理论指导构建Cu-O-Ti-Ov活性位点及其高效电催化还原硝酸根研究

doi:10.1016/S1872-2067(23)64618-2

催化学报 ›› 2024, Vol. 59: 293-302.DOI: 10.1016/S1872-2067(23)64618-2

理论指导构建Cu-O-Ti-O_v活性位点及其高效电催化还原硝酸根研究

聂翼飞^a^,¹, 颜红萍^a^,¹, 鹿苏微^a, 张宏伟^a, 齐婷婷^a^,^*(), 梁诗景^a^,^b^,^*(), 江莉龙^a^,^b

^a福州大学化肥催化剂国家工程研究中心, 福建福州 350002
^b清源创新实验室, 福建泉州 362801

收稿日期:2024-01-04 接受日期:2024-02-04 出版日期:2024-04-18 发布日期:2024-04-15
通讯作者: *电子邮箱: qtt@fzu.edu.cn (齐婷婷), sjliang2012@fzu.edu.cn (梁诗景).
作者简介:
¹共同第一作者.
基金资助:
国家自然科学基金(22221005);国家自然科学基金(22378060);国家重点研发计划(2021YFB3801600)

Theory-guided construction of Cu-O-Ti-O_v active sites on Cu/TiO₂ catalysts for efficient electrocatalytic nitrate reduction

Yifei Nie^a^,¹, Hongping Yan^a^,¹, Suwei Lu^a, Hongwei Zhang^a, Tingting Qi^a^,^*(), Shijing Liang^a^,^b^,^*(), Lilong Jiang^a^,^b

^aNational Engineering Research Center of Chemical Fertilizer Catalyst Fuzhou University, Fuzhou 350002, Fujian, China
^bQingyuan Innovation Laboratory, Quanzhou 362801, Fujian, China

Received:2024-01-04 Accepted:2024-02-04 Online:2024-04-18 Published:2024-04-15
Contact: *E-mail: qtt@fzu.edu.cn (T. Qi), sjliang2012@fzu.edu.cn (S. Liang).
About author:
¹ Contributed equally to this work.
Supported by:
The National Natural Science Foundation of China(22221005);The National Natural Science Foundation of China(22378060);The National Key R&D Program of China(2021YFB3801600)

摘要/Abstract

摘要：

面向国家绿色低碳战略目标, 变革化石资源合成氨技术路线变得尤为迫切, 开发可再生能源制“绿氨”将成为合成氨领域未来的重要发展方向. 将工业废水中的硝酸根(NO₃^-)电催化还原为氨(NO₃RR), 既可有效回收氨, 又能消除硝酸根污染影响. 然而, NO₃RR涉及缓慢的八电子转移过程, 含有多种反应中间体, 其反应机理复杂不明. 此外, 水系电解液中存在的析氢竞争反应也为高效NO₃RR催化剂的开发设计带来了巨大的挑战. 为突破高效催化剂的发展瓶颈, 本文通过理论模拟, 在低成本的催化剂上设计了高效的NO₃RR催化活性位点, 并利用简单的制备策略合成了目标催化剂. 同时, 结合原位表征技术, 阐明了NO₃RR的反应路径及催化机理.

本文通过密度泛函理论(DFT)计算发现, Cu/TiO₂催化剂上的Cu-O-Ti-O_v结构具有较好的NO₃^-还原活性, 该结构不仅能够促进反应中间体NO_x^-的吸附和活化, 还能有效抑制竞争析氢反应, 从而降低NO₃RR的反应能垒. 在该结构上, NO₃RR的反应路径为: NO₃^* → NO₂^* → HONO^* → NO^* → ^*NOH → ^*N → ^*NH → ^*NH₂ → ^*NH₃ → NH₃. 基于理论计算结果, 分别采用浸渍法和尿素水解法制备了系列富含Cu-O-Ti-O_v结构的Cu/TiO₂催化剂. 氮气等温吸附-脱附曲线、拉曼光谱(Raman)、电子顺磁共振波谱、X射线光电子能谱(XPS)和傅立叶红外光谱等结果发现, 相比于采用浸渍法制备的系列Cu/TiO₂催化剂, 采用尿素水解法制备的Cu/TiO₂(CT-U)催化剂具有更大的比表面积以及更多的Cu-O-Ti-O_v位点, 说明尿素水解法可提高Cu颗粒在TiO₂载体表面的分散度, 增强Cu颗粒与TiO₂载体之间的相互作用, 提高Cu/TiO₂催化剂表面的Cu-O-Ti-O_v位点含量. 将以上制备出的催化剂应用于催化NO₃RR中, 结果表明, 在-1.0 V vs. RHE还原电位下, CT-U催化剂上氨产率可达3046.5 μg h^-1 mg_cat^-1, 高于大多数文献报道结果. 循环稳定性测试结果表明, 在Cu/TiO₂催化剂上构建Cu-O-Ti-O_v位点还能显著抑制电催化反应过程中Cu物种从Cu/TiO₂催化剂上溶出, 从而显著增强催化剂的稳定性. 此外, 设计制备了不含氧空位的Cu/TiO₂, TiO_2-_x, Cu, Cu₂O以及CuO催化剂, 并将其用于催化NO₃RR. 结果发现, 上述催化剂上的氨产率皆明显低于CT-U催化剂, 说明Cu, Ti以及O_v构成的Cu-O-Ti-O_v结构具有较好的催化协同作用, 从而显著提升了NO₃RR反应活性. 最后, 通过原位Raman及原位XPS表征检测反应中间体, 验证了由DFT模拟出的NO₃RR反应路径.

综上, 通过在Cu/TiO₂催化剂上理论指导构建Cu-O-Ti-O_v活性位点, 实现了NO₃RR性能的有效提升. Cu-O-Ti-O_v结构中的多位点协同作用不仅促进了NO_x^-的吸附和活化, 而且抑制了电催化过程中Cu物种从催化剂上的溶出, 从而提高了催化剂的稳定性. 本研究为设计高效稳定的NO₃RR催化剂提供了新思路.

关键词: 电催化硝酸盐还原, 合成氨, Cu-O-Ti-O_v位点, 协同催化, Cu/TiO₂催化剂

Abstract:

Electrocatalytic nitrate reduction reaction (NO₃RR) has been capturing immense interest in the industrial application of ammonia synthesis, and it involves complex reaction routes accompanied by multi-electron transfer, thus causing a challenge to achieve high efficiency for catalysts. Herein, we customized the Cu-O-Ti-O_v (oxygen vacancy) structure on the Cu/TiO₂ catalyst, identified through density functional theory (DFT) calculations as the synergic active site for NO₃RR. It is found that Cu-O-Ti-O_v site facilitates the adsorption/association of NO_x^- and promotes the hydrogenation of NO₃^- to NH₃ via adsorbed ^*H species. This effectively suppresses the competing hydrogen evolution reaction (HER) and exhibits a lower reaction energy barrier for NO₃RR, with the reaction pathways: NO₃^* → NO₂^* → HONO^* → NO^* → ^*NOH → ^*N → ^*NH → ^*NH₂ → ^*NH₃ → NH₃. The optimized Cu/TiO₂ catalyst with rich Cu-O-Ti-O_v sites achieves an NH₃ yield rate of 3046.5 μg h^-1 mg_cat^-1 at -1.0 V vs. RHE, outperforming most of the reported activities. Furthermore, the construction of Cu-O-Ti-O_v sites significantly mitigates the leaching of Cu species, enhancing the stability of the Cu/TiO₂ catalyst. Additionally, a mechanistic study, using in situ characterizations and various comparative experiments, further confirms the strong synergy between Cu, Ti, and O_v sites, which is consistent with previous DFT calculations. This study provides a new strategy for designing efficient and stable electrocatalysts in the field of ammonia synthesis.

Key words: Electrocatalytic nitrate reduction, Ammonia synthesis, Cu-O-Ti-O_v site, Synergic catalytic effect, Cu/TiO₂ catalyst

聂翼飞, 颜红萍, 鹿苏微, 张宏伟, 齐婷婷, 梁诗景, 江莉龙. 理论指导构建Cu-O-Ti-O_v活性位点及其高效电催化还原硝酸根研究[J]. 催化学报, 2024, 59: 293-302.

Yifei Nie, Hongping Yan, Suwei Lu, Hongwei Zhang, Tingting Qi, Shijing Liang, Lilong Jiang. Theory-guided construction of Cu-O-Ti-O_v active sites on Cu/TiO₂ catalysts for efficient electrocatalytic nitrate reduction[J]. Chinese Journal of Catalysis, 2024, 59: 293-302.

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图/表 6

Fig. 1. (a) The adsorption energy of NO3- on the Cu-O-Ti-Ov, Ti-Ov-Ti and Cu-O-Ti structure. (b) The energy profiles for HER on the Cu-O-Ti-Ov and Cu-O-Ti structure. (c) The energy profiles for NO3RR on the Cu-O-Ti-Ov structure.

Fig. 2. (a) Scheme for the synthesis of CT-U. (b) TEM image of TiO2 (inset: HRTEM image of TiO2). (c) TEM image of CT-4 (inset: HRTEM image of CT-4). (d) TEM image of CT-U (inset: HRTEM image of CT-U). (e) Elemental mapping of CT-U.

Fig. 3. (a) XRD patterns of TiO2, CT-4, and CT-U. (b) Raman spectra of CT-x and TiO2. (c) Comparison of Raman spectra for TiO2, CT-4 and CT-U. (d) EPR spectra of TiO2, CT-4 and CT-U. O 1s (e) and Ti 2p (f) of TiO2, CT-4 and CT-U. Cu 2p (g) and Cu LMM XPS (h) spectra of CT-4 and CT-U.

Fig. 4. (a) LSV curves of CT-4 with and without NO3-. (b) NH3 yield rates of TiO2, CT-x, and CT-U. (c) Faradaic efficiency of CT-x, TiO2 and CT-U. (d) Controlled experiments for CT-U. (e) Comparison of NH3 yield rate detected by indophenol blue method (UV) and ion chromatography (IC) on CT-U. (f) Comparison of the NO3RR activity of the CT-U with other catalysts reported in the literature.

Fig. 5. (a) The consecutive cycles for CT-4 and CT-U. (b) O 1s XPS spectra of original CT-U, CT-U after 8 cycles, and heat-treated CT-U. (c) The catalytic performances for original CT-U, CT-U after 8 cycles, and heat-treated CT-U. (d) Concentration of NO3- and NO2- in the reaction process.

Fig. 6. In situ electrochemical FTIR (a) and Raman (b) spectra for NO3RR on CT-U.

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理论指导构建Cu-O-Ti-O_v活性位点及其高效电催化还原硝酸根研究

Theory-guided construction of Cu-O-Ti-O_v active sites on Cu/TiO₂ catalysts for efficient electrocatalytic nitrate reduction

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理论指导构建Cu-O-Ti-Ov活性位点及其高效电催化还原硝酸根研究

Theory-guided construction of Cu-O-Ti-Ov active sites on Cu/TiO2 catalysts for efficient electrocatalytic nitrate reduction

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理论指导构建Cu-O-Ti-O_v活性位点及其高效电催化还原硝酸根研究

Theory-guided construction of Cu-O-Ti-O_v active sites on Cu/TiO₂ catalysts for efficient electrocatalytic nitrate reduction