Bismuth oxychloride nanoflake assemblies as a new anode for potassium ion batteries

Article abstract of DOI:10.1039/c9cc01937e

This work reports the first demonstration of bismuth oxyhalides as anode materials in potassium-ion batteries. BiOCl nanoflake assemblies deliver high capacities of 367 mA h g^-1 at 50 mA g^-1 and 175 mA h g^-1 at 1 A g^-1. The formation of K-Bi alloys at an early stage of potassiation is observed.

Full text of DOI:10.1039/c9cc01937e

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DOI: 10.1039/C9CC01937E
BiOCl is demonstrated as the first bismuth oxyhalide compound serving as a new
anode material for potassium ion batteries.

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Bismuth oxychloride nanoflake assemblies as a new anode for
potassium ion batteries
Wei Li,a Yang Xu,*b,c Yulian Dong,a Yuhan Wu,b Chenglin Zhang,b Min Zhou,b Qun Fu,a Minghong
Received 00th January 20xx,
Accepted 00th January 20xx
Wu,*a and Yong Lei *b
DOI: 10.1039/x0xx00000x
This work reports the first demonstration of bismuth oxyhalides as consists of [X-Bi-O-Bi-O-X] slices stacking by the van der Waals
anode materials in potassium-ion batteries. BiOCl nanoflake interaction through the halogen atoms along the c axis.9,10 The
assemblies deliver high capacities of 367 mAh g-1 at 50 mA g-1 and layered structure is featured by strong intralayer covalent
175 mAh g-1 at 1 A g-1. The formation of K-Bi alloys at an early stage bonding and weak interlayer van der Waals interaction, which
of potassiation is observed.
results in highly anisotropic electrical, mechanical and optical
properties, endowing BiOX with potential applications in
various fields.11-15 However, there has been very little study of
BiOX in the application of rechargeable alkali-metal ion
batteries (LIBs16,17 and Na-ion batteries (NIBs)18). It is surprising
because BiOX meets the two criteria. On the one hand, the van
der Waals gaps in BiOX naturally serve as two-dimensional (2D)
ion diffusion pathways. On the other hand, metallic Bi can be
formed by the conversion reaction to enhance the electronic
conductivity of electrode matrix. Thus, it is urgent yet rational
to exploit the potential of BiOX in the emerging field of KIBs.
In this work, we report the first application of BiOX
compounds in KIBs by taking BiOCl as a demonstrator. BiOCl
nanoflake assemblies (NFAs) are prepared and characterized by
a submicron hierarchical structure that consists of square-
shaped flake nanounits. The electrochemical mechanism study
reveals the formation of K-Bi alloys at the initial stage of
potassiation, which has not been observed in lithiation and
sodiation of BiOX. BiOCl NFAs deliver a high capacity of 367 mAh
g-1 and retain 58% capacity after 50 cycles at 50 mA g-1. They
also show great rate capability by delivering a capacity of 175
mAh g-1 at 1 A g-1. To the best of our knowledge, the NFAs
exhibit the best electrochemical performance among all the
BiOX compounds tested in alkali-metal ion batteries.
BiOCl NFAs are fabricated by a solvothermal reaction, where
NH4Cl not only serves as the Cl precursor, but also lowers the
pH value of the reaction solution to reduce the hydrolysis rate
of Bi(NO3)35H2O.19 The lowered hydrolysis rate and the
viscosity of ethylene glycol (EG) as the reaction solvent can
affect the growth of the nanoflakes and lead to the formation
of assemblies.20 The X-ray diffraction (XRD) pattern (Fig. 1a) can
be well indexed to tetragonal phase BiOCl (JCPDS No. 06-0249)
with a space group of P4/nmm. Good crystallinity can be
verified by the sharpness of the peaks.21,22 (001), (002) and (003)
Investigation of the feasibility of K-ion batteries (KIBs) has been
greatly prompted during the past few years.1-5 There are two
important advantages of KIBs that encourage researchers to
proceed from Li-ion batteries (LIBs) to KIBs. First, K has a lower
standard redox potential than Li in nonaqueous electrolytes,
which can be translated to a higher cell voltage of KIBs.1 Second,
nonaqueous K electrolytes have a higher ionic conductivity than
Li electrolytes and lower interfacial reaction resistance deriving
from the lower desolvation activation energy.2,3 Study of KIB
cathodes is mainly focused on intercalation-type materials,6,7
but there is a great variety of KIB anodes because of the various
electrochemical mechanisms to store K-ions.1,4,8 It can be
anticipated that the mechanisms in KIBs might be beyond our
expectations and different from those in LIBs even given the
same material. Despite the diverse mechanisms, two criteria
are important to obtain satisfactory KIB performance: (i)
suitable ion diffusion pathways exist in the anode’s structure to
ensure fast ionic transport and (ii) high electronic conductivity
is achievable to ensure fast electronic transport.
As a group of V-VI-VII ternary compounds, bismuth
oxyhalides BiOX (X = Cl, Br and I) are a classic type of layer-
structured materials. They crystallize into
a tetragonal
matlockite (PbFCl-type) structure (space group P4/nmm) that
a. Institute of Nanochemistry and Nanobiology, School of Environmental and
Chemical Engineering, Shanghai University, Shanghai 200444, China. E-mail:
mhwu@shu.edu.cn
b. Fachgebiet Angewandte Nanophysik, Institut für Physik & ZMN MacroNano (ZIK),
Technische Universität Ilmenau, Ilmenau 98693, Germany. E-mail: yong.lei@tu-
ilmenau.de
c. Department of Chemistry, University College London, London WC1H 0AJ, UK. E-
mail: y.xu.1@ucl.ac.uk
† Electronic Supplementary Information (ESI) available: experimental details, TEM,
SEM after ultrasonic and cycling, survey XPS, O 1s and Cl 2p XPS after the first cycle,
schematic of reaction pathways. See DOI: 10.1039/x0xx00000x
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peaks are broader than (110) and (200) peaks, indicating that be assigned to {110} facets. A schematic diagrVaiemw A(rtFicilge.On2lidne)
the crystallite size along the c-axis, which is regarded as the provides a direct visualization of the DaOtIo: m10.i1c03a9r/rCa9nCgCe0m19e3n7Et
thickness of the flakes, is smaller than that of the a-b plane, as characterized in HRTEM. One can see that the minimum unit in
will be seen in Fig. 2. The relatively strong (110) peak suggests the (001) plane is in a square shape (white lines). This
that the flakes favour the growth along the (110) orientations microscopic feature at atomic level agrees with the macroscopic
which are perpendicular to the c-axis, forming thin slabs.23 BiOCl morphology of the square-shaped nanoflakes (Fig. 2b).
has a typical layered structure (Fig. 1b) where [Bi2O2]2+ stabs
stack along the c axis while being sandwiched by two stabs of
Cl-, forming [Cl-Bi-O-Bi-Cl] units along the same axis. This
enables the expose of (001) facets and the 2D K-ion diffusion
pathways between the [Bi2O2]2+ stabs. X-ray photoelectron
spectroscopy (XPS) survey spectrum (Fig. S1, ESI†) shows the
presence of only Bi, O, Cl and C. Bi 4f spectrum (Fig. 1c) shows
two peaks located at 159.0 and 164.3 eV that can be assigned
to Bi 4f5/2 and 4f7/2 spin-orbital components of Bi3+. Cl 2p
spectrum (Fig. 1d) consists of Cl 2p3/2 and 2p1/2 peaks located
at 197.1 and 198.7 eV, respectively. The peaks agree well with
previous reports.24,25
Fig. 2 (a and b) SEM images, (c) HRTEM image (inset is SAED
pattern) of BiOCl NFAs, and (d) schematic diagram of the crystal
structure along the c axis.
The potassium storage mechanism of BiOCl NFAs is studied
by using half cells at the current density of 50 mA g-1 in a voltage
window of 0.01-2.0 V. The cyclic voltammetry (CV) curves of
Cycle1 (Fig. 3a) show four cathodic peaks. The strong peak at
1.5 V is attributed to the conversion of BiOCl to Bi.16,17 The two
small peaks (0.72 and 0.54 V) and another strong peak at 0.1 V
correspond to the multi-phase K-Bi alloying reactions, while the
two anodic peaks at 0.65 and 1.25 V correspond to the de-
alloying reactions.26,27 In Cycle2 and Cycle3, the cathodic peak
at 1.5 V disappears, indicating the irreversibility of the
conversion reaction in Cycle1, as will be discussed later. Other
peaks remain almost unchanged except for the slight shift of the
anodic peak (0.71 V) and the occurrence of two shoulder peaks
(0.2 and 0.83 V). Thus, the two redox pairs of 0.1(0.2)/0.71(0.83)
V and 0.72/1.25 V are established, indicating the stabilization of
the alloying/de-alloying reactions. The Cycle1 charge/discharge
profiles (Fig. 3b) agree well with the observations in the CV
curves. There are two discharge plateaus at 1.6 and 0.2 V as well
as a slope in between, while two charge plateaus at 0.6 V and
1.2 V can be observed. The cell delivers initial discharge and
charge capacities of 781 and 340 mAh g-1, respectively, resulting
in an initial columbic efficiency (CE) of 43.5%. Six discharge-
charge states (as indicated in Fig. 3b) are selected for the ex-situ
XRD measurement (Fig. 3c). When discharging to 1.1 V, the
strong Bi peak demonstrates a conversion reaction (BiOCl→Bi)
has occurred at the initial stage of potassiation, which is
correlated to the cathodic peak at 1.5 V in CV curves and the
plateau at 1.6 V in the discharge profile. Surprisingly, not only is
Bi formed but K-Bi alloys also appear at this stage in the
compositions of KBi and K3Bi2.26,28 Early formation of alkali-
metal-Bi alloys has not been observed in the lithiation and
Fig. 1 (a) XRD pattern, (b) crystal structure, (c) Bi 4f, and (d) Cl
2p XPS spectra of BiOCl NFAs.
Fig. 2a shows the panoramic-view scanning electron
microscope (SEM) image of the NFAs. It reveals a high yield of
hierarchical assemblies with an erythrocyte-like shape and a
typical diameter of 800 nm-1 μm. Zoom-in SEM image (Fig. 2b)
transmission electron microscope (TEM) image (Fig. S2, ESI†)
show the assemblies consist of nanoflakes with the thickness of
35-40 nm. The nanoflakes are square shaped with clearly
corners and smooth surface. The hierarchical structure is still
intact after a lengthy (1 h) ultrasonic treatment (Fig. S3, ESI†),
indicating the good structural stability. The high-resolution TEM
(HRTEM) image of a single nanoflake (Fig. 2c) displays two sets
of continuous lattice fringes with the spacing of 0.2 and 0.28 nm
that correspond to the (200) and (110) planes of tetragonal
BiOCl, respectively. The selected-area electron diffraction
(SAED) pattern (Fig. 2c, inset) reveals that the electron beam
can be indexed to the [001] zone, suggesting the exposed
surface to be the (001) plane. HRTEM image at the corner of the
nanoflake (Fig. S4, ESI†) shows that the four lateral surfaces can
2 | J. Name., 2012, 00, 1-3
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sodiation of BiOCl.16-18 Thus, it is likely that reduction of BiOCl to Bi. The profiles of Cycle2 and 3 exhibit the mixed features of
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DOI: 10.1039/C9CC01937E
and alloying between K and Bi occur concurrently, producing Bi those of the reported Bi anodes in KIBs, supporting the
and K-Bi alloys. When discharging to 0.4 V, the amount of KBi previously discussed electrochemical mechanism. During
and K3Bi2 decreases while another alloy K3Bi appears.26,29 At the discharge, the slope between 1.5 and 0.4 V could be mainly
end of discharge (0.01 V), only Bi and K3Bi can be observed. ascribed to the formation of KBi and K3Bi2,26,28 and the
During the charge process, de-alloying reactions occur. It leads subsequent plateau is characteristic for the formation of
to the gradually decreased amount of K3Bi and K3Bi2 and the K3Bi.26,28,29 The charge profile agrees with those of the Bi
final composition of KBi and Bi at 2.0 V. Thus, the BiOCl structure anodes, suggesting a reversible dealloying process. It is
is not restored, which explains the relatively low initial CE and interesting to note that the intermediate phases are different
the disappearance of the peak at 1.5 V in the CV curves (Fig. 3a). from one report to another (KBi2,26 K5Bi4,27 KBi,28 and K3Bi229),
Ex-situ XPS results can provide additional support to the possibly due to the different size and morphology of the Bi
electrochemical mechanism. In Fig. 3d, both Bi 4f peaks shift to anodes; thus, it is not surprise that the NFAs exhibit mixed
lower bonding energies after discharge, suggesting the features of the phase transition process. BiOCl NFAs deliver
reduction of BiOCl to Bi upon inserting K-ions.17 The peak most of the discharge capacity below 0.4 V in a voltage window
positions remain unchanged after charge, indicating the BiOCl up to only 2 V, which makes BiOCl favourable in assembling full-
structure is not restored when K-ions are extracted. The cells compared to oxides,31 dichalcogenide KIB anodes32-34 and
decomposition of BiOCl can also be evidenced by the evolution even carbons.35,36 The NFAs delivered Cycle2 capacity of 367
of the O 1s peaks (Fig. S5, ESI†). The major component of the O mAh g-1 and retained 213 mAh g-1 after 50 cycles (Fig. 4b). It is
bonding changes from Bi-O at the pristine state to K-O after worth pointing out that the obtained cyclability is far beyond
cycle, implying that the decomposition process is accompanied the reported limitation of 15 cycles in LIBs and NIBs.16-18 The
by the formation of potassium oxides.17,30 The absence of their electrode was characterized by SEM after 50 cycles. The yellow
XRD peaks may be due to their highly amorphous nature. In dashed squares (Fig. S8, ESI†) highlight that the hierarchical
addition, the Cl 2p peak intensity (Fig. S6, ESI†) dramatically structure is maintained after repetitive cycles, and the flakes
decreases after discharge and charge, suggeting the formation can be identified, which contributes to the observed cyclability.
of soluble KCl accompanies the decomposition of BiOCl, which Unlike Bi anodes that need the incorporation of carbon to
can be seen from the KCl peak in all the ex-situ patterns (Fig. maintain the structural integrity,27-29 the NFAs exhibit good
3c). Based on the above analysis, the overall reaction pathways structural stability without any carbon incorporation. It also can
are schematically summarized in Fig. S7, ESI†.
be seen that the diameter of the NFAs increases due to the
volume expansion of the K-Bi alloying reaction, which might be
responsible for the slow decay of the capacity over cycles.
Strikingly, BiOCl NFAs exhibit better rate performance than in
LIBs and NIBs,16-18 and even some Bi anodes (Bi/rGO27 and Bi/C
composites28). They delivered capacities of 346, 314, 272 and
223 mAh g-1 at the current densities of 50, 100, 200 and 500 mA
g-1, respectively (Fig. 4c). Half of the capacity (175 mAh g-1) was
retained when the current density increased to 1 A g-1.
Moreover, the low discharge plateau is well maintained when
the current density increases by 20 times (Fig. 4d). To the best
of our knowledge, this is the first demonstration of bismuth
oxyhalides that can sustain at a high rate of 1 A g-1 in alkali-metal
ion batteries. The obtained performance of BiOCl NFAs can be
ascribed to three factors. First, the interlayer space in the
microstructure of BiOCl serves as 2D K-ion diffusion pathways
that could reduce the diffusion resistance.37 Second, the
formation of Bi and the alloying reaction naturally enhance the
electronic conductivity of the electrode matrix, and this has an
even more significant role in determining the rate capability of
the NFAs. Third, the macroscopic rigidity keeps the hierarchical
structure of the NFAs intact despite the volume change during
the alloying reaction. The combination of microstructural,
mechanism and macrostructural merits results in the obtained
electrochemical performance of BiOCl NFAs. Moreover, unlike
the reported Bi anodes,26-29 the presented performance is
obtained without carbon incorporation and ether-based
electrolytes, thereby holding the advantages of the ease of
synthesis and low-cost.
Fig. 3 (a) CV curves of Cycle1-3, (b) discharge/charge profiles of
Cycle1, (c) XRD patterns at discharge/charge states, (d) Bi 4f XPS
spectra at pristine state, after discharge and charge states.
The electrochemical performance of BiOCl NFAs is fully
demonstrated in Fig. 4. The discharge/charge profiles of Cycle2
and Cycle3 at the current density of 50 mA g-1 (Fig. 4a) well
overlap with each other. A pair of plateaus at 0.2 V
(discharge)/0.6 V (charge) can be clearly identified. Compared
to Cycle1 (Fig. 3b), the discharge plateau at 1.6 V disappears,
which can be ascribed to the irreversible conversion from BiOCl
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Fig. 4 (a) discharge/charge profiles of Cycle2 and 3, (b) cycling
performance at 50 mA g-1, (c) rate performance, and (d)
discharge/charge profiles at various current densities from 50
mA g-1 to 1 A g-1.
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In summary, we have shown the promise of BiOCl as a
potential KIB anode material by studying its electrochemical
mechanism to store K-ions and evaluating its electrochemical
performance. The mechanism study revealed potassiation of
BiOCl proceeds through a conversion reaction of transforming
BiOCl to Bi and the alloying reactions of forming KBi, K3Bi2 and
K3Bi. We observed that K-Bi alloying processes proceed
concurrently with the conversion process at the initial stage of
potassiation, which is different from the previously reported
lithiation and sodiation of bismuth oxyhalides. The
electrochemical evaluation showed great cyclability and rate
capability of BiOCl, exhibiting the best performance among all
the reported bismuth oxyhalides in the battery research. This is
the first demonstration of bismuth oxyhalides used as KIB
electrode materials, and the demonstration is expected to
promote future work of these compounds in this exciting field.
This work was supported by the German Research
Foundation (DFG: LE2249/4-1 and LE2249/5-1), and National
Natural Science Foundation of China (21577086).
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Conflicts of interest
There are no conflicts to declare.
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