馄饨结构的KB@Co-C3N4在中性电解质中作为锌空气电池的高活性和稳定性氧催化剂

doi:10.1016/S1872-2067(24)60007-0

催化学报 ›› 2024, Vol. 60: 178-189.DOI: 10.1016/S1872-2067(24)60007-0

馄饨结构的KB@Co-C₃N₄在中性电解质中作为锌空气电池的高活性和稳定性氧催化剂

吴维凡^a^,^b, 范晋歌^a^,^b, 赵振宏^a, 潘建敏^a^,^b, 杨静^a, 阎兴斌^c, 詹怡^a^,^b^,^*()

^a中山大学化学工程与技术学院, 广东珠海 519082
^b中山大学低碳化学与节能工程重点实验室, 广东广州 510275
^c中山大学材料科学与工程学院, 光电材料与技术国家重点实验室, 广东广州 510275

收稿日期:2023-12-23 接受日期:2024-02-27 出版日期:2024-05-18 发布日期:2024-05-22
通讯作者: *电子信箱: zhany9@mail.sysu.edu.cn (詹怡).
基金资助:
广东省基础与应用基础研究基金(2023A1515010134)

Wonton-structured KB@Co-C₃N₄ as a highly active and stable oxygen catalyst in neutral electrolyte for Zinc-air battery

Wei-Fan Wu^a^,^b, Jin-Ge Fan^a^,^b, Zhen-Hong Zhao^a, Jian-Min Pan^a^,^b, Jing Yang^a, Xingbin Yan^c, Yi Zhan^a^,^b^,^*()

^aSchool of Chemical Engineering and Technology, Sun Yat-sen University, Zhuhai 519082, Guangdong, China
^bThe Key Lab of Low-Carbon Chemistry & Energy Conservation of Guangdong Province, Sun Yat-sen University, Guangzhou 510275, Guangdong, China
^cState Key Laboratory of Optoelectronic Materials and Technologies, Department of Materials Science and Engineering, Sun Yat-sen University, Guangzhou 510275, Guangdong, China

Received:2023-12-23 Accepted:2024-02-27 Online:2024-05-18 Published:2024-05-22
Contact: *E-mail: zhany9@mail.sysu.edu.cn (Y. Zhan).
Supported by:
Guangdong Basic and Applied Basic Research Foundation, China(2023A1515010134)

摘要/Abstract

摘要：

金属和氮共掺杂碳(M-N-Cs)由于具有高原子利用率、良好的活性和选择性, 因而被认为是具有潜力的氧电催化剂. 但其热力学氧化势较低, 碳材料在高电位下容易腐蚀. 在放电过程中, 锌空气电池正极的电位始终比碳氧化的热力学电位高约0.5 V, 这导致阴极中碳的严重腐蚀. 对于M-N-C, 腐蚀会破坏金属氮配位(M-N_x)活性位点, 导致活性比表面积减少, 同时还会改变孔隙形貌和表面特性, 进而降低其催化活性. 在充电(即氧气析出反应, OER)过程中, 这种腐蚀现象会进一步加剧. 因此, 开发一种既具有高效双功能催化活性, 又具有良好抗电化学腐蚀性能的M-N-C催化剂, 对于解决上述问题至关重要.

本文利用氮化碳(g-C₃N₄)支撑钴氮配位(Co-N_x)活性位点, 同时包覆科琴黑(KB)形成馄饨结构, 制备了双功能氧催化剂KB@Co-C₃N₄. 首先, 将剥离的C₃N₄与KB混合后煅烧, 得到C₃N₄包覆的KB材料(KB@C₃N₄); 随后, 再次煅烧将Co单原子引入KB@C₃N₄中, 形成具有高活性和高稳定性的KB@Co-C₃N₄氧催化剂. 红外光谱结果证实了, KB@Co-C₃N₄中存在C₃N₄成分. 透射电镜和元素标记结果表明, C₃N₄均匀包覆在KB基底上. 同步辐射测试确定了Co单原子的配位环境为CoN₄结构. 在0.5 mol L^‒1 NH₄Cl溶液中测试了KB@Co-C₃N₄氧催化剂ORR/OER的催化活性和稳定性. 结果表明, KB@CoC₃N₄表现出较好的ORR性能, 半波电位为0.723 V, 显著优于商业铂碳催化剂(0.673 V)和普通Co-N-C催化剂(0.694 V). 经过40000圈加速耐久性测试, KB@Co-C₃N₄仅衰减9 mV, 而商业铂碳和Co-N-C在7500圈测试后分别衰减41和44 mV. 在OER方面, KB@Co-C₃N₄在10 mA cm^‒2时的过电位为550 mV, 优于氧化钌的560 mV和Co-N-C的600 mV. 经过20000圈测试, KB@Co-C₃N₄的OER过电位几乎保持不变, 而氧化钌和Co-N-C经过4000圈测试后分别增加了37和20 mV. 透射电镜观察发现, KB@Co-C₃N₄在实验前后形貌未发生明显变化, 证明了其较好的稳定性. 理论计算揭示, C₃N₄能够优化Co金属活性位点的电子结构, 改善Co中心的电荷分布并增强Co‒N键强度; 同时, C₃N₄对KB基底的包覆有效避免了KB在高电位下的腐蚀, 确保了KB@Co-C₃N₄的高稳定性和催化活性. 将KB@Co-C₃N₄应用于中性锌空气电池中, 该电池展现出1.52 V的开路电压, 并在5 mA cm^‒2的高电流密度下稳定循环运行超过985 h, 性能优于大多数报道的采用碳基材料作为阴极催化剂的中性锌空气电池.

综上所述, 馄饨结构的KB@Co-C₃N₄具有较好的氧催化活性和稳定性, 为设计高稳定性高活性的M-N-C催化剂提供了一定的参考.

关键词: 氧电催化, 单原子催化剂, 中性电解液, 抗腐蚀

Abstract:

This work addresses the challenges faced by oxygen catalysis applications in neutral media, which are hindered by sluggish kinetics and severe carbon corrosion. To overcome these issues, a bifunctional oxygen catalyst (KB@Co-C₃N₄) was developed by utilizing graphitic carbon nitride (g-C₃N₄) to support Co-N_x active sites and simultaneously to wrap Ketjen black (KB) to form a wonton structure. The resulting catalyst exhibited excellent ORR/OER activity and good stability in neutral electrolytes. The KB@Co-C₃N₄ catalyst demonstrated a half-wave potential (E_1/2) of 0.723 V and only a 9 mV decay after 40000 cycles of ORR accelerated durability test (ADT). In terms of OER, the overpotential at 10 mA cm^-2 (η₁₀) of KB@Co-C₃N₄ was 550 mV, with negligible increase observed even after 20 k cycles of OER ADT. The zinc-air battery incorporating KB@Co-C₃N₄ exhibited superior performances over other benchmark bifunctional counterparts in open-circuit voltage (1.52 V), galvanostatic discharge/charge performance and cycling duration (985 h at 5 mA cm^-2). The theoretical investigation revealed that the engineered electronic structures of the metal active sites enable precise regulation of the charge distribution of Co centers, leading to optimized adsorption and desorption of oxygenated intermediates. The high stability of the catalyst is attributed to the chemically stable C₃N₄, which strengthens Co-N_x active sites and protects KB against carbon corrosion by wrapping KB to form the wonton structure.

Key words: Oxygen electrocatalysis, Single-atomic catalysts, Neutral electrolyte, Corrosion resistance

吴维凡, 范晋歌, 赵振宏, 潘建敏, 杨静, 阎兴斌, 詹怡. 馄饨结构的KB@Co-C₃N₄在中性电解质中作为锌空气电池的高活性和稳定性氧催化剂[J]. 催化学报, 2024, 60: 178-189.

Wei-Fan Wu, Jin-Ge Fan, Zhen-Hong Zhao, Jian-Min Pan, Jing Yang, Xingbin Yan, Yi Zhan. Wonton-structured KB@Co-C₃N₄ as a highly active and stable oxygen catalyst in neutral electrolyte for Zinc-air battery[J]. Chinese Journal of Catalysis, 2024, 60: 178-189.

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链接本文: https://www.cjcatal.com/CN/10.1016/S1872-2067(24)60007-0

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Fig. 1. (a) The synthesis process of the KB@Co-C3N4 catalyst. TEM (b-d), HAADF-TEM images and the corresponding elemental mapping images (e) of the KB@Co-C3N4 catalyst. (f) HAADF-STEM images of the KB@Co-C3N4 catalyst with the atomic dispersion of Co atoms.

Fig. 2. High-resolution XPS spectra of Co 2p (a), N 1s (b), and C 1s (c) for the KB@Co-C3N4 catalyst. (d) Co K-edge k2-weighted FT spectra of the KB@Co-C3N4 catalyst and the reference samples. (e) The Co K-edge XANES (Inset: maximum absorption peak energy (E0) of KB@Co-C3N4 and r reference samples from 1st derivative of XANES). (f) FT-EXAFS fitting for the KB@Co-C3N4 catalyst at R space (inset: schematic model of Co-N4). WT-EXAFS contour plots of KB@Co-C3N4 (g), Co foil (h), CoO (i) and Co2O3 (j).

Fig. 3. (a) ORR LSV curves of different catalysts. (b) ORR LSV curves of different catalysts before and after ADT. (c) OER LSV curves of different catalysts. (d) OER LSV curves of different catalysts before and after ADT. (e) ORR LSV curves of different catalysts before and after OER ADT. (f) Overall oxygen bifunctional activity of different catalysts. Comparison of the δE1/2 (g) and ΔE (h) of the KB@Co-C3N4 catalyst and the previously reported catalysts. All above were tested in O2-saturated 0.5 mol L?1 NH4Cl at 1600 r min?1.

Fig. 4. Chronopotentiometric curves of KB@Co-C3N4 (a) and RuO2 (b) at different current densities. Visible spectra of the electrolytes with KI after electrolysis with a delivered charge of 30 C cm?2 and the average OER proportion of KB@Co-C3N4 (c) and RuO2 (d) at the indicated current densities.

Fig. 5. (a) The Co?N bond energy and the adsorption configurations of KB@Co-C3N4 (left) and Co-N-C (right) based on DFT, the brown, off-white, blue, red and white balls represent C, N, Co, O and H atoms respectively. (b) The Gibbs free energy diagrams of ORR at U = 1.23 V for KB@Co-C3N4 and Co-N-C.

Fig. 6. (a) Schematic illustration of a ZAB. (b) Open-circuit voltage of liquid ZAB with KB@Co-C3N4 and Pt/C+RuO2 as cathode catalysts respectively. Rate performance (c) and Nyquist plots (d) of liquid ZAB. (e) LSV curves of liquid ZAB. (f) Galvanostatic discharge-charge cycling curves of KB@Co-C3N4 and Pt/C+RuO2 ZABs at 5 mA cm?2. (g) Comparison of performances of the KB@Co-C3N4 based-ZAB with other neutral rechargeable ZABs with carbon-based catalysts as cathodes in the literature in terms of current density and cyclic life.

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馄饨结构的KB@Co-C₃N₄在中性电解质中作为锌空气电池的高活性和稳定性氧催化剂

Wonton-structured KB@Co-C₃N₄ as a highly active and stable oxygen catalyst in neutral electrolyte for Zinc-air battery

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