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ISSN : 1226-0088(Print)
ISSN : 2288-7253(Online)
Membrane Journal Vol.34 No.5 pp.253-261
DOI : https://doi.org/10.14579/MEMBRANE_JOURNAL.2024.34.5.253

FeCO3/rGO Composites Prepared by CO2 Capture and Carbonate Conversion: Anode Material in Lithium-Ion Batteries with Enhanced Performance

Sanglim Lee*, Gahwi Gu*, Daeung Park*, Hwiyun Im*, Yongjae Lee*, Junseok Moon*, Weonho Shin**, Hiesang Sohn*†
*Department of Chemical Engineering, Kwangwoon University, Seoul 01897, Republic of Korea
**Department of Electronic Material Engineering, Kwangwoon University, Seoul 01897, Republic of Korea

1 The authors equally contributed to this work.


†Corresponding author(e-mail: sonisang@hanmail.net; http://orcid.org/0000-0002-4164-9397)
September 30, 2024 ; October 15, 2024 ; October 15, 2024

Abstract


Carbon capture, utilization, and storage (CCUS) technology is gaining attention as a key strategy for achieving carbon neutrality. In this study, CO2 was permanently fixed as carbonate through mineral carbonation and applied as an anode material for lithium-ion batteries (LIBs). Such a fixed carbonate by CO2 was used for the preparation of FeCO3 composited with rGO and PVP to be applied as active material for negative electrode in LIBs. Specifically, the rGO plays an important role to increase electrical conductivity and prevent particle aggregation while PVP could stabilize the particle surface and strengthened structural stability as a surfactant. Electrochemical tests showed that the LIB anode material based on FeCO3/rGO composite maintained a capacity of 400 mAh/g after 50 cycles at a current density of 1,620 mA/g. This study suggests the converting CO2 into valuable battery materials can contribute to future energy storage technologies.


lithium ion battery , CO2 capture , FeCO3 , anode , rGO

이산화탄소 포집 및 탄산염 전환 통해 제조된 FeCO3/rGO 복합체: 리튬이온 전지향 고성능 음극재

이상림*, 구가휘*, 박대웅*, 임휘윤*, 이용재*, 문준석*, 신원호**, 손희상*†
*광운대학교 화학공학과
**광운대학교 전자재료공학과

초록


탄소중립을 달성하기 위해 이산화탄소를 포집, 활용, 저장하는 CCUS(carbon capture, utilization, and storage) 기술이 주목받고 있다. 본 연구에서는 광물 탄산화 공정을 통해 이산화탄소를 탄산염으로 고정하고, 이를 전이금속 탄산염 기반 리튬이온배터리(LIB) 음극재로 적용하였다. CO2를 탄산염으로 고정후, 이를 이용해 FeCO3를 제작하고, rGO와 PVP와 복합화하여 음극활물질에 적용하였다. rGO는 전기전도도를 높이고 입자의 응집을 방지해 부피 팽창을 완화했으며, PVP는 계면활성제로서 입자 표면을 안정화하여 구조적 안정성을 강화하였다. FeCO3-PVP-rGO 복합체 기반한 음극재에 대한 전기화학 테스트를 진행한 결과, FeCO3/rGO 복합체는 1,620 mA/g의 전류 밀도에서 50 사이클 이후에도 400 mAh/g의 용량을 유지하였다. 본 연구는 CO2를 고부가가치 배터리 소재로 전환하여 차세대 에너지 저장 기술에 기여할 가능성을 시사한다.


    1. Introduction

    The drastic climate change and environmental pollution have become globally significant issue[1-3]. Carbon dioxide (CO2) emissions from industrial processes have been identified as one of the major causes of global warming[4-5]. Therefore, it is crucial to develop technologies that can capture and convert CO2 into useful substances. carbon capture and utilization (CCU) and carbon capture, utilization, and storage (CCUS) technologies have gained attention for storing CO2 in a stabilized form by converting it into useful materials. Specifically, mineral carbonation technology is an effective method to convert CO2 into chemically stable storage form of carbonates with high environmental safety[6-9].

    Graphite, the conventional anode material for lithium- ion batteries (LIBs), has a limited energy density due to its low theoretical capacity of 372 mAh/g, facing to be changed with alternative anode material with high capacity including metal oxide, Si and lithium [10-20]. Among them, transition metal carbonates have been highlighted as the potential alternative anode to significantly improve LIB performance due to their high reversible capacity. However, the existing transition metal carbonate anodes failed to be commercialized due to its low electrical conductivity and volume expansion, hindering their practical application towards LIB anode with high electrochemical performance[21-23].

    In this regards, iron carbonate (FeCO3) is an appropriate transition metal carbonate for LIB anode. Specifically, FeCO3 is low-cost and non-toxic material which can be prepared by CO2 conversion. However, the practical application of iron carbonate towards LIB anode is limited by its poor electrochemical performance due to low electrical conductivity and volume expansion of FeCO3[24-26].

    In this study, we report a novel CCUS technology including mineral carbonation of CO2 to be utilized as LIB anode material through simple and facile process. Briefly, we first prepare FeCO3 by serial process of CO2 capture and sodium carbonate conversion followed by metathesis. For the enhancement of conductivity and volume expansion of FeCO3, a composite of reduced graphene oxide (rGO) and polyvinylpyrrolidone (PVP) and FeCO3 was prepared through hydrothermal process and high temperature sintering. The material and electrochemical properties of the synthesized nanocomposites were analyzed to evaluate the applicability of nanocomposite towards LIB anode.

    2. Experimental

    2.1. Materials

    Sodium hydroxide (NaOH, 99.5%), sodium chloride (NaCl, 99.0%), L-ascorbic acid (C6H8O6, AA, 99.0%), ethylene gylcol (EG, 99.5%), hydrochloric acid (HCl, 35.0%), sulfuric acid (H2SO4, 95.0%), potassium permanganate (KMnO4 99.3%), hydrogen peroxide (H2O2, 30.0%) were purchased from Duksan Chemical. Iron(III) chloride hexahydrate (FeCl3 6H2O, 99.0%), graphite (99%), phosphoric acid (H3PO4, 85.0%), ethyl ether (99.0%) were purchased from Daejung chemical. All materials were used as-received for synthesis without further purification.

    2.2. Synthesis of sodium carbonate through mineral carbonation

    The sodium carbonate was prepared through carbonation and low-temperature crystallization with 2M NaOH under a constant temperature (35°C). The initial pH of the NaOH solution was approximately 14 while CO2 (95 vol.%, 200 cc/min) was then injected into the NaOH solution until the pH of solution reached to 11. After the CO2 injection, the reactor temperature was lowered to 10°C for the facilitated CO2 conversion into bicarbonate and carbonate ions. The injection of CO2 was continued for the crystallization at 2°C until the pH of the mixture reached to 7. After the crystallization, the white precipitate was formed in the solution and was separated through filtration.

    The overall chemical reaction for Na2CO3 formation can be described as follows:

    Initial reaction with NaOH to form sodium bicarbonate:

    NaOH + CO 2 → NaHCO 3
    (1)

    Further reaction of sodium bicarbonate with NaOH to form sodium carbonate:

    NaHCO 3 + NaOH → Na 2 CO 3   +   H 2 O
    (2)

    In this experiment, 10.2 g of CO2 was injected into the NaOH solution, leading to the formation of 8.1 g of Na2CO3. Considering the molar weights of CO2 and Na2CO3, and assuming a 1:1 molar conversion ratio, the theoretical Na2CO3 yield was calculated. The actual yield achieved, 8.1 g, corresponds to a percentage yield of approximately 32.9%. These data provide a quantitative measure of the CO2 conversion efficiency under these experimental conditions and indicate that around 1.26 g of CO2 is required to produce 1 g of Na2CO3.

    2.3. Synthesis of FeCO3/rGO composite

    For the preparation of FeCO3/rGO composite, the previously synthesized sodium carbonate was used as a carbonate precursor to be mixed with graphene oxide. Specifically, graphene oxide (GO) dispersed in the distilled water was mixed with the solution of FeCl3 in an ethylene glycol (EG)-water mixture (1:1 volume ratio). Then, ascorbic acid (AA) and polyvinylpyrrolidone (PVP) were subsequently added to the mixed solution of GO and FeCl3 for the preparation of precursor for the subsequent hydrothermal synthesis. The as-prepared precursor was transferred to a teflon-lined autoclave to be synthesized as FeCO3/GO composite at 180°C for 12 hours. In the end, FeCO3/rGO composite can be prepared by high temperature reduction by sintering at 500°C for 4 hours under a nitrogen (N2) atmosphere.

    2.4. Material characterization

    The crystal structure and chemical composition of the sodium compound, FeCO3, and FeCO3/rGO composite were characterized with physical and chemical analytical instruments. The crystal structure of the material was analyzed by X-ray diffractometer (XRD, Rigaku) at a 2θ range of 20~60° using CuKα (= 0.154059 nm) as radiation source. Surface chemical functionality (chemical bonds and molecular vibrations) for materials were analyzed mounted on ZnSe crystal at a wavenumber range of 750~2500 nm with Fourier Transform Infrared Spectroscopy (FT-IR, JASCO). The morphological information of the materials were obtained with Scanning Electron Microscopy (FE-SEM, Hitachi) using a secondary electron detector (SE) under an acceleration voltage of 5 kV and a working distance of 8 mm.

    2.5. Electrochemical characterization

    The electrochemical properties of the material was characterized by analyzing their symmetric cell performance and electrochemical impedance spectroscopy (EIS). The cell electrodes was prepared with pasted slurry mixtures of the active material, Super P, and PVDF at 7:2:1 on the Cu foil. The as-prepared cell electrode was then cut into discs and assembled to coin type electrochemical cells containing lithium foil, separator (celgard 2400), and electrolytes (1 mol/L LiPF6 in ethylene carbonate (EC)/dimethyl carbonate (DMC)). Galvanostatic cycling tests were conducted using a battery tester (WBCS3000, Wonatech) system over the voltage range of 0.01~3.0 V. Electrochemical impedance spectroscopy (EIS) was performed in the frequency range 100 kHz to 0.1 Hz with a potentiostat.

    3. Results and Discussion

    3.1. Material characterization

    Fig. 1. displays the crystal structure of FeCO3 and FeCO3/rGO composite. All the peaks of the samples can be indexed into rhombohedral FeCO3 (R3c space group, PDF Card No.: 5000036). Different from the characteristic peaks of FeCO3, a weak and broad band of FeCO3/rGO suggests the presence of rGO due to the decreased crystallinity and a reduced grain size of FeCO3[28]. As-calcuated grain sizes for FeCO3 and FeCO3/rGO are estimated to be 7.82 and 2.31 nm, respectively, attributing to the suppressed aggregation of FeCO3 nanoparticles uniformly distributed on the rGO nanosheets[29].

    Fig. 2 shows the FT-IR spectra of Na2CO3 prepared by CO2 capturing and FeCO3 synthesized using Na2CO3 as a carbonate precursor. As shown in the FT-IR spectra, strong absorption peaks at 1,390 cm-1 and 880 cm-1 observed in Na2CO3, indicates the stretching and bending vibrations of CO32-, indicating the successful carbonate ions formation of Na2CO3 [13]. Similarly, strong absorption peaks at 1,420 cm-1 and 892 cm-1 observed in FeCO3 can be assigned to CO32-, indicating the carbonate ions formed in FeCO3, similarly with that of Na2CO3[19]. As demonstrated in the chemical functionality of materials, the successful CO2 capturing have been performed through the effective storage as carbonate form and subsequently converted to FeCO3[30].

    As displayed in the Fig. 3, the morphological structure of as-synthesized FeCO3 and FeCO3/rGO composite were analyzed with scanning electron microscopy (SEM). As shown in Fig. 3a, as-synthesized FeCO3 microparticles by the solvothermal process are visible to have an irregular shape with the size of ca. 5~7 μm. As for the morphology for the rGO/FeCO3 composite (Fig. 3b), as-formed FeCO3 nanoparticles are observed as particles homogeneous distributed on rGO nanosheet with a mitigated size of 500~800 nm [31]. Such the different size and morphology of FeCO3/rGO composite from that of FeCO3 is attributed to the controlled growth of FeCO3 nanoparticles in the rGO based composite matrix[15].

    3.2. Electrochemical analysis

    Fig. 4 compares the electrochemical properties for FeCO3 and FeCO3/rGO composite as the anode for lithium ion battery, As displayed in voltage profiles (Fig.s 4(a) and 4(b)) for charge/discharge at various cycles (1st, 2nd, 10th, and 50th cycles) at 1.62 A/g and 0.01 to 3 V, the large irreversible capacity losses are observed for FeCO3 (1,325 mAh/g→747 mAh/g) and the FeCO3/rGO composite (1,490 mAh/g→908 mAh/g) at the initial and second cycles due to the solid electrolyte interface (SEI) film formation and and the degradation by the irreversible electrolyte/electrode reactions[11-18]. As-formed SEI and irreversible reactions reduce the available capacity for subsequent cycles by consumption of lithium ions[32]. Specifically, the declined plateaus are observed in the first discharge for the FeCO3 (from 0.71 V to 0.43 V) and for the FeCO3/rGO composite (from 0.78 V to 0.53 V) attributed to the iron reduction (Fe²⁺ to metallic Fe⁰), and carbon reduction (C4+ to C0)[32]. As shown in the voltage profiles, the plateau curve above 0.5 V indicates the SEI layer formation in the composite[33]. Note that, the diminished plateau with stabilized voltage profile after 10 cycles suggests the reversible elec-trochemical reactions leading to the improved longterm cycle stability[34-35]. Furthermore, although the charge/discharge profiles show gradually decreased capacity at the elongated cycles (10th and 50th cycles) for both FeCO3 and FeCO3/rGO composites, FeCO3/rGO composite displays much improved electrochemical performance compared to that of FeCO3. Specifically, FeCO3/rGO composite shows 557 mAh/g in the 10th cycle while the pristine FeCO3 exhibits a capacity reduction to 159 mAh/g at the identical condition, indicating the more stabilized SEI layer and the reduced irreversible reactions of FeCO3/rGO composite without continuous consumption of lithium ions [15-19]. Note that, FeCO3/rGO composite shows the retained capacity (396 mAh/g) at elongated cycle (50th cycle) superior to that of FeCO3 (103 mAh/g) at identical condition. Such the better capacity retention (cycle stability) of FeCO3/rGO composite than that of pristine FeCO3 indicates the mitigated structure degradation of FeCO3 in the rGO composite due to structural stability and enhanced electronic conductivity by rGO nanosheet[17].

    Fig. 4(c) compares the electrochemical performance (cycling stability and capacity) of FeCO3 and FeCO3/ rGO composite. The FeCO3/rGO nanocomposite exhibited the retained capacity (ca. 395 mAh/g) after 50 cycles, much superior to that of pristine FeCO3 (95 mAh/g) at identical condition. Such the significantly improved performance (cycle stability and capacity retention) of the FeCO3/rGO composite suggests effectively alleviated strain induced from FeCO3 volume change and enhanced conducitivity of composite by introduction of rGO in to composite.

    As displayed in Fig. 4(d), the resistance of the samples were compared with electrochemical impedance spectroscopy (EIS) analyses. The semicircle observed in high-frequency corresponds to the charge- transfer resistance (Rct). As displayed in the EIS results, FeCO3/rGO composite exhibit much lower resistance (Rct, 93.09 Ω) than that of bare FeCO3 (121.62 Ω), indicating facilitated charge transfer and improved ion mobility in the composite electrode[35].

    4. Conclusion

    In this study, we demonstrated a composite of FeCO3 and rGO by carbonate based CO2 capture/conversion and subsequent metathesis into FeCO3 and rGO compositing to be applied as an anode material for LIBs.

    As-prepared composite of FeCO3 and rGO exhibited a superior electrochemical performance (retained cycle stability and capacity (400 mAh/g) after 50 cycles at 1.62 A/g) as LIB anode to that of pristine FeCO3 based LIB anode (95 mAh/g) under the same test condition by overcoming the limitations of conventional transition metal carbonate anodes with the enhanced conductivity and alleviated strain of composite via introduction of rGO nanosheets. In addition, the FeCO3/ rGO composite exhibited a lower charge transfer resistance (Rct) of 93.1 Ω than that for bare FeCO3 (121.6 Ω), suggesting enhanced electron mobility and ionic conductivity of our composite.

    As-demonstrated in this report, our study highlights the potential of wasted CO2 utilization to address environmental issues (carbon neutrality) by CO2 conversion into high-valued LIB materials[34].

    Acknowledgement

    This work was supported by Korea Electric Power Corporation (KEPCO) (Grant Number: R22XO05-09) and an NRF grant funded by the Ministry of Science and ICT (MSIT) of Korea (grant number NRF-RS- 2023-0022 2124).

    Figures

    MEMBRANE_JOURNAL-34-5-253_F1.gif

    Crystal structure analyses: XRD patterns of FeCO3 and FeCO3/rGO composite.

    MEMBRANE_JOURNAL-34-5-253_F2.gif

    Surface chemical functionality analyses: FT-IR spectra of sodium carbonate (Na2CO3) and iron carbonate (FeCO3) synthesized via mineral carbonation.

    MEMBRANE_JOURNAL-34-5-253_F3.gif

    Morphological analyses: SEM images of (a) FeCO3 microparticles and (b) FeCO3/rGO nanocomposites.

    MEMBRANE_JOURNAL-34-5-253_F4.gif

    Discharge/charge voltage profiles: (a) FeCO3 (b) FeCO3/rGO composite; (c) Cycling performance of FeCO3 and FeCO3/rGO composite; (d) EIS curves of FeCO3 and FeCO3/rGO composite.

    Tables

    Comparison of Anode Materials

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