具有蜂窝碳结构的杂原子掺杂NiX/Ni纳米复合催化剂高效电催化H2O2合成

doi:10.1016/S1872-2067(24)60121-X

催化学报 ›› 2024, Vol. 66: 212-222.DOI: 10.1016/S1872-2067(24)60121-X

具有蜂窝碳结构的杂原子掺杂NiX/Ni纳米复合催化剂高效电催化H₂O₂合成

刘梦然^a^,¹, 刘灿豫^a^,¹, 杨天芳^b, 胡仕祥^a, 李思韵^a, 刘仕哲^b, 刘洋^a, 陈野^a, 葛炳成^a^,^*(), 高书燕^a^,^b^,^*()

^a河南师范大学材料科学与工程学院, 河南新乡 453007
^b河南师范大学化学化工学院, 河南新乡 453007

收稿日期:2024-07-01 接受日期:2024-08-22 出版日期:2024-11-18 发布日期:2024-11-10
通讯作者: *电子信箱: shuyangao@htu.cn (高书燕),gebingcheng@htu.edu.cn (葛炳成).
作者简介:¹共同第一作者.
基金资助:
国家自然科学基金(U52272293);中国博士后科学基金(2021M701116);中国博士后科学基金(2021M690930)

High-efficiency electrochemical H₂O₂ synthesis by heteroatom-doped NiX/Ni nanocomposites with honeycomb-like porous carbon

Mengran Liu^a^,¹, Canyu Liu^a^,¹, Tianfang Yang^b, Shixiang Hu^a, Siyun Li^a, Shizhe Liu^b, Yang Liu^a, Ye Chen^a, Bingcheng Ge^a^,^*(), Shuyan Gao^a^,^b^,^*()

^aSchool of Materials Science and Engineering, Henan Normal University, Xinxiang 453007, Henan, China
^bSchool of Chemistry and Chemical Engineering, Henan Normal University, Xinxiang 453007, Henan, China

Received:2024-07-01 Accepted:2024-08-22 Online:2024-11-18 Published:2024-11-10
Contact: *E-mail: shuyangao@htu.cn (S. Gao),gebingcheng@htu.edu.cn (B. Ge).
About author:¹Contributed equally to this work.
Supported by:
National Natural Science Foundation of China(U52272293);Fellowship of China Postdoctoral Science Foundation(2021M701116);Fellowship of China Postdoctoral Science Foundation(2021M690930)

摘要/Abstract

摘要：

通过二电子(2e^-)氧还原反应(ORR)合成过氧化氢(H₂O₂)是有望取代传统能源密集型蒽醌工艺的技术之一, 但是2e^- ORR生成H₂O₂途径与4e^-生成H₂O途径存在竞争关系, 因此制备高选择性、高活性的催化剂是有效促进电催化ORR合成H₂O₂的关键. 基于密度泛函理论(DFT)得到的火山图结果表明, 在电催化2e^- ORR中碳负载镍基催化剂(Ni@NC)靠近火山图顶点, 具有巨大应用潜力, 然而Ni@NC仍存在Ni位点与关键中间体*OOH吸附强度不佳的问题, 因此增强中间体*OOH的吸附强度以提高其选择性是一项挑战.

本文采用强电负性O/S原子掺杂调控催化活性中心Ni原子电子结构, 利用盐酸多巴胺聚合的碱性氛围制备富O/S掺杂的前驱体, 结合自牺牲模板铸造法通过控制煅烧温度成功合成一种NiO或者NiS掺杂的具有多孔结构蜂窝状纳米复合催化剂(NiO/Ni@NCHS或NiS₆/Ni@NCHS). X射线衍射(XRD)和X射线光电子能谱(XPS)等分析测试结果明确了催化活性中心组分及局域原子配位环境对催化活性位点的影响. 与Ni配位的O/S原子可以调节Ni原子的电子结构, 从而改善Ni原子与中间体*OOH的吸附能力. 采用自牺牲模板法构造高比表面积、介孔分布的蜂窝状结构聚苯乙烯(PS)微球, 加速了活性物种在电解质中的转移, 提高了活性位点暴露程度, 改善了电催化活性. 得益于蜂窝状结构和O/S杂原子掺杂的共同作用, 在700 ºC下合成的催化剂(NiO/Ni@NCHS-700)在碱性电解液中0.1-0.6 V的电位范围内表现出89.1%的H₂O₂选择性, 并且H₂O₂产率高达1.47 mol g-1 cat h^-1@0.2 V, 优于大多数先进的催化剂. 同时, NiS₆/Ni@NCHS催化剂表现出91.3%的2e^- ORR选择性, 1.85 mol g-1 cat h^-1@0.3 V的H₂O₂产率等较好的电催化性能. 通过原位红外(ATR-FIIR)光谱技术和拉曼测试追踪氧还原反应过程的中间体, 结果表明, OOH_ad在NiO/Ni@NCHS催化剂的ORR过程中起主要作用. 密度泛函理论计算了ORR每一步所需的热力学自由能, 验证了NiO/Ni@NCHS(或NiS₆/Ni@NCHS)中杂原子的掺入有效调节了Ni的强吸附特性. 同时, 金属Ni及其氧化物(或硫化物)之间的协同效应显著增强了催化活性.

综上, 本文研究了新型多组分催化剂的制备策略, 通过调控掺杂元素、孔结构和比表面积, 实现优化催化性能与反应选择性, 为高效Ni基2e^- ORR电催化剂的合理设计与调控提供思路, 为推动电催化2e^- ORR产H₂O₂技术发展提供参考.

关键词: NiX/Ni@NCHS复合催化剂, 2e^-氧还原反应, 蜂窝状多孔碳, 密度泛函理论, 电催化

Abstract:

Transition metal Ni anchored in carbon material represents outstanding 2e^- oxygen reduction reaction (ORR) catalytic selectivity, but enhancing the adsorption strength of intermediate *OOH to promote its selectivity remains a major challenge. Herein, the NiX/Ni@NCHS composite catalyst with heteroatom doping (O,S) is modulated by controlling partial pyrolysis strategies on honeycomb-like porous carbon to manipulate the electronic structure of the metal Ni. With the synergistic effect of honeycomb structure and O atom, NiO/Ni@NCHS-700 exhibits an exceptional H₂O₂ selectivity of above 89.1% across a wide potential range from 0.1 to 0.6 V in an alkaline electrolyte, and an unexpected H₂O₂ production rate up to 1.47 mol g_cat^-1 h^-1@0.2 V, which outperforms most of the state-of-the-art catalyst. Meanwhile, NiS/Ni@NCHS exhibits excellent electrocatalytic performance, with 2e^- ORR selectivity of 91.3%, H₂O₂ yield of 1.85 mol g_cat^-1 h^-1@0.3 V. Density functional theory simulations and experiments results reveal that the heteroatom doping (O,S) method has been employed to regulate the adsorption strength of Ni atoms with *OOH, and combined with the self-sacrificing template-assisted pyrolysis approach to improve the microstructure of catalysts and optimize the active site. The heteroatom doping method in this work provides significant guidance for promoting 2e^- ORR electrocatalysis to produce H₂O₂.

Key words: NiX/Ni@NCHS composite catalyst, 2e^- oxygen reduction reaction, Honeycomb-like porous carbon, Density functional theory, Electrocatalysis

刘梦然, 刘灿豫, 杨天芳, 胡仕祥, 李思韵, 刘仕哲, 刘洋, 陈野, 葛炳成, 高书燕. 具有蜂窝碳结构的杂原子掺杂NiX/Ni纳米复合催化剂高效电催化H₂O₂合成[J]. 催化学报, 2024, 66: 212-222.

Mengran Liu, Canyu Liu, Tianfang Yang, Shixiang Hu, Siyun Li, Shizhe Liu, Yang Liu, Ye Chen, Bingcheng Ge, Shuyan Gao. High-efficiency electrochemical H₂O₂ synthesis by heteroatom-doped NiX/Ni nanocomposites with honeycomb-like porous carbon[J]. Chinese Journal of Catalysis, 2024, 66: 212-222.

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链接本文: https://www.cjcatal.com/CN/10.1016/S1872-2067(24)60121-X

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图/表 6

Scheme 1. Schematic illustration for the synthesis of the NiO/Ni@NCHS-700 composite catalyst with a honeycomb structure (a) and the NCSS-700 catalyst with a solid structure (b).

Fig. 1. Compositions and morphologies of NiO/Ni@NCHS-700. (a,b) FESEM images; (c,d) TEM images; (e,f) HR-TEM images; (g) HAADF images, and corresponding EDS maps.

Fig. 2. N2 adsorption-desorption isotherms (a), pore size distributions by the DFT method (b), BET specific area and total pore volume information (c), XRD patterns (d), Raman spectra (e), and FT-IR spectra (f) of NiO/Ni@NCHS-700 and counterparts.

Fig. 3. (a) Full spectrum of NCHS-700, NCSS-700, NiO/Ni@NCHS-700, and NiO/Ni@NCSS-700. High-resolution XPS spectra of C 1s (b). (c) Element contents of different samples. N 1s (d), O 1s (e) and Ni 2p (f) spectra of catalysts XPS.

Fig. 4. LSV curves (a), limiting disk current density (jL) and onset potential (Eon) (b), H2O2 selectivity and electron transfer number (n) (c) of NCHS-700, NCSS-700, NiO/Ni@NCHS-700, and NiO/Ni@NCSS-700. (d) Performance comparison of electrochemical H2O2 production on NiO/Ni@NCHS-700 and other reported catalysts based on RRDE performance map of Eon and maximum H2O2 selectivity. (e) Tafel plots of NiO/Ni@NCHS-700. (f) The calculated H2O2 productivity and Faradaic efficiency of NiO/Ni@NCHS-700 at 0.2, 0.3, 0.4, 0.5, and 0.6 V vs. RHE, respectively (Error bars from three measurements at different potentials). (g) Stability measurement of NiO/Ni@NCHS-700. (h) Performance comparison of electrochemical H2O2 production on NiO/Ni@NCHS-700 and other recently reported catalysts performance map of jL and durability.

Fig. 5. (a) The ATR-FIIR spectra of NiO/Ni@NCHS for the 2e- ORR in the potentiostatic step. (b) In situ Raman spectra of NiO/Ni@NCHS. (c,d) Free energy diagram of the Ni@NCHS, NiO@NCHS, NiS6@NCHS, NiO/Ni@NCHS, and NiS6/Ni@NCHS. (e) PDOS for the d-orbitals. (f,g) Charge density differences of NiO/Ni@NCHS and NiS6/Ni@NCHS, where the electron accumulation and depletion regions are shown in yellow and green, respectively. (h) Volcano plot for 2e- ORR activity with the *OOH descriptor. (i) Schematic diagrams of NiO/Ni@NCHS reaction processes.

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具有蜂窝碳结构的杂原子掺杂NiX/Ni纳米复合催化剂高效电催化H₂O₂合成

High-efficiency electrochemical H₂O₂ synthesis by heteroatom-doped NiX/Ni nanocomposites with honeycomb-like porous carbon

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