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DOI: 10.1039/D2CC06915F (Communication) Chem. Commun., 2023, 59, 4356-4359

Single-cell-array biomass-templated architecture of hierarchical porous electrocatalysts for Zn–air and Zn–H2O2 batteries†

Zhenjiang Zhu a, Liangyu Jin a, Meng Zhou a, Kui Fu a, Fancheng Meng a, Xiangfeng Wei a and Jiehua Liu *ab
aFuture Energy Laboratory, School of Materials Science and Engineering, Hefei University of Technology, Hefei 230009, China. E-mail: liujh@hfut.edu.cn
bKey Laboratory of Advanced Functional Materials and Devices of Anhui Province, Engineering Research Center of High-Performance Copper Alloy Materials and Processing, Ministry of Education, Hefei 230009, China

Received 19th December 2022 , Accepted 6th March 2023

First published on 7th March 2023

Abstract

Hierarchically macro–meso–microporous ZIF-67/nori-derived electrocatalysts were synthesized by using single-cell-array nori and ZIF-67 as macroporous and microporous templates, and KOH as a meso/micropore-forming reagent. The ZIF-67/nori-800-based Zn–H2O2 battery achieved a high maximum power density, of 476 mW cm−2, and a specific energy density of 964 W h kg−1 at 50 mA cm−2.

Zn–H2O2 batteries are becoming one of the research hotspots in the field of energy storage due to their advantages over Zn–air cells including high energy density, low cost, high safety, and environmental friendliness.1 Compared to Zn–air cells, Zn–H2O2 batteries can achieve higher power for multiple applications, because of their superior oxygen storage in hydrogen peroxide.2 Highly efficient bifunctional catalysts of the oxygen reduction reaction (ORR) and oxygen evolution reaction (OER) are desired for Zn–H2O2 batteries as well as Zn–air batteries. Noble-metal-based catalysts have become important commercial ORR catalysts (e.g., Pt/C) as well as OER catalysts (RuO2, IrO2, etc.) in acidic and basic solutions.3 However, their application in Zn–air or Zn–H2O2 batteries is limited due to their high costs.4 It has been a challenge to develop non-noble-metal-based catalysts displaying excellent ORR and OER catalytic activity.5

Nitrogen-doped carbon-based electrocatalysts have attracted extensive attention due to their high catalytic activity levels; these enhanced levels are due to the enhanced electron donor tendency and the enhanced adsorption of O2 resulting from the altering of the electron cloud density of adjacent carbon atoms.6 In addition, transition metals have been used as hydroxyl acceptors to adsorb protons and improve OER performance.7 Cobalt oxide has been reported to yield excellent ORR activity,8 and is expected to replace noble-metal-based catalysts.9 More importantly, gas–solid–liquid (three-phase) interfacial catalysis of ORR/OER has been improved by the presence of hierarchical pores.10 The meso/microporous structure is usually produced by controlling the carbon activation process, including physical and chemical activation, heat treatment, and impregnation. However, macropores (>50 nm) are often neglected in heterogeneous electrocatalysis, because they have been obtained on only a small scale using hard templates such as SiO2,11 MgO,12 or polymer microspheres.13

Nori is a highly abundant single-cell-thick biomass with a micro-cell-array sheet structure and natural macropores,14 and has the important characteristic of being able to adsorb toxic metal ions. Herein, we developed a novel route for synthesizing ZIF-67/nori-based electrocatalysts by using nori as a single-cell-layered template with a natural macropore array, which offered a sheet-like network of the conductive structure. The optimized catalyst (ZIF-67/nori-800) exhibited a high half-wave potential and overpotential for the OER (0.85 V and 1.46 V). The ZIF-67/nori-800-based Zn–H2O2 battery showed a high specific energy density of 964 W h kg−1 at a high rate of 50 mA cm−2 and achieved a high maximum power density of 476 mW cm−2.

There were three roles for the nori cell array in the processes used to prepare ZIF-67/nori, namely providing stability in water, respiration in ethanol/H2O, and fixed Co(II) ions, as shown in Fig. 1a. Nori was observed to have a unique micro-cell-array sheet structure with a single-cell thickness as shown in optical micrographs of nori, purified nori, and ZIF-67/nori (Fig. 1b–d). The nori cells were observed to be dark purple when they were infiltrated by deionized water (Fig. 1b). The ability of nori to provide respiration in ethanol/H2O was quite interesting (Fig. S1, ESI†). The nori material was found to become transparent when soluble impurities such as pigments and inorganic salts were removed from it (Fig. 1c). A sample of nori was immersed in Co(II) solution to form Co2+-adsorbed nori (nori-Co2+). After 2-methylimidazole was added, ZIF-67/nori was obtained by in situ synthesis of ZIF-67 in the interior and interface of nori cells (Fig. 1d). Samples subjected to annealing at 700, 800, and 900 °C were denoted as ZIF-67/nori-700, ZIF-67/nori-800, and ZIF-67/nori-900, respectively.


image file: d2cc06915f-f1.tif
Fig. 1 (a) Schematic of the route used to synthesize ZIF-67/nori. (b–d) Optical microscope photographs of (b) nori, (c) purified nori, and (d) ZIF-67/nori, scale bars each represent 100 μm.

Preliminary cyclic voltammetry (CV) tests showed better electrocatalytic activity displayed by ZIF-67/nori-800 than by ZIF-67/nori-700 and ZIF-67/nori-900 (Fig. S2, ESI†). Therefore, ZIF-67/nori-800 was characterized systematically in the following analysis. Field emission scanning electron microscope (FESEM) images of ZIF-67/nori-800 were obtained to describe its morphology. As shown in Fig. 2a, macropores with diameters of specifically 0.2–2 μm were found in ZIF-67/nori-800. Sub-macroscopic pores, with diameters of 40–200 nm, were observed distributed on the top view and cross-section of ZIF-67/nori-800 (Fig. 2b and c). Many macropores, derived from the micro-cell-array of nori, were observed.


image file: d2cc06915f-f2.tif
Fig. 2 (a–c) FESEM, (d and e) TEM, and (f) HRTEM images of ZIF-67/nori-800. (g) HAADF-STEM image of ZIF-67/nori-800 with mapping of C, N, O, and Co elements.

Fig. 2d includes a transmission electron microscope (TEM) image of ZIF-67/nori-800; here, many mesopores with diameters of several nanometers were observed distributed in the catalyst. As shown in Fig. 2e, ZIF-67/nori-800 also showed the presence of micropores. An HRTEM image of ZIF-67/nori-800 showed an amorphous non-crystalline structure (Fig. 2f). The HAADF-STEM image acquired of ZIF-67/nori-800 and the corresponding mappings of C, N, O, and Co elements are provided in Fig. 2g. N, O, and Co elements were uniformly distributed, as was the C element. Furthermore, the Co mapping overlapped with the N and O mappings, indicative of the presence of Co–O and Co–N bonds in ZIF-67/nori-800 (Fig. S3, ESI†).

X-Ray diffraction (XRD) patterns of ZIF-67/nori-derived catalysts are provided in Fig. S4a (ESI†). No obvious peak was observed for ZIF-67/nori-700, ZIF-67/nori-800, and ZIF-67/nori-900, indicating that the Co element was distributed as single atom sites or amorphous structures. As shown in Fig. S4b (ESI†), the Raman spectra of the samples showed two prominent peaks, at about 1360 cm−1 and 1589 cm−1, corresponding to the defect (D) and graphite (G) bands, respectively.15 As the temperature was increased, the ratios of the intensity of the D band to that of the G band (ID/IG) were measured to be 1.29 (700 °C), 1.02 (800 °C), and 1.01 (900 °C), indicating increasing the temperature to be beneficial, specifically for increasing the graphitization of samples.

N2 adsorption–desorption measurements were taken to investigate the interfacial properties and pore structure of the catalysts (Fig. S4c, ESI†). Type IV hysteresis curves in the P/P0 range 0.4–1.0 nm were observed for ZIF-67/nori-700, ZIF-67/nori-800, and ZIF-67/nori-900, and were due to capillary condensation, indicating the presence of micro/mesoporous structures in the three samples.16 The specific BET surface areas were 834.8, 1454.3, and 2861.3 m2 g−1 for ZIF-67/nori-700, ZIF-67/nori-800, and ZIF-67/nori-900, respectively. The increasing surface area with increasing temperature might have been due to an increasing pore-forming effect of the activator with increasing temperature. Fig. S4d (ESI†) shows the micro/mesopore-size distributions of the ZIF-67/nori-derived catalysts based on N2 adsorption–desorption isotherms calculated using the QSDFT method. The mesopore diameters of ZIF-67/nori-800 and ZIF-67/nori-900 were mainly between 2 and 12 nm, and their micropore diameters were mainly 0.5–2 nm.

The atomic percentages on the surfaces of the catalysts were determined using X-ray photoelectron spectroscopy (XPS), with the results summarized in Table S1 (ESI†). Nitrogen contents of 29.03, 9.03, and 4.46 at% were observed for ZIF-67/nori-700, ZIF-67/nori-800, and ZIF-67/nori-900, with these values significantly higher than that for ZIF-67/nori-R1 (without melamine added). Co–O and Co–Nx bonds in general have high catalytic activity for the OER and ORR.5b,17 The high-resolution Co 2p region of the XPS spectrum of ZIF-67/nori-800 was fitted by five peaks typical for Co (Fig. S5, ESI†): at 780.5 eV and 796.4 eV attributed to the Co(II)–O species,2a Co 2p satellite peaks at 786.8 eV and 802.7 eV, and at 782.5 eV belonging to Co–Nx.17 Peaks for Co–Nx in ZIF-67/nori-700, ZIF-67/nori-800, and ZIF-67/nori-900 were identified, in contrast to the lack of any clear Co–Nx peak for ZIF-67/nori-R1.18 More detailed information is provided in Fig. S6 and Table S2 (ESI†).

In Fig. S7 (ESI†), four peaks were fitted at 398.2, 398.9, 400.1, and 401.5 eV, corresponding to pyridinic-N, pyrrolic-N, graphite-N, and Co–Nx.19 As shown in Table S3 (ESI†), no Co–Nx bonds except pyrrolic-N bonds in ZIF-67/nori-R1 have been identified. The contents of pyridinic-N (1.52 at%), pyrrolic-N (3.93 at%), graphitic-N (3.27 at%), and Co–Nx (0.29 at%) bonds of ZIF-67/nori-800 were found to be much higher than those of ZIF-67/nori-900 (0.8, 1.6, 1.9, 0.09 at%) and ZIF-67/nori-R1 (pyrrolic-N 1.57 at%). Pyridinic-N and pyrrolic-N bonds in general could enhance ORR kinetics through the synergistic effect of Co and N elements.20 The high-resolution O 1s XPS spectra of the catalysts are shown in Fig. S8 and Table S4 (ESI†). The presence of Co–O bonds on the surface of the material could provide strong chemisorption for the adsorption of O2 molecules.21 The 11.45 at% content of oxygen in ZIF-67/nori-800 suggested a high oxygen adsorption capacity for this catalyst.22

Linear sweep voltammetry (LSV) curves were acquired to accurately evaluate the ORR performances at 1600 rpm. As displayed in Fig. 3a, ZIF-67/nori-800 showed an excellent ORR performance with a half-wave potential (E1/2) of 0.85 V and onset potential (Eonset) of 1.01 V, values much higher than those of commercial Pt/C catalyst (E1/2 = 0.82 V, Eonset = 1.00 V) and ZIF-67/nori-900 (E1/2 = 0.84 V, Eonset = 1.01 V). The limiting current density of ZIF-67/nori-800 was 5.14 mA cm−2, higher than those of Pt/C and ZIF-67/nori-R1. The good ORR catalytic activity of ZIF-67/nori-800 may have been due to a synergistic effect of hierarchical macro–meso–micropores and high-dispersion of N/Co atoms.


image file: d2cc06915f-f3.tif
Fig. 3 (a) ORR curves and (b) Tafel slopes for the ORR of the catalysts.

OER performances of ZIF-67/nori-derived catalysts were evaluated by acquiring the LSV curves of O2-saturated 1 M KOH solutions of these catalysts at 1600 rpm. In Fig. S9 (ESI†), the overpotential of ZIF-67/nori-800 at 10 mA cm−2 was 230 mV, better than that of RuO2 (363 mV), indicating a better OER performance of ZIF-67/nori-800 than that of RuO2. In Fig. 3b, the Tafel slope of the ZIF-67/nori-800 catalyst was determined to be only 89 mV dec−1, better than the 148 mV dec−1 value for commercial Pt/C. And the Tafel slope of ZIF-67/nori-900 was close to that of ZIF-67/nori-800, indicating good OER kinetic reactions for both ZIF-67/nori-800 and ZIF-67/nori-900. In Fig. S10 (ESI†), electron transfer number (n) values of 3.61–3.75 were calculated, using the K–L equation, for ZIF-67/nori-800 at various potentials ranging from 0.5 to 0.7 V; this result was consistent with the predominance of a four-electron ORR pathway.

Fig. S11 (ESI†) shows the LSV curves of the ZIF-67/nori-800 catalyst before and after 5000 cycles of the ORR in 1 M KOH: over the course of the 5000 cycles, a decrease of only 7 mV was observed, and the limiting current density at 5000 cycles was 94.1%, together indicative of the good stability of the ZIF-67/nori-800 catalyst.

A Zn–air battery was fabricated using ZIF-67/nori-800 as the electrocatalyst of the air cathode and metal Zn sheet as the anode. Fig. 4a shows the discharge voltages of Zn–air batteries with ZIF-67/nori-800 and Pt/C catalysts at current densities ranging from 20 to 150 mA cm−2. The discharge voltages were 1.27, 1.2, and 1.08 V for the ZIF-67/nori-800-based Zn–air battery at the high current densities of 20, 50, and 150 mA cm−2; these discharge voltage values were much higher than those of the Pt/C-based Zn–air battery. Fig. 4b shows the polarization and power density curves of the cells. The maximum power density was 284 mW cm−2 for the ZIF-67/nori-800-based Zn–air battery, superior to the value of 179 mW cm−2 for the Pt/C-based Zn–air battery. In our opinion, the maximum power density of ZIF-67/nori-800 may have originated from its unique porous structure. As shown in Fig. S12 (ESI†), the open-circuit voltage (Voc) was 1.41 V for the ZIF-67/nori-800-based Zn–air battery, a bit higher than the 1.39 V value of the Voc for the Pt/C-based Zn–air battery. The specific energy density and specific capacity of the ZIF-67/nori-800-based Zn–air battery were 871 W h kg−1 and 771 mA h g−1 at 50 mA cm−2, much higher than those of the Pt/C-based Zn–air battery (Fig. 4c and Fig. S13, ESI†). A high specific energy density, specifically 992 W h kg−1, was measured for the ZIF-67/nori-800-based Zn–air cell at 10 mA cm−2 (Fig. S14, ESI†).


image file: d2cc06915f-f4.tif
Fig. 4 (a) Rate performances, (b) discharge polarization curves and corresponding power density plots, and (c) specific energy density curves of Zn–air and Zn–H2O2 batteries with ZIF-67/nori-800 and Pt/C as ORR catalysts.

Fig. S15 (ESI†) shows the cycling stability of Zn–air batteries at a current density of 10 mA cm−2. The Zn–air battery with ZIF-67/nori-800 showed a long lifetime of up to 200 h, much better than that of Pt/C–RuO2 (90 h). The charge and discharge voltages of the ZIF-67/nori-800-based Zn–air battery were 1.92 V and 0.97 V, and the difference between them (ΔV) was only 0.95 V, superior to that of the Pt/C–RuO2-based Zn–air battery with a ΔV of 1.06.

ZIF-67/nori-800 was further investigated in Zn–H2O2 batteries, which could work in non-oxygen or hypoxic environments. Fig. 4a shows the high-rate performances of Zn–H2O2 batteries with ZIF-67/nori-800 and Pt/C electrocatalysts. The discharge voltages were 1.29 (20 mA cm−2), 1.25 (50 mA cm−2), 1.20 (100 mA cm−2), and 1.15 V (150 mA cm−2), which were much higher than those of the Pt/C-based Zn–air/Zn–H2O2 batteries. The polarization and power density curves of the cells are shown in Fig. 4b. The maximum power density of the ZIF-67/nori-800-based Zn–H2O2 battery was 476 mW cm−2, much better than those of the Pt/C-based Zn–air/Zn–H2O2 battery (179 mW cm−2/271 mW cm−2) and ZIF-67/nori-800-based Zn–air battery (284 mW cm−2). The Voc of ZIF-67/nori-800 in the Zn–H2O2 battery was 1.44 V, higher than those of other Zn–air/Zn–H2O2 batteries. Importantly, the specific energy density and specific capacity of the ZIF-67/nori-800-based Zn–H2O2 battery were 964 W h kg−1 and 800 mA h g−1 at 50 mA cm−2, superior to those of the Pt/C-based Zn–air/Zn–H2O2 battery and ZIF-67/nori-800-based Zn–air battery (871 W h kg−1/771 mA h g−1).

In summary, we have developed highly efficient bifunctional ORR/OER electrocatalysts with unique hierarchical porous structures by using single-cell-layered biomass (nori) as a macropore-array template and KOH as a meso/micropore-forming reagent. ZIF-67/nori-800 yielded an excellent power density performance (476 mW cm−2) and specific energy density (964 W h kg−1) in the reported Zn–air/Zn–H2O2 batteries. The ZIF-67/nori-800-based Zn–H2O2 battery is a promising alternative high-power battery in low-oxygen or nonoxygen environments where Zn–air batteries do not work properly.

This research was supported by the National Natural Science Foundation of China (U1832136 and 21303038).

Conflicts of interest

There are no conflicts to declare.

Notes and references

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Footnote

† Electronic supplementary information (ESI) available: See DOI: https://doi.org/10.1039/d2cc06915f
This journal is © The Royal Society of Chemistry 2023
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