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Vol. 9. Issue 1.
Pages 984-993 (January - February 2020)
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Vol. 9. Issue 1.
Pages 984-993 (January - February 2020)
Original Article
DOI: 10.1016/j.jmrt.2019.11.038
Open Access
The preparation of V2CTx by facile hydrothermal-assisted etching processing and its performance in lithium-ion battery
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Libo Wanga,
Corresponding author
wanglibo537@hpu.edu.cn

Corresponding authors.
, Darong Liua, Weiwei Liana, Qianku Hua, Xuqing Liub, Aiguo Zhoua,
Corresponding author
zhouag@hpu.edu.cn

Corresponding authors.
a School of Materials Science and Engineering, Henan Polytechnic University, Jiaozuo, Henan 454000, China
b School of Materials, University of Manchester, Oxford Road, Manchester, M13 9PL UK
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Tables (2)
Table 1. Surface atomic concentration (%) of samples obtained from XPS.
Table 2. Electrochemical performance of V2CTx and similar materials in other literature.
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Abstract

In this study, high-purity V2CTx MXene was successfully synthesized by etching V2AlC with fluoride and hydrochloric acid mixed solution using a hydrothermal-assisted method. This method is more concise and effective and has a low level of danger. The morphology and structure of the V2CTx MXene was characterized by X-ray diffraction, field emission scanning electron microscopy, and X-ray photoelectron spectroscopy. The electrochemical properties were investigated as an anode material for lithium ion batteries. The results show that the prepared V2CTx had a higher purity and showed excellent electrochemical properties as an anode of lithium-ion batteries. And V2CTx prepared with different etching system can he obtained with high yield and excellent purity by changing the reactive conditions of the system. However, electrochemical performance of V2CTx MXene obtained at different etching system is quite different. V2CTx synthesized in the mixed solution of ammonium fluoride and hydrochloric acid has the best performance, which originates from more accessible active sites for ion in the enlarged interlayer distance, and the smaller impedance of V2CTx.

Keywords:
MXene
V2CTx
Hydrothermal
Lithium ion battery
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1Introduction

MXenes are a new type of 2D transition metal carbides and/or nitrides nanomaterials, which was firstly synthesized by selective etching of the Al element layers from MAX phase Ti3AlC2 with hydrofluoric acid (HF) in 2011 by Naguib et al. [1]. Generally, a MXene is synthesized by exfoliating MAX phases with hydrofluoric acid, which is not safe or environmentally friendly. Therefore, the method for MXene synthesis using the solution of fluoride salt and hydrochloric acid has been developed. As the precursor of MXene, MAX phase has a chemical general formula of Mn+1AXn (n = 1,2,3…), where M is an early transition metal element, A belongs to the main groups III/IV elements, and X represents C or/and N elements [2,3]. The diversity of MAX gives the designability of composition and structure of MXene, such as Ti3C2[1,4], Ti2C [5,6], V2C [7], Nb2C [8], Mo2C [9,10], Ti3CN [4,11], Nb4C3[12], (Ti0.5Nb0.5)2C [4], and (V0.5Cr0.5)3C2[4]. A large amount of theoretical calculations and experiments indicate that MXenes have many excellent physical and chemical properties and were widely used in many fields such as adsorption materials [13–15], catalytic materials [16–19], polymer reinforced materials [20–22], lubricant additives [23,24], and especially energy storage materials [25–29].

Among the MXene materials, V2CTx have a better performance than many other MXenes and has attracted great attention due to its novel properties. Theoretical analysis indicates that V2CTx MXene is a promising material as a highly active catalyst for hydrogen evolution reaction [30], uranium capture materials for nuclear waste treatment [31,32], hybrid material for the CO2 and temperature responsive [33] and an energy storage material for batteries [7,34]. Naguib et al. [35] and Sun et al. [36] found that V2CTx MXene is an ideal material for Li ion batteries (LIBs) with the theoretical capacity of up to 940 mA h g−1, which is much higher than that of Nb2C and Ti2C.

Up until now, the main method of preparing V2CTx is to etch V2AlC in HF solution or in the mixed solution of fluoride salts and hydrochloric acid. However, because of the high formation energies of V2C from V2AlC [27], the complete exfoliation of V2AlC is difficult, and the obtained V2CTx tends to contain a certain amount of unreacted V2AlC. Therefore, the transformation efficiency of V2AlC into V2C are still to be improved, which is of great importance for the further applications of V2CTx MXene.

In this paper, based on the previous studies of our work [7,37], the highly pure V2CTx MXene was successfully prepared by a simple hydrothermal-assisted method. Effects of the reactants, time and temperature on the yield of the product were studied in details. Meanwhile, the electrochemical performance as an anode for LIBs were also investigated. This method for MXene V2CTx synthesis has moderate reaction conditions and is much safer, easier and more efficient compared with other methods.

2Experimental2.1Sample preparation

V2AlC powders were pre-made by a tube furnace in Ar atmosphere and passed in 500 mesh sieves [38]. In a typical synthesis, 2 g V2AlC powders were added into 40 mL mixed solution of 0.05 mol lithium fluoride (sodium fluoride, potassium fluoride and ammonium fluoride) and 40 mL hydrochloric acid (6 M) by magnetic stirring. The reaction mixture was sealed in a Teflon-lined stainless-steel autoclave with 100 mL capacity, kept at 90 °C for 5 days, and then allowed to cool to room temperature naturally. Black precipitates were centrifugally collected and washed several times by deionized water and absolute ethanol. Finally, the precipitates were dried under vacuum at 60 °C for 12 h. The samples obtained with lithium fluoride, sodium fluoride, potassium fluoride and ammonium fluoride were named V2CTx-Li, V2CTx-Na, V2CTx-K and V2CTx-N. To understand the influence of temperature (60, 90 and 120℃) and time (3, 5 and 7 days) on the exfoliating process, more experiments were carried out in the same reaction system.

2.2Measurements and observations

X-ray diffraction (XRD) pattern was obtained by D8 Advance Bruker X-Ray diffractometer equipment with Cu Ka radiation. The sample was scanned over the range (2θ) 5–80° with a scanning rate of 15° min−1 to identify the crystal structure. The morphology and microstructures of the samples were examined using a field emission scanning electron microscopy (FESEM, Merlin Compact, Carl Zeiss NTS, acceleration voltage = 15 kV) with energy-dispersive X-ray spectroscopy (EDX) and transmission electron microscopy (TEM, JEOL JEM-2010, Japan, acceleration voltage = 100 kV). X-ray photoelectron spectroscopy (XPS) analysis was carried out to reveal the chemical state of the elements of V2CTx MXene surface on PHI-5702 multifunctional X-ray photoelectron spectrometer, Mg Ka radiation was used as an exciting source, using the binding energy of contaminated carbon (C1s: 284.8 eV) as reference.

2.3Electrochemical characterization

The electrochemical tests were carried out in a standard CR2016 coin cell. The anode electrodes were prepared by mixing the active material, Super P, and a polyvinylidene fluoride (PVDF) binder in a mass ratio of 8:1:1 in a solution of N-methyl-2-pyrrolidinone (NMP) and stirred for several minutes. The resulting slurry was then pasted on a Cu foil and dried in a vacuum oven at 110℃ for 12 h. The battery was assembled in an argon-filled glove box (H2O<1 ppm, O2 <1 ppm) using lithium metal as the counter electrode. The electrolyte was 1 M LiPF6 in a mixture of ethylene carbonate (EC), dimethyl carbonate (DMC), and ethylmethyl carbonate (EMC) in a 1:1:1 volume ratio. The coin cells were tested on a XINWEI workstation, with a current density ranging from 50 mA g−1 to 1000 mA g−1 with a voltage range from 0.01–3.0 V. Cyclic voltammetry (CV) measurements were performed on an EQCM440 workstation (Shanghai Chenhua, China) at a scan rate of 0.2 mV s−1. Electrochemical impedance spectroscopy (EIS) was measured on an electrochemical workstation (Parstat 2273, Princeton) with a frequency range from 50 mHz to 100 kHz.

3Results and discussion

The influence of fluoride salts has an important effect on the etching process. The XRD patterns of V2CTx synthesized by etching V2AlC with different fluoride salt and time are shown in Fig. 1. The diffraction peaks with 2θ values at 13.5, 35.6, 36.2, 39.0, 41.3 and 55.5° correspond to the crystal plane (002), (100), (101), (103), and (106) of crystalline V2AlC, respectively (PDF 29-0101). After the etching of V2AlC with different mixture solution of fluorine salt and hydrochloric acid, the characteristic diffraction peaks of V2AlC disappeared gradually and the characteristic diffraction peaks of V2CTx appeared with the reaction time extending. The characteristic diffraction peak with 2θ about 7.4° can be assigned to the (002) plane of MXene V2CTx[7,30]. From Fig. 1, it can be found that the reaction system of NaF and HCl mixture solution has the fastest etching rate than other system, the V2AlC precursor have almost been etched in three days. While the reaction system of KF has the slowest etching rate, which needs seven days. In addition, the position of characteristic diffraction peaks of V2CTx of alkali system (LiF, NaF and KF) are almost identical. However, the diffraction peak of V2CTx prepared with NH4F has significantly shifted to a small angle. The enlarged interlayer distance means more accessible active sites for ion in the interlayer space, which will greatly enhance the performance of V2CTx materials in energy storage devices [39].

Fig. 1.

The XRD patterns of V2CTx synthesized by etching V2AlC with (a) LiF, (b) NaF, (c) KF and (d) NH4F in different time at 90℃.

(0.29MB).

Fig. 2 is the FESEM images of V2CTx prepared with four mixture solution of LiF, NaF, KF, and NH4F with HCl in different time at a temperature of 90 ℃. As shown in Fig. 2, it can be observed that the reaction is very weak in a short time of three days. Indeed, the changing of the surface morphology is weak, especially for the V2AlC etched at KF and HCl mixture solution. With the increase of the reaction time, HF produced by the fluoride salts and hydrochloric acid increased and impel the etching process of V2AlC to become significant and quasi-2D MXene sheets were obtained. Hence, from the figure, it can be seen that the V2AlC in different mixture solution are almost exfoliated into the layered structure.

Fig. 2.

FESEM images of V2CTx prepared with four mixture solution in different time at 90℃.

(0.39MB).

To understand the influence of temperature on the exfoliating process, more experiments were carried out. Fig. 3 shows the XRD patterns of the samples exfoliated with different temperature. From the XRD patterns, it can be seen that the etching reaction was very weak at low temperature of 60℃, and the etching efficiency is very low. The intensity of diffraction peaks of V2AlC is still strong, only a very weak diffraction peak of V2CTx appeared. When the temperature increased to 90℃, V2CTx peaks appeared obviously and the diffraction peaks of V2AlC almost disappeared, with the exception of V2AlC etched at KF and HCl mixture solution, which means most V2AlC were exfoliated to V2CTx. If the reaction temperature was increased to 120℃, the V2AlC peaks all disappeared. The characterization shows that the width of XRD diffraction peak of V2CTx gets broader, and the diffraction peak of V2CTx significantly shifts to a smaller angle, meaning the enlarging of interplanar crystal spacing. However, something unknown was observed in the position of 2θ about 25°, which may be the residual aluminum fluoride or hydroxide crystals that cannot be easily washed off.

Fig. 3.

The XRD patterns of V2CTx synthesized by etching V2AlC with (a) LiF, (b) NaF, (c) KF and (d) NH4F at different temperature for five days.

(0.22MB).

Fig. 4 is the FESEM images of V2CTx samples prepared at different temperatures for five days. It was found that temperature has a direct effect on the etching process. In the low temperature of 60℃, lots of V2AlC was still in its original form, especially in the mixture of KF and HCl system, which means the etching reaction was difficult to happen. With etching temperature increasing from 60 to 90 and/or 120℃, it was observed that V2CTx MXene stacks become more separated. This illustrates that HF is easier penetrate into the layer and selectively etching the Al-layer in V2AlC, and V2CTx is finally generated.

Fig. 4.

FESEM images of V2CTx prepared with four mixture solution at different temperature for five days.

(0.89MB).

In order to obtain the surface information of V2CTx prepared with different fluoride salt, XPS analysis were carried out and the results are shown in Fig. 5 and the surface atomic concentration of samples are shown in Table 1. XPS shows that the main composition of these samples are V, C, O, F, and Cl. Because of adventitious carbon always co-existing with MXene, this results in higher C concentration being detected by XPS. Chlorine element on the surface of V2CTx comes from the absorption of chloridion, while the Al element in the system of NH4F and HCl may be coming from the tiny amounts of aluminum salt residue. Interestingly, it was found that the atomic concentration of fluoride salt ions has a large difference on the surface of V2CTx. Li-ion has the maximum capacity, while K-ion has zero atomic concentration and Na-ion concentration is in the middle. This phenomenon shows that Li-ion is easier embedded in V2CTx than Na-ion and K-ion, which may be due to the minimum ionic radius. In addition, nitrogen element was also found on the surface of V2CTx, which means that NH4+ had intercalated into the layers of V2CTx. This led to an increase of d-spacing and reducing the Van der Waals force of V2CTx layers, which will contribute to exfoliate V2CTx into a single layer [40].

Fig. 5.

XPS spectra of V2CTx prepared by different mixture solution for 5d.

(0.26MB).
Table 1.

Surface atomic concentration (%) of samples obtained from XPS.

Samples  V2p  C1s  F1s  O1s  Cl2p  Li/Na/K/N 
LiF+HCl  9.73  58.10  9.52  14.12  0.67  7.87 
NaF+HCl  12.27  65.69  5.33  15.71  0.48  0.53 
KF+HCl  10.62  62.86  6.80  18.99  0.74  0.00 
NH4F+HCl  9.49  58.70  3.54  24.09  0.53  1.41 

To better understand the chemical states of the V elements on the surface of V2CTx, deconvolution of the V2p region of the high resolution XPS spectra of V2CTx obtained with different fluoride salts are shown in Fig. 6. Deconvolution of the V2p region reveals the presence of V2+ (∼513.5 eV), V3+ (∼514.6 eV) and V4+ (∼516.6 eV). The peaks at ∼513.3 eV and ∼521.1 eV (V2+) correspond to the incomplete etching of V2AlC MAX phase in the produced V2CTx MXene, as reported in previous studies. [41–43] The peaks around ∼514.6 eV (V3+), ∼516.7 eV (V4+) and ∼524.1 eV (V3+), ∼524.1 eV (V4+) are attributed to the existence of a monolayer oxide/vanadium oxide mixture on the surface of V2CTx MXene nanosheets. [35,42] From the high resolution XPS spectra of V2p, it can be found that the relative intensity of the V2+ peaks of V2CTx obtained with NH4F is weakest, which means that the method with NH4F has a highest yield of V2CTx and a minimum residual amount of incomplete etched V2AlC MAX phase.

Fig. 6.

The high resolution XPS spectra of V2p of V2CTx. (a) LiF, (b) NaF, (c) KF, (d) NH4F.

(0.32MB).

The charge-discharge profiles of different V2CTx samples as the LIBs anode, at different cycles with a current density of 50 mA/g in the voltage range from 0.01–3.0 V are shown in Fig. 7, respectively. The first discharge capacities of V2CTx-Li, V2CTx-Na, V2CTx-K and V2CTx-N are 1123.3, 613.6, 574.1, and 943.6 mAhg−1, respectively, and the first charge capacities are 675.3, 373.4, 350.0, and 719.0 mAhg−1, respectively. The first charge and discharge coulombic efficiencies of V2CTx-Li, V2CTx-Na, V2CTx-K and V2CTx-N are 60, 61, 61, and 76%, respectively. The low efficiency in the first cycle was mainly because of the formation of the SEI on the surface. Among them, V2CTx-N has maximum coulombic efficiencies.

Fig. 7.

Charge–discharge profiles of different V2CTx electrode at different cycles with a current density of 50 mA/g.

(0.4MB).

Fig. 8(a–d) shows the typical cyclic voltammetry (CV) plots of lithium storage behavior of the different V2CTx electrodes, with an electrochemical window of 3.0 V–0.01 V at a scan rate of 0.2 mV s−1. As shown in Fig. 8a-d, the CV curve shape of V2CTx is similar to that reported in the literature [44]. Cyclic voltammetry curves of V2CTx do not exhibit a distinct reduction peak. The main weakly reduction peak of the V2CTx electrode is about 1.1 V in the first lithiation process, and then disappears in the following Li-ion intercalation process. This could mainly be due to the formation of SEI companion on the electrode surface to trapping of Li+ on the sheets of V2CTx[45]. In the cycle for the oxidation process, a peak at about 2.0 V maybe caused by Li ion extraction from the V2CTx layers. The cycling performances of MXene V2CTx samples electrodes at different current densities were tested, and the results are shown in Fig. 8e. In the first ten cycles at a current density of 50 mA·g−1, the capacities of all four electrodes were unstable, and this was due to the formation of the SEI film [46]. From the first 60 cycles, it can be seen that the V2CTx-N electrode has a high capacity at a different rate and that the capacity has no obvious attenuation. In the latter 50 cycles, when the current density was reduced back to 1000 mA g−1, the cell maintained a stable capacity, and the efficiency remained at almost 100%. In all of the cycles, V2CTx-N had a higher time capacity than V2CTx-Li, V2CTx-Na, and V2CTx-K. The increase of the capacity of V2CTx-N materials in LIBs may be due to the enlarged interlayer distance (as shown in XRD and SEM), which can provide more accessible active sites for ion in the interlayer space. By contrast, the electrochemical results of V2CTx-N are better than other similar materials in some previous reports in Table 2.

Fig. 8.

Characterization of Li-ion batteries made using different V2CTx anodes, including (a–d) Cyclic voltammetry curves, (e) Rate performance and (f) Electrochemical impedance spectroscopy Nyquist plots.

(0.59MB).
Table 2.

Electrochemical performance of V2CTx and similar materials in other literature.

Materials  Method  1st discharge mAh/g  Cycling performance-discharge Capacity (nth) mAh/g  Refs. 
N-Nb2CTx  Nitrogen-doped  380 at 0.2C  360 (100th) at 0.2C  [50] 
V2CTx  HCl + NaF-etching  467 at 50 mA/g  243 (500th)at 50 mA/g  [7] 
V4C3Tx-HF  HF-etching  164.1 at 100 mA/g  125 (300th) at 100 mA/g  [51] 
Ti3C2-TiO2  Freeze-drying  367 at 200 mA/g  267 (500th) at 200 mA/g  [52] 
Nb4C3Tx  HF-etching  231.4 at 100 mA/g  69 (100th) at 100 mA/g  [53] 
Mo2CTx  HCl + LiF-etching  323 at 50 mA/g  274.85 (300th) at 50 mA/g  [54] 
Ti3C2Tx  HF-etching  335.5 at 50 mA/g  70 (1000th) at 1000 mA/g  [55] 
rGO  Freeze-dried  267 at 66.7 mA/g  208.26 (100th) at 66.7 mA/g  [56] 
V2CTx-N  Hydrothermal etching  943.6 at 50 mA/g  233 (50th) at 1000 mA/g  This work 

Fig. 8f is the electrochemical impedance spectroscopy of the V2CTx electrodes. From the spectroscopy, it can be found that V2CTx obtained from NH4F and HCl etching system has the smallest semicircular diameter in the high frequency region, meaning a better charge transfer efficiency in the four electrodes [47]. Moreover, V2CTx-Li, V2CTx-Na and V2CTx- K had the maximum impedance. The straight line in the low frequency region was due to the diffusion of Li+ on the electrode [48,49]. V2CTx-N sample has the smaller diffusion resistance in low frequency, meaning the better diffusion of Li ion from electrolyte. The straight line in low frequency region of V2CTx-K has a maximum value and slope among four samples. This indicated that the V2CTx-K sample has high impedance, corresponding to the cycling performances of MXene V2CTx samples electrodes at different current densities.

4Conclusion

In summary, this paper provides a simple and efficient hydrothermal-assisted etching method to prepare V2CTx MXene. From analysis of aforementioned results, reaction temperature and time are important factors in influencing the fabrication of V2CTx MXene. Compared to previous literature [7,34], this method can highly improve the purity and yield of V2CTx sample. When used as an anode for Li-ion batteries, the as prepared V2CTx MXene present excellent cycling capability and good reversibility. Among the samples, V2CTx etching by ammonium fluoride and hydrochloric acid mixed solution can provide a large electrochemically active surface and a rapid channel for ion and electron transfer with lower resistance, and shows higher specific capacitance with the capacity of 233 mAhg−1 at the current of 1000 mAg−1. Hence, the present study expands on the efficient preparation of V2CTx MXene as an electrode material for high performance Li-ion batteries.

Conflict of interest

We declare that we have no financial and personal relationships with other people or organizations that can inappropriately influence our work, there is no professional or other personal interest of any nature or kind in any product, service and/or company that could be construed as influencing the position presented in, or the review of, the manuscript entitled, “The preparation of V2CTx by facile hydrothermal-assisted etching processing and its performance in lithium-ion battery”.

Acknowledgement

This work was supported by National Natural Science Foundation of China (51772077), Natural Science Foundation of Henan Province (182300410228), Project of science and technology tackling key of Henan (172102210284), Program for Innovative Research Team (in Science and Technology) in the University of Henan Province (No. 19IRTSTHN027).

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