4d金属掺杂液态Ga用于宽N2浓度下的高效氨电合成

doi:10.1016/S1872-2067(24)60144-0

催化学报 ›› 2024, Vol. 67: 194-203.DOI: 10.1016/S1872-2067(24)60144-0

• 论文 • 上一篇

4d金属掺杂液态Ga用于宽N₂浓度下的高效氨电合成

魏莹莹, 孙昱垚, 于耀东, 石月, 吴哲, 王磊, 赖建平()

青岛科技大学化学与分子工程学院, 生态化工国家重点实验室基地, 生态化学工程与绿色制造国际科技合作基地, 山东青岛 266042

收稿日期:2024-08-31 接受日期:2024-09-11 出版日期:2024-11-30 发布日期:2024-11-30
通讯作者: 赖建平
基金资助:
国家自然科学基金(52272222);泰山学者青年专家计划(tsqn201909114);泰山学者青年专家计划(tsqn201909123);山东省高校青年创新团队(202201010318)

4 d Metal-doped liquid Ga for efficient ammonia electrosynthesis at wide N₂ concentrations

Yingying Wei, Yuyao Sun, Yaodong Yu, Yue Shi, Zhe Wu, Lei Wang, Jianping Lai()

State Key Laboratory Base of Eco-Chemical Engineering, International Science and Technology Cooperation Base of Eco-chemical Engineering and Green Manufacturing, College of Chemistry and Molecular Engineering, Qingdao University of Science and Technology, Qingdao 266042, Shandong, China

Received:2024-08-31 Accepted:2024-09-11 Online:2024-11-30 Published:2024-11-30
Contact: Jianping Lai
Supported by:
National Natural Science Foundation of China(52272222);Taishan Scholar Young Talent Program(tsqn201909114);Taishan Scholar Young Talent Program(tsqn201909123);University Youth Innovation Team of Shandong Province(202201010318)

摘要/Abstract

摘要：

工业使用的氨主要采用Haber-Bosch工艺生产, 该过程耗能巨大, 且每年工业生产氨会排放约4.2亿吨二氧化碳, 与当前低碳环保理念不符. 电催化氮还原反应(eNRR)是一种很有前途的氨合成途径, 该反应由太阳能或可再生能源提供电能, 在常温常压下进行. 然而, 目前研究的eNRR都是在N₂饱和的环境中进行的, 并且使用高纯度的N₂作为原料, 成本较高. 因此, 设计和开发适用于大范围N₂浓度的高效电催化eNRR催化剂是非常有吸引力和挑战性的. p嵌段金属由于其高丰度和低成本被广泛研究用于eNRR. 更重要的是, p嵌段金属占据的p轨道给N₂未占据的反键轨道提供电子, 从而有效地削弱N≡N. 许多关于p嵌段金属基电催化剂的设计和调控及其性能改进策略的研究已经被报道. 虽然有报道称3d元素的掺杂可以在一定程度上降低加氢过程的能垒, 但所报道的催化剂中间体吸附能力较弱, 产物脱附困难, 影响了催化性能. 因此, 相似的吸附能导致增强了中间体吸附和促进产物脱附之间的内在矛盾, 这反过来又阻碍了p嵌段金属基催化剂实现高效合成氨. 结合最近的研究, 与3d元素相比, 4d元素能够通过轨道间相互作用有效地调节电子结构.

本文引入了一种协同策略, 通过将超低含量的4d元素Ru加入液态金属Ga中, 来调节Ga的电子结构和促进活性位点的持续暴露. 该策略为解决关键中间体覆盖率低和产物解吸困难的问题提供了新的思路, 并在较宽的N₂浓度下实现了高效的eNRR. 优化后的催化剂以高纯N₂为原料气时, 在‒0.3 V vs. RHE的过电位下实现了高达126.0 μg h^‒1 mg_cat^‒1的氨产率, 在‒0.1 V vs. RHE下法拉第效率高达60.4%. 在较低N₂浓度时, 该催化剂的氨产率均大于100 μg^‒1 mg_cat^‒1, 法拉第效率高于47%. 此外, 为了研究Ru_0.06/LM@C催化剂在eNRR中的实际应用潜力, 制备了气体扩散电极来提高气体对电化学界面的可及性, 并在阴离子交换膜(AEM)电解槽中测试了催化剂的eNRR性能. 将催化剂应用于AEM电解槽阴极时, 在1.7 V的电压下可以稳定运行100 h, 产氨法拉第效率为26.34 ± 2.23%, 能量效率为11.47 ± 0.97%. X射线光电子能谱和密度泛函理论(DFT)计算结果表明, Ru的掺杂有效地调节了Ga的电子结构, 导致电子向N₂转移, 使催化剂和N₂之间形成更强的共价相互作用, 更有利于N₂的吸附和活化. 此外, Ru的引入也降低了中间体生成的能垒, 更有利于加氢过程的进行. DFT计算证明了Ru_0.06/Ga@C (Ru的质量含量为0.06时)材料本身具有促进产物解吸的作用. 此外, 液体催化剂利用其流动性能够提供更高密度的活性位点. 原位红外光谱和N₂-程序升温脱附证实了Ru掺杂、材料的促进产物脱附能力以及液态催化剂更高密度的活性位点间的协同作用, 优化了N₂的传质途径, 使得关键中间体具有高覆盖率.

总之, 本文提出了一种将4d元素Ru掺杂与液态催化剂流动性相结合的策略. 一系列实验和DFT计算证实, Ru掺杂和液态催化剂流动性的协同效应优化了N₂传质路径, 降低了氢化能垒, 从而提高了关键中间体的覆盖率, 进而在较宽的N₂浓度范围内实现了高氨产量, 本文策略的实现也为电催化的其他领域提供了新思路.

关键词: 液态催化剂, 电催化, 氮还原反应, 氨合成, 电催化剂

Abstract:

Electrocatalytic nitrogen reduction reaction under ambient conditions is a promising pathway for ammonia synthesis. Currently nitrogen reduction reactions are carried out in N₂-saturated environments and use high-purity nitrogen as feedstock, which is costly. Here, we prepared carbon-coated ultra-low 4d metal Ru-doped liquid metal Ga (Ru_0.06/LM@C) for NRR over a wide range of N₂ concentrations. Comprehensive analyses show that the introduction of the ultra-low 4d element Ru can effectively adjust the electronic structure through orbital interactions, thus enhancing the adsorption of nitrogen-containing intermediates. The liquid catalyst utilized its mobility to provide a higher density of active sites. In addition, the material Ru_0.06/Ga@C itself has the ability to promote product desorption. The three act synergistically to optimize the N₂ mass transfer path, thereby increasing the *NNH coverage and further improving the ammonia yield over a wide range of N₂ concentrations. The maximum NH₃ yield of the catalyst can reach 126.0 μg h^-1 mg_cat^-1 (at -0.3 V vs. RHE) with high purity N₂ as feed gas, and the Faraday efficiency is 60.4% at -0.1 V vs. RHE. Over a wide range of N₂ concentrations, the NH₃ yield of the catalyst was greater than 100 μg h^-1 mg_cat^-1 with a Faraday efficiency higher than 47%. The catalytic performance is much higher than that of solid Ga@C and reported p-block metal-based catalysts.

Key words: Liquid catalyst, Electrocatalysis, Nitrogen reduction reaction, Ammonia synthesis, Electrocatalyst

魏莹莹, 孙昱垚, 于耀东, 石月, 吴哲, 王磊, 赖建平. 4d金属掺杂液态Ga用于宽N₂浓度下的高效氨电合成[J]. 催化学报, 2024, 67: 194-203.

Yingying Wei, Yuyao Sun, Yaodong Yu, Yue Shi, Zhe Wu, Lei Wang, Jianping Lai. 4 d Metal-doped liquid Ga for efficient ammonia electrosynthesis at wide N₂ concentrations[J]. Chinese Journal of Catalysis, 2024, 67: 194-203.

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链接本文: https://www.cjcatal.com/CN/10.1016/S1872-2067(24)60144-0

https://www.cjcatal.com/CN/Y2024/V67/I12/194

图/表 5

Fig. 1. Morphology and composition characterizations of Ru0.06/LM@C catalyst. (a) SEM image. (b) TEM image. (c) The corresponding EDS elemental mappings. HRTEM image (d) and enlarged images (e). (f) XRD patterns. XPS spectra of the Ru0.06/LM@C catalyst: (g) Ga 2p; (h) Ru 3p1/2; (i) C 1s.

Fig. 2. Electrochemical nitrogen reduction performance of Ru0.06/LM@C catalysts. (a) LSV curves in high-purity N2 and Ar atmospheres. (b) The obtained NH3 yield and corresponding FEs at the given potential in high-purity N2 atmospheres with a constant flow rate of 30 mL min-1. (c) NH3 yield and FE at different N2 partial pressures. (d) Comparison of the NRR performance of Ru0.06/LM@C with that of other reported catalysts. The orange balls represent the performance of this work. The unit of NH3 yield in the graph is μg h-1 mgcat-1. (e) Recycling test for 12 times of Ru0.06/LM@C catalyst at -0.3 V vs. RHE.

Fig. 3. Performance of Ru0.06/LM@C catalyst on AEM electrolyzer. (a) Schematic diagram of the AEM electrolyzer. (b) LSV curves of Ru0.06/LM@C (-) || RuO2 (+) in the AEM electrolyzer. (c) Current density-dependent FE and voltage in an AEM electrolyser. Error bars represent the standard deviation of three independent measurements. (d) Chronoamperometric current curves of Ru0.06/LM@C (-) || RuO2 (+) at a cell voltage of 1.7 V (blue dots are Ammonia FE, green line is current density).

Fig. 4. DFT calculation. (a) Free energy of H2O dissociation process on Ga@C and Ru0.06/Ga@C. (b) The charge difference of N2 adsorbed on Ga@C (left) and Ru0.06/Ga@C (right). (c) The DOS patterns of Ga@C. (d) The DOS patterns of Ru0.06/Ga@C. (e) Gibbs free energy diagrams of NRR on the Ru0.06/Ga@C and Ga@C.

Fig. 5. Exploration of NRR mechanism on Ru0.06/LM@C. (a) In situ FTIR spectra of Ru0.06/LM@C catalyst in 0.1 mol L?1 KOH at different potentials. (b) The variable temperature in situ FTIR spectra. (c) N2-TPD of Ru0.06/LM@C and Ga@C. (d) Simplification of the NH3 generation mechanism on Ru0.06/LM@C.

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4d金属掺杂液态Ga用于宽N₂浓度下的高效氨电合成

4 d Metal-doped liquid Ga for efficient ammonia electrosynthesis at wide N₂ concentrations

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