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a r t i c l e i n f o a b s t r a c t
Article history: Two-dimensional (2D) layered metal carbides materials called MXenes (e.g., Ti3C2) are significantly atten-
Received 24 January 2022 tioned as electrode material for lithium-ion capacitors (LICs) because of its large surface-to-volume ratio
Revised 29 April 2022 and ultra-high electronic conductivity. Whereas, as anode electrode material, the performance and appli-
Accepted 6 May 2022
cation prospects of Ti3C2 are severely restricted to its lower theoretical capacity. In this work, a straight-
Available online 11 May 2022
forward and effective strategy to surmount the restrictions was developed to combine layered Ti3C2
nanosheets with dual Co/Zn metal–organic framework (MOF) polyhedrons derivatives through electro-
Keywords:
static assembly. Co3O4/ZnO polyhedrons could prevent the stacking of Ti3C2 nanosheets and provide
MXene conductive network
MOF derivatives
prominent lithium storage capacity. Furthermore, the advanced structure of Ti3C2@Co3O4/ZnO as anode
Hierarchical structure material could provide short Li+ paths, large electrolyte channels and excellent structural stability to
Li-ion capacitor enhance the electrochemical performance for LICs. As a result, the prepared Ti3C2@Co3O4/ZnO composite
exhibited a specific capacity of 585.7 mAh/g at 0.1 A/g, and the electrode still delivered a capacity of 229
mAh/g at 2 A/g after 1000 cycles with 93% capacity retention in lithium-ion half cell. In addition, by
assembling with activated carbon (AC) as cathode and Ti3C2@Co3O4/ZnO as anode, the LIC revealed an
ultra-high energy density of 196.8 Wh/kg at a power density of 174.9 W/kg, and delivered a high energy
output of 87.5 Wh/kg even at a power density of 3500 W/kg. And its capacitance retention reaches 75%
after 6000 cycles at 2 A/g. The advanced structure, handy preparation, and outstanding performance of
layered carbon-based material Ti3C2@hollow polyhedrons composite might provide promising applica-
tions in LICs.
Ó 2022 Published by Elsevier Inc.
⇑ Corresponding author at: School of Material Science and Engineering, Shaanxi Key Laboratory of Green Preparation and Functionalization for Inorganic Materials, Shaanxi
University of Science and Technology, Xi’an 710021, PR China.
E-mail address: wuwenling@sust.edu.cn (W. Wu).
https://doi.org/10.1016/j.jcis.2022.05.038
0021-9797/Ó 2022 Published by Elsevier Inc.
W. Wu, C. Zhao, H. Liu et al. Journal of Colloid and Interface Science 623 (2022) 216–225
217
W. Wu, C. Zhao, H. Liu et al. Journal of Colloid and Interface Science 623 (2022) 216–225
fully prepared by electrostatic assembly and partly hydrogen [16]. These results also further substantiated the successful prepa-
bonding. ration of Ti3C2@Co3O4/ZnO. In addition, the fourier transform infra-
red spectoscopy (FT-IR) spectra of prepared materials are shown in
Fig. S1, the peaks at 1439 and 1609 cm1 are attributed to the
3. Results and discussion
vibration of C@O and OAH bonds, respectively. The intensity of
OAH in Ti3C2@Co3O4/ZnO composite obviously was increased com-
In the process of Ti3C2@Co3O4/ZnO synthesis, X-ray diffraction
pared to Co3O4/ZnO. This phenomenon can be explained by the in-
(XRD) and Raman patterns were tested to characterize the phases
situ formation of the dipole–dipole hydrogen bonds (OAH O) and
of the materials. XRD pattern (Fig. 2a) of Ti3C2 clearly displayed the
could contribute to the structure stability for enhanced lithium
peaks at 8.6° and 60.9°, indicating the 2D microstructure of Ti3C2.
storage.
In addition, all the diffraction peaks appearing in XRD pattern of
To detect surface elemental constituents and chemical bonding
Co3O4/ZnO distinctly disclose the coexistence of Co3O4 and ZnO
state of the Ti3C2@Co3O4/ZnO composite, X-ray photoelectron
phases. The peaks at 19.0°, 31.3°, 36.9°, 38.6°, 44.8°, 55.7°, 59.4°
spectroscopy (XPS) spectra of the composite were demonstrated
and 65.3° corresponded one by one to (1 1 1), (2 2 0), (3 1 1),
in Fig. 3. As a whole, the wide-scan survey XPS spectrum shown
(2 2 2), (4 0 0), (4 2 2), (5 1 1), (4 4 0) facets of Co3O4 (JCPDS No.76–
in Fig. 3a revealed the binding energy of Ti 2p, Co 2p, Zn 2p, C
1802). The other peaks at 31.8°, 34.5°, 36.3°, 47.6°, 56.7°, 63.0°
1 s and O 1 s, demonstrating the successful preparation of the Ti3-
and 66.5° corresponded to (1 1 0), (0 0 2), (1 0 1), (1 0 2), (1 1 0),
C2@Co3O4/ZnO composite. Furthermore, in the high-resolution Ti
(1 0 3), (2 0 0) facets of ZnO (JCPDS No.75–0576). In addition, XRD
2p spectrum region of the composite, distinct Ti–C covalent bonds
pattern of the composite contained the characteristic peaks of
located at 454.6 eV and 458.2 eV, validating the existence of Ti3C2.
Ti3C2, Co3O4 and ZnO with no impure phase. Moreover, Raman
The Ti-O peak at 460.3 eV can be ascribed to TiO2, revealing that
spectra were also characterized to demonstrate the Ti3C2 composi-
Ti3C2 was slightly oxidized over the preparation process.
tion of Ti3C2@Co3O4/ZnO composite. The composite displayed char-
[19,20,39] And the high-resolution spectrum of Co 2p (Fig. 3c)
acteristic Raman bands positioned at 1322 cm1 and 1578 cm1
were classified as two distinctive spin–orbit doublets of 2p1/2 and
corresponding to the D-band and G-band of Ti3C2, respectively
Fig. 2. (a) X-ray diffraction patterns of Ti3C2, Co3O4/ZnO and Ti3C2@Co3O4/ZnO (b) Raman patterns of Ti3C2, Co3O4/ZnO and Ti3C2@Co3O4/ZnO.
218
W. Wu, C. Zhao, H. Liu et al. Journal of Colloid and Interface Science 623 (2022) 216–225
Fig. 3. (a) X-ray photoelectron spectroscopy wide spectrum of Ti3C2@Co3O4/ZnO. High-resolution XPS spectra of Ti3C2@Co3O4/ZnO (b) Ti 2p, (c) Co 2p, (d) Zn 2p, (e) C 1 s, and
(f) O 1 s.
2p3/2 and obvious satellite peaks (named as Sat.). The peaks situ- The microstructure and morphology of the prepared materials
ated at 779.7 eV and 795.2 eV were assigned to Co3+ and the peaks could be observed well via the images of scanning electron micro-
located at 781.5 eV and 796.7 eV were allocated to Co2+ in Co3O4 scopy (SEM) and transmission electron microscopy (TEM). It was
[37]. In addition, two prominent peaks of Zn 2p spectrum at observed in Fig. 4a that Ti3C2 of 2D microstructure is successfully
1021.6 eV. and 1044.7 eV were attributed to 2p3/2 and 2p1/2, prepared. The layered structure was complete and the surface of
respectively. The fitting results indicated that the chemical states the Ti3C2 was smooth. The SEM images in Fig. 4(d-f) showed poly-
of Zn in the composite are the same [29]. For the high-resolution hedron structure of MOF derivatives. The morphology of the
spectrum of O 1 s (Fig. 3d), two peaks centred at 529.6 eV and derivatives Co3O4/ZnO was uniform and the side length of the poly-
531.6 eV were matched with the lattice oxygen in Co3O4 and hedron was about 900 nm. Furthermore, the images of Ti3C2@Co3-
ZnO, which also further verifies the presence of MOF derivatives O4/ZnO composite were exhibited in Fig. 4(g-f). The Co3O4/ZnO
[41]. polyhedrons were uniformly loaded on the surface and interlayer
219
W. Wu, C. Zhao, H. Liu et al. Journal of Colloid and Interface Science 623 (2022) 216–225
Fig. 4. The SEM images for (a-c) Ti3C2, (d-f) Co3O4/ZnO, (g-i) Ti3C2@Co3O4/ZnO, and (j) image of Ti3C2@Co3O4/ZnO and the corresponding mapping images.
of the layered Ti3C2. The polyhedron and layered structure of the In addition, the more visual morphology and lattice information
composite were well preserved, which also further suppressed of Co3O4/ZnO and Ti3C2@Co3O4/ZnO were analyzed by TEM. As can
the accumulation of Ti3C2 nanosheets. In addition, the energy- be observed in Fig. 6a and b, there was distinct polyhedron struc-
dispersive X-ray (EDX) elemental mappings of Ti3C2@Co3O4/ZnO ture composed of Co3O4/ZnO particles (MOF derivatives). Its partic-
was shown in Fig. 4j display the well-distributed Co, Zn, Ti, C and ular hollow polyhedron structure can provide abundant Li+
O through the composite. The positions of Co, Zn and O elements diffusion paths, accelerate the effective conduct of Li+ in electro-
in the EDX diagram indicated the successful synthesis of Co3O4/ chemical reactions, and hence could enhance the electrochemical
ZnO, and the presence of Ti element also indicated the loading of properties of Ti3C2@Co3O4/ZnO electrode materials. The magnified
Co3O4/ZnO on the surface of Ti3C2 sheet. TEM diagram (Fig. 6b) displayed that the Ti3C2 as a network struc-
Moreover, to study the specific surface area and pore volume of ture is connected to the Co3O4/ZnO polyhedrons, which is consis-
the prepared electrodes, the nitrogen adsorption–desorption iso- tent with the SEM images. Furthermore, in the high-resolution
therms and the pore size distribution were analyzed. As shown TEM (HRTEM) image, some distinct lattice fringes were displayed
in Fig. 5, Ti3C2, Co3O4/ZnO and Ti3C2@Co3O4/ZnO displayed typical in Fig. 6d with interplanar distances of 0.241 nm and 0.279 nm,
type-IV curves. Compared to the surface areas and pore volumes of matching with the (3 1 1) lattice planes of Co3O4 and the (1 0 0) lat-
Ti3C2 (2.6 m2 g1, 0.05 cm3 g1) and Co3O4/ZnO (38.1 m2 g1, tice planes of ZnO. Accordingly, the TEM results were consistent
0.16 cm3 g1), it was clear that the surface area and pore volume with the XRD and EDS data, proving the successful synthesis of Ti3-
of Ti3C2@Co3O4/ZnO composite (77.2 m2 g1, 0.32 cm3 g1) was C2@Co3O4/ZnO composite.
greatly increased. This result of the Brunauer-Emmett-Teller In addition, Fig. 7 described schematic illustration of Li+ paths
(BET) data could be attributed to the Co3O4/ZnO polyhedra inserted and electron transport on Ti3C2@Co3O4/ZnO electrode. Obviously,
on surface of Ti3C2 nanosheets, forming hierarchical structure com- polyhedrons structure can provide abundant Li+ diffusion paths,
posite fuhe and effectively preventing the agglomeration of Ti3C2 accelerate the effective conduct of Li+ in electrochemical reactions.
sheets. The increase in the specific surface area and pore volume Furtthermore, Ti3C2 nanosheet as stable and conductive substrate
of Ti3C2@Co3O4/ZnO electrode can provide large electrolyte chan- was served as a charge-transporting interconnector, further
nels and faster charge/Li+ transfer, which could enhance the elec- enhancing the charge transfer rate and structural stability of this
trochemical performance of the composite electrode. hierarchical architecture. The synergistic effect of MOF derivatives
220
W. Wu, C. Zhao, H. Liu et al. Journal of Colloid and Interface Science 623 (2022) 216–225
Fig. 5. Nitrogen adsorption–desorption isotherms and the pore size distribution of Ti3C2, Co3O4/ZnO and Ti3C2@Co3O4/ZnO.
221
W. Wu, C. Zhao, H. Liu et al. Journal of Colloid and Interface Science 623 (2022) 216–225
Fig. 8. Electrochemical properties in Li-half cell (a) Cyclic voltammetry curves of Ti3C2@Co3O4/ZnO at a scan rate of 0.1 mV/s. (b) Galvanostatic discharge and charge curves in
the first three cycles for Ti3C2@Co3O4/ZnO at 0.1 A/g. (c) Rate performances of Ti3C2, Co3O4/ZnO and Ti3C2@Co3O4/ZnO at various current densities. (d) Cycling performances of
Ti3C2, Co3O4/ZnO and Ti3C2@Co3O4/ZnO electrodes over 1200 cycles at 2 A/g. (e) CV curves of the Ti3C2@Co3O4/ZnO anode at various scan rates from 0.1 to 2 mV/s. (f) The
determination of b-values based on cathodic and anodic peaks for Ti3C2@Co3O4/ZnO. (g, h) Contribution of capacitive-controlled capacities at various scan rates.
þ
ZnO þ 2Li þ 2e ! Zno þ Li2 O ð2Þ Ti3C2 nanosheets, which enhanced the electrical conductivity of
electrode material. The discharge capacities of Ti3C2, Co3O4/ZnO
þ
Zno þ Li þ e $ LiZn ð3Þ and Ti3C2@Co3O4/ZnO were tested to be 177.1 mAh/g, 401.2
mAh/g and 585.7 mAh/g at current density of 0.1 A/g. Furthermore,
þ after rate performance test, the capacities of the Ti3C2, Co3O4/ZnO
LiZn $ Zno þ Li þ e $ ZnO ð4Þ and Ti3C2@Co3O4/ZnO were also maintained at 155.5 mAh/g,
275.2 mAh/g and 401.4 mAh/g once the current density was
þ
Ti3 C2 Tx þ yLi þ ye $ Liy Ti3 C2 Tx ð5Þ adjusted to 0.1 A/g. In addition, Fig. 8d exhibited the long cycle per-
formance of the prepared electrodes. It was particularly obvious
During the discharge process, the cathodic peak observed at
that as the current density increased to 2 A/g, the discharge capac-
around 1 V can be ascribed to the alloying reaction of LiZn, while
ity of single MOF derivatives electrode was greatly reduced, but
the anodic presented at 1.7 V corresponds to the de-alloying reac-
Ti3C2@MOF derivatives electrode could still deliver a discharge
tions of Li-Zn alloy and the formation of ZnO. Fig. 8c showed the
capacity of 229 mAh/g after 1000 cycle with 93% capacity reten-
rate capability of Ti3C2, Co3O4/ZnO and Ti3C2@Co3O4/ZnO from
tion. In addition, the electrochemical performance of Ti3C2@Co3O4
0.01 to 3 V at various current densities of 0.1, 0.2, 0.5, 1, 2 A/g. It
were shown in Fig. S2 and the results indicated that Ti3C2@Co3O4/
can be obviously observed that Ti3C2@Co3O4/ZnO electrode dis-
ZnO electrode exhibted higher specific capacity and better cycle
played much higher capacity than the Ti3C2 and Co3O4/ZnO elec-
stability than Ti3C2@Co3O4 material. The excellent electrochemical
trodes at different current densities. This reason might be that
properties of the Ti3C2@Co3O4/ZnO composite indicated that with
hollow structure MOF derivative of Co3O4/ZnO were embedded in
222
W. Wu, C. Zhao, H. Liu et al. Journal of Colloid and Interface Science 623 (2022) 216–225
Ti3C2 nanosheets as stable conducting substrates, the Ti3C2@Co3O4/ AC as a cathode to form an LIC (Fig. 9a). The morphology and struc-
ZnO electrode material could remain relatively intact structurally ture information about activated carbon were shown in Fig. S3. To
and the material was not deactivated under different current den- explore the practical applications of the LIC, the electrochemical
sity impacts. performance of LIC device was characterized by galvanostatic
Moreover, to better study the capacity behavior of Ti3C2@Co3O4/ charge and discharge (GCD) and impedance spectroscopy (EIS)
ZnO electrode material, CV curves of the material were measured measurement. Fig. 9b showed the CV curves of the Ti3C2@Co3O4/
at diverse scan rates. The charge storage mechanism could be char- ZnO//AC LIC at different scan rates from 2 mV/s to 100 mV/s with-
acterized by analyzing the peak currents (i) and scan rates (m) of out obvious deviation. In addition, GCD curves of the LIC at differ-
the CV curves using Eqs. (6) and (7): ent current densities (1 A/g to 10 A/g) were exhibited in Fig. 9c. For
LIC, the electrochemical performance was calculated by the follow-
i ¼ av b ð6Þ ing equations:
Fig. 9. (a) Schematic representation of the construction of Ti3C2@Co3O4/ZnO//AC LIC. (b) CV curves of Ti3C2@Co3O4/ZnO//AC LIC at different scan rates; (c) charge discharge
curves of Ti3C2@Co3O4/ZnO//AC LIC at different current densities from 0.1 A/g to 2 A/g; (d) Nyquist plots of Ti3C2, Co3O4/ZnO and Ti3C2@Co3O4/ZnO (e) Ragone plots of
Ti3C2@Co3O4/ZnO//AC LIC; (f) cycle performance of Ti3C2@Co3O4/ZnO//AC LIC at a current density of 2A/g.
223
W. Wu, C. Zhao, H. Liu et al. Journal of Colloid and Interface Science 623 (2022) 216–225
output of 88 Wh/kg. Furthermore, Fig. 9e also showed the perfor- 2016GBJ-10), and China Postdoctoral Science Foundation (Grant
mance comparison of the prepared Ti3C2@Co3O4/ZnO and other No. 2019M653611).
materials used as LICs anode, such as CNT@pLTO//GF (101.8 Wh/
kg at 436.1 W/kg) [8], Co3O4@TiO2-2//AC (72 Wh/kg at 420 W/
kg) [43], Co3O4-NS//JFAC (118 Wh/kg at 120 W/kg) [44], CoP/r- Appendix A. Supplementary data
GO//AC (119.3 Wh/kg at 175 W/kg) [45], and NiMn-LDH/MXene//
AC (122.7 Wh/kg at 199 W/kg) [35]. And the cycle stability of the Supplementary data to this article can be found online at
LIC was shown in Fig. 9f; the capacity could maintain 75% after https://doi.org/10.1016/j.jcis.2022.05.038.
6000 cycles. Further exploring practicality, the Ti3C2@Co3O4/
ZnO//AC LIC could light a blue light-emitting diode (LED) light. References
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This work was financially supported by the National Natural [21] J. Zhang, R. Chu, Y. Chen, H. Jiang, Y. Zeng, X. Chen, Y. Zhang, N.M. Huang, H.
Science Foundation of China (51803113 and 51572158), the Guo, MOF-derived transition metal oxide encapsulated in carbon layer as
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Yorkshireman likes to be complimented on his foresight and good
sense by an acknowledged expert.
“I wonder if he would paint my wife,” said Mr. Crosby of the Foreign
Office.
“You can ask him, my dear fellow,” said the expert.
“Would he want a stiff figure?” said Mr. Crosby, who had a very
practical mind.
“It would cost you a cool thousand, I dare say,” said Cheriton, before
Kendal could announce that it had cost him five hundred.
“Stiff, ain’t it, for an unknown man?” said Mr. Crosby.
“He is going to be the man, my dear fellow,” said Cheriton. “What do
you say, Caroline? You have seen some of his work.”
“I agree with you, Cheriton,” said the flattered Caroline, who knew as
much about pictures as Ponto did. “He has painted two of my nieces,
and in my opinion they are excellent likenesses.”
“Have you two nieces, Caroline?” said the Marquis. “That is
interesting. When are we to have the opportunity of seeing the other
one?”
“Next season—perhaps.”
As yet there had been no formal announcement of Cheriton’s
engagement, but it was known to many. It is true that those who
were best acquainted with him maintained an attitude of incredulity.
So many times in the past had there been talk of entertaining at
Cheriton House. Yet there was a consensus of opinion that he really
meant to settle down at last; and while all disinterested people could
not fail to admire his taste, the critical were a little inclined to doubt
his wisdom. Still, there was no doubt about the beauty and the
docility of his choice, and in her quaint way she had unmistakably
the bel air. She was a good honest girl, a Wargrave, and the old
woman of Hill Street could well afford to do something in the matter.
Still, the knowing ones “could not see it at all”; those who were not
so knowing thought that “Cheriton might have done worse.”
All the same, Miss Perry was famous and she was popular. Her
simplicity was something that was growing very rare; she was
unaffectedly good to everybody, and everybody could not help being
grateful to her for her goodness, because it sprang straight from the
heart. No matter whether people were important or unimportant, it
made no difference to her. Great beauty and an absolute friendliness
which is extended to all, which keeps the same gracious smile for
the odd man about the stables that it has for the wearer of the
Garter, will go far towards the conquest of the world.
Miss Perry had conquered her world. All agreed that Cheriton had
done well. Yet the creature was not in the least happy. So much
practice, however, had the Wargraves had in the course of the
centuries in dissembling their unhappiness and in offering their
heads to the block, that only four persons were able to suspect that a
brave, smiling, and bountiful exterior concealed a broken heart.
Jim Lascelles was one. He knew for certain. Miss Burden was
another. Caroline Crewkerne was no believer in broken hearts. For
one thing, she had never had a heart of any sort to break. But she
had seen those great damp splotches on the correspondence with
her father, she had noticed that the creature’s appetite was not what
it was; and there were half a dozen other symptoms that enabled her
to put two and two together. As for the fourth person, it was Cheriton
himself. He was a man of immense practical sagacity. The Lascelles
affair was perfectly familiar to him in all its bearings. He himself was
primarily responsible for it. And none knew better than did he that
youth will be served.
During Jim’s stay at Barne Moor, Cheriton went out of his way to
show him consideration. He behaved like a habitually courteous and
broad-minded man of the world, who, so to speak, knew the whole
alphabet of life, and if necessary could repeat it backwards.
“You have no right to be here, my dear fellow,” he said tacitly to Jim
Lascelles; “but since my Yorkshire friend, Kendal, has blundered, as
one’s Yorkshire friends generally do, and you find yourself in the
wrong galley, behave just as you would under ordinary
circumstances, and, if you have the courage, take up the parable
more or less where you left it. After all, you were brought up together,
and I am only an interloper, and an old one at that.”
It was bold and it was generous of Cheriton to take this course. But
the young fellow Lascelles had behaved so well that he was bound
to respect him. And he had a genuine liking for him too. Therefore he
raised no objection to their spending long hours upon the moors with
only one another for company, while he gossiped and shot birds, and
fribbled and idled away his time indoors among more mature
persons.
Still, it was trying Jim Lascelles somewhat highly. The test was a
severer one than perhaps Cheriton knew. For Jim was confident that
he had only to speak the word for the Goose Girl to marry him by
special license at Barne Moor parish church. Once, indeed, they
found themselves in it, since the Goose Girl was by way of being a
connoisseur in churches; and they had a pleasant and instructive
conversation with the vicar.
However, all’s well that ends well, as Shakespeare informs us. Jim
Lascelles did not obtain a special license, but returned to his mother
like a good son and, shall we say, a man of honor. For it would have
been such a fatally easy and natural thing to marry the Goose Girl at
Barne Moor parish church. If you came to think about it, why should
she be offered for sacrifice? Dickie, of course, would be able to go to
Sandhurst, and Milly would be able to go to the boarding school; but
all the same, it was desperately hard on the Goose Girl.
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