanosheets or
capping the edge/defect sites by polyanionic salts.[7, 9] Apply-
ing reductive capping agents like sodium L-ascorbate can save
the MXenes in solution for 21 days at a low cost but still
cannot meet the desire of long-term storage.[10] The difficulty
in complete removal of these strongly adsorbed species from
MXene surface also makes it hard to restore the intrinsic
properties and chemical compatibility of MXenes. Hydrogen
annealing also works effectively to improve the stability of the
MXenes but causes a loss of redispersibility and surface
reactivity.[11] More recently, Ti3C2Tx MXene with better
oxidation resistance was fabricated from Al-rich Ti3AlxC2
precursor with higher crystallinity.[12] Nevertheless, there is
still a lack of immediately commercializable ways for low-cost
and environmentally sustainable storage of MXenes in long
term.
Besides dissolved oxygen, the water molecules also play
a critical role in damage of MXene structure. They act as not
only a solvent of dissolved oxygen but also a proton source to
degrade the MXenes to methane and metal oxides.[13]
Replacing the water by non-aqueous polar solvents (e.g.,
isopropanol, NMP, DMSO, ethanol) is reasonably beneficial
to prevent the MXenes from water attacking.[13a, 14] Never-
theless, the negative effect of dissolved oxygen on MXene
stability is still predominant or even worse in organic solvents
with higher oxygen solubility relative to water. Poor disper-
sibility of MXenes in most organics and tedious removal of
these toxic solvents further raise the processing complexity
and cost for MXene storage.
Herein, we report a cost-effective and environmentally
sustainable way for long-term storage of MXenes in aqueous
solution by hydration chemistry of inorganic salts with
nontoxicity, abundant reserve and low cost (e.g., NaCl, LiCl
and CaCl2) under ambient conditions (Figure 1). Their
hydration effect is utilized to decrease the ratio of free
water molecules in solution and their interplay with MXenes.
A low residue of free water simultaneously restricts the
oxygen solubility in solution to suppress MXene oxidation,
which is difficultly achieved by replacing water with organic
solvents. Benefited from a synergistic reduction of oxygen and
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Figure 1. Schematic illustration of the protection mechanism of
MXenes by hydration chemistry.
water attacking, the storage life of Ti3C2Tx MXene could be
prolonged to up to 400 days in saturated saline solution with
less sacrifice of their intrinsic properties. Upon use, the salt
protectants can be readily rinsed out to restore the good
dispersibility of MXenes, over 90 % of which can be recycled
for better cost-effectiveness and processing sustainability.
The effectiveness of hydration chemistry on protecting
MXenes is firstly demonstrated in aqueous NaCl solution by
taking extensively used Ti3C2Tx MXene as an example. Fresh
Ti3C2Tx MXene has a typical nanosheet morphology with
a flat surface (Figure 2 a, Figure S1a). The Ti 2p X-ray
photoelectron spectroscopy (XPS) spectrum of such MXene
can be divided into four 2p3/2/2p1/2 doublets at 455.2/460.8,
456.2/461.9, 457.3/463.0 and 458.9/464.3 eV for Ti-C, Ti2+, Ti3+
Figure 2. a) TEM image of fresh MXene; b) XPS spectra of fresh
MXene and MXene after saving in saturated NaCl solution for one
month. c) TEM image of NaCl-protected MXene. d) XRD, e) Raman
and f) FT-IR spectra of fresh and NaCl-protected MXene.
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Chemie
and Ti-O species, respectively (Figure 2 b). After storage in
saturated NaCl solution for one month, the original nano-
sheet shape of Ti3C2Tx MXene is well retained at ambient
condition (Figure 2 c, Figure S1b). Good retention of the
chemical structure of MXene is revealed by a similar Ti 2p
spectrum with fresh one in terms of peak position and
intensity (Figure 2 b). Compared to fresh MXene (4 % Ti-O,
50 % Ti-C), the ratio of Ti-O species is slightly increased to
9 % while the amount of Ti-C species remains nearly the same
to reveal a high reserve of conductive Ti3C2 backbone. In
sharp contrast, the Ti3C2Tx MXene is rapidly oxidized to TiO2
without any residue after one-month storage in pure water
(Figure S2a, Figure S3a). The X-ray diffraction (XRD) anal-
ysis validates the good retention of crystalline structure for
Ti3C2Tx MXene protected in saturated NaCl solution. Both
fresh and NaCl-protected Ti3C2Tx MXene exhibit similar
XRD patterns with fingerprint (002) diffraction along with
weak peaks from the (004), (0010) and (110) planes of
hexagonal Ti3C2 lattice (Figure 2 d). The NaCl-protected
Ti3C2Tx MXene also resembles the structural and electronic
properties of fresh one, indicated by similar A1g out-of-plane
vibration modes at 204 and 720 cm 1 for C and Ti atoms, and
the Eg in-plane vibration modes at 283, 375, and 623 cm 1 for
C, Ti and surficial groups in Raman spectra, respectively
(Figure 2 e). No signals from TiO2 are detected by both XRD
and Raman analysis, indicating low oxidation of NaCl-
protected Ti3C2Tx MXene after one month. Fourier transform
infrared spectroscopy (FT-IR) spectra reveal the reserve of
surface chemistry for NaCl-protected Ti3C2Tx MXene. It is
characterized by strong adsorption bands of -OH asymmetric
stretching (3429 cm 1), asymmetric vibration (2890 cm 1),
and bending vibration of -OH (1630 cm 1) that resembles
fresh MXene (Figure 2 f). The UV-vis spectra of NaCl-
protected Ti3C2Tx MXene reprint the pattern of fresh one
with two broad plasmonic bands in a wavelength range of
200–400 nm and 700–850 nm, implying a negligible loss of
electronic structure after storage (Figure S4a). Benefited
from greatly suppressed oxidation, the NaCl-protected
Ti3C2Tx MXene exhibits a comparable electrical conductivity
of 4834 S cm 1 to fresh one (4977 S cm 1) after one-month
storage in saturated NaCl solution. The salt can be readily
removed by several centrifugation-separation cycles due to its
high solubility in water and weak adsorption on MXene. After
rinsing NaCl out, the Ti3C2Tx MXene can restore good
dispersibility to form a homogenous aqueous colloid with an
apparent Tyndall effect (Figure S5) and a similar Zeta
potential with that of fresh one (Figure S6). XPS analysis
shows that the Cl residue in rinsed MXene is as low as
2.36 at.%, comparable to that of fresh sample (1.67 at.%),
showing efficient removal of NaCl from MXene surface.
Water is the only solvent for the storage and separation of
MXene. Over 90 % of NaCl can be recycled in high purity by
simple evaporation of final waste liquor for repeated use
(Figure S7), rendering high cost-effectiveness, processing
sustainability and environmental benefit.
The stability of Ti3C2Tx MXene tends to increase with
NaCl concentration rising in aqueous solution, manifesting as
a reduction of Ti O bond ratio but increase of Ti C bond
ratio in XPS spectra (Figure S2, Figure S3) In solution with
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< 3.0M NaCl, the MXene experiences reduced but still
apparent oxidation after one-month storage, visualized by
the coverage of white deposit on black MXene along with the
rise of TiO2 peaks in XRD pattern (Figure 3 a, b and
Figure S8). No MXene is left after saving in pure water for
one month at all. The intensity of normalized UV-vis peak at
a wavelength (l) of 785 nm, where the Ti3C2Tx MXene
reaches maximum absorption in the near-infrared region
(NIR), is used as an indicator to detect the oxidation degree
of MXene (Figure S4). It decreases rapidly to nearly zero for
Ti3C2Tx MXene in pure water within 30 days by fast oxidation
to TiO2 (Figure 3 c). In contrast, the MXene degradation is
largely mitigated once introducing the NaCl into the aqueous
solution. The oxidation kinetics of MXene is getting slower
with NaCl concentration increasing until a rather slow rate in
saturated NaCl solution (Figure 3 c). The curve of oxidation
kinetics for Ti3C2Tx MXene in NaCl solution follows an
empirical law of A = Aunre + Are e t/t, where Aunre and Are stand
for the unreactive and reactive MXene, and t is the time
constant (days).[15] A larger t means a longer time scale of
MXene against oxidation on average, namely, the better
stability in aqueous solution. For Ti3C2Tx MXene in pure
water, the t is as short as 10.4 days, indicating poor stability. In
contrast, it can be significantly prolonged to 53.5, 125.2 and
a maximum of 480.7 days by storage in solution with 1.0M,
3.0M and saturated NaCl, respectively. Such a dramatic
t improvement indicates the high effectiveness of NaCl in
stabilizing the MXene in aqueous systems.
Figure 3. a) Optical photos and b) XRD patterns of Ti3C2Tx MXene
after one-month storage in NaCl solution with various concentrations.
c) The intensity of normalized UV-vis peak of Ti3C2Tx MXene stored in
NaCl solution with different concentrations at l = 785 nm for different
times. The dot lines are the curves fitted to the empirical law
(A = Aunre + Are e t/t). A correlation between dissolved oxygen concen-
tration or water activity and d) NaCl concentration or e) Ti-O ratio in
Ti3C2Tx MXene. f) A relationship of time scale (t) of Ti3C2Tx MXene
against oxidation with dissolved oxygen concentration or water activity
in NaCl solution with different concentrations.
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Chemie
The ionic shielding effect may work but not play a vital
role in stabilizing the MXene in NaCl solution. Distinct to
polyanionic salts,[7, 9] the inorganic salts with a small anionic
size are not sufficient to protect the defect/edge sites of
MXene from attacking by oxygen and water molecules. Thats
why the MXene made by popular way of LiF/HCl etching still
encounters fast oxidation although they naturally have Li+
and Cl on the surface. Noted that water molecules play
a dual role of proton source and solvent of dissolved oxygen in
triggering oxidation of MXene. The improvement of MXene
stability in NaCl solution may be primarily related to
a reduction of free water molecules by strong hydration
effect enabled by its small ionic radius (Na+: 102 pm, Cl :
184 pm) and high hydration enthalpy (Na+: 406 kJ mol 1,
Cl : 364 kJ mol 1). To confirm this mechanism, the corre-
lation of NaCl concentration with water activity, a descriptor
of the ratio of free water in solution, and dissolved oxygen
concentration is examined (Figure 3 d). The water activity is
decreased from 1.00 to 0.76 with NaCl concentration rising
from zero to saturated level (ca. 5.5M at room temperature).
This phenomenon indicates the lowering of the free water
ratio in solution with NaCl concentration increasing. Such
effect not only mitigates the attacking of MXene by water but
also effectively reduces the dissolved oxygen concentration by
up to 5.5 folds with respect to pure water. With the water
activity and dissolved oxygen concentration decreasing in
concentrated NaCl solution, the degradation of Ti3C2Tx
MXene to TiO2 is significantly restricted to reduce the ratio
of Ti O bonds (Figure 2 b, Figure 3 e and Figure S2). Accord-
ingly, the time scale of MXene against oxidation can be
extended by up to 48 times relative to those saved in pure
water (Figure 3 f). Such correlations highlight the significant
effect of hydration chemistry on suppressing MXene degra-
dation in aqueous solution.
The above results suggest the water activity may be a good
indicator to direct the choice of salt protectant for stabilizing
MXene in aqueous solution. Soluble inorganic salts consisting
of smaller ionic size tends to exhibit a lower water activity,
reflecting a lower ratio of free water molecules in solution to
protect the MXene better (Figure 4 a).[16] The salts consisting
of both the cation and anion with ionic radius blow 102 pm
(e.g., Li+, Na+, Ca2+, Zn2+) and 196 pm (e.g., F , Cl , Br ,
NO3 , OH ) can greatly reduce the water activity. This
phenomenon can be understood by stronger ion-dipole
interactions of smaller ions with water, which effectively
binds the free water molecules to reduce the water activity
and attacking of MXene by them and dissolved oxygen.
Specifically, the salts containing the Li+, Na+, Ca2+, Zn2+ and
Cl would be good candidates of MXene protectant due to
their reserve abundance, high solubility, low toxicity and
chemical reactivity. Among them, the CaCl2 with a similar
cation radius (100 pm) to that of NaCl (102 pm) but a higher
charge number and water solubility (ca. 6M) can further
reduce the water activity to 0.36 in saturated solution. It
works effectively to save Ti3C2Tx MXene for over six months
with a slight increase of the Ti-O ratio from 4 % to 12.2 %
(Figure 4 b). A water activity of as low as 0.12 can be achieved
by saturated solution of LiCl with rather high solubility
(> 13M), hydration enthalpy ( 520 kJ mol 1) but a smaller
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Figure 4. a) Water activity of saturated solution of various inorganic
salts with different cation and anion radii. The salts with anion and
cation size in the blue shaded area induce low water activity for better
protection of MXene(marked by the red stars). b) XPS spectrum and
optical photo (the inset) of Ti3C2Tx MXene stored in saturated CaCl2
solution after six months. c) The intensity of normalized UV-vis peak
of Ti3C2Tx MXene stored in saturated LiCl solution at l = 785 nm for
different times. It is well fitted to the empirical law with a t of 1203.9
days. d) XPS spectrum of MXene stored in saturated LiCl solution after
400 days.
cation radius (76 pm). It can dramatically extend the time
constant (t) of Ti3C2Tx MXene against oxidation to as long as
1203.9 days. After saving in saturated LiCl solution for
400 days, the ratio of Ti-O species in Ti3C2Tx MXene is
increased to only 16.8 % relative to the fresh sample, showing
the exceptional effect on stabilizing the MXene in solution.
Good retention of protected MXene in intrinsic surface
chemistry is demonstrated by using Ti3C2Tx MXene saved in
saturated LiCl solution for 400 days for surface reaction
dominated supercapacitor, one of the most popular applica-
tions of MXene.[17] Cyclic voltammetry (CV) reveals similar
pseudocapacitive behavior of LiCl-protected and fresh
Ti3C2Tx MXene for charge storage in a voltage window of
0.6 to 0.3 V (vs. Ag/AgCl) in 3M H2SO4 (Figure 5 a). Both
MXenes exhibit a pair of redox peaks at ca. 0.25/ 0.37 V
(vs. Ag/AgCl) for reversible faradic process on electrochemi-
cally active groups (e.g., -O, -OH) grated to their surface.[18] It
thus indicates a high reserve of surface reactivity of MXene
after long-term LiCl protection. Galvanostatic charge/dis-
charge curves confirm the same charge storage behavior of
LiCl-protected and fresh MXene (Figure 5 b, Figure S9). Both
of them show low ohm drops and charge transfer resistance
(Rct = 3.61 and 2.43 W for LiCl-protected and fresh MXene,
respectively) due to good retention of metallic conductivity of
LiCl-protected Ti3C2 backbone (Figure S10). The LiCl with
relatively weak interaction with MXene can be largely rinsed
out to restore high dispersibility of Ti3C2Tx MXene for the
reserve of high electrochemical active surface area (ECSA).
This benefit is validated by the comparable double-layered
capacitance of LiCl-protected (Cdl = 12.77 mF cm 2) and fresh
Ti3C2Tx MXene (Cdl = 13.67 mF cm 2) in 3M H2SO4 (Fig-
ure 5 c, Figure S11). A less aggregation of MXene also
facilitates fast ionic diffusion upon electrochemical reactions,
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Chemie
Figure 5. a) CVs at a scan rate of 20 mVs 1, b) galvanostatic charge/
discharge curves at a current density of 1.0 A g 1 for LiCl-protected
MXene, fresh Ti3C2Tx MXene, and MXene-derived TiO2 in 3 M H2SO4.
c) The Cdl determined by the plots of Dj/2 against various scan rates at
0.25 V vs. Ag/AgCl for these electrodes. d) Capacitance retention of
these electrodes at various current densities. e) Polarization curves of
LiCl-protected MXene, fresh Ti3C2Tx MXene, and MXene-derived TiO2
at a scan rate of 10 mVs 1 in 0.5 M H2SO4 with (solid lines) and
without (dot lines) NIR irradiation (808 nm, 5.2 Wcm 2). The red
shaded area indicates the HER under NIR irradiation. f) The response
of redox current to NIR light on-off cycles for these catalysts.
manifested as close relaxation time constant of LiCl-pro-
tected (1.99 s) and fresh MXene (1.25 s)(Figure S12). Work-
ing together with high utilization of surficial redox capaci-
tance, the LiCl-protected Ti3C2Tx MXene exhibits good
capacitance retention of 180–280 F g 1 at rapidly varied scan
rates from 5 to 100 mV s 1, which is slightly lower but still
comparable to the performance of fresh MXene (Figure 5 d,
Figure S13a,b). In contrast, the MXene saved in pure water
lost almost all the pseudocapacitance due to complete
degradation to TiO2 (Figure S13c).
The MXene is known as good plasmonic material with
a strong localized surface plasmon resonance (LSPR) effect in
the solar spectrum.[3] The decay of light excited energetic
localized surface plasmon (LSP) in metallic MXene can
induce hot carrier injection accompanied by a significant
thermoplasmonic effect.[2b] A synergy of these effects may
boost the activity of MXenes for electrocatalysis of hydrogen
evolution reaction (HER) in full pH range.[2b] This finding is
utilized to demonstrate the effectiveness of hydration chemis-
try for reserving the bulk carrier properties of MXene
backbone by using HER as a probe reaction. The Ti3C2Tx
MXene exhibits a strong LSPR effect at l = 785 nm in the
NIR region. After saving in saturated LiCl for 400 days, it
exhibits similarly poor HER activity with fresh MXene in
0.5M H2SO4. However, when subject to NIR irradiation at l =
808 nm and light power of 5.2 W cm 2, the overpotential for
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achieving a current density of 10 mA cm 2 (hj=10) and Tafel
slope of LiCl-protected MXene can be dramatically reduced
by 240 mV and 19 mV dec 1 relative to fresh one (476 mV,
136 mV dec 1), respectively (Figure 5 e, Figure S14). The NIR
light on-off induces an immediate and pronounced change of
redox current, which further validates the significant effect of
LSPR on the electrocatalytic properties of MXene (Fig-
ure 5 f). In contrast, the LSPR affect negligibly on HER
activity of TiO2 derived from Ti3C2Tx MXene stored in pure
water since it has no plasmonic properties. Apparently, the
hydration chemistry can work effectively for a high reserve of
not only surface chemistry but also the bulk carrier properties
of MXenes.
In summary, an immediately commercializable way has
been developed for long-term storage of MXene in terms of
hydration chemistry. The hydration effect of inorganic salts
can significantly reduce both the water activity and concen-
tration of dissolved oxygen in aqueous solution. As a result,
the attacking of MXene by free water and oxygen molecules
can be largely suppressed to prolong their shelf life to up to
400 days with negligible loss of surface chemistry and carrier
properties. The MXene can be readily rinsed out to restore
good dispersibility and intrinsic properties for use. This
strategy avoids the use of expensive and toxic reagents, as
well as tedious separation. The salt protectant can be largely
recycled by evaporation of waste liquor to maximize the cost-
effectiveness and processing sustainability.
Acknowledgements
This work was supported by the National Natural Science
Foundation of China (NSFC, No. 51772040, 51972040), Talent
Program of Liaoning (No. XLYC1807032), Innovation Pro-
gram of Dalian City (No. 2018RJ04) and the Fundamental
Research Funds for the Central Universities (No.
DUT20TD203).
Conflict of Interest
The authors declare no conflict of interest.
Keywords: hydration chemistry · inorganic salts · MXene ·
stability · water activity
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Manuscript received: October 14, 2021
Accepted manuscript online: November 2, 2021
Version of record online: November 17, 2021
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