Solid State Ionics 320 (2018) 70–75

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Solid State Ionics

journal homepage: www.elsevier.com/locate/ssi

A super-long life rechargeable aluminum battery T

a,b a a a a a
Zahid Ali Zafar , Sumair Imtiaz , Ruirui Li , Jinghao Zhang , Rameez Razaq , Ying Xin ,
⁎
Qian Lia, Zhaoliang Zhanga, , Yunhui Huangc
a
School of Chemistry and Chemical Engineering, Shandong Provincial Key Laboratory of Fluorine Chemistry and Chemical Materials, University of Jinan, No. 336, West
Road of Nan Xinzhuang, Jinan 250022, China
b
Department of Physical and Macromolecular Chemistry, Faculty of Science, Charles University, Prague 12843, Czech Republic
c
School of Materials Science and Engineering, State Key Laboratory of Material Processing and Die & Mould Technology, Huazhong University of Science and Technology,
Wuhan, Hubei 430074, China

A R T I C L E I N F O A B S T R A C T

Keywords: High energy and power density rechargeable batteries with low cost, long cycle life and high safety remain a
Rechargeable aluminum battery great demand of portable electronics and grid storage systems. Recently, rechargeable aluminum batteries
Cathode (RABs) have attracted much attention owing to its high volumetric capacity (8046 mAh cm−3), low cost and
CMK-3 ultra-safety. However, harsh reaction conditions and complicated processes are usually used in preparation of
Ordered mesoporous
electrode materials, hindering the practical application. Herein, a commercial ordered mesoporous carbon
Super-long life
(CMK-3) as a cathode for RABs is proposed, which shows a super-long life of > 36,000 charge/discharge cycles
with a high coulombic efficiency of > 97% and excellent rate performance up to 3000 mA g−1. Moreover, The
Al/CMK-3 battery has a high energy density of ~45 Wh kg−1. Last, the structure changes and (de)intercalation of
chloroaluminate anions into the mesopores of CMK-3 during the charge/discharge process were checked by ex-
situ scanning electron microscopy (SEM), high-resolution transmission electron microscopy (HRTEM), Raman
and X-ray photo spectroscopy (XPS). Commercially availability and affordable cost of the cathode material make
Al/CMK-3 battery more promising for wearable and portable appliances.

1. Introduction
Sustainable and environmentally friendly energy storage and con-
version systems have attracted intense attention, especially electro-
chemical batteries. Li metal-based rechargeable batteries offer high
capacity and energy density but high cost and low safety [1–4].
Therefore, in the past decade, the research focus has shifted abruptly
towards the quest of post-lithium based rechargeable batteries [5–10].
Therein, rechargeable aluminum batteries (RABs) have demonstrated
potential applications in the near future due to its ultrahigh volumetric
capacity (8046 mAh cm−3), low cost and very high safety without any
fire risks [11–13].
Recently, a wide range of cathode materials have been reported for
RABs, for instance, metal oxides, sulfides, chlorides, carbon-based, and
many others [14–36]. Nevertheless, the research of cathodes for RABs
has elucidated that the carbon-based materials are of great significance
for the stable, long life and high operating voltage RABs
[21,28,30,35,37–39]. However, the reported carbon-based cathode
materials involve complex and high-cost synthesis processes, which are
hard to commercialize [21,28,30,38,40]. As a typical example, the
defect-free graphene which exhibits very long cycle life in RABs was
synthesized at a high temperature of 3000 °C [38]. Accordingly, the
carbon-based materials which are inexpensive or already commercially
available would be expected as practical cathode materials without
compromising electrochemical performance of RABs and can bring
RABs from lab scale to large production lines.
Owing to its high surface areas (1000–2000 m2 g−1) and pore vo-
lumes (0.5–1 cm3 g−1) as well as excellent conductivity, [41–43] the
ordered mesoporous carbon, CMK-3 has been widely explored in the
fields of catalysis, pollutant absorbents, hydrogen storage, super-
capacitors and batteries [42,44–48]. Importantly, it is already com-
mercially available with affordable costs. In this communication, CMK-
3 is reported for the first time as a cathode material for RABs. The
resultant Al/CMK-3 battery shows > 36,000 reversible cycles at a cur-
rent density of 980 mA g−1 (15C, where 1C = ~60 mAh g−1
[37]), > 97% coulombic efficiency and ~45 Wh kg−1 energy density.
The intercalation/deintercalation of chloroaluminate anions into CMK-
3 during the charge/discharge process was confirmed by ex situ scan-
ning electron microscopy (SEM), high resolution transmission electron
microscopy (HRTEM), Raman and X-ray photoelectron spectroscopy

⁎
Corresponding author.
E-mail address: chm_zhangzl@ujn.edu.cn (Z. Zhang).

https://doi.org/10.1016/j.ssi.2018.02.037
Received 15 January 2018; Received in revised form 6 February 2018; Accepted 25 February 2018
Available online 02 March 2018
0167-2738/ © 2018 Elsevier B.V. All rights reserved.
Z.A. Zafar et al.
Fig. 1. Demonstration of the Al/CMK-3 pouch cell fabrication (top), and the practical application of the battery in digital wristwatch (bottom).
(XPS). This work not only reports a low cost and commercial cathode
material but paves an avenue for the commercialization of RABs.
2. Experimental
2.1. Preparation of CMK-3 electrode
In order to obtain uniform slurry for the fabrication of cathode film,
CMK-3 was mixed with PTFE binder dissolved in NMP disperser
(25 mg ml−1). Additionally, Super-P was also added to enhance overall
conductivity of the cathode. All cathode components, CMK-3, Super-P
and PTFE dissolved in NMP were added in the ratio of 7:2:1 and mixed
in a mortar and pestle to get homogenous slurry. The as-obtained slurry
was pasted on molybdenum (Mo) current collector by using a doctor
blade with a film thickness of 150 μm. Later, the slurry was dried in an
oven at 60 °C for overnight before cutting into rectangular shaped
(1.5 mm × 1.0 mm) cathodes for the fabrication of pouch cells.
2.2. Preparation of [EMIm]AlxCly IL electrolytes
A room temperature IL electrolyte was prepared by mixing 1-ethyl-
3methyl-imaidazolium chloride [EMIm]Cl (TCI-Japan, 97%) and an-
hydrous AlCl3 (Sigma-Aldrich, 99.999%). The room temperature
[EMIm]AlxCly IL electrolyte was prepared in a glove box under an
Argon atmosphere (H2O and O2 < 0.01 ppm) as both components of
electrolyte are highly hygroscopic. AlCl3 and [EMIm]Cl were mixed
together with a molar ratio of 1.3. Finally, the resulting light-yellow
transparent liquid was stirred at room temperature for 10–20 min.
2.3. Fabrication of Al/CMK-3 pouch cells
The pouch cells were fabricated in a glovebox (H2O and
O2 < 0.01 ppm) to avoid any contact with moisture or air. The as-
71
Solid State Ionics 320 (2018) 70–75
prepared CMK-3 cathode (1.5 mm × 1.0 mm) was utilized against the
ultrapure Al foil (0.2 mm, 99.9999%, Alfa-Aesar) anode which was
separated by a single layer of microglass fiber filter (GF/D) separators
(Fig. 1, top). After the injection of IL electrolyte, all of the battery
components were sealed inside aluminum laminate sheet (C80-400) by
utilizing an impulse heating sealer machine (Bleuets FR-300B).
2.4. Characterizations
X-ray diffraction (XRD) patterns were recorded on a Rigaku D/max-
2500/PC diffractometer employing Cu Kα radiation (λ = 1.5418 Å)
operating at 50 kV and 200 mA. The Brunauer-Emmett-Teller (BET)
surface area and pore structure were measured by N2 adsorption/des-
orption using a Micromeritics 2020 M instrument. Before exposure to
N2, the sample was outgassed at 300 °C for 5 h. Field-emission scanning
electron microscopy (FESEM) was performed on a Hitachi SU-70 mi-
croscope. High resolution transmission electron microscopy (HRTEM)
was conducted on a JEOL JEM-2010 microscope at an accelerating
voltage of 200 kV. XPS data were obtained on an AXIS-Ultra instrument
from Kratos Analytical using monochromatic Al Kα radiation (225 W,
15 mA, 15 kV) and low-energy electron flooding for charge compensa-
tion. To compensate for surface charging effects, the binding energies
were calibrated using the C1s hydrocarbon peak at 284.80 eV.
2.5. Electrochemical performance measurements
The galvanostatic charge/discharge, cycle life and rate capability
tests were performed at a LAND (Wuhan) charge/discharge apparatus
at constant charging and discharging current densities in the voltage
range of 0.5 to 2.3 V at 25 ± 1 °C. The electrochemical impedance
spectroscopy (EIS) measurements were conducted on SP-300 at a fre-
quency range of 100 kHz to 100 mHz.
Z.A. Zafar et al.
Fig. 2. The electrochemical performance of the Al/CMK-3 battery. (a) Long cycle life tests; (b) Rate performance; and (c) Mean-voltage and specific energy density.
Fig. 3. EIS for the Al/CMK-3 battery.
3. Results and discussion
Electrochemical performance of the Al/CMK-3 battery was in-
vestigated in pouch cell configurations. Fig. 1 (top) shows schematically
fabrication of the Al/CMK-3 pouch cells. CMK-3 (JCNANO INC.) was
used as received without any further treatments. Highly amorphous
nature of CMK-3 is confirmed by XRD (Fig. S1). The specific BET sur-
face area, pore volume and average pore diameter from N2 absorption/
desorption are 960 m2 g−1, 1.17 cm3 g−1 and 3.8 nm, respectively for
the pristine CMK-3 (Fig. S2). The as-prepared CMK-3 cathode is
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Solid State Ionics 320 (2018) 70–75
implemented against ultrapure Al foil anode, which is separated by a
single layer of glass fiber filter paper in an IL electrolyte (see
Experimental section). All operations for the preparation of pouch cells
and electrolytes were conducted in a glove box (H2O and
O2 < 0.01 ppm) to avoid any potential risk of moisture or oxygen
contamination.
Fig. 2 shows the electrochemical performance of the Al/CMK-3
battery within the voltage ranges of 0.5–2.3 V. At a relatively low
current density of 100 mA g−1 (1.5 C), the charging capacity of nearly
42 mAh g−1 was recorded, but the discharge capacity was a bit low
around 35 mAh g−1 (Fig. S3a). The reduced discharge capacity and
coulombic efficiency at low rates can be attributed to side reactions
possibly at oxygen-containing functionality within CMK-3 [32]. How-
ever, at high current densities, the charge and discharge capacities were
almost the same and Coulombic efficiency was reached > 97%.
After > 1500 cycles at 15 C, the reversible capacity of 33 mAh g−1 was
obtained (Fig. S3b). Although the evident plateaus are not observed, the
voltage profile remained identical throughout charge/discharge, which
was also reported previously for RABs with other carbon-based cath-
odes [18,32,49,50], suggesting that RABs with carbon-based cathode
materials containing high defects demonstrate capacitive properties
with the combination of (de)intercalation and surface deposition phe-
nomena.
Significantly, a super-long life of > 36,000 cycles was observed for
the Al/CMK-3 battery at a high rate of 15 C (980 mA g−1) with high
Coulombic efficiency of > 97% (Fig. 2a). The initial capacity was a bit
low but after hundreds of cycles the capacity was improved, because
the intercalation of chloroaluminate anions (AlCl4− = 0.528 nm) might
have widened the intercalation paths of CMK-3. Fig. 2b shows the rate
Z.A. Zafar et al.
Fig. 4. (a) SEM image of the pristine CMK-3, (b) as-prepared cathode, (c) after fully charged state, (d) after discharged state; (e) HRTEM image of the pristine CMK-3, and (f) after
3000 cycles.
performance of the Al/CMK-3 battery. High capacities were observed at
low current densities, but at the cost of a bit low Coulombic efficiency.
Even at very high current densities, the capacity drop was not evident.
In detail, a reversible capacity of 32 mAh g−1 was obtained at 4.5 C
with a coulombic efficiency of ~94%. However, it dropped to
24 mAh g−1 at an extremely high rate of 50 C (3000 mA g−1), while
Coulombic efficiency was increased above 99%. Once back to the low
current densities, the Al/CMK-3 battery retrieved the initial capacity
with a minor improvement, in accordance with other carbon-based
RABs [30,37]. The excellent rate performance of the Al/CMK-3 battery
can be attributed to the highly ordered mesoporous structure and good
conductivity of CMK-3. The former provides open paths for the
73
Solid State Ionics 320 (2018) 70–75
penetration of electrolyte and shortens the diffusion paths for the
transportation of ions, whereas the latter helps in the fast electron
transportation during the charge/discharge process.
In addition, the average mid-voltage of the Al-CMK-3 battery is
1.4 V (Fig. 2c). The ~45 Wh kg−1 energy density is comparable to
aqueous LIBs and lead-acid batteries, but higher than those of the re-
ported RABs utilizing carbon paper (36 Wh kg−1) and 3D–graphitic
foam (40 Wh kg−1) [21,39,51,52].
Fig. 3 shows the electrochemical impedance spectroscopy (EIS) of
the Al/CMK-3 battery before and after 4000 cycles. The resistance was
very low before the cycling due to the good electronic conductivity of
CMK-3 that enables fast electronic diffusions. Moreover, no obvious
Z.A. Zafar et al. Solid State Ionics 320 (2018) 70–75

the CMK-3 cathode during the charge/discharge process suggests the

D G occurrence of the intercalation/deintercalation of chloroaluminate an-
ions. The HRTEM images give more direct evidence. As shown in
Fig. 4e, the pristine CMK-3 shows a highly ordered mesoporous struc-
ture. After > 3000 charge/discharge cycles, the ordered mesopores are
Discharged interrupted but the coherent structure is still distinguishable, which
also verifies the robust structure of CMK-3.
Fig. 5 shows ex situ Raman spectroscopy. The D-band and G-band of
Charged the pristine CMK-3 were located at 1326.38 and 1597.42 cm−1 with an
ID/IG ratio of 2.44, which indicates poor graphitization (amorphous as
shown by XRD) and defects such as the presence of oxygen-containing
functional groups, i.e. OH– and O−. The presence of many defects could
Pristine be a reason for the limited capacity of the CMK-3 cathode for RABs,
because the anode Al metal and IL electrolyte are highly prone to get
affected by the presence of O2 or oxygen-containing functional groups
600 900 1200 1500 1800 2100 2400 [13,21]. The graphene-based cathodes with high numbers of defects
-1
Raman shift (cm ) have also showed similar results in RABs [38]. However, the ID/IG ratio
Fig. 5. Raman spectra for the pristine, fully charged and discharged CMK-3 cathodes. was reduced to 1.90 with a little shift in the G-band for the fully
charged CMK-3 cathode, suggesting the intercalation of chlor-
oaluminate anions. As expected, for the discharged cathode, the ID/IG
resistance increase is observed after 4000 cycles, suggesting that there
ratio (2.26) was nearly recovered and the position for G-band was also
is no excess solid electrolyte interphase (SEI) film growth [24,53].
back to its original position. The minor difference in the ID/IG ratio
In order to confirm the intercalation/deintercalation of chlor-
could be addressed as the depth of discharge (DOD) was not 100%.
oaluminate anions into the mesopores of CMK-3, ex situ SEM, HRTEM,
Namely, even at discharged state, a few intercalated chloroaluminate
Raman and XPS were performed for the pristine CMK-3, the as-prepared
anions were remained in the CMK-3 structure. Raman results bear
and fully charged/discharged cathodes.
witness to highly stable structure of CMK-3 before and after the charge/
The SEM images of the pristine CMK-3 and the as-prepared cathode
discharge process, which is crucial for the long cycle life and excellent
containing CMK-3 active material, the conductive Super-P and PTFE
rate capability.
binder are shown in Fig. 4a and b, respectively. After charging, the
Fig. 6 shows ex situ XPS to confirm the existence of chloroaluminate
morphology of CMK-3 looks slightly different from that of the as-pre-
anions in CMK-3. Al and Cl are not present in the pristine CMK-3
pared cathode (Fig. 4c). However, after fully discharging, the original
(Fig. 6a and b). After charging, the presence of the intense peaks of Al
morphology is almost recovered (Fig. 4d). The morphological change of
and Cl indicates the intercalation and surface deposition of

Fig. 6. XPS spectra of Al 2p (a), Cl 2p (b) and O 1s (c) for the pristine, fully charged and discharged CMK-3 cathodes.

74
Z.A. Zafar et al.
chloroaluminate anions. Correspondingly, after discharging, the in-
tensity of Al and Cl peaks decreased, indicating the deintercalation of
chloroaluminate anions from CMK-3. However, the Al and Cl peaks did
not disappear completely after discharging, because the DOD was set to
0.5 V, as indicated above. In addition, the O1s spectra was also ob-
served in the pristine CMK-3 (Fig. 6c), confirming the existence of
oxygen-containing functional groups on CMK-3. The intensity change of
the O1s peaks during charge/discharge shows similar tendency with
those of Al and Cl, confirming the participation of oxygen functional
groups in the intercalation/deintercalation process of chloroaluminate
anions. This is also the reason why the Al/CMK-3 battery has a limited
reversible capacity.
In the present Al/CMK-3 battery, the utilization of electrolytes was
also optimized to 180 μL per mg of the cathode material in order to
reduce the overall cost. As a practical application, the Al/CMK-3 battery
can keep powering a digital wristwatch > 70 h at fully charged state
(Fig. 1 bottom). This also demonstrates the Al/CMK-3 battery can be
used in the wearable and portable appliances.
4. Conclusions
In summary, a commercial ordered mesoporous carbon, CMK-3 was
reported for the first time as a cathode in RABs: (1) The Al/CMK-3
battery demonstrated surpassing long cycle life of > 36,000 reversible
cycles with excellent Coulombic efficiency of > 97%; (2) The Al/CMK-3
battery outputs splendid rate capability and stable performance even at
extremely high current density up to 3000 mA g−1 (50 C). (3) The Al/
CMK-3 battery has high gravimetric energy density of ~45 Wh kg−1.
Such unprecedented results have not been reported for any commercial
carbon-based cathode material for RABs. The excellent electrochemical
performance, low cost and commercial availability of CMK-3 have
projected the Al/CMK-3 battery more practical and feasible for the
wearable and portable appliances.
Acknowledgements
This work was supported by National Natural Science Foundation of
China (No. 21477046) and Key Technology R&D Program of Shandong
Province (No. 2016ZDJS11A03).
Appendix A. Supplementary data
The wide-angle XRD pattern, N2 adsorption/desorption curves along
with pore size distribution for CMK-3, and charge-discharge curves of
the Al/CMK-3 battery are presented in the Supporting Information.
Supplementary data to this article can be found online at https://doi.
org/10.1016/j.ssi.2018.02.037.
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