Journal of Alloys and Compounds 857 (2021) 157571

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Journal of Alloys and Compounds

journal homepage: http://www.elsevier.com/locate/jalcom

BN nanosheets in-situ mosaic on MOF-5 derived porous carbon

skeleton for high-performance lithium-ion batteries
Dandan Jia, Ruoyan Tong, Liangmin Ning, Zewen Yang, Yuting Zhang, Wen Gu*, Xin Liu**
Key Laboratory of Advanced Energy Materials Chemistry (MOE), Tianjin Key Laboratory of Metal and Molecule Based Material Chemistry, Collaborative
Innovation Centre of Chemical Science and Engineering, Nankai University, Tianjin, 300071, China

a r t i c l e i n f o a b s t r a c t

Article history: Graphite anode (specific capacity is only 372 mA h g
1) for lithium-ion batteries (LIBs) is not enough for
Received 28 August 2020 high energy and high power density demands. In this work, MOF-5 was used as a precursor to prepare a
Received in revised form porous carbon material embedded with BN (Boron Nitride), while B and N elements will enhance the
29 September 2020
electron transport speed thus improving the conductivity simultaneously. A large specific surface area of
Accepted 12 October 2020
Available online 13 October 2020
1790.19 m2 g
1 was provided with this material because of embedding of lamellar BN, therefore it caused
excellent cycling stability and high capacity characteristics in LIBs. The capacity retention is 1290 mA h
g
1 at 200 mA g
1 and 683 mA h g
1 at 2000 mA g
1. This material provides a solution for improving the
Keywords:
Lithium-ion batteries
performance of LIBs, and it can also be a reference for the development in other fields.
BN nanosheets © 2020 Published by Elsevier B.V.
MOF-5
Porous carbon
High capacity

1. Introduction
Lithium-ion batteries due to the advantages of high energy den-
sity, high output voltage, good cycling performance and low self-
discharge phenomenon, have been widely used in portable elec-
tronic devices [1e5]. In recent years, the research of LIBs anode ma-
terials mainly focuses on porous carbon materials, carbon nanotubes
and graphene owing to the advantages of rich resources, strong
reproducibility, low cost and high conductivity [6e9]. The
morphology of carbon-based anode materials exhibits fiber (wire)
[10], sheet [11], and sphericala [12e14], which are conducive for Liþ
insertion/extraction and can improve the conductivity and stability of
the electrodes. In addition, doping B, N, S or P is an effective strategy to
increase the conductivity of carbonaceous materials, thereby
enhancing electron transport and providing more Liþ storage/reac-
tion active sites [7,15,16]
Metal-organic-frameworks (MOFs) with periodic network struc-
ture is a suitable choice to be a precursor for preparing carbon ma-
terials [17e19]. Due to its structure, MOFs usually have a relatively
large specific surface area and abundant pores, which facilitates the
* Corresponding author.
** Corresponding author.
E-mail addresses: guwen68@nankai.edu.cn (W. Gu), liuxin64@nankai.edu.cn
(X. Liu).
rapid transfer and reaction of lithium ions [20]. Modification of the
ligands or using their framework structure during MOFs synthesis
process can achieve the doping of different elements [21,22]. Song
et al. [23] reported a MOF-derived nitrogen-doped core-shell hier-
archical porous carbon (N-CSHPC) with interconnected meso/mi-
cropores to effectively confine Se for high-performance LieSe
batteries. Ma et al. [7] investigated MOF-derived tri-doped (N, P, S)
hollow carbon shells (NPSC). The porous hollow shells were suc-
cessfully doped with N, S and P. With the doping of heteroatoms, the
performance of the batteries have been significantly improved.
BN can be used to achieve B and N doping at the same time [24].
The structure of BN is similar to graphite and belongs to sp2 hybrid
[25]. In the 2D layer of BN, the B and N atoms are alternately arranged
in the form of ABAB to form a planar network structure and the B, N
atoms are connected by strong BeN covalent bonds [26,27]. Ultra-
thin Boron Nitride nanosheets (BNNs) have been demonstrated to
be beneficial for enhancing the performance of electrodes [28e31].
Duan et al. [32] loaded Fe3O4 on flexible ultra-thin BNNs and used in
lithium batteries. The volume change of traditional electrode mate-
rials during the deintercalation and insertion of lithium ions can be
well reduced by thin layer of boron nitride. Recently, Hersam et al. [33]
applied ultra-thin BNNs to commercial polypropylene separator for
lithium batteries. The super-strong mechanical properties of BNNs
can effectively suppress the puncture of the separator during charge
and discharge processes.

https://doi.org/10.1016/j.jallcom.2020.157571
0925-8388/© 2020 Published by Elsevier B.V.
D. Jia, R. Tong, L. Ning et al.
Therefore, heteroatom-doped porous carbon materials with
large specific surface area are recognized as excellent electrode
materials for lithium-ion batteries [22,34e37]. In order to obtain
this type of material, MOF-5 was used as the precursor of the entire
carbon skeleton. 2D BNNs were introduced into MOF-5 during the
synthesis process. As a result, a tetrahedral material with a MOF-5
structure and uniformly embedded with BNNs on the surface was
prepared named MDC/BNNs (MOF-5 derived carbon material
embedded with BNNs). This material achieved a high specific sur-
face area of 1790.19 m2 g
1 due to BNNs embedded, while the
structure of two-dimensional BNNs is conducive to the insertion
and extraction of lithium ions, N doping enhances the electron
transport characteristics. The corresponding lithium-ion batteries
showed excellent cycling stability and high capacity characteristics.
The capacity retention is 1290 mA h g
1 at a current density of
200 mA g
1 and 683 mA h g
1 at 2000 mA g
1.
2. Experiment
2.1. Materials
All the reagents used in the experiment were of analytical grade
and used without further purification. Zinc nitrate hexahydrate
(Zn(NO3)2$6H2O), terephthalic acid and BN were purchased from
Aladdin Reagent Co., Ltd. Triethanolamine, N,N-
Dimethylformamide, ethylenediamine and methanol were pur-
chased from Tianjin Hengshan Chemical Co., Ltd. Deionized water
was used in all experiments.
2.2. Preparation of BNNs
The BNNs was fabricated according to the former reported
article [56]. BN powder (0.3 g) was added into a 100 mL flask, and
triethanolamine (30 mL) was added as dispersion solvent. The
milky white liquid was stirred at a rate of 1000 rpm for 8 h, then
centrifuged at 4500 rpm for 30 min, and the supernatant was taken.
The supernatant was placed in a 500 mL glass beaker, 400 mL of
deionized water was added, stirred for 1 min, and ultrasonicated
for 30 s to thoroughly mix the dispersion with deionized water,
suction filtration. The filter and the product were taken out
together and placed again in 500 mL glass beaker. In the beaker,
400 mL deionized water was added, and the mixture was washed
four times in a cycle, and the solvent was changed to DMF in the last
time. Finally, the products on the filter were placed in 50 mL,
100 mL, 200 mL DMF to prepare different concentrations of BNNs
DMF dispersion solutions, named BNNs-0.5, BNNs-1.0 and BNNs-
2.0.
2.3. Preparation of MOF-5/BNNs-x
Zn(NO3)2$6H2O (1.2 g) and terephthalate (0.6 g) were added to
60 mL of ethylene glycol, stirred until completely dissolved, then
96 mL different concentrations of BNNs DMF dispersion solutions
were added and stirred for 3 h. The sample was transferred to a
25 mL polytetrafluoroethylene-lined steel autoclave, and reacted at
150  C for 6 h by a simple hydrothermal synthesis method, cooled
to room temperature, and the white product was separated on a
filter paper, each of dichloromethane and methanol. Washed three
times, dried naturally, and then washed three times with DMF and
methanol to prepare MOF-5/BNNs-x.
2.4. Preparation of MDC/BNNs-x
The prepared MOF-5/BNNs-x was placed in a quartz boat and
carbonized at 1000  C for 5 h under an argon atmosphere with a
2
Journal of Alloys and Compounds 857 (2021) 157571
heating temperature rate of 5  C min
1. Finally, the sample MDC/
BNNs-x were obtained.
2.5. Structural characterization
The morphologies and microstructures were surveyed by
Transmission Electron Microscope (TEM) (Talos F200X G2, AEMC)
and Sanning Electron Microscope (SEM) (JEOL JSM7500F) with Pt-
coated before examination. N2 adsorption-desorption isotherms
were measured on the Quantachrome Instruments (NoVA 2200e).
The surface areas were calculated by the Brunauere-Emmette-
Teller (BET) method while the pore size distributions were gained
from the desorption branches of the N2 adsorption-desorption
isotherms with the Barrette-Joynere-Halenda (BJH) method. X-ray
diffraction (XRD) data were collected from Rigaku Mini Flexll
diffractometer using Cu Ka radiation (l ¼ 1.5408 Å) in the 2q range
of 3e80 at a scan rate of 5 min
1. Raman spectra were recorded
on a confocal Raman microscope (532 nm Arþ laser) (DXR, Thermo
Fisher Scientific) in ambient air. X-ray photoelectron spectrometry
(XPS) analysis was conducted on a Kratos Analytical Axis Ultra DLD
spectrometer with 284.6 eV adjusted for C 1s.
2.6. Electrochemical measurements
The electrochemical performance was evaluated using LIR2032-
type coin cells, which are assembled in an Ar-filled glovebox, using
lithium foil as both the counter and reference electrodes, Celgard
2325 membrane as separator, and 1 M LiPF6 in a 50:50 (w/w)
mixture of ethylene carbonate (EC) and dimethyl carbonate (DMC)
as electrolyte. The working electrode slurries were prepared by
mixing active material (MDC/BNNs-x), carbon black and poly-
vinylidene fluoride (PVDF) with a mass ratio of 7:2:1 in N-methyl-
2-pyrrolidone. Afterwards, the slurry was carefully coated on a
copper foil and dried at 60  C for 12 h. The loading mass of the
active material is approximately 0.6e0.8 mg cm
2 for each elec-
trode. Galvanostatic discharge/charge tests were performed on a
LAND-CT2001A battery testing system. Voltage window range of
cyclic voltammetry (CV) from 0.01 to 3 V and electrochemical
impedance spectroscopy (EIS) collected in the frequency range
from 100 kHz to 10 mHz were conducted on a CHI660 electro-
chemical measurement system. All specific capacities and current
densities mentioned in the paper are calculated based on the
content of active material.
Fig. 1. Preparation process diagram.
D. Jia, R. Tong, L. Ning et al.
3. Results and discussion
3.1. Synthesis and structural characterization
The synthesis strategy of the MDC/BNNs is schematically shown
in Fig. 1a. First, the BN powder was dispersed into the triethanol-
amine solution and peeled off by stirring and centrifugation to
prepare BNNs. Then, the BNNs was dispersed into different doses of
DMF by filtration and washing to prepare different concentrations
of dispersion solutions (label the different concentrations x as 0.5,
1.0 and 2.0). MOF-5/BNNs-x were composited through adding
Zn(NO3)2$6H2O, terephthalic acid and ethylene glycol to different
concentrations of BNNs in DMF dispersion. Finally, MDC/BNNs-x
were synthesized by simple high-temperature calcination.
MOF-5/BNNs-x with BNNs neatly embedded on the surface
were prepared by a simple hydrothermal method. In the XRD
pattern of Fig. S1a [38], the prepared MOF-5 corresponds to the
diffraction peaks of the standard XRD card, confirming the suc-
cessful preparation of MOF-5. After incorporating with BNNs, the
diffraction peak position of the material has changed (Fig. S1a), and
the diffraction peak has also become wider. From the scanning
electron microscope image of Fig. S2a, it can be seen that the
Fig. 2. (a-b) SEM images of MDC/BNNs-1.0. (c-d) TEM images of MDC/BNNs-1.0. (e-i) SEM/EDS element mapping of MDC/BNNs-1.0.
3
Journal of Alloys and Compounds 857 (2021) 157571
incorporation of BNNs makes the surface of MOF-5 rough, thereby
destroying the original MOF-5 crystal face to make the crystallinity
deteriorates. The BNNs are neatly arranged on the surface, causing
interlayer gaps to expose other crystal planes inside MOF-5, thus
changing the position of diffraction peaks [39]. As shown in Fig. S2b
and Fig. S2d, the surface of MOF inlaid with BNNs is obviously
roughened, but the shape is basically unchanged. It is obvious that
after the high temperature calcination (Fig. 2a, Fig. 2d), the overall
shape of the material almost completely retains the regular shape
of the MOF-5 precursor, proving that the material has stable char-
acteristics. The pore structure appearing on the surface of the
material after calcination can be observed, which is conducive to
improving the electron transport capability of lithium-ion batteries
and the infiltration of electrolyte, thus further improve the per-
formance of the battery. The transmission electron micrographs
(TEM) of Fig. 2c and d also proved the mosaic arrangement of BNNs
on the surface of the material. As shown in Fig. 2f, the element
mapping shows a uniformly distribution of C, O, N and B of the
MDC/BNNs-1.0.
The XRD pattern of MDC/BNNs-1.0 is shown in Fig. 3a. It can be
observed that the XRD pattern of the sample has a bulge at
2q z 20 e30 , which corresponds to amorphous carbon.
D. Jia, R. Tong, L. Ning et al.
Fig. 3. (a) XRD pattern of MDC/BNNs-1.0. (b) Raman spectrum of MDC and MDC/BNNs-1.0. (c) N2 adsorption-desorption isotherms and (d) pore size distributions of MDC/BNNs-1.0.
Meanwhile, there are two peaks at 2q z 26.0 and 43.7, which
correspond to the (002) and (100) crystal planes of graphitic carbon
(JCPDS: 26e1076) [40]. It is proved that the prepared carbon material
has a partially amorphous structure. Through Raman spectroscopy
(Fig. 3b), it can be seen that MDC/BNNs-1.0 has two independent
characteristic bands, the D band at around 1350 cm
1 reflects the
structural defects in the graphitic structure, while the G band at
around 1588 cm
1 corresponds to the in-plane vibration of sp2
carbon atoms. The calculated peak intensity ratio of ID/IG is~0.93,
revealing that the MDC/BNNs-1.0 has been partially graphited during
annealing, which is beneficial to achieving a better electronic con-
duction [41,57]. A typical hysteresis loop is observed in Fig. 3c, which
indicates the presence of mesopores in the material, and the
Brunauer-Emmett-Teller (BET) surface area is calculated to be
1790.19 m2 g
1, while the BJH method reveals that the material
mainly has a pore size of 6 nm (Fig. 3d). For the electrode, the
mesoporous structure can not only provide a lot of channels for the
rapid transmission of lithium ions, but also provide good conditions
for the rapid transmission of lithium ions [15,42].
The XPS of the samples before and after doping with BNNs are
shown in Fig. S3, Fig. S4. In the comparison results of the total
spectrum, in addition to the basic elements Zn, O and C corre-
sponding to MOF-5, B elements appear in the samples doped with
BNNs. The N 1s spectrum and the B 1s spectrum also correspond
well to the BN bond in BN, which confirms the synthesis of MOF-5
with BNNs embedded on the surface. The chemical composition
and valence state of the MDC/BNNs-1.0 material were researched
by XPS (Fig. 4a). The O, N, C and B elements can be clearly observed,
which is consistent with the previous element distribution dia-
gram. The C1s spectrum can be divided into peaks at 284.6, 285.6
and 288.6 eV, which can correspond to C]C, CeC and C]O,
respectively (Fig. 4b). The high resolution spectrum of O1s can be
divided into two peaks, located at 532.6 eV and 534 eV, which are
4
Journal of Alloys and Compounds 857 (2021) 157571
related to (CeO, CeOOH) and H2O, respectively (Fig. 4c). The N 1s
spectrum can be divided into four types of N, pyridine N, CeNeB
bond (398.3 eV), pyrrolic N (400.8 eV) and graphite N (401.2 eV)
(Fig. 4d). Nitrogen doping can strengthen the interaction between
electrode materials [43,44]. The NeB bond proves that BNNs are
embedded in MOF-5. Similarly, the high resolution spectrum of B 1s
(Fig. 4e) shows a peak of BeN bond at 190.5 eV, which corresponds
to the N 1s spectrum, and proves the existence of BNNs [45].
3.2. Electrochemical performance evaluation and the mechanism
research
In order to evaluate the practical application ability of the ma-
terial, MDC/BNNs-1.0 was evaluated as the anode material for
lithium-ion batteries. Fig. 5a shows the CV curves of the first four
cycles of the MDC/BNNs-1.0 electrode. It shows the typical CV curve
of carbon material as the anode of lithium ion battery, which fits well
with the curve of the charge and discharge process (Fig. 5b) [46].
Except for the first charge and discharge, the CV curves of the
remaining cycles are highly overlapping. The first coulombic effi-
ciency of the material is lower because it occured some irreversible
capacity, which is mainly due to the consumption of some lithium
ions to form the SEI (solid electrolyte interphase) film on the surface
of the electrode material, and the existing of some micropores or
heteroatoms in the material cause some irreversible deintercalation
of lithium ions [47]. As shown in Fig. S5, the CV curves of MDC, MDC/
BNNs-0.5 and MDC/BNNs-2.0 are almost the same as MDC/BNNs-1.0,
confirming that BNNs can improve the performance of the battery
without changing the charging and discharging mechanism. As
shown in Fig. 5b, Fig. S5, during the second cycle, MDC/BNNs-1.0 still
maintains a discharge capacity of 1293.8 mA h g
1 and a charging
capacity of 1503.9 mA h g
1. The capacity retention rate after 100
cycles was 93%, and the coulombic efficiency reached 99.97%,
D. Jia, R. Tong, L. Ning et al.
Fig. 4. XPS spectra for the MDC/BNNs-1.0 (a) Survey, (b) C 1s, (c) O 1s, (d) N 1s and (e) B 1s level spectra.
showing high reversibility of the material. MDC/BNNs-1.0 shows a
higher specific capacity, compared with MDC, MDC/BNNs-0.5 and
MDC/BNNs-2.0. After 200 cycles, MDC/BNNs-1.0 can still maintain a
specific capacity of 1290 mA h g
1. It also has remarkable high ca-
pacity and excellent cycle stability at high current density (Fig. 5e),
after circulating for 1000 cycles at a large current density of
2000 mA g
1, the capacity of battery also remained 683 mA h g
1. It
is worth noting that in the first 400 cycles, the capacity showed an
upward trend, due to the continuous activation of the electrode
material during the initial charge and discharge, and then gradually
stabilized [48].
As shown in Fig. 6a, with specific currents of 100, 300, 500, 1000
and 2000 mA g
1, average specific capacities of 1050, 765, 602, 478
and 409 mA h g
1 were obtained, respectively. When the charging
rate was reset to 100 mA g
1, a reversible capacity of 1042 mA h g
1
was obtained, which indicates excellent capacity retention ability. It is
worth mentioning that as the amount of BNNs added increases, the
resistance of the battery shows an increasing trend (Fig. 6b). This
phenomenon may be due to the stable and insulating nature of BN.
5
Journal of Alloys and Compounds 857 (2021) 157571
Meanwhile the stripped BNNs are inserted into MOF-5 in the form of
thin sheets and are neatly arranged, which can shorten the ion
transmission path to improve the battery performance due to the
characteristics of the two-dimensional layered structure. Thus, the
battery performance of MDC/BNNs-1.0 is better than MDC. However,
the excessive doping ratio of BNNs leads to excessive internal resis-
tance of the battery and the battery performance degrades. Therefore,
by comparing the electrochemical performance, MDC/BNNs-1.0 is
selected as the material with the best doping ratio of BNNs [49].
Representative specific capacitance of previously reported N, B doped
carbon anode materials for LIBs anodes comparison with our result,
(see Table 1), MDC/BNNs-1.0 shows the best performance.
To further fully investigate the capacitive behavior of these
MOF-derived composites, their kinetics was also analyzed with CV
measurements. As clearly shown in Fig. 7a, the CV profiles at
different scan rates increased from 0.2 to 3.2 mV s
1 displaying a
much similar shape. Normally, the scan rate (v) and the measured
current (i) obey the following relationship.
D. Jia, R. Tong, L. Ning et al. Journal of Alloys and Compounds 857 (2021) 157571

Fig. 5. (a) Cyclic voltammetry curves of MDC/BNNs-1.0. (b) Galvanostatic discharge/charge curves. (c) Cycling performance of MDC, MDC/BNNs-0.5, MDC/BNNs-1.0 and MDC/BNNs-
2.0 at 200 mA g
1. (d-e) Cycling performance of MDC/BNNs-1.0 at 200 mA g
1 and 2000 mA g
1.

i ¼ abv (1) logi ¼ b,logv þ loga (2)

Specifically, when the value of b is less than 0.5, it indicates that

Fig. 6. (a) Rate performance of MDC/BNNs-1.0 at various current densities. (b) Nyquist plots of MDC, MDC/BNNs-0.5, MDC/BNNs-1.0 and MDC/BNNs-2.0 under different cyclic states
at 100 mA g
1.

6
D. Jia, R. Tong, L. Ning et al. Journal of Alloys and Compounds 857 (2021) 157571

Table 1
Representative specific capacitance of previously reported N, B doped carbon anode materials for LIBs anodes comparison with our result.

Samples Cycles Current density Specific capacity References

(mA g
1) (mAh g
1)

MDC/BNNs 200 200 1290 This work

MDC/BNNs 1000 1000 683 This work
BN-3D graphene 100 10 1000 [50]
N-doped carbon fibers 500 500 316 [51]
NHBCM 1000 5000 104 [52]
BCN nanotubes 100 100 963 [53]
3D porous carbon 180 100 606 [54]
Porous carbon nanosheets 100 100 743 [55]

Fig. 7. (a) CV curves of the MDC/BNNs-1.0 electrode at different scan rates. (b) The peak current plotted against the scan rates. (c) the capacitive contribution at the scan rate of
0.8 mV s
1 marked by the green region. (d) Capacitive and diffusion controlled contributions at different scan rates. (For interpretation of the references to colour in this figure
legend, the reader is referred to the Web version of this article.)

the battery is diffusion controlled, and when the value of b is close
to 1, it indicates that the battery is controlled by capacitance. From
Fig. 7b, it shows that the b values corresponding to the positive and
negative electrodes of the MDC/BNNs-1.0 electrode are 0.81 and
0.90, respectively. This experimental result shows that most of the
charging process shows capacitive characteristics. At a specific scan
rate, the current response (i) of a specific potential (v) can be obey
the following relationship, where K1 and K2 are constants at a
specific scan rate.
i ¼ K1 v þ K2 v1=2

1
For example, at a given 0.8 mV s sweep rate, the CV profile for
the capacitive current compared with that of the total measured
current is displayed in Fig. 7c, in which 41% is quantified as
capacitive. As the scan rate increases, the capacitance contribution
gradually increases (Fig. 7d). When the scan rate is 6.4 mV s
1, the
capacitance contribution of the MDC/BNNs-1.0 electrode is as high
as 85% [52,56].
4. Conclusion
In conclusion, by embedding BNNs into MOF-5 precursor and
calcination, a dodecahedral porous carbon material with neatly
arranged nanosheets arrays were successfully prepared. Then, the
best MDC/BNNs-1.0 anode material was obtained by screening the
electrochemical performance of BNNs with different doping levels.
After 1000 cycles at a large current density of 2000 mA g
1, the
specific capacity can be stabilized at around 683 mA h g
1. It is
worth noting that the material is embeded with 2D BNNs, and
doped with B and N elements at the same time, which causes the
(3) surface activity of the material improved since the lamellar surface
structure is beneficial to the insertion and extraction of ions.
Meanwhile, it also has a larger specific surface area
(1790.19 m2 g
1), so it achieves a higher capacity and better elec-
trochemical stability. The materials prepared by this simple and
effective method will have broad application potential in lithium-
ion batteries and other fields.
7
D. Jia, R. Tong, L. Ning et al.
CRediT authorship contribution statement
Dandan Jia: Experiments, Methodology, Software, Writing.
Ruoyan Tong: Experiments, Software. Liangmin Ning: Validation,
Formal analysis. Zewen Yang: Data curation. Yuting Zhang: Re-
sources. Wen Gu: Writing - review & editing. Xin Liu: Writing -
review & editing.
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 work was supported by the National Natural Science
Foundation of China (21875117), 111 project (B12015).
Appendix A. Supplementary data
Supplementary data to this article can be found online at
https://doi.org/10.1016/j.jallcom.2020.157571.
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