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Article

Enhancement on PrBa0.5Sr0.5Co1.5Fe0.5O5 Electrocatalyst Performance in the Application of Zn-Air Battery

by
Chengcheng Wang
1,†,
Ziheng Zheng
1,†,
Zian Chen
1,
Xinlei Luo
1,
Bingxue Hou
2,
Mortaza Gholizadeh
3,
Xiang Gao
1,
Xincan Fan
1,* and
Zanxiong Tan
1,*
1
School of Entrepreneurship and Innovation, Shen Zhen Polytechnic, Shenzhen 518055, China
2
Aviation Engineering Institute, Civil Aviation Flight University of China, Guanghan 618037, China
3
Faculty of Chemical and Petroleum Engineering, University of Tabriz, Tabriz 51666, Iran
*
Authors to whom correspondence should be addressed.
†
These authors contributed equally to this work.
Catalysts 2022, 12(7), 800; https://doi.org/10.3390/catal12070800
Submission received: 23 June 2022 / Revised: 11 July 2022 / Accepted: 13 July 2022 / Published: 20 July 2022
(This article belongs to the Special Issue Pt-M (M = Ni,Co,Cu, etc.)/C Electrocatalysts)
Browse Figures
Review Reports Versions Notes

Abstract

:
Due to the insufficient stability and expensive price of commercial precious metal catalysts like Pt/C and IrO2, it is critical to study efficiently, stable oxygen reduction reaction as well as oxygen evolution reaction (ORR/OER) electrocatalysts of rechargeable Zn-air batteries. PrBa0.5Sr0.5Co1.5Fe0.5O5 (PBSCF) double perovskite was adopted due to its flexible electronic structure as well as higher electro catalytic activity. In this study, PBSCF was prepared by the citrate-EDTA method and the optimized amount of PBSCF-Pt/C composite was used as a potential ORR/OER bifunctional electrocatalyst in 0.1 M KOH. The optimized composite exhibited excellent OER intrinsic activity with an onset potential of 1.6 V and Tafel slope of 76 mV/dec under O2-saturated 0.1 M KOH. It also exhibited relatively competitive ORR activity with an onset potential of 0.9 V and half-wave potential of 0.78 V. Additionally, Zn–air battery with PBSCF composite catalyst showed relatively good stability. All these results illustrate that PBSCF-Pt/C composite is a promising bifunctional electrocatalyst for rechargeable Zn-air batteries.

1. Introduction

Nowadays, the increasing demand for safe, clean and renewable energy in society has inspired scientists to conduct extensive research on electrochemical energy storage and conversion technologies. Due to their rich resources, high specific energy density and the fact that it is environmentally benign, metal-air batteries have become the main research hotspots. Zn-air battery [1,2,3,4] is considered an efficient metal-air battery with a cheap price, good energy density and safety. However, its wide application is greatly restricted by the slow kinetics of ORR [5] and OER [6] due to complicated reduction, oxidation processes including breaking OH bonds and forming O=O bonds. Therefore, this greatly affects the efficiency and practicability of these electrochemical energy devices. Precious metal catalysts such as Pt/C, IrO2 etc. are widely adopted to achieve superior ORR and OER performance [6], but their high price and scarcity limit significantly their wide application in the energy devices. Moreover, they are quite unstable when being used in alkaline condition. Hence, it is urgent to develop a cheap, high-performing and stable electrocatalyst. Much more attention has been paid to prepare non-precious-metal ORR and OER electrocatalysts by using transition metal oxides and carbon-based electrocatalysts [7,8,9]. Transition metal oxides composites exhibiting high bifunctional ORR and OER activities have been extensively studied due to their easily tailoring surface properties as well as sufficient catalytic activity.
Among transition metal oxides composites, perovskites are one of the most suitable electrocatalysts due to their easy preparation method as well as tunable structure by adjusting A site or B site cations in the ABO3 compound [10,11,12,13]. Firstly, Suntivich et al. [14,15] prepared excellent OER perovskite electrocatalysts because of eg orbital of the transition metal. Ba0.5Sr0.5Co0.8Fe0.2O3−δ (BSCF) [14] exhibits higher OER compared to IrO2. However, BSCF is not stable after long-time operation due to the amorphous structure. There are many studies regarding the optimization of ORR and OER performances of perovskites by different site doping [16,17,18,19,20,21,22,23]. Our group [24] ever reported that La0.5Sr0.5Ni0.4Fe0.6O3−δ was a promising catalyst with high OER activity under alkaline condition; however, the long-term stability of the perovskite electrocatalysts was not extensively studied yet. SrCo0.95P0.05O3−δ (SCP) [18] perovskite electrocatalysts were studied by Yilong Zhu et al., who found that OER activity as well as the stability can be enhanced by doping with a certain amount of P element into B site. Recently, their group continuously investigated Sr(Co0.8Fe0.2)0.95P0.05O3−δ bifunctional electrocatalysts in Zn-air batteries. Their studies indicated that the optimized amount of Sr(Co0.8Fe0.2)0.95P0.05O3−δ-Pt composite can exhibit excellent ORR/OER activity [25]. In addition, they showed that the initial discharge potential was 1.25 V, while the charge potential was 2.02 V with excellent stability at 5 mA/cm2. Therefore, there are many ways to develop perovskite catalysts with better activity in the field of Zn-air batteries.
More attention is given to double perovskites due to the flexible electronic structure, defect introduction, surface modification, nanostructures as well as higher activity. Moreover, they were much cheaper than commercial precious metal electrocatalysts. NdBa0.5Sr0.5Co1.5Fe0.5O5 catalysts exhibited better activity and stability than single perovskite electrocatalysts [26]. Shao Z.P. et al. [27] also reported that Ba2CoMo0.5Nb0.5O6 was an active OER catalyst under alkaline conditions and it had excellent stability in an alkaline medium. In this study, PrBa0.5Sr0.5Co1.5Fe0.5O5 electrocatalysts were synthesized by the traditional EDTA-citrate method and evaluated as potential bifunctional ORR/OER electrode materials for aqueous rechargeable Zn-air battery under alkaline condition. It was also used in the solid Zn-air battery [28,29,30,31,32]. Additionally, the structure and electrochemical performance of PrBa0.5Sr0.5Co1.5Fe0.5O5 electrode were studied. This work not only represents the advancement direction in highly efficient bifunctional electrocatalysts, but also widens the application of these electrocatalysts in rechargeable metal-air batteries, especially solid Zn air batteries.

2. Results and Discussion

2.1. Phase as well as Microstructure Identification

Figure 1a shows the XRD pattern of PBSCF combusted at 1000 °C for 5 h with the double pervoskite phase, which was in accordance with other researchers’ reported results [16]. The main perovskite phase was similar to JCPDS card 46-0335. The minor peaks that appeared at 26°, 36° and 43° might referred to Sr2Fe2O5, which might need more investigations. According to the SEM image, PBSCF particles were mostly dispersing uniformly with a particle size of 100–200 nm, which was similar to TEM results as shown in Figure 1c. Interestingly, it is worth mentioning that there were some tiny particles observed in Figure 1b as well. EDX results showed that these particles were still mainly composed of PBSCF elements, and the peak intensity of Sr and Fe was more obvious, which might indicate that Sr-related compounds formed. This was similar to XRD results of minor peaks. The d-spacing of 0.297 nm was indexed to the (110) plane of perovskites The selected-area electron diffraction (SAED) pattern of nanoparticles was shown in Figure 1d, which demonstrated that PBSCF showed Debye Scherer rings, which confirms that it has a crystalline structure.
The oxidation states of PBSCF were evaluated by XPS to investigate the origin of the electrocatalytic activity. Figure 2a shows the survey scan of the catalysts for PBSCF electrocatalysts, indicating the presence of Ba, Sr, Co, Fe and O elements. Some unknown peaks might be due to contamination during the tests like Na, Cl and so on. Deconvoluted O 1s spectra is shown in Figure 2b. The peaks were divided into four individual species like surface adsorbed water species OH−, O−, and O2−. The relative amount of O− was related to the concentration of surface oxygen species contributing to superior oxygen reduction electrcatalytic activity [25].

2.2. Electrocatalytic Activity

Figure 3a,b shows ORR activity of Pt/C from 400 to 2500 rpm, PBSCF, and PBSCF composite electrodes under O2-saturated 0.1 M KOH at 10 mV/s at 1600 rpm. The onset potential and half wave potential of the PBSCF electrode were 0.7 V, and 0.5 V, respectively. While onset potential as well as half wave potential of PBSCF composite were 0.9 V and 0.78 V, respectively. Obvious synergistic effect of PBSCF and Pt/C might be accounted for this phenomenon. The outstanding electrochemical activities observed might be explained by analysing the O peak of the XPS result, and the relative amount of these oxidative oxygen species (O2−/O−) was closely correlated with the concentration of surface oxygen species, which contributed to good ORR and OER activities. For commercial Pt/C, onset potential and half wave potential was 0.9 V, 0.8 V, respectively. OER activity of Pt/C, PBSCF, and PBSCF composite electrodes was also evaluated at the same condition (Figure 3c). Onset potential of PBSCF composite was 1.58 V, which was 60 mV higher than IrO2 (1.52 V). Maximum current density measured at 1.9 V was 12 mA/cm2, which was higher than IrO2 (9 mA/cm2). Moreover, the onset potential of PBSCF was around 1.62 V. Remarkably, PBSCF composite afforded current density (10 mA/cm2) at 1.81 V.
Figure 3d shows ORR kinetics evaluated by Koutecky-Levich (K-L) equation. Electron transfer numbers for Pt/C and PBSCF composite were nearly 4.0. 4e− reduction was predominant for PBSCF composite. Figure 3e shows Tafel slope plots of PBSCF, IrO2 and PBSCF composite measured under O2 saturated 0.1 M KOH at 0.1 mV/s. Tafel slope for PBSCF composite was 76 mV/dec, while PBSCF was 89 mV/dec. Zhu. reported that Tafel slope for SrNb0.1Co0.7Fe0.2O3 and BSCF were 76 and 94 mV/dec, respectively [16]. The Tafel slope of IrO2 was 60mV/dec. The relatively lower Tafel slopes for PBSCF composite might indicate the synergistic effect for Pt and PBSCF.
Chronopotentiometry ORR stability for PBSCF composite was also studied at a constant potential of 0.75 V (Figure 3f) with the same loading condition. PBSCF composite showed good ORR stability. It initially reached 4.9 mA/cm2 and then became 5.2 mA/cm2 after 10,000 s. Chronoamperometry OER stability for PBSCF composite was obtained at 10 mA/cm2 (Figure 3f). The initial potential for PBSCF composite was 1.6 V, and it was approximately 1.62 V after 10 h.

2.3. Cell Performance

PBSCF composite electrocatalyst assembled in an aqueous rechargeable Zn-air battery was tested. Three Zn-air batteries could power the LED screen continuously (Figure 4). OCVs of PBSCF composite-based Zn air battery was 1.5 V. Zn-air battery achieved maximum peak power density of 175 mW/cm2 at 200 mA cm−2.
The stability of the rechargeable Zn-air battery was tested by charging and discharging for 10 min individually with repeated cycles at 5 mA cm−2. Its voltage gap (Δη) was 0.77 V initially, and the round trip efficiency was 61.9%. After 48 h, the voltage gap increased to 0.86 V and round-trip efficiency decreased to 57.6%, respectively. Such phenomenon might be due to the irreversible Zn plating-stripping process. PBSCF-composite Zn-air battery exhibits good rechargeability, and its performance is comparable to other results reported in the literature [33,34]. Moreover, PBSCF-composite is cheaper than IrO2 and 20 Pt/C, which shows its high economic potential.

3. Experimental

3.1. Powder Preparation

PrBa0.5Sr0.5Co1.5Fe0.5O5 (PBSCF) was prepared by EDTA-citrate sol-gel method. A stoichiometric amount of Pr(NO3)3.H2O, Ba(NO3)2, Sr(NO3)2, Co(NO3)3, and Fe(NO3)3.9H2O (Sigma) were weighted and mixed with distilled water, and then citric acid(CA) and EDTA (Sigma, Saint Louis, MO, USA) were added. The mole ratio of n(CA):n(Mn+):n(EDTA)=1:1:1.5. Mn+ indicates the total mole amount of metal ions in the mixture. After all, chemicals were mixed with water, they were heated to 80 °C for 4 h to form a dark sol. Then, it was heated to 200 °C to form a gel. In the next stage, the powders produced were combusted at 1000 °C for 5 h. PBSCF was mixed with commercial 20 wt% Pt/C from Johnson Matthey (JM). The composite obtained was denoted as PBSCF composite, in which the weight ratio of PBSCF and Pt/C was 2:1.

3.2. Electrode Preparation

Firstly, catalyst inks were prepared by mixing 10.0 mg catalyst powders, 16 μL Nafion solution and 250 μL ethanol, Secondly, they were sonicated to obtain homogeneous inks. Finally, it was dried for 5 min. Ink (5 μL) was dipped onto glassy carbon disk electrodes to achieve uniform thin film working electrodes.

3.3. Cell Preparation

2 mg PBSCF, 8 mg acetylene black, 5 mg Pt/C, 600 µL of Nafion and ethanol (1:1) were mixed together to form cell ink, and it was coated on a carbon cloth with Ni-foam. Carbon cloth and polished zinc plate were assembled in a Zn-air battery by 6 M KOH and 0.2 M ZnCl2. The detailed schematic diagram used is shown in Figure 5.

3.4. Electrocatalyst Characterizations

XRD was used to analyse the powder phase (Bruker D8 Advances). XPS was used to test the element valence of powders by the ESCALAB 250Xi instrument (Thermo Fisher, Waltham, MA, USA). The morphology was studied by SEM (ZEISS). HRTEM images and SAED were operated at 300 kV by the JEOL-3000 instrument.

3.5. Electrocatalytic Activity Test

ORR and OER activities were measured by three-electrode method with Pt wire as a counter electrode, saturated calomel electrode as reference electrode, and glassy carbon electrode as the working electrode. Princeton electrochemical workstation with RDE system was adopted.
For the ORR test, linear sweep voltammetry (LSV) curves were tested by 10 mV/s from −1 to 0 V at different rotation speeds from 400 rpm to 2500 rpm under 0.1 M KOH. Tafel curve was also obtained under the same condition by 1 mV/s. Chronopotentiometry data was tested at a constant potential of 0.75 V (vs. RHE). For OER tests, LSV curves were tested from 0 to 1 V (vs. RHE) by 10 mV/s and at 1600 rpm. Chronoamperometry data was conducted at a constant current density of 10 mA/cm2.
Charge and discharge data of aqueous rechargeable Zn-air battery was tested at 5 mA cm−2 by LAND CT2001A testing device. Polarization curves for the discharge process were tested by CHI6000A at 0.5 mA/s. The as-prepared catalyst is being used in the solid Zn-air battery in this research, and the detailed preparation process can be found in the published paper [35].

4. Conclusions

A highly active and stable ORR/OER bifunctional Pt/C-PrBa0.5Sr0.5Co1.5Fe0.5O5 double perovskite electrocatalyst was used in alkaline media and its performance was monitored. PrBa0.5Sr0.5Co1.5Fe0.5O5 catalyst was prepared by the sol-gel method and its composite materials showed better intrinsic ORR-OER activity and better stability in O2-saturated 0.1 M KOH. Rechargeable Zn-air battery on PBSCF composite demonstrated good initial discharge and charge potential. In addition, it also exhibited high cycling stability after 48 h. Overall, all these results illustrate that PBSCF composite is an economical electrocatalyst for rechargeable Zn-air batteries.

Author Contributions

Conceptualization, C.W.; methodology, Z.Z.; software, Z.C.; validation, X.L.; formal analysis, B.H.; investigation, M.G.; resources, X.G.; data curation, X.F.; writing—original draft preparation, Z.T.; funding acquisition, C.W. All authors have read and agreed to the published version of the manuscript.

Funding

This research was funded by 2022 Shenzhen Science and Technology Program (GJHZ20210705142006020), 2022 Research Funding of Shenzhen Polytechnic (6022310007K), Sichuan science and technology program (2020YJ0501,2022YFH0044).

Acknowledgments

The authors acknowledge the facilities, the scientific and technical assistance from Hoffman Research Institute in Shenzhen Polytechnic.

Conflicts of Interest

The authors declare no conflict of interest.

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Catalysts 12 00800 g001 550
Figure 1. XRD for PrBa0.5Sr0.5Co1.5Fe0.5O5 (PBSCF) (a) powders prepared by EDTA-citrate method fired at 1000 °C for 5 h. SEM images of as-prepared PBSCF (b). TEM images of the as-prepared PBSCF (c) the diffraction pattern as shown in (d), and the EDS of selected point was shown in (e).
Figure 1. XRD for PrBa0.5Sr0.5Co1.5Fe0.5O5 (PBSCF) (a) powders prepared by EDTA-citrate method fired at 1000 °C for 5 h. SEM images of as-prepared PBSCF (b). TEM images of the as-prepared PBSCF (c) the diffraction pattern as shown in (d), and the EDS of selected point was shown in (e).
Catalysts 12 00800 g001
Catalysts 12 00800 g002 550
Figure 2. Survey Scan of PBSCF of XPS spectra (a), High resolution deconvoluted of O 1s spectra of PBSCF electrocatalysts (b).
Figure 2. Survey Scan of PBSCF of XPS spectra (a), High resolution deconvoluted of O 1s spectra of PBSCF electrocatalysts (b).
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Catalysts 12 00800 g003 550
Figure 3. ORR activity of LSV curves for (a) 20 Pt/C, (b) PBSCF, and PBSCF composite, (c) OER activity of LSV curves for PBSCF, 20 Pt/C, and PBSCF composite, (d) K-L plots for PBSCF, 20 Pt/C, and PBSCF composite, (e) Tafel plots for PBSCF, 20 Pt/C, and PBSCF composite, (f) Chronopotentiometry curves of ORR for PBSCF composite at 0.41 V. (g) Chronoamperometry curves of OER for PBSCF composite at 10 mA cm−2 tested at 1600 rpm in O2-saturated 0.1 M KOH solution.
Figure 3. ORR activity of LSV curves for (a) 20 Pt/C, (b) PBSCF, and PBSCF composite, (c) OER activity of LSV curves for PBSCF, 20 Pt/C, and PBSCF composite, (d) K-L plots for PBSCF, 20 Pt/C, and PBSCF composite, (e) Tafel plots for PBSCF, 20 Pt/C, and PBSCF composite, (f) Chronopotentiometry curves of ORR for PBSCF composite at 0.41 V. (g) Chronoamperometry curves of OER for PBSCF composite at 10 mA cm−2 tested at 1600 rpm in O2-saturated 0.1 M KOH solution.
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Figure 4. (a) OCV for three PBSCF composite Zn air batteries. (b) Power supplying for LED. (c) I–V and P–V curves for two PBSCF composite Zn-air battery cells. (d) Galvanostatic charge–discharge profiles of Zn-air batteries at 5 mA cm−2.
Figure 4. (a) OCV for three PBSCF composite Zn air batteries. (b) Power supplying for LED. (c) I–V and P–V curves for two PBSCF composite Zn-air battery cells. (d) Galvanostatic charge–discharge profiles of Zn-air batteries at 5 mA cm−2.
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Figure 5. Schematic diagram of ORR/OER of PBSCF composite-based electrocatalysts and the assembling of rechargeable Zn-air battery.
Figure 5. Schematic diagram of ORR/OER of PBSCF composite-based electrocatalysts and the assembling of rechargeable Zn-air battery.
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Wang, C.; Zheng, Z.; Chen, Z.; Luo, X.; Hou, B.; Gholizadeh, M.; Gao, X.; Fan, X.; Tan, Z. Enhancement on PrBa0.5Sr0.5Co1.5Fe0.5O5 Electrocatalyst Performance in the Application of Zn-Air Battery. Catalysts 2022, 12, 800. https://doi.org/10.3390/catal12070800

AMA Style

Wang C, Zheng Z, Chen Z, Luo X, Hou B, Gholizadeh M, Gao X, Fan X, Tan Z. Enhancement on PrBa0.5Sr0.5Co1.5Fe0.5O5 Electrocatalyst Performance in the Application of Zn-Air Battery. Catalysts. 2022; 12(7):800. https://doi.org/10.3390/catal12070800

Chicago/Turabian Style

Wang, Chengcheng, Ziheng Zheng, Zian Chen, Xinlei Luo, Bingxue Hou, Mortaza Gholizadeh, Xiang Gao, Xincan Fan, and Zanxiong Tan. 2022. "Enhancement on PrBa0.5Sr0.5Co1.5Fe0.5O5 Electrocatalyst Performance in the Application of Zn-Air Battery" Catalysts 12, no. 7: 800. https://doi.org/10.3390/catal12070800

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