Citation: Shi-Sheng HOU, Ze-Tong XU, You-Kai ZHANG, Kui XIE, Li-Zhen GAN. Enhanced CO2 Electrolysis with Mn-doped SrFeO3-δ Cathode[J]. Chinese Journal of Structural Chemistry, ;2020, 39(9): 1662-1668. doi: 10.14102/j.cnki.0254-5861.2011-2672 shu

Enhanced CO2 Electrolysis with Mn-doped SrFeO3-δ Cathode

  • Corresponding author: Li-Zhen GAN, lzgan@fafu.edu.cn
  • Received Date: 20 November 2019
    Accepted Date: 8 February 2020

    Fund Project: the National Natural Science Foundation of China 21902025the National Natural Science Foundation of China 91845202the National Natural Science Foundation of China 21750110433Innovative Project of the Education Department of Fujian Province JAT170174Natural Science Foundation of Fujian Province 2018J05012Dalian National Laboratory for Clean Energy DNL180404Strategic Priority Research Program of Chinese Academy of Sciences XDB2000000

Figures(6)

  • Solid oxide carbon dioxide electrolysers are expected to play a key role in carbon-neutral energy landscape. However, the limited activity of traditional ceramic cathodes still restricts the electrochemical performance. Here we report the doping of Mn at the B site of SrFeO3-δ cathode to improve CO2 electrolysis. The oxygen vacancy concentration is increased by ~30% with Mn doping while the surface oxygen exchange coefficients are enhanced by ~10 times. The chemisorption of CO2 indicates the presence of chemical intermediate state between CO2 molecule and carbonate ion on the oxygen-deficient cathode surface which therefore leads to the desorption temperature of ~800 ℃. The Mn-doped SrFeO3-δ enhances CO2 electrolysis with no performance degradation being observed even after high-temperature operation of 100 hours.
  • Solid oxide electrolysers have demonstrated tremendous benefits of using renewable electricity to efficiently convert CO2 into fuel[1-3]. The high operation temperature delivers enhanced dynamic and thermodynamic advantages. By applying an external potential, CO2 can be directly electrolyzed into CO and O2 in an oxygen-ion-conducting solid oxide electrolyser[4-7].

    Traditional Ni-YSZ composite electrode has been widely used for CO2 electrolysis; however, the inherent oxidation-reduction instability of Ni–YSZ limits its application when performing direct CO2 electrolysis without reducing gas atmosphere[8-12]. It is reported that CO2 electrolysis using perovskite ceramics electrodes would be highly promising[13]. Perovskite oxide electrode materials have been therefore extensively studied[14, 15], which is due to that perovskite oxides are very good parent materials for tailoring chemical composition through the control of element doping in A and B sites. And some of them have shown long-term stability, carbon deposition resistance, sulfur poisoning resistance and excellent transport properties.

    The ABO3-type perovskite oxide could provide layered lattice structure that has huge potential for the cation doping strategy for the development of new electrode materials[16]. Perovskite SrFeO3-δ oxide has been intensively studied as the cathode of solid oxide fuel cells and they have shown good electrochemical performance[17-19]. SrFeO3-δ oxide is a typical conductor while it still demonstrates high conductivity in reducing atmosphere[20]. As a cathode, it has been proven to be effective for steam electrolysis in a solid oxide electrolyser. Enhancing the concentration of oxygen vacancy with dopant would be highly favourable to improve electrode activity. In this case, oxygen defects would not only improve the transport properties but also facilitate the chemisorption of CO2 on oxide surfaces at high temperature.

    In this work, we dope Mn into the B-site of SrFeO3-δ lattice to increase oxygen vacancy concentration towards CO2 electrolysis. The electrical properties and surface oxygen exchange coefficient of the materials are investigated. We perform CO2 electrolysis with Mn-doped cathode.

    SrFeO3-δ and SrFe0.85Mn0.15O3-δ are synthesized by a solid state reaction method with heat treatment at 1300 ℃[21, 22]. Reduced samples are prepared by treating the samples in 5%H2/Ar at 800~1000 ℃ for 3~5 hours. La0.9Sr0.1Ga0.8-Mg0.2O3-δ (LSGM) electrolyte powders are prepared using a solid state reaction method with heat treatment at 1000 ℃. (La0.8Sr0.2)0.95MnO3-δ (LSM) and Ce0.8Sm0.2O2-δ (SDC) powders are synthesized using a glycine-nitrate combustion method[23, 24]. The phase formation of powder samples is analyzed using X-ray diffraction (D/MAX2500V). About 2.0 g of SrFeO3-δ or SrFe0.85Mn0.15O3-δ powder is pressed into a bar and sintered at 1300 ℃ for 6 h in air for conductivity test using a DC four-terminal method (Keithley 2000)[25]. Electrical conductivity relaxation (ECR) method is used to test the surface oxygen exchange coefficient with oxygen partial pressure shifting between 10-18 and 10-12 atm at 800 ℃[26, 27]. In our work, we use the atmospheres of CO/CO2 by changing the ratio between CO and CO2 to get the two different oxygen partial pressures.

    LSGM electrolyte is prepared by pressing the powder sample and sintered at 1500 ℃ for 10 hours in air. SrFeO3-δ/SDC and SrFe0.85Mn0.15O3-δ/SDC slurries are prepared by milling the SrFeO3-δ or SrFe0.85Mn0.15O3-δ with SDC at a weight ratio of 65:35 in alpha-terpineol with suitable cellulose additive. Single cells are assembled using screen printing method and then heat-treated at 1100 ℃. The microstructures of single cells are observed using a scanning electron microscope (SEM, JEOL Ltd). Electrochemical measurement of CO2 electrolysis is recorded using an electrochemical station (IM6, Zahner, Germany). Pure CO2 (50 mL·min-1) is fed to cathode while the anode is exposed to air. The generation of CO is analyzed using an online gas chromatograph (GC2014, Shimazu).

    Fig. 1a and 1b present the XRD patterns of the powder samples in oxidized and reduced states, respectively. The SrFeO3-δ is in a tetragonal phase while the Mn-doped SrFe0.85Mn0.15O3-δ in a cubic phase. After reduction, a phase transition to orthorhombic phase is observed both for SrFeO3-δ and SrFe0.85Mn0.15O3-δ[28]. We therefore obtain Sr2Fe2O5 phase which is the active phase for CO2 electrolysis at high temperature. The doping of Mn changes the cell parameters as confirmed by the shift of diffraction peaks. As shown in Table 1, we use iodometric method[24, 29] to analyze the oxygen nonstoichiometry of SrFeO3-δ and SrFe0.85Mn0.15O3-δ in oxidized and reduced states, respectively. The oxygen deficiency is 0.2880 for SrFeO3-δ while it is enhanced to 0.3386 for SrFe0.85Mn0.15O3-δ through doping of Mn in lattice.

    Figure 1

    Figure 1.  XRD patterns of (a) oxidized forms of samples and (b) reduced forms of samples

    Table 1

    Table 1.  Oxygen Deficiency in Oxidized and Reduced Samples
    DownLoad: CSV
    Chemical formula Oxidized (3-δ) Chemical formula Reduced (5-δ)/2 Oxygen loss
    SrFeO3-δ 2.7227 Sr2Fe2O5-δ 2.4347 0.2880
    SrFe0.85Mn0.15O3-δ 2.6375 Sr2Fe0.17Mn0.3O5-δ 2.2989 0.3386
    The oxygen nonstoichiometry is determined using iodometric titration.

    Fig. 2a shows the conductivity of sintered samples in the temperature range of 200 to 800 ℃ in 5%H2/Ar. The SrFeO3-δ and SrFe0.85Mn0.15O3-δ samples show typical p-type conduction in air with conductivity reaching ~8 S·cm-1 at 800 ℃. In reducing atmosphere, the conductivity of the two samples both gradually decreases and finally reaches ~1 S·cm-1. Fig. 2b shows that the doping of Mn significantly reduces the re-equilibrium time in the ECR tests. The conductivity shifts from ~0.6 to 1.6 S·cm-1 for SrFe0.85Mn0.15O3-δ while the conductivity shifts from ~1.2 to 2.2 S·cm-1 for the SrFe0.85Mn0.15O3-δ during the conductivity relaxation test. The doping of Mn leads to the increase of oxygen vacancy, which accordingly decreases the concentration of charge carrier of hole and thereby reduces the mixed conductivity. The surface exchange coefficient, k value, of the SrFe0.85Mn0.15O3-δ samples is enhanced by ~10 times to 3.5 × 10-3 cm·s-1 in contrast to 4.7 × 10-4 cm·s-1 for SrFeO3-δ. The increase of oxygen vacancy is favorable to the enhancement of surface oxygen exchange process that is extremely important to electrode activity.

    Figure 2

    Figure 2.  (a) Conductivities of different samples in 5%H2/Ar ranging from 200 to 800 ℃; (b) Surface oxygen exchange coefficients of the two samples with oxygen partial pressure shifting between 10-12 and 10-18 atm

    Fig. 3a shows FT-IR spectrum of the CO2 chemisorption on reduced SrFe0.85Mn0.15O3-δ sample at 800 ℃. The band at 2270~2400 cm-1 is associated with CO2 molecule while the wave number at 1440~1600 cm-1 represents the presence of CO32- on sample surface[6]. The chemisorbed CO2 is therefore supposed to be in an intermediate state between the molecular CO2 and carbonate ions. Fig. 3b shows the temperature programmed desorption of the samples in CO2 atmosphere. It is observed that the chemisorption takes place at ~800 ℃ which is normally close to the decomposition temperature of carbonates. And stronger desorption is observed for the Mn-doped sample which further validates the enhancement of CO2 chemisorption with increased oxygen vacancy concentration on oxide surfaces. We further correlate the desorption volume of CO2 with the surface areas of materials. The adsorption capacity of CO2 is 0.06 and 0.04 mL·mcatal2 for SrFe0.85Mn0.15O3-δ and SrFeO3-δ materials, respectively.

    Figure 3

    Figure 3.  (a) FT-IR spectroscopy of CO2 adsorbed on the reduced SrFe0.85Mn0.15O3-δ at 800 ℃. (b) Temperature programmed desorption of the two samples in CO2 atmosphere

    Direct electrolysis of pure CO2 is studied based on SrFeO3-δ and SrFe0.85Mn0.15O3-δ cathodes at 800 ℃. Fig. 4a shows the typical I-V curves of CO2 electrolysis with the two cathodes. For SrFe0.85Mn0.15O3-δ cathode, the current density reaches 0.53 A·cm-2 at 1.6 V which is much higher than 0.44 A·cm-2 based on the SrFeO3-δ cathode under same conditions. This indicates that the Mn-doped cathode enhances CO2 electrolysis through improving electrode activity including surface oxygen exchange process and chemisorption in composite cathode. Fig. 4b shows the short-term performance of CO2 electrolysis under different applied voltages, which further confirms the enhanced current densities with Mn-doped cathode. Fig. 4c and 4d show the production of CO and the Faradaic efficiency with the two cathodes. The production of CO reaches 2.25 mL·min-1·cm-2 for SrFe0.85Mn0.15O3-δ, which is ~20% higher than 1.92 mL·min-1·cm-2 for SrFeO3-δ at 1.5 V. The maximum current efficiency reaches 82.3% and 74.8% for SrFe0.85Mn0.15O3-δ and SrFeO3-δ cathodes at 1.1~1.5 V, respectively.

    Figure 4

    Figure 4.  (a) I-V curves, (b) Short-term performances, (c) CO production rate and (d) Current efficiency of CO2 electrolysis with SrFeO3-δ and SrFe0.85Mn0.15O3-δ cathodes at 800 ℃

    Fig. 5 presents the AC impedance of CO2 electrolysis recorded at 1.2~1.6 V. In general, the values of Rs are generally stable while the Rp values considerably decrease with the voltage increasing to 1.5 V. We observe the Rp values at 0.62 and 0.46 Ω·cm2 for SrFeO3-δ and SrFe0.85Mn0.15O3-δ cathodes at 1.5 V, respectively, which is comparable to the electrode activity of Sr2Fe1.6Mo0.5O6-δ for CO2 electrolysis[24]. The doping of Mn effectively improves electrode activity and therefore reduces the electrode polarization resistance. Fig. 6a shows the cell microstructure with a configuration of the SrFe0.85Mn0.15O3-δ/LSGM/(La0.8Sr0.2)0.95MnO3-δ, which presents the uniform porous electrode microstructure and very dense electrolyte support. Fig. 6b shows the long-term performance of CO2 electrolysis at 1.3 V at 800 ℃. No degradation is observed even after operation of 100 hours, which further indicates the good stability of the Mn-doped cathode.

    Figure 5

    Figure 5.  AC impedance for electrolysers based on (a) SrFeO3-δ and (b) SrFe0.85Mn0.15O3-δ at various voltages

    Figure 6

    Figure 6.  (a) Scanning electron microscopy of the single cell with SrFe0.85Mn0.15O3-δ cathode. (b) Long-term performance of CO2 electrolysis with SrFe0.85Mn0.15O3-δ at 800 ℃ under 1.3 V

    In this work, enhanced CO2 electrolysis is achieved with Mn-doped SrFe0.85Mn0.15O3-δ cathode. The doping of Mn increases the concentration of oxygen vacancy and surface oxygen exchange process, which therefore improves the electrode activity toward CO2 splitting. The increase of oxygen vacancy also facilitates the chemisorption of CO2 with the desorption temperature at ~800 ℃. We then demonstrate enhanced CO2 electrolysis with no degradation being observed even after high temperature operation of 100 hours.


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