Recycling cathode materials for lithium-ion batteries via Hydro-to-Cathode® method

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EDITED BY
Rachid Essehli,
Oak Ridge National Laboratory (DOE),
United States

REVIEWED BY
Nitin Muralidharan,
Indian Institute of Technology Madras, India

*CORRESPONDENCE
Jong Hyun Shim,

[jshim@ascendelements.com](mailto:jshim@ascendelements.com)

RECEIVED 06 March 2024

ACCEPTED 11 December 2024

PUBLISHED 03 January 2025

CITATION
Shim JH (2025) Recycling cathode materials for
lithium-ion batteries via Hydro-toCathode® method.

Front. Batteries Electrochem. 3:1397122.
doi: [10.3389/fbael.2024.1397122](https://doi.org/10.3389/fbael.2024.1397122)

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[TYPE](https://www.frontiersin.org/journals/batteries-and-electrochemistry#editorial-board) Mini [Review](https://www.frontiersin.org/journals/batteries-and-electrochemistry#editorial-board)

PUBLISHED 03 January 2025

DOI [10.3389/fbael.2024.1397122](https://doi.org/10.3389/fbael.2024.1397122)

# Recycling cathode materials for lithium-ion batteries via Hydro-to-Cathode ® method

Jong Hyun Shim*

Ascend Elements, Westborough, MA, United States

KEYWORDS

recycling, lithium-ion battery, Hydro-to-Cathode ®, cathode material,
closed-loop system

## 1 Introduction

Since the concept of the lithium-ion battery (LIB) was formalized by John Goodenough,
Stanely Wittingham and Akira Yoshino, the LIB was broadly applied to a variety of
industries such as electronic devices, military applications, and electric vehicles (EVs) (Bai
et al., 2020b; Kim, 2022; Sim et al., 2023). More specifically, the market for EVs has
dramatically increased; forecasting 140 million EVs to be operated worldwide by
2030 Chemical and Engineering News (2019). When compared to conventional
combustion engine vehicles, EVs have relatively simple mechanical systems. They also
generate low outgas emissions, resulting in greater attention relative to lower
environmental impact.

Despite those advantages, the initial version of EVs has been challenging because of
limited driving distance per single charge of the LIB. Following the first designed
cathode material produced for commercial use, the ternary system of Li [NixMnyCoz]O2
(x + y + z = 1) (NMC) LIB cathode material has been in the spotlight. High Ni NMC
based LIB cathode material [Li(NixMnyCo1-x-y)O2, x ≥ 0.8] demonstrated particularly
high energy density (200–250 mA h/g) and high operating voltage (≥4.3 V vs. Li + /Li)
compared to LiFePO4 (LFP), LiMn2O4 (LMO), and LiCoO2 (LCO) based cathode
materials, making it sufficient to meet the growing demand of the EV market (Li W.
et al., 2020). That said, the high Ni NMC system demonstrates relatively insufficient
cycling performance due to poor structural stability (Duan et al., 2019). To compensate

Due to the rising price and limited resource supply chain of Li [NixMnyCoz]O2 (x +
y + z = 1) (NMC) cathode material, lithium-ion battery (LIB) recycling technologies
have been emerging as the best solution to address the price issue. Mainly,
conventional hydrometallurgy processes have been applied to the LIB recycling
field in recognition of its value. One remarkable advantage of the hydrometallurgy
method is that it serves as a bridge to enable the Hydro-to-Cathode® method.

method is that it serves as a bridge to enable the Hydro-to-Cathode® method.

However, using recycled raw materials in the production of precursor cathode
materials needs to be studied in parallel with the impurity (dopant) effect. The
insufficient selective impurity removal technology leads to unexpected
electrochemical properties in the final NMC cathode active material, which
can be doped by several different impurities. Consequently, scrutinizing
dopant elements (inorganic and organic) is critical if we want to consider the
Hydro-to-Cathode® method as a major recycling process of NMC cathode

Hydro-to-Cathode® method as a major recycling process of NMC cathode

material.

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FIGURE 1
Direct and indirect recycling methods for NMC cathode material.

for this limitation, researchers have been studying techniques for
doping, coating, and tailoring crystalline structure by
introducing different elements and solid-state reaction skills
(Ko et al., 2023; Susai et al., 2023; Tang et al., 2023; Hong
et al., 2024).

Nevertheless, the LIB must be replaced every 5–10 years, at
which it reaches end of life (EOL) due to the degradation of internal
parts and materials (Mishra et al., 2022). Consequently, permanent
use of the LIB is mostly impossible. The serious degradation of the
cathode active material over time is a major cause of the reduced life
of LIB. Cathode materials are an essential part of LIB, as they not
only can determine performance of EVs, but also constitute more
than half of the entire manufacturing cost of the LIB (Houache
et al., 2022).

Consequently, due to the high demand of the LIB cathode
materials, over time the prices of the LIB raw materials have
lacked both control and consistency globally. Li is an essential
raw material for cathode material as a source of electrochemical
potential compared to others and has been designated as a strategic
material for all countries (Bae and Kim, 2021). Ni and Co are also
important elements, in terms of energy density and structural
stability respectively (Ye et al., 2021). Therefore, many countries
have focused on securing these materials. As a result, the price of Li,
Ni, and Co have been rising recently. To overcome high price
concerns, recycling technologies for LIB cathode materials are
considered more commonly in both academic and industrial
applications (Jung et al., 2021). In this review, we will cover
several recycling methods and subsequent obstacles during the
recycling process.

## 2 Recycling methods

2.1 Direct recycling

In terms of LIB recycling, there are two substantive approaches
to accomplish the demanding task. The first, direct recycling, is an
affordable method to meet goals such as cost reduction and
suppressing environmental crisis. Compared to indirect recycling
methods (pyrometallurgy and hydrometallurgy), direct recycling is
more advantageous in terms of simplicity, efficiency, and
conservation of energy. It can be broken down into three steps
including grinding/delamination, separation, and regeneration
(Figure 1). After collecting EOL LIB, they go directly through the
grinding process or manual disassembly. From there, cathode
material must be separated from grinded powder or delaminated
film, which may contain anode, current collectors, and separator.
Finally, the refined cathode material would be regenerated through
proper treatments (Bai et al., 2020a; Xu et al., 2020; Kim et al., 2021).

When it comes to the regeneration process, it requires relithiation treatment via heat treatment because the most common
failure of cathode material is attributed to Li loss during processing.
Typically, the heat treatment process can be proceeded by using
Li2CO3 as a Li source and has been widely studied due to its high
accessibility (Zhang et al., 2013; Ji et al., 2023). Mainly, the
regeneration of LMO and LFP based cathode materials has been
studied due to low material cost and simple chemical composition.
As the cost of those materials is very inexpensive, the conventional
recycling method is not needed in this case (Lv et al., 2018). Besides,
LCO and NMC cathode materials have been considered for direct

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recycling by using Li2CO3 as a Li source (Nie et al., 2015; Shi et al.,
2018). For heat treatment, duration time and temperature should be
the most critical factors in addition to the Li source as the primary
influencing factor. Though Li2CO3 is commonly utilized for relithiation studies, LiOH and LiNO3 sources were verified from little
research. The LiOH source was selected for the hydrothermal relithiation process which follows heat treatment (Figure 1) (Sloop
et al., 2020). The hydrothermal treated recycled cathode materials
showed relatively high cell cycling performance (Xu et al., 2021).
Interestingly, there is a way to dramatically reduce lithiation
temperature. Huang et al. reported that degraded Li

[Ni0.6Mn0.2Co0.2]O2 (NMC622) material was sintered with LiOHLiNO3 molten salt for not only re-lithiation but also conversion to
single crystal particle to allow for a single body type of cathode
material that demonstrated high cycling properties (Huang
et al., 2022).

Nonetheless, the direct recycling method lacks the flexibility to
obtain different cathode chemistries. For instance, the used Li [Ni1/

3 Mn 1/3 Co 1/3 ]O 2 (NMC111), Li [Ni 0.5 Mn 0.3 Co 0.2 ]O 2 (NMC532), and
NMC622 chemistries could only be recycled to the exact same NMC
chemistry. Therefore, direct recycling cannot satisfy the demand for
high Ni NMC cathode materials (Neumann et al., 2022). Even if
there is no disruption in the supply of used high Ni NMC, due to the
lack of structural stability it is realistically difficult to adopt the direct
recycling method for high Ni NMC (Gao et al., 2022). In addition,
due to the nature of this recycling concept, electrode, or LIBs cell
current collectors such as Cu and Al must be perfectly separated
after crushing. It is also worth noting that achieving perfect
separation between cathode material and polyvinylidene fluoride
(PVDF)/carbon is very challenging considering current technologies
(Zhan et al., 2020). In summary, the direct recycling method is not
fully applicable to support scaling up to industrial levels as it lacks
required technologies.

2.2 Indirect recycling

The second predominant recycling method, indirect recycling, is
based on deconstruction through smelting and leaching, and is
widely preferred in the industry. Therefore, the pyrometallurgy and
hydrometallurgy methods are prevailing routes for the execution of
recycling LIB cathode material (Figure 1) (Bae and Kim, 2021; Kader
et al., 2021; Latini et al., 2022; Mishra et al., 2022). In terms of
recycling process simplicity, pyrometallurgy offers greater simplicity
compared to hydrometallurgy. Considering both powder containing
pretreated precious metals (black mass) from pretreatments
(grinding and separation) or disassembled LIB can directly go
through the smelting process, pyrometallurgy offers a simple
operation and shortened process time (Latini et al., 2022).
However, the smelting process is not viable in terms of energy
saving and environmental impact because of high energy
consumption and carbon emissions, respectively (Kader et al.,
2021). Furthermore, extraction of Li is challenging because it can
be incorporated into slag (Makuza et al., 2021; Miao et al., 2022). To
overcome the impediments of the pyrometallurgy method, pyrolysis,
roasting, and calcination processes have been introduced, allowing
relatively low temperature conditions and higher recovery rates of Li
(~93%) and Co (~99%) (Makuza et al., 2021). Nevertheless, the

pyrometallurgy method always requires a leaching process to
retrieve precious metals as a post treatment.

Accordingly, the hydrometallurgy method has been selected for
many years in the LIB cathode material recycling industry. The
hydrometallurgy approach is based upon dissolution of spent LIBs
via high acidic treatment and extract processes (Lv et al., 2018; Kader
et al., 2021; Latini et al., 2022). The entire process involves multiple
steps. During acidic treatment, unpleasant gas emissions and a
significant volume of wastewater generation are unavoidable
(Latini et al., 2022). However, the hydrometallurgy method can
achieve high recovery yield as well as high purity of recycled
metals. Particularly, the hydrometallurgy method encompasses
several different processes such as pretreatment of the battery cell,
leaching by acidic solution, selective precipitation of metal, impurity
removal, and solvent extraction for drawing Li, Co, Ni, and Mn,
separately. Among these processes, the leaching process has been
actively studied - not only is the rate of recovery efficiency directly
related to the high final yield of precious metals, but it is also directly
linked to environmental pollution due to the generation of tons of
wasted water after the process (Jung et al., 2021). Naturally, many
researchers have been searching for highly efficient and minimally
toxic leaching agents. Organic acids are a remarkable leaching agent in
terms of environmental benefit. However, the high hurdle for
adopting them at industrial scale has deterred widespread use.
Therefore, inorganic acids have been broadly utilized for industrial
purposes (Or et al., 2020). More specifically, the H2SO4 leaching
system is widely studied for various methodologies of process through
diversification. The H2SO4 system has relatively high adaptability to
industrial scale compared to other inorganic acids such as HCl, HNO3
and H3PO4. Therefore, different concentrations of H2SO4, leaching
temperature, additives, etc. can be controlled in terms of different
leaching efficiencies for targeted precious LIB materials (Li, Ni, and
Co) (Or et al., 2020; Chan et al., 2021; Jung et al., 2021).

2.3 Hydro-to-Cathode® method

The H2SO4 leaching system can also allow direct resynthesizing
via a co-precipitation process using the purified leached metal
solution (Figure 1). This concept was originally patented by Yan
Wang et al. in United States, and they named it the Hydro-toCathode ® method for the very first time (Wang et al., 2013). The
Hydro-to-Cathode ® method is advantageous for both cost reduction
and precursor cathode materials design. The concept itself is
designed for creating a closed-loop system, which provides a
better solution than conventional recycling methods to improve
process time and cost in the LIB material industry. Therefore,
research on the Hydro-to-Cathode ® concept is actively being
conducted in both commercial and academic fields. Ascend
Elements plans to open a new large scale LIB precursor cathode
and cathode materials plant in the United States using the Hydro-toCathode ® method (Recycling Today, 2022). Compared to the direct
recycling approach, the Hydro-to-Cathode ® method not only allows
increased accessibility to various cathode chemistries, but also
tailoring crystalline structure and surface morphology of
precursor cathode material for certain models of battery cells.
The Yan Wang group conducted a preliminary study to verify
the potential of the Hydro-to-Cathode ® method. They showed a

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direct comparison between recycled and virgin raw NMC metal
solutions by a co-precipitation process to evaluate final
cathode materials.

The Yan Wang group then went through a leaching process with
mixed cathode materials [LCO, LMO, NMC111, and LFP]. During
this process, Fe was properly removed by pH adjustment and Li2CO3
was recovered. After that, Ni1/3Mn1/3Co1/3(OH)2 was synthesized by
a recycled metal solution. Furthermore, final cathode material was
prepared by using the recovered Li2CO3. The recycled cathode
material showed a similar range to commercial grade of
electrochemical performance. They have also reported recycled
cathode material is more economical compared to the normal
process. (Zou et al., 2013).

Beyond academic field study, they recycled actual LIBs for
getting final NMC111 product. Before the leaching process,
pretreatments (shredding, magnetic removal, aluminum
dissolution, and sieving) were systematically proceeded. For
characterization, the final product was analyzed by X-ray
diffraction (XRD) measurement, and the peaks matched well
with layered structure without any abnormal impurity peaks
(Gratz et al., 2014).

They also reported that four different feedstocks of EOL LIBs
from various manufacturers were utilized for the Hydro-toCathode ® method. Four precursor cathode materials were coprecipitated to obtain Ni1/3Mn1/3Co1/3(OH)2. The final cathode
materials were evaluated with coin cell testing to characterize
their electrochemical properties. All four samples showed similar
rate capability to commercial cathode material at low C-rates, while
they exhibited superior capability in high C-rates. Therefore, they
could conclude that the Hydro-to-Cathode ® method has minimal
impact on the final recycled cathode material (Zheng et al., 2018).

Lastly, they executed one batch experiment with up to 30 kg of
spent LIBs from different EV manufacturers. The recycled cathode
material was compared with commercial cathode material by both
coin cell and single layer pouch cell tests. Recycled and commercial
cathode materials showed similar properties through discharge
ΔSOC (state of charge) tests and direct current resistance tests.
This was the first trial for the scaling-up process, so they could
confirm Hydro-to-Cathode ® is a suitable method in terms of
scalability (Chen et al., 2019).

Other groups further investigated the effects of impurities in
final cathode material. Beak et al. verified that actual recycled NMC
metal solution can affect morphology control of precursor cathode
material [Ni1/3Mn1/3Co1/3(OH)2]. They reported after converting to
cathode material, high levels of metallic impurities could have an
unfavorable impact on initial charge/discharge capacity and capacity
retention at 55 cycles at coin half-cell test (3.0–4.3 V). They also
argued that metallic and nonmetallic impurities are advantageous as
dopants in cathode material to get better rate capability than nondoped cathode material (Beak et al., 2022).

Kauppinen et al. introduced recycled and purified Mn for Li

[Ni0.8Mn0.1Co0.1]O2 (NMC811) cathode material. They synthesized
precursor cathode materials with three different metal sulfate
solutions which contain different levels of metallic impurities
(Zn, Ca, K, Mg, and Fe). Following proper sintering processes,
they assessed the electrochemical property through pouch cell
testing (2.8–4.2 V). After 1,100 cycles, capacity retention showed
over 80% and initial discharge capacity reached 184 mA h/g.

Therefore, they concluded the recycled raw material is feasible
for high Ni NMC cathode material (Kauppinen et al., 2023).

2.4 Impurity (dopant) control for the Hydroto-Cathode® method

The mentioned experiments with NMC based cathode materials
can be considered important because they have studied the real
possibilities of the Hydro-to-Cathode ® method. The types and levels
of impurities would not be easily controllable by impurity removal
during the recycling process. Even a small ppm level of impurities
could have severe influence on electrochemical properties as a
dopant. Furthermore, the combination of impurities with two or
three elements can provide different aspects of cell performance
rather than what we expected (Tian et al., 2023). Therefore,
scrutinizing the doping effect on cathode materials is
indispensable if we rely on precursor NMC cathode material
synthesized via co-precipitation with recycled metal raw materials.

In the last decade, doping effects of specific elements have been
investigated through NMC cathode material. In accordance with the
operation mechanism of doping in the NMC system, we can divide into
two main doping strategies (Figure 2). The first scheme involves
introducing similar size of element to either Li or transition metal
atoms. These specific elements make it possible to substitute either
transition metal atoms or Li. Among all possible elements, Al, Ti, Zr,
and Nb are especially considered as structural stabilizers due to their
high bonding with the neighbor transition metal atoms (Schipper et al.,
2016; Liu et al., 2018; Song et al., 2018; Xin et al., 2019; 2022; Yang et al.,
2019; Zhang et al., 2019; Park et al., 2020; Zhou et al., 2021; Bizzotto
et al., 2023). Therefore, they can lead to high cycling performance and
capable performance under high voltage conditions. Other feasible
dopants are Na, Mg, and Zn, which can play a pivotal role in
improving rate capability by replacing the Li site as a pillar (Du
et al., 2015; Huang et al., 2016; Li et al., 2019; Li L. et al., 2020; Liu
et al., 2019; Sattar et al., 2020; Gomez-Martin et al., 2022).

The second strategy involves tailoring a preferentially aligned
NMC cathode crystalline structure, rather than chemically bonding
with a heterogeneous element and the main NMC structure to
mitigate collapse of cathode material crystalline structure. For
instance, a radial columnar structure, which is designed to extend
outward from the center, could be advantageous for getting
enhanced electrochemical performance. This uniquely oriented
crystalline structure can diminish internal stress and strain
caused by charge and discharge, allowing dramatically improved
cycling performance to be achievable. B, Ta, W, Sn, and Mo have
been studied for forming controlled radial columnar structure by
many researchers (Park et al., 2018; Lee et al., 2019; Ryu et al., 2019;
Kim et al., 2020; Sun et al., 2021; Thien Nguyen et al., 2021). In
particular, B has been acknowledged as a key dopant in terms of
structural controlling of NMC cathode material. Because the B
doped cathode materials exhibited enhanced cycling performance
and discharge capacity, it can be attributed to alleviated internal
compressed stress and increased delivery of lithium ions during the
charging and discharging processes. Ryu et al. conducted a direct
comparison between NMC and Li [NixCoyB1-x-y]O2 (NCB) systems
to observe B doping effect undoubtedly. They also demonstrated
that different doping amounts and sintering temperature could be

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FIGURE 2
Two strategies of impurity (dopant) effect on NMC cathode material.

an adjustable factor to find optimum crystalline structure (Ryu
et al., 2020).

## 3 Discussion and future works

In this mini review, we have discussed several recycling methods for
obtaining precious materials from the EOL LIB. It can be divided into two
broad categories including direct and indirect recycling methods. The
direct recycling method is an attractive approach in terms of saving cost,
time, and energy due to the simple nature of the process. However, its
technical challenges and limited freedom of NMC composition will limit
its utilization in the commercial LIB industry. In contrast, the indirect
recycling method provided relatively clear direction toward industrial
application. The indirect recycling method is approachable through
pyrometallurgy or hydrometallurgy processes. Technically, these
processes require completely different paths to break down into
precious major raw materials such as Li, Ni, and Co. However, both
methods mandatorily go through leaching and extraction processes to
draw the raw materials. Therefore, the hydrometallurgy method is
advantageous for industrial application. Moreover, the Hydro-toCathode ® method, which is an advanced variation of the
hydrometallurgy method, showed positive signs to attain a closedloop system. The remaining ppm level of impurities can be doped
into the precursor cathode materials, so that the final cathode material
will exhibit significantly improved electrochemical properties compared
to the virgin cathode material. The improved performance of the cathode
material can be attributed to two doping strategies including
strengthened structure and oriented crystallite structure. Consequently,
the Hydro-to-Cathode ® method would be successfully adopted into the
industrial field with a genuine understanding of dopant (impurity)
impact and precise adjustment skill for impurity control.

## Author contributions

JS: Funding acquisition, Writing–original draft, Writing–review
and editing.

## Funding

The author(s) declare that financial support was received for the
research, authorship, and/or publication of this article. This study
received funding from Ascend Elements, Inc.

## Acknowledgments

The author would like to express appreciation to Sarah Jose for
helpful discussion and support.

## Conflict of interest

Author JS was employed by Ascend Elements, Inc.

## Publisher’s note

All claims expressed in this article are solely those of the authors
and do not necessarily represent those of their affiliated
organizations, or those of the publisher, the editors and the
reviewers. Any product that may be evaluated in this article, or
claim that may be made by its manufacturer, is not guaranteed or
endorsed by the publisher.

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