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\begin{document}

\title{Improving the electrical performance of Lithium-ion battery using
SilicaCarbon anode through technique}



\author[1]{Loan Phung Le}%
\author[1]{Xuan My Nguyen}%
\author[1]{Kha Le}%
\author[1]{Quan Phung}%
\author[2]{Duc Truong}%
\author[1]{Hoang Nguyen}%
\author[1]{Quynh Nguyen}%
\author[1]{Man Tran}%
\affil[1]{Vietnam National University Ho Chi Minh City University of Science}%
\affil[2]{Battery Cell Institute}%


\vspace{-1em}



  
  \date{May 26, 2024}


\begingroup
\let\center\flushleft
\let\endcenter\endflushleft
\maketitle
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\selectlanguage{english}
\begin{abstract}
Nowadays, a hybrid composite SiO2/C has been paid attention to improving
battery performance in Li-ion batteries (LIBs) as the anode. However,
this material unexpectedly suffers from initial active lithium loss
caused by the solid electrolyte interface (SEI) formation leading to low
initial Coulombic efficiency and significantly reducing the initial
capacity. In order to solve these issues, pre-lithiation has been
considered an effective approach to limit active lithium loss and
increase cycling performance. This work focuses on the two most common
techniques, including the direct contact method (CM) and the
electrochemical method in half-cell (EM). After the pre-lithiation
process, the anodes would be evaluated in full-cell with
LiNi0.6Mn0.2Co0.2O2 (NMC622) cathode. According to electrochemical
properties evaluations, pre-lithiation could enhance discharged capacity
and initial coulombic efficiency. Without the pre-lithiation method, the
discharged capacity in full-cell only witnessed 66.9 mAh.g-1, while CM
and EM methods illustrated a better battery performance. In detail, EM
exhibited a higher discharged capacity and initial coulombic efficiency
(137.06 mAh.g-1 and 99.08\%, respectively) compared to CM (99.08 mAh.g-1
and 93.23\%) method. Besides, the capacity retention using EM achieved
71.4\% and the discharged capacity illustrated 97.87 mAh.g-1 after 100
cycles, which is better than using CM, which only showed 71.40 mAh.g-1.%
\end{abstract}%



\sloppy


\textbf{1. Introduction}

Nowadays, the depletion shortage of non-renewable natural fossil
resources and environmental damages has led to the development of
battery storage energy. Therein, energy storage through electrochemical
cells has been considered the most satisfactory solution due to its high
energy density, high power density, flexibility, and simplicity of
maintenance. Moreover, as shown as the state-of-the-art technology for
various applications, LIBs are required to show lightweight, long
lifespans, high specific capacity, and good retention capacity.
{[}1-4{]}

In recent years, the silicon-based anode has attracted more attention
because of its superior theoretical capacity of 3579
mAh.g\textsuperscript{-1}. {[}5{]} However, the formation of
Li\textsubscript{x}Si\textsubscript{y} alloy makes the silicon anode
suffers a high-volume expansion (over 280\%), which leads to concerns
related to the safety and disconnection of electric contact, and then a
severe decrease of capacity after the first cycles. Therefore, silica
materials have been alternatives to develop silicon-based anodes owing
to less volume expansion and high capacity of 635.7
mAh.g\textsuperscript{-1} for LIBs. {[}6-7{]}

Although those materials overcome the weakness of silicon anode, their
low conductivity is one of the main reasons to prevent
commercialization. As a solution, a hybrid composite
SiO\textsubscript{2}/C was used to enhance battery performance. In
detail, the hard carbon in the SiO\textsubscript{2} structure enhances
the ionic and electronic conduction and the kinetic migration of
Li\textsuperscript{+} inside the materials by creating a linking network
to boost electrons movements to convert SiO\textsubscript{2} into Si and
co-products faster. {[}8-10{]} Nevertheless, SiO\textsubscript{2}/C
based as an anode suffers from significant active lithium loss, which
leads to low initial Coulombic efficiency in Li-ion batteries. This
phenomenon is caused by some Li\textsuperscript{+} ions trapped in an
anode structure. In detail, the irreversible reaction and volume
expansion create cracks inside the electrode, which need a large amount
of the electrolyte. As a result, the thickness of the SEI layer
increases after the first cycle, causing a significant amount of
Li\textsuperscript{+} ions to be trapped inside the electrode by the SEI
layer. {[}11-12{]}

To deal with this challenge, the pre-lithiation process was used to
compensate for the active lithium loss of the anode to enhance the
practical battery performance. {[}13-17{]} In this research, the two
common pre-lithiation methods were used, which include the direct
contact method (CM) using lithium foil and the half-cell electrochemical
method (EM). {[}18-22{]} These techniques were applied for the composite
anode SiO\textsubscript{2}/C, before matching in the full-cell with
NMC622, cathode. In CM, the time for anode directly contacted with
lithium was investigated. Meanwhile, regarding the electrochemical
method, the anode was assembled in half-cell and pre-lithiated at
various cycles to activate prior to the full-cell assembly. This study
hopefully brings new insights into selecting an appropriate approach to
successfully construct a high-performance lithium full-cell with
silica/carbon-based anode.

\textbf{2. Experiment}

\textbf{2.1. Experimental samples}

\textbf{Table 1.} List of full cells, detailed anodes component and
techniques used for pre-lithiation.\selectlanguage{english}
\begin{longtable}[]{@{}llll@{}}
\toprule
\textbf{Full cell} & \textbf{Anode} & \textbf{Cathode} &
\textbf{Method}\tabularnewline
\midrule
\endhead
100GR & 100 wt.\% graphite: 1.5 wt.\% CMC: 2.5 wt.\% SBR & NMC622 &
Without pre-lithiation method\tabularnewline
Baseline & 80 wt.\% graphite: 20 wt.\% SiO\textsubscript{2}/C: 1.5 wt.\%
CMC: 2.5 wt.\% SBR & NMC622 & Without pre-lithiation
method\tabularnewline
CM10 & & NMC622 & CM method within 10 min\tabularnewline
CM20 & & NMC622 & CM method within 20 min\tabularnewline
CM30 & & NMC622 & CM method within 30 min\tabularnewline
CM40 & & NMC622 & CM method within 40 min\tabularnewline
EM1C & & NMC622 & EM method with one cycle\tabularnewline
EM2C & & NMC622 & EM method with two cycles\tabularnewline
EM3C & & NMC622 & EM method with three cycles\tabularnewline
EM4C & & NMC622 & EM method with four cycles\tabularnewline
\bottomrule
\end{longtable}

In this work, ten different samples were investigated for pre-lithiation
techniques, namely 100GR, baseline, CM10, CM20, CM30, CM40, EM1C, EM2C,
EM3C, and EM4C, respectively (\textbf{Table 1} ). Among them, 100GR was
represented for full-cell consisting of 100 wt.\% graphite: 1.5 wt.\%
CMC: 2.5 wt.\% SBR as anode and NMC622 as cathode. The other samples
included 80 wt.\% graphite: 20 wt.\% SiO\textsubscript{2}/C: 1 wt.\%
C65: 1.5 wt.\% CMC: 2.5 wt.\% SBR as anode and NMC622 as cathode. In
detail, the 100GR and baseline were named full-cells without
prelithiated anode. In contrast, the CM samples mean the anode using the
direct contact method. For instance, ``CM10'' indicates that full-cell
was assembled using the anode contacted with lithium foil for 10
minutes. Meanwhile, the EM samples describe the anode using the
electrochemical method, whereas the anode was assembled in half-cell and
cycled in several cycles. For example, ``EM1C'' indicates that the
full-cell was assembled by the anode using an electrochemical technique
and activated by one cycle.

\textbf{2.2. Electrode preparation}

The anode was prepared by mixing conductive carbon (C65, Imerys,
Belgium), synthesized silica-carbon composite (SiO\textsubscript{2}/C)
{[}23,24{]}, and carboxymethyl cellulose binder (CMC, MTI, USA). After
being mixed in a planetary mixer (Thinky, Japan) at 2000 rpm for 20
minutes, an amount of graphite was added into a mixture and continuously
mixed for the next 20 minutes. Then, SBR binder was incorporated and
mixed for the last 5 minutes. The homogeneous slurry with the
aforementioned ratio was cast on copper foil and then dried in a vacuum
oven at 80 \textsuperscript{o}C for 12 h. The electrode film was finally
punched into a 15 mm diameter round plate. The mass loading of the anode
was around 12 mg.cm\textsuperscript{-2}.

The positive electrode was fabricated by mixing an active material of
LiNi\textsubscript{0.6}Mn\textsubscript{0.2}Co\textsubscript{0.2}O\textsubscript{2}(NMC622,
MTI, USA), C65, polyvinylidene fluoride (PVdF, Sigma-Aldrich, USA) in
the weight ratio of 96:2:2, respectively. All powder materials were
dispersed in N-methylpyrrolidone (NMP, Merck) solvent in a container.
After mixing for 20 minutes, the homogeneous slurry was cast on an
aluminum foil and dried in the same condition as the anode. Then, the
cathode film was punched into a round shape (12 mm diameter). The mass
loading of the cathode was around 18 mg.cm\textsuperscript{-2}.

\textbf{2.3. Coin cell assembly process}

In the CM method, the anodes were brought face to face with Li foil for
a period, then taken out and assembled in the full-cell configuration
with the NMC622 cathodes. On the other hand, in EM treatment, the anodes
were pre-lithiated by half-cell with lithium metal as counter electrode
using the electrolyte of 1.2 M LiPF\textsubscript{6} dissolved in EC:
EMC (3:7, v/v) and a polypropylene separator (PP, Sigma-Aldrich) to
achieve the pre-lithiation process. Then, these anodes were disassembled
from half-cell and used again for matching in full-cell. All the steps
were carried out in an Ar-controlled glovebox (MBRAUN, Germany). After
the pre-lithiation process, these anodes were assembled in full-cell
with NMC622 cathode material.

\textbf{2.4. Testing model}

In the EM method, the anodes assembled in half-cells were tested to
activate by Galvanostatic Cycling with Potential Limitation (GCPL),
performed on CT2001A Lanhe Battery Testing System (China). In detail,
the activated test was evaluated at current density C/10 (1C = 400
mA.g\textsuperscript{-1}) from 0.01 to 2.0 V. In full-cell
configuration, the cells were cycled at a constant current density of
C/3 (1C = 150 mA.g\textsuperscript{-1}) at 30 \textsuperscript{o}C with
a cut-off voltage range of 2.65 -- 4.3 V using a battery testing system
Lanhe.

\textbf{3. Results and discussion}

\textbf{3.1. Structure of SiO\textsubscript{2}/C material}\selectlanguage{english}
\begin{figure}[H]
\begin{center}
\includegraphics[width=0.70\columnwidth]{figures/image1/image1}

\end{center}
\end{figure}

\textbf{Figure 1.} XRD patterns of SiO\textsubscript{2}/C composite
material prepared from rice husks.

As shown in \textbf{Figure 1} , the structure of silica carbon material
prepared from rice husk as raw material was characterized by X-ray
diffraction. The synthesis process of SiO\textsubscript{2}/C anode
material was reported elsewhere. {[}23{]} XRD patterns of silica carbon
material exhibited broad peak spreading from 20 --
27\textsuperscript{o}confirming the presence of amorphous silica and
carbon. In addition, the diffraction peak of 43 -- 44\textsuperscript{o}
is represented for the amorphous carbon. {[}9{]} As a result,
SiO\textsubscript{2}/C synthesized has no impurities which are
compatible for anode application.

\textbf{3.2. Electrochemical properties}\selectlanguage{english}
\begin{figure}[H]
\begin{center}
\includegraphics[width=0.70\columnwidth]{figures/image2/image2}

\end{center}
\end{figure}

\textbf{Figure 2.} (a) Voltage profile at first cycle, (b) Voltage
profile at 80th cycle, (c) Cycling performance\textbf{,} and (d)
Coulombic efficiency of GR100 and baseline samples with NMC622
full-cells.

The battery performance of 100GR and the baseline with NMC622 full-cells
are shown in \textbf{Figure 2} . The 100GR full cell exhibits an initial
discharge capacity of 140.27 mAh.g\textsuperscript{-1}, while the
baseline only displays an initial value of 48.16
mAh.g\textsuperscript{-1} (\textbf{Figure 2} a). After 80 cycles, the
100GR full cell delivered a specific capacity of 51.35
mAh.g\textsuperscript{-1} (\textbf{Figure 2} b), which was reduced by
63.4\% compared to the first cycle. Meanwhile, the baseline one displays
a capacity of 32.50 mAh.g\textsuperscript{-1}, which only decreased by
32.9\% compared to the first cycle. These results could be explained by
the porous and amorphous structure of SiO\textsubscript{2}/C facilitated
a considerable amount of Li\textsuperscript{+} ions from the NMC cathode
to intercalate in by shortening the Li\textsuperscript{+} ion diffusion
pathway, resulting in the significant charging capacity. {[}10{]}
However, the superior specific surface area of SiO\textsubscript{2}/C
material reacted strongly with electrolyte to consume
Li\textsuperscript{+} ions for SEI layer formation, which indicated
``active lithium loss''. Hence the discharged capacity of the baseline
is lower than the 100GR.

Furthermore, the cycling performance and Coulombic efficiency of the
baseline were more stable than 100GR (\textbf{Figure 2} c, d). Although
the 100GR sample possesses a much higher discharged capacity than the
baseline sample, capacity retention is lower (\textbf{Figure 2} c). Minh
et al. reported that the 100GR\textbar{}\textbar{}NMC622 full-cell using
the same electrolyte solution (1.2 LiPF\textsubscript{6}, EC: EMC 3:7
v/v) with N/P ratio of 1.24 delivered a discharged capacity of only
140.5 mAh.g\textsuperscript{-1} and remained 9.8 \% after 30 cycles,
respectively. {[}25{]} Moreover, the previous study reported that the
well-designed graphite\textbar{}\textbar{}NMC622 batteries retained
about 50\% initial capacity during the cell lifespan. {[}14{]} This
rapid capacity fading of graphite anode full-cell may associate with
active lithium loss due to the growth of the SEI layer or physical
delamination of the graphite particles. {[}26{]} Aiping Wang et al.
showed that the decomposition of ethylene carbonate (EC) during the
cycling process would thicken the SEI layer and consequently decrease
capacity retention. {[}14{]} In order to enhance the long-cycling
performance of the baseline sample, the CM and EM methods were carried
out to optimize the full-cell capacity.

Regarding the pre-lithiation SiO\textsubscript{2}/C using the direct
contact method (CM) with lithium foil for a defined time, it can be
expected that an adjustable amount of Li\textsuperscript{+} can be used
for compensating active lithium loss during the first cycles for
SiO\textsubscript{2}-based anode without promoting the Li dendrite
formation. \textbf{Figure 3} shows the battery performance in various
contact times, including 10, 20, 30, and 40 minutes. The CM30 sample
shows the highest capacity, while the baseline sample only displays the
lowest capacity in the first and 80\textsuperscript{th} cycles
(\textbf{Figure 3} a, b). The first reversible capacity of CM30 is 99.08
mAh.g\textsuperscript{-1}, wh\selectlanguage{ngerman}ích declines by 27.94\% after 80 cycles,
while these values for the baseline sample are 48.43
mAh.g\textsuperscript{-1} and 32.50 mAh.g\textsuperscript{-1},
respectively. According to cycling performance and Coulombic efficiency
(\textbf{Figure 3} c, d), the CM30 sample continually witnesses the
highest capacity during the testing time and maintains stable Coulombic
efficiency of around 98\% for 80 cycles. Furthermore, increasing the
contact time enhances not only the discharged capacity but also improves
the coulombic efficiency. Indeed, by increasing the contact time, the
initial Coulombic efficiency increases from 84.42\% (CM10 sample) to the
highest of 93.23 \% for the CM30 before declining by the time in CM40.
Recently, similar results were demonstrated by Gerrit Michael Overhoff
et al. with Si/C\textbar{}\textbar{}NMC811 full-cell by varying the
contact times. {[}21{]} As a result, the amount of Li\textsuperscript{+}
ion was compensated to enhance battery performance by the CM method.
Nevertheless, increasing the contacting time (over 30 minutes) leading
to the deposition of lithium metal on the surface of the anode as well
as the thickness of the SEI layer are the main reasons to explain the
fast decrease of performance in the CM40 sample.\selectlanguage{english}
\begin{figure}[H]
\begin{center}
\includegraphics[width=0.70\columnwidth]{figures/image3/image3}

\end{center}
\end{figure}

\textbf{Figure 3.} (a) Voltage profile at first cycle, (b) Voltage
profile at 80\textsuperscript{th} cycle, (c) Cycling performance, and
(d) Coulombic efficiency of baseline, CM10, CM20, CM30, and CM40 samples
with NMC622 full-cells.

FT-IR Spectroscopy was further performed to evaluate the formation of
the SEI layer on the anode surface by analyzing the vibrational state of
chemical bonds. \textbf{Figure 4} exhibits similar qualitative spectra
but differentiates quantitatively in peak intensity, indicating the
heterogenous formation of the SEI layer. In general, there are three
main frequency regions observed, and each of these regions is associated
with typical group frequencies: 4000 -- 3000 cm\textsuperscript{-1}
assigned for the O -- H stretching, 3000 -- 1750 cm\textsuperscript{-1}
for the C -- H stretching, and 1700 -- 800 cm\textsuperscript{-1} for
the C = O stretching regions, as earlier reported by Guorong V. Zhuang
et al. {[}27{]} The wavenumber region of 2800 -- 2000
cm\textsuperscript{-1} might represent the CO\textsubscript{2} molecular
absorbed by LiOH or Li\textsubscript{2}O, which happens during sample
reservation and testing process (\textbf{Figure 4} ). In addition, the
SEI layer was reported to be composed of
Li\textsubscript{2}CO\textsubscript{3} and lithium alkyl carbonate
(ROCO\textsubscript{2}Li) compounds due to the decomposition of ethyl
carbonate (EC) electrolyte. {[}28{]} Thereby, IR fingerprints of these
samples proved the present of Li\textsubscript{2}CO\textsubscript{3} on
the electrode surface by the broad band of 920 -- 800
cm\textsuperscript{-1} and the double peak at 1520 -- 1380
cm\textsuperscript{-1} wavelength. It can be observed that the peak
intensity of Li\textsubscript{2}CO\textsubscript{3} also increases with
the longer contact duration, which is consistent with the explanation of
the thick SEI layer. Additionally, three wavelength regions including
1820 -- 1740 cm\textsuperscript{-1}, 1100 -- 1000
cm\textsuperscript{-1}, and 780 -- 600 cm\textsuperscript{-1} represent
organic carbonate from ROCO\textsubscript{2}Li compounds was observed
and also increased with the contact time. {[}28{]}\selectlanguage{english}
\begin{figure}[H]
\begin{center}
\includegraphics[width=0.70\columnwidth]{figures/image4/image4}

\end{center}
\end{figure}

\textbf{Figure 4.} FT-IR of pre-lithiated samples in different contact
times with CM method.\selectlanguage{english}
\begin{figure}[H]
\begin{center}
\includegraphics[width=0.70\columnwidth]{figures/image5/image5}

\end{center}
\end{figure}

\textbf{Figure 5} . (a) Voltage profile at first cycle, (b) Voltage
profile at 80\textsuperscript{th} cycle, (c) Cycling performance, and
(d) Coulombic efficiency of baseline, EM1C, EM2C, EM3C, and EM4C samples
with NMC622 full-cells.

\textbf{Figure 5} shows a significant improvement in electrochemical
performance by the EM method. Specifically, the three samples presented
significantly higher capacity than the baseline sample, and the capacity
decreased following the order: EM4C \textless{} EM2C \textless{} EM3C,
respectively. Obviously, the sample EM4C delivers the highest initial
capacity of 137.06 mAh.g\textsuperscript{-1} (\textbf{Figure 5} a) and
maintains 97.87 mAh.g\textsuperscript{-1} in the
80\textsuperscript{th}cycle (\textbf{Figure 5} b). Moreover, the EM4C
continually illustrates stable coulombic efficiency, around 99\% for 80
cycles. . Meanwhile, regarding the sample EM2C and EM3C, there is no
significant difference in the capacity behavior, showing a low initial
value of 48.43 mAh.g\textsuperscript{-1}, and the capacity declines to
32.50 mAh.g\textsuperscript{-1} after 80 cycles (\textbf{Figure 5} d).
By activating anodes with the EM method, an artificial SEI layer is
formed on anode's surface and becomes a stable SEI layer. Indeed, the
full-cells using these anode pre-lithiated by EM method do not lose the
capacity to stabilize the SEI layer. Furthermore, the EM method can
enhance the mobility of Li\textsuperscript{+} ions to optimize the
lithiation mechanism, which makes the charge transfer process more
accessible since the Li\textsuperscript{+} ions are not trapped.
{[}29-32{]} Therefore, the initial Coulombic efficiency and battery
performance increase when increasing the cycles for pre-lithiation.

\textbf{Table 2.} Battery performance of 100GR, baseline, CM30, and EM4C
sample.\selectlanguage{english}
\begin{longtable}[]{@{}lllll@{}}
\toprule
& Discharge capacity in the 1\textsuperscript{st} cycle
(mAh.g\textsuperscript{-1}) & Discharge capacity in the
80\textsuperscript{th} cycle (mAh.g\textsuperscript{-1}) & Capacity
retention (\%) & Coulombic efficiency in the 80\textsuperscript{th}
cycle (\%)\tabularnewline
\midrule
\endhead
100GR & 140.27 & 51.35 & 36.6 & 98.78\tabularnewline
Baseline & 48.43 & 32.50 & 67.1 & 98.73\tabularnewline
CM30 & 99.08 & 71.40 & 72.1 & 99.80\tabularnewline
EM4C & 137.06 & 97.87 & 71.4 & 99.56\tabularnewline
\bottomrule
\end{longtable}\selectlanguage{english}
\begin{figure}[H]
\begin{center}
\includegraphics[width=0.70\columnwidth]{figures/image6/image6}

\end{center}
\end{figure}

\textbf{Figure 6.} (a) Cycling performance and (b) Energy density in the
80\textsuperscript{th} cycle.

The battery performance of four samples, including 100GR, baseline,
CM30, and EM4C (\textbf{Table 2} ) is shown in \textbf{Figure 6} .
Overall, the discharged capacity of all samples decreases after testing
time. Indeed, the 100GR sample drops dramatically in discharge capacity,
from 140.27 to 51.35 mAh.g\textsuperscript{-1} (\textbf{Figure 6} a).
Meanwhile, the battery performance increase when using the
pre-lithiation method. In detail, the CM30 and EM4C show the capacity of
99.08 and 137.06 mAh.g\textsuperscript{-1} in the first cycle,
respectively, which is increased around 2-3 times compared to the
baseline sample. Therefore, the energy density of the EM4C is much
higher than the others, which is 98.68 mWh.g\textsuperscript{-1}. As a
result, the EM method effectively enhanced the battery performance.

\textbf{4. Conclusion}

In conclusion, the pre-lithiation method could effectively enhance the
battery performance compared to CM. In particular, the EM4C sample shows
the highest battery performance with the discharged capacity of 137.06
and 97.87 mAh.g\textsuperscript{-1} in the first and
80\textsuperscript{th} cycle, while the CM30 demonstrates a capacity of
71.40 mAh.g\textsuperscript{-1} in the 80\textsuperscript{th} cycle,
respectively. In addition, the EM4C exhibits remarkable cycling
performance, with a retention capacity of 71.4\% after 80 cycles at a
C/3 current density compared to the other samples. The remarkable
improvement in the performance of
SiO\textsubscript{2}/C\textbar{}\textbar{}NMC622 full-cell using the EM
technique can be attributed to a stable artificial SEI layer on the
anode surface which enhance the mobility of Li\textsuperscript{+} ions
and remained enough Li\textsuperscript{+} ions stored capacity for
stabilizing the SEI layer. Therefore, the EM is a promising
pre-lithiation method for the silicon or silicon-based anode material to
enhance battery performance in LIB applications.

\textbf{Author contributions}

Xuan My Nguyen Thi: performed the analysis, collected the data, wrote
the paper. Kha Minh Le: conceived and designed the analysis, data
interpretation, edited the paper. Quan Phung: contributed to analysis
tool. Duc Quang Truong: contributed to analysis tool. Hoang Van Nguyen:
contributed to analysis tool, edit the paper. Quynh Nhu Nguyen: data
interpretation, wrote, reviewed and format the paper. Man Van Tran:
contributed to analysis tool. Phung My Loan Le: conceived and designed
the analysis, reviewed the paper.

\textbf{Conflicts of interest}

There are no conflicts to declare.

\textbf{Acknowledgements}

This work was funded by University of Science, Vietnam National
University Ho Chi Minh city through the grant number T2022-41.

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\end{enumerate}

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