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Cited by 108Advanced Battery Technologies ResearchAdvancements in Battery MaterialsExtraction and Separation Processes

Low‐temperature reversible capacity loss and aging mechanism in lithium‐ion batteries for different discharge profiles

Open access
Wu, Weixiong, Wu, Wei, Qiu, Xianghui, Wang, Shuangfeng·2019·International Journal of Energy Research
DOI 10.1002/er.4257
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Abstract

In this paper, reversible capacity loss of lithium-ion batteries that cycled with different discharge profiles (0.5, 1, and 2 C) is investigated at low temperature (−10°C). The results show that the capacity and power degradation is more severe under the condition of low discharge rate, not the widely accepted high discharge rate. To shed some light on the aging phenomena, noninvasive electrochemical methods, ie, incremental capacity and differential voltage analysis, are applied to identify and quantify the effects of different degradation modes (DMs). Apart from the resistance increase, the DMs include the loss of lithium inventory (LLI) and the loss of active material (LAM). Both LLI and LAM decay to a greater extent for the cell cycled with lower discharge rate, and the growth of LAM is higher than that of LLI. Further, the analysis of state of charge (SOC) window shows that the earlier cutoff of the high discharge rate can lead to less mechanical and thermal stress on cathode materials, thus a lower degradation rate. Another cause is that the lithium plating on the anode materials can be mitigated by increasing the charging temperature which results from preceding high rate discharging.

AI snapshot

Written from the paper’s full text.

TL;DR

In commercial 18650 graphite/NCA cells cycled at −10°C, a lower discharge rate (0.5 C) caused more severe capacity and power degradation than 1 C or 2 C, contrary to the usual expectation. Noninvasive IC-DV analysis attributed aging to resistance increase plus loss of active material (LAM) and loss of lithium inventory (LLI), with LAM growing more than LLI.

Key findings

  • After 150 cycles, discharge capacity retention at 1 C was about 92% for the 1 C- and 2 C-cycled cells, while the 0.5 C-cycled cell retained only 78%.
  • Internal resistance at 0.5 SOC increased by 39.4% for the 0.5 C cell, compared with 20.5% and 16.2% for the 1 C and 2 C cells, respectively.
  • IC-DV analysis showed LAM and LLI as main degradation modes besides resistance increase; for the 0.5 C cell, LAM grew from 0% to 25.7% over RPT, while LLI grew to 15.4%, making LAM the larger contribution.
  • The discharge SOC window was about 0.0–0.8 for 0.5 C, 0.2–0.8 for 1 C, and 0.3–0.8 for 2 C; higher-rate earlier cutoff and self-heating (surface temperature at end of first discharge: −3.7°C, 8.5°C, and 17.2°C for 0.5, 1, and 2 C) were linked to less cathode stress and mitigated lithium plating.

Methods

  • Commercial cylindrical 18650 graphite/NCA cells with rated capacity 3100 mAh and voltage window 2.5–4.2 V were cycled at −10°C for 150 cycles. Charging was CC-CV at 0.5 C to 4.2 V then CV to 50 mA; discharging was at 0.5 C (cell A), 1 C (cell B), or 2 C (cell C) to 2.5 V.
  • Reference performance tests (RPTs) at 25°C were performed every 30 cycles and included 1 C and 0.2 C capacity tests, a 0.1 C microdischarge for IC-DV curves, and HPPC at SOC 0.9 to 0.1.
  • Noninvasive IC-DV analysis quantified LLI and LAM growth from DV offsets and IC peak heights; HPPC calculated discharge resistance, T-type thermocouples measured surface temperature, and SOC windows were calculated from first low-temperature charge/discharge capacities.

Limitations

  • The paper states that only surface temperature was measured, so there can be a radial discrepancy between surface and internal temperatures, more evident at high discharge rates and sometimes above 10°C.
  • Evident from the text: one cell per discharge rate, a single cell chemistry/format (18650 graphite/NCA), one low temperature (−10°C), and one charge protocol were used, with no ex situ/postmortem validation reported, limiting generalizability.

Model-written summary. Check it against the paper before relying on it.

Integrity signals

Registry

Crossref · 10.1002/er.4257

Cites

54 of 54 references verified0 citation errors · 0 not checkable

Statistics

Nothing to recompute.

Claims the paper makes

0 of 22 cited sources checked · 0 supported · 0 flagged

  • Findingown data

    At -10°C, capacity and power degradation is more severe for cells cycled with lower discharge rate (0.5 C) than for those cycled with higher discharge rates (1 and 2 C), contrary to the widely accepted high-discharge-rate acceleration.

    “The results show that the capacity and power degradation is more severe under the condition of low discharge rate, not the widely accepted high discharge rate.”
    • Also stated in: § 3.1 | Capacity fade · plain
      “It is interesting that the capacity degradation is more severe under the condition of low discharge rate, not the widely accepted high discharge rate.”
    • Also stated in: § 4 | CONCLUSIONS · plain
      “It is showed that the cell cycled with low discharge rate has a quicker degradation rate, which is counterintuitive to what would be expected from previous studies.”
    Quote in the paperSubstantial claim
  • Findingown data

    Apart from resistance increase, the degradation modes include loss of lithium inventory (LLI) and loss of active material (LAM).

    “Apart from the resistance increase, the DMs include the loss of lithium inventory (LLI) and the loss of active material (LAM).”
    • Also stated in: § 3.3 | Degradation modes · plain
      “It can be seen that apart from resistance increase, LAM and LLI are the main DMs.”
    • Also stated in: § 4 | CONCLUSIONS · plain
      “This reveals that except of the resistance increase, the pertinent DMs consist of LAM and LLI.”
    Quote in the paperSubstantial claim
  • Findingown data

    The discharge capacities in stage 1 for all cells at 25°C (RPT 1) remain at the same level (about 3045 mAh).

    “According to the results of primary test (RPT 1) at a temperature of 25°C, the discharge capacities in stage 1 for all cells remain at the same level (about 3045 mAh).”
    Quote in the paperNot a substantial claim
  • Findingnone given

    The IC peaks decay to a greater degree in intensity and position for the cell cycled with lower discharge rate.

    “In addition, the peaks decay to a greater degree in intensity and position for the cell cycled with lower discharge rate.”
    Quote in the paperNot a substantial claim
  • Findingown data

    The range of the SOC window follows the sequence cell A > cell B > cell C.

    “As a result, the range of SOC window follows a sequence: cell A > cell B > cell C.”
    Quote in the paperSubstantial claim
    • The authors state this as an assumption: The inherent capacity of the reference performance test (RPT) is the same as the following first low-temperature cycle.
  • May combine two claims. 17
  • Classified as probably not a substantial claim. 13

  • May combine two claims.

    Findingown data

    With cycling, the difference in capacity between 0.2 and 1 C for cell B and cell C remains steady, but the gap for cell A diverges.

    “In addition, with cycling, the difference in capacity between 0.2 and 1 C for cell B and cell C remains steady, but the gap for cell A is diverged.”
    Quote in the paperNot a substantial claim

  • May combine two claims.

    Findingown data

    The discharge capacity retention of cells B and C after 150 cycles is about 92% at 1 C, while the capacity of cell A is only 78%.

    “To be specific, the discharge capacity retention of cells B and C after 150 cycles is about 92% at 1 C, while the capacity of cell A is only 78%.”
    Quote in the paperSubstantial claim

  • May combine two claims.

    Findingown data

    The reversible capacity decreases with cycling, and the degradation rate follows the order cell A > cell B > cell C.

    “It is shown that the reversible capacity decreases with cycling, while the degradation rate follows the order of cell A > cell B > cell C.”
    Quote in the paperSubstantial claim

  • May combine two claims.

    Findingown data

    The SOC of cell A at the beginning of discharging decreases gradually with cycling, while cell B and cell C stay relatively stable (ca. 80%).

    “It can be seen that the SOC of cell A at the beginning of discharging decreases gradually with cycling, while cell B and cell C stay relatively stable (ca.80%).”
    Quote in the paperSubstantial claim
    • The authors state this as an assumption: The inherent capacity of the reference performance test (RPT) is the same as the following first low-temperature cycle.

  • May combine two claims.

    Findingown data

    The LAM of cell A grows exponentially over RPT from 0% to 25.7%, while LLI grows from 0% to 15.4%.

    “For instance, the LAM of cell A grows exponentially over RPT from 0% to 25.7%, while LLI grows from 0% to 15.4% showing that the contribution of LAM as capacity loss percentage is more significant.”
    • Also stated in: § 4 | CONCLUSIONS · plain
      “The LAM of the 0.5 C discharge rate-cycled cell grows exponentially over RPT from 0% to 25.7%, while LLI only grows to 15.4%, showing that the contribution of LAM as capacity loss percentage is more significant.”
    Quote in the paperSubstantial claim

  • May combine two claims.

    Findingown data

    The SOC window of cells A, B, and C during the discharging process is about 0.0 to 0.8, 0.2 to 0.8, and 0.3 to 0.8, respectively.

    “In this study, the SOC window of cells A, B, and C during the discharging process is about 0.0 to 0.8, 0.2 to 0.8, and 0.3 to 0.8, respectively.”
    • Also stated in: § 4 | CONCLUSIONS · plain
      “The SOC window of the cells during the discharging process of 0.5, 1, and 2 C is about 0.0 to 0.8, 0.2 to 0.8, and 0.3 to 0.8, respectively.”
    Quote in the paperSubstantial claim
    • The authors state this as an assumption: The inherent capacity of the reference performance test (RPT) is the same as the following first low-temperature cycle.

  • May combine two claims.

    Findingown data

    The IC curves of RPT 1 for all cells show highly distinct peaks around 3.37, 3.55, 3.85, and 4.05 V for discharging, and with cycling the peak intensity and position change; the peak around 3.37 V decays significantly until it disappears.

    “The IC curves of RPT 1 for all cells show highly distinct peaks around 3.37, 3.55, 3.85, and 4.05 V for discharging, while with cycling, the peak intensity and position change.Specially, the peak around 3.37 V decays significantly until it disappears.”
    Quote in the paperSubstantial claim

  • May combine two claims.

    Findingown data

    The SOC at the end of discharging displays a remarkable difference among these cells, and the cell cycled at higher discharge rate has a higher b_i.

    “The SOC at the end of discharging displays a remarkable difference among these cells, and the cell cycled at higher discharge rate has a higher b i .”
    Quote in the paperSubstantial claim
    • The authors state this as an assumption: The inherent capacity of the reference performance test (RPT) is the same as the following first low-temperature cycle.

  • May combine two claims.

    Findingown data

    After low-temperature cycling, the cells cycled at 1 and 2 C discharge rates show an R_d increase of 20.5% and 16.2%, while the 0.5 C-discharge-rate-cycled cell shows an R_d increase of 39.4%.

    “The cells cycled at 1 and 2 C discharge rates show an R d increase of 20.5% and 16.2%, while the 0.5 C-dischargerate-cycled cell suffers from significant increase in R d by 39.4% after low-temperature cycling test.”
    Quote in the paperSubstantial claim

  • May combine two claims.

    Findingown data

    At higher discharge rate, significantly higher temperature rise is observed; the recorded surface temperature at the end of discharge is -3.7°C, 8.5°C, and 17.2°C for 0.5, 1, and 2 C, respectively.

    “As anticipated, at higher discharge rate, significantly higher temperature rise is observed.The recorded surface temperature at the end of discharge is -3.7°C, 8.5°C, and 17.2°C for 0.5, 1, and 2 C, respectively.”
    Quote in the paperSubstantial claim

  • May combine two claims.

    Interpretationown data

    The capacity loss at low temperature is not completely irreversible; it can be recovered by higher temperature activation.

    “However, the delivered capacity could be returned to a certain value when the cells are brought back to the RPT 6, indicating that the capacity loss is not completely irreversible; rather, it could be recovered by higher temperature activation.”
    Quote in the paperSubstantial claim

  • May combine two claims.

    Interpretationown data

    The IC peaks shift toward lower voltages and DV peaks show no change, suggesting an increase in internal resistance.

    “In general, the IC peaks shift toward lower voltages and no change for DV peaks suggesting an increase in internal resistance.”
    Quote in the paperSubstantial claim

  • May combine two claims.

    Interpretationreasoning

    The reversible capacity loss is caused by the loss of either lithium inventory or electrode active material.

    “Thus, it can be concluded that the reversible capacity loss is caused by the loss of either lithium inventory or electrode active material.”
    Quote in the paperSubstantial claim

  • May combine two claims.

    Interpretationown data

    Under low-temperature cycling, a lower discharge rate has a more harmful effect not only on capacity but also on power capability.

    “These results suggest that under low-temperature cycling, a lower discharge rate has a more harmful effect not only on the capacity but also on the power capability.”
    Quote in the paperSubstantial claim

  • May combine two claims.

    Interpretationreasoning

    The voltage rebound at 2 C is caused by self-heating: high initial internal resistance at low temperature generates heat, raising temperature, improving reaction rate and reducing resistance.

    “Since the high initial internal resistance at low temperature, most heat is generated by battery, which helps to raise its temperature.This selfheating effect can improve the reaction rate and reduce the resistance, leading to a voltage rebound.”
    Quote in the paperSubstantial claim

  • Probably not a substantial claim: may not pass S3 (load-bearing).

    Premisecitation

    LAM is attributed to material dissolution, particle isolation, and structural transformations.

    “LAM is attributed to the material dissolution, particle isolation, and structural transformations.26”
    Quote in the paperNot a substantial claim0 of 1 sources checked
    • cites [26]

      Couldn’t be matched to a paper in Crossref, so it can’t be checked.

  • Probably not a substantial claim: may not pass S3 (load-bearing).

    Premisecitation

    The poor performance of LIBs at low temperature can be attributed to several factors such as low ionic conductivity of electrolyte, limited solid-state diffusivity of Li-ion, and increased interfacial charge-transfer resistance.

    “The poor performance of LIBs at low temperature can be attributed to several factors such as the low ionic conductivity of electrolyte, 12 limited solid-state diffusivity of Li-ion, 13 and increased interfacial chargetransfer resistance.14,15”
    Quote in the paperNot a substantial claim0 of 4 sources checked
    • cites [12]

      Couldn’t be matched to a paper in Crossref, so it can’t be checked.

    • cites [13]

      Couldn’t be matched to a paper in Crossref, so it can’t be checked.

    • cites [14]

      Couldn’t be matched to a paper in Crossref, so it can’t be checked.

    • cites [15]

      Couldn’t be matched to a paper in Crossref, so it can’t be checked.

  • Probably not a substantial claim: may not pass S3 (load-bearing).

    Premisecitation

    The IC-DV method has been widely used to investigate the degradation mechanisms of LIBs with high fidelity and availability.

    “Recently, the IC-DV method has been widely used to investigate the degradation mechanisms of LIBs with high fidelity and availability.33,34”
    Quote in the paperNot a substantial claim0 of 2 sources checked
    • cites [33]

      Couldn’t be matched to a paper in Crossref, so it can’t be checked.

    • cites [34]

      Couldn’t be matched to a paper in Crossref, so it can’t be checked.

  • Probably not a substantial claim: may not pass S3 (load-bearing). May combine two claims.

    Premisecitation

    The state of health (SOH) is determined by the discharge capacity of an aged cell compared to its initial value, and a SOH < 80% is commonly used to represent the end of life of cells.

    “In the light of the USABC testing procedures, the state of health (SOH) is determined by the discharge capacity of an aged cell compared to its initial value, and a SOH < 80% is commonly used to represent the end of life of cells.39”
    Quote in the paperNot a substantial claim0 of 1 sources checked
    • cites [39]

      Couldn’t be matched to a paper in Crossref, so it can’t be checked.

  • Probably not a substantial claim: may not pass S3 (load-bearing).

    Study design and conductnone given

    The battery testing system had current and voltage accuracy of ±0.1%.

    “The charge and discharge processes are controlled by the computer connected to a battery testing system (CT-4008, Shenzhen Neware Electronics Co., Ltd., China), current and voltage accuracy of which are ±0.1%.”
    Quote in the paperNot a substantial claim

  • Probably not a substantial claim: may not pass S3 (load-bearing). May combine two claims.

    Study design and conductnone given

    Only the surface temperature is measured, and there can be a radial discrepancy between the surface and internal temperatures.

    “It should be noted that only the surface temperature is measured here and there can be a radial discrepancy between the surface and internal temperatures.”
    Quote in the paperNot a substantial claim

  • Classified as probably not a substantial claim.

    Premisecitation

    Lithium plating is more likely to happen during the charging process because of the low lithiation potential of anode.

    “Therefore, lithium plating is more likely to happen during the charging process because of the low lithiation potential of anode.22,23”
    Quote in the paperSubstantial claim0 of 2 sources checked
    • cites [22]

      Couldn’t be matched to a paper in Crossref, so it can’t be checked.

    • cites [23]

      Couldn’t be matched to a paper in Crossref, so it can’t be checked.

  • Probably not a substantial claim: may not pass S3 (load-bearing).

    Premisecitation

    The acknowledged degradation mechanisms can be grouped into three modes: increase of resistance, loss of active materials (LAM), and loss of lithium inventory (LLI).

    “In general, the acknowledged degradation mechanisms can be grouped into three modes: the increase of resistance, loss of active materials (LAM), and loss of lithium inventory (LLI).25”
    Quote in the paperNot a substantial claim0 of 1 sources checked
    • cites [25]

      Couldn’t be matched to a paper in Crossref, so it can’t be checked.

  • Probably not a substantial claim: may not pass S3 (load-bearing).

    Premisecitation

    The SOC window can be used to understand the degradation.

    “According to previous research, 20 the SOC window can be used to understand the degradation.”
    Quote in the paperNot a substantial claim0 of 1 sources checked
    • cites [20]

      Couldn’t be matched to a paper in Crossref, so it can’t be checked.

  • Classified as probably not a substantial claim.

    Study design and conductnone given

    All cells were cycled and characterized in a temperature and humidity programmable chamber to assure constant temperature conditions.

    “All cells are cycled and characterized in a temperature and humidity programmable chamber (BTH-150C, DongGuan Bell Experiment Equipment Co., Ltd., China) in order to assure constant temperature conditions.”
    Quote in the paperSubstantial claim

  • Classified as probably not a substantial claim.

    Study design and conductnone given

    Three cells were put into the chamber at -10°C for 3 hours to reach thermal equilibrium before cycling.

    “Three cells were firstly put into the chamber at -10°C for 3 hours to reach thermal equilibrium.”
    Quote in the paperSubstantial claim

  • Classified as probably not a substantial claim.

    Premisecitation

    Under low-temperature condition, lithium plating was highly responsible for the performance degradation of LIBs.

    “It has been found that under low-temperature condition, lithium plating was highly responsible for the performance degradation of LIBs.21”
    Quote in the paperSubstantial claim0 of 1 sources checked
    • cites [21]

      Couldn’t be matched to a paper in Crossref, so it can’t be checked.

  • Classified as probably not a substantial claim.

    Premisereasoning

    It is still unclear how the low-temperature cycling performance and corresponding degradation mechanisms depend on the discharge profile.

    “However, it is still unclear how the lowtemperature cycling performance and corresponding degradation mechanisms depend on the discharge profile.This is the main purpose of this study.”
    Quote in the paperSubstantial claim0 of 2 sources checked
    • cites [22]

      Couldn’t be matched to a paper in Crossref, so it can’t be checked.

    • cites [24]

      Couldn’t be matched to a paper in Crossref, so it can’t be checked.

28 of 28

  • The authors state this as an assumption.

    The inherent capacity of the reference performance test (RPT) is the same as the following first low-temperature cycle.

    “It is assumed that the inherent capacity of RPT is the same as the following first low-temperature cycle.”
1 of 1

Self-check

Percentages, sums and reported differences re-computed from the paper’s own numbers.

Each contradiction between two passages listed here was confirmed by an independent check.

  • Figure 7 panel range differs between text and caption

    Minor

    The text says the SOC windows are shown in panels B through D, but the Figure 7 caption identifies only panels B through C.

1 of 1

Cites

Flagged first, then by citations

Research works printed but not linked: 1

  1. Balewski KB, 1967, J.P. a new method for the study of the electrochemical reactivity of manganese dioxide, Electr Technol, 5, 527

Cited by

Sorted by citations

Related

Authors
Wu, W., Wu, W., Qiu, X., & Wang, S.
Affiliations
South China University of Technology (CN)
Corresponding author
Wang, Shuangfeng
ORCID
Venue
International Journal of Energy Research
Publisher
Wiley
Published
2018-10-18
Volume
43
Issue
1
Pages
243-253
ISSN
  • 0363-907X (ISSN-L)
  • 1099-114X
DOI
10.1002/er.4257
OpenAlex
W2896248624
Semantic Scholar
c35c7dd6c83ecc3842c9c9f85d8aed9638c4ec4c
Cited by
108
References
49
Citations by year
2026: 6 · 2025: 21 · 2024: 13 · 2023: 12 · 2022: 20 · 2021: 14 · 2020: 11 · 2019: 11
FWCI
4.74
Type
journal article
Language
en
Open access
Licence
Locations
International Journal of Energy Research (publishedVersion)
Funders
National Natural Science Foundation of China (51536003)
Topics
  • Physical Sciences › Engineering › Automotive Engineering › Advanced Battery Technologies Research
  • Physical Sciences › Engineering › Electrical and Electronic Engineering › Advancements in Battery Materials
  • Physical Sciences › Engineering › Mechanical Engineering › Extraction and Separation Processes
Keywords
lithium-ion batteries, low-temperature cycling, reversible capacity loss, battery aging mechanisms, discharge rate, degradation modes, lithium inventory loss, active material loss, lithium plating, incremental capacity analysis, differential voltage analysis, charging temperature

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