构筑富含磷空位缺陷的磷化钯催化剂实现高效和抗CO毒化的碱性氢氧化反应

doi:10.1016/S1872-2067(23)64570-X

催化学报 ›› 2024, Vol. 56: 176-187.DOI: 10.1016/S1872-2067(23)64570-X

• 论文 • 上一篇

构筑富含磷空位缺陷的磷化钯催化剂实现高效和抗CO毒化的碱性氢氧化反应

杨玉婷^a^,^b^,¹, 石路岩^a^,¹, 梁沁睿^a, 刘奕^a, 董家新^a, 王宝^c, 杨秀林^a^,^*()

^a广西师范大学化学与药学学院, 广西低碳能源材料重点实验室, 广西桂林541004, 中国
^b中山大学环境科学与工程学院, 广东广州510275, 中国
^c中国科学院过程工程研究所, 生化工程国家重点实验室, 北京100190, 中国
^d阿卜杜拉国王科技大学的沙特阿拉伯基础工业公司, 图瓦勒, 沙特阿拉伯

收稿日期:2023-09-11 接受日期:2023-11-07 出版日期:2024-01-18 发布日期:2024-01-10
通讯作者: *电子信箱: xlyang@gxnu.edu.cn (杨秀林), isimjant@sabic.com (Tayirjan Taylor Isimjan).
作者简介:¹共同第一作者.
基金资助:
国家自然科学基金(52363028);国家自然科学基金(21965005);广西自然科学基金(2021GXNSFAA076001);大学生创新创业训练项目(202210602045);广西研究生教育创新计划项目(YCSW2023140);广西科技基地与人才课题(GUIKE AD20297039)

Uleashing efficient and CO-resilient alkaline hydrogen oxidation of Pd₃P through phosphorus vacancy defect engineering

Yuting Yang^a^,^b^,¹, Luyan Shi^a^,¹, Qinrui Liang^a, Yi Liu^a, Jiaxin Dong^a, Tayirjan Taylor Isimjan^d^,^*(), Bao Wang^c, Xiulin Yang^a^,^*()

^aGuangxi Key Laboratory of Low Carbon Energy Materials, School of Chemistry and Pharmaceutical Sciences, Guangxi Normal University, Guilin 541004, Guangxi, China
^bSchool of Environmental Science and Engineering, Sun Yat-sen University, Guangzhou 510275, Guangdong, China
^cState Key Laboratory of Biochemical Engineering, Institute of Process Engineering, Chinese Academy of Sciences, Beijing 100190, China
^dSaudi Arabia Basic Industries Corporation (SABIC) at King Abdullah University of Science and Technology (KAUST), Thuwal 23955-6900, Saudi Arabia

Received:2023-09-11 Accepted:2023-11-07 Online:2024-01-18 Published:2024-01-10
Contact: *E-mail: xlyang@gxnu.edu.cn (X. Yang), isimjant@sabic.com (T. T. Isimjan).
About author:¹Contributed equally to this work.
Supported by:
National Natural Science Foundation of China(52363028);National Natural Science Foundation of China(21965005);Natural Science Foundation of Guangxi Province(2021GXNSFAA076001);Innovation and entrepreneurship training for college students(202210602045);Innovation Project of Guangxi Graduate Education(YCSW2023140);Guangxi Technology Base and Talent Subject(GUIKE AD20297039)

摘要/Abstract

摘要：

碱性阴离子交换膜燃料电池(AEMFCs)可以直接将氢的化学能转化为电能, 被认为是新兴绿色氢经济的基石技术. 但其阳极氢氧化反应(HOR)动力学缓慢, 严重依赖于Pt基催化剂. 由于Pt基催化剂极易被CO毒化、动力学过程复杂以及价格昂贵, 极大限制了其商业化应用. 因此, 亟需开发高效、稳定和抗CO毒化能力强的新型HOR催化剂. Pd具有与Pt相似的氢键结合能, 并且比Pt储量丰富, 有望成为实现HOR的候选催化剂. 然而, Pd的本征催化活性和Pt相比仍有很大差距. 近年来, 磷化钯因具有功能多样性和高催化活性被广泛关注. 此外, 缺陷工程可以有效调控催化剂的表面结构, 改善中间体的吸附强度, 提高催化剂的催化活性. 因此, 构建富含缺陷的磷化钯催化剂有望提高其HOR的性能. 然而, 该方向研究较少, 反应机理尚不清楚. 因此, 阐明空位缺陷对于提高磷化钯催化剂HOR性能的作用机制, 对促进AEMFCs电催化反应具有重要意义.

本文通过溶胶-凝胶法以及低温磷化策略合成了一种碗状半球结构的富含磷空位Pd₃P@C (V_p-Pd₃P@C)催化剂, 并用于碱性HOR. 在磷化过程中, 通过调整Pd前驱体和磷源比例以及煅烧温度, 在碳碗状半球载体上合成具有不同晶相组成(Pd/Pd₃P@C, Pd_3.20P₁₂@C, Pd₃P@C, 和Pd₅P₂@C)的Pd_xP_y@C催化剂. 扫描电镜和透射电镜证实了催化剂为碗状半球形貌. 利用电子顺磁共振波谱研究了Pd_xP_y@C催化剂的磷空位浓度, 结果表明, Pd/P比例为1:3时, 在350 °C下煅烧得到的V_p-Pd₃P@C具有最高的磷空位浓度. X射线光电子能谱证实了磷空位促进了d-p轨道杂化, 增强了Pd和磷之间的电子相互作用. 电化学测试结果表明, V_p-Pd₃P@C具有最高的HOR性能, V_p-Pd₃P@C在50 mV的质量活性为1.66 mA μg_Pd^-1, 交换电流密度为3.2 mA cm^-2, 优于Pd₃P (0.45 mA μg_Pd^-1, 1.78 mA cm^-2)和商业Pt/C (0.3 mA μg_Pt^-1, 2.29 mA cm^-2). 同时, 该催化剂在50 mV的电位下能稳定运行20 h. 此外, 即使在CO浓度高达1000 ppm时, V_p-Pd₃P@C催化剂仍表现出较好的HOR活性. 紫外光电子能谱证实了V_p-Pd₃P@C中的Pd原子呈现缺电子状态, 这不利于Pd 4d轨道对CO 2π*轨道的电子反馈, 降低了Pd和CO的键合强度, 进而减弱了Pd对CO分子的吸附, 从而增强了其抗CO中毒的能力. 密度泛函理论计算结果表明, 相较于磷空位浓度较少的Pd₃P@C催化剂, 富含磷空位缺陷的V_p-Pd₃P@C催化剂能够优化和平衡反应中间体(H_ads和OH_ads)的吸附强度, 使速率决定步骤从H₂O*的解吸转换到H₂O的形成, 促进了Volmer反应(H_ads + OH_ads → H₂O + 2*sites)的进行, 进而提升了催化活性. 系统实验和表征结果表明, V_p-Pd₃P@C较好的HOR性能可归因于以下3个因素: (1) 空心碗状结构大大地增加了固-液-气三相接触点, 加速了HOR的传质过程; (2) 磷空位产生的局部反应活性和有利的电子结构优化了H_ads和OH_ads的吸附强度, 极大地促进了Volmer步骤; (3) 丰富的磷空位打破了原有的周期性晶体结构, 形成了新的电子结构, 有效地抑制了电子从Pd 4d轨道到CO 2π*轨道的反馈, 提高了V_p-Pd₃P@C对CO的耐受能力.

综上, 本文通过缺陷工程策略调控了V_p-Pd₃P@C中活性位点与HOR关键中间体的相互作用, 明确了空位缺陷浓度与HOR活性之间的构效关系. 并从碱性HOR反应机理, CO分子与金属催化剂的轨道相互作用以及结构设计三个方面总结了高效和稳定的HOR催化剂的设计原则. 目前, 由于界面环境的复杂性和缺乏原位技术, 催化剂表面上痕量中间体的光谱信息难以获得, 未来可在开发原位技术监测HOR过程中间体和催化剂的组分变化方面做出更多的努力, 以促进AEMFCs的商业化应用.

关键词: 氢氧化反应, CO耐受性, 磷空位, V_p-Pd₃P@C, 碗状半球

Abstract:

A high-performance and highly CO-resilient hydrogen oxidation reaction (HOR) electrocatalyst is heralded as core material to solve the commercial deployment of hydrogen fuel cells. Phosphorus vacancies, as a type of delicate point defect, could effectively and flexibly modulate the catalytic performance. Therefore, based on the vacancy design philosophy of “less is more”, we synthesize a phosphorus-vacancy-rich Pd₃P@C (V_p-Pd₃P@C) catalyst with bowl-like hemisphere structure for alkaline HOR, for the first time. The V_p-Pd₃P@C catalyst exhibits remarkable mass activity and exchange current density of 1.66 mA μg_Pd^-1 and 3.2 mA cm^-2, respectively, surpassing those of Pd₃P@C (0.45 mA μg_Pd^-1, 1.78 mA cm^-2) and commercial Pt/C (0.3 mA μg_Pt^-1, 2.29 mA cm^-2). Intriguingly, the catalyst can tolerate 1000 ppm CO that Pt/C catalyst lacks. Density functional theory calculations uncover that the optimal local coordination environment and favorable electronic structure that rooted from phosphorus vacancy enable optimum adsorption kinetics of hydrogen and hydroxyl while concomitantly suppressing Pd 4d → CO 2π* back donation, contributing to the remarkable HOR reactivity and CO tolerance.

Key words: Hydrogen oxidation reaction, CO tolerance, Phosphorus vacancy, V_p-Pd₃P@C, Bowl-like hemisphere

杨玉婷, 石路岩, 梁沁睿, 刘奕, 董家新, 王宝, 杨秀林. 构筑富含磷空位缺陷的磷化钯催化剂实现高效和抗CO毒化的碱性氢氧化反应[J]. 催化学报, 2024, 56: 176-187.

Yuting Yang, Luyan Shi, Qinrui Liang, Yi Liu, Jiaxin Dong, Tayirjan Taylor Isimjan, Bao Wang, Xiulin Yang. Uleashing efficient and CO-resilient alkaline hydrogen oxidation of Pd₃P through phosphorus vacancy defect engineering[J]. Chinese Journal of Catalysis, 2024, 56: 176-187.

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https://www.cjcatal.com/CN/Y2024/V56/I1/176

图/表 6

Fig. 1. (a) Schematic protocol of the synthesis strategy for Vp-Pd3P@C. SEM images of SiO2/SiO2@RF (b), bowl-like hemispheres (c) and Vp-Pd3P@C (d). TEM (e) and HRTEM (f) images of the Vp-Pd3P@C (inset: the corresponding FFT pattern). (g) HAADF-STEM image and corresponding elemental mappings of Vp-Pd3P@C.

Fig. 2. (a,b) Powder XRD patterns of synthesized palladium phosphides (PdxPy@C). (c) Crystal structures of various palladium phosphides spanning a range of temperature and Pd:P mass ratios. (d) EPR spectra of PdxPy@C.

Fig. 3. High-resolution XPS spectra of Pd 3d (a,b), and P 2p (c) spectra of regions in PdxPy@C. (d) Pdδ+ and Pδ- percentages in PdxPy@C.

Fig. 4. (a) HOR polarization curves of Vp-Pd3P@C, Pd3P@C, Pd@C, commercial Pd/C and commercial Pt/C, respectively. (b) HOR polarization curves for Vp-Pd3P@C at various rotation speeds. Inset in b shows corresponding Koutecky-Levich plots at an overpotential of 75 mV. (c) Tafel plots. (d) Linear current potential region around the equilibrium potential of studied catalysts. (e) Comparison of apparent exchange current density (j0), kinetic current density (jk) at 50 mV, mass activity (MA) at 50 mV, ECSA, and specific activity (SA) at 50 mV of the comparative catalysts. (f) Comparison of mass activity at 50 mV and j0 with other recently reported excellent HOR catalysts. (g) HOR polarization curves for Vp-Pd3P@C and Pt/C in H2-saturated 0.1 mol L?1 KOH with (dashed lines) and without (solid lines) the presence of 1000 ppm CO. (h) HOR polarization curves for Vp-Pd3P@C in H2-saturated 0.1 mol L?1 KOH before and after 1000 cycles, respectively. Inset shows chronoamperometry (j-t) responses recorded on Vp-Pd3P@C at 50 mV.

Fig. 5. (a) Schematic diagram of σ-type/π-type orbital interactions between metal catalysts and CO molecules. (b) UPS spectra. (c) Band structure alignment of the Vp-Pd3P@C, Pd3P@C, and Pd@C. (d) CO stripping curves in N2-statured 0.1 mol L?1 KOH of Vp-Pd3P@C, Pd3P@C, and Pd@C. (e) Zeta potential of Vp-Pd3P@C, Pd3P@C, and Pd@C. Error bars represent the standard deviation for triplicated experiments.

Fig. 6. (a) Charge-density distribution of the Vp-Pd3P@C model, yellow and cyan areas indicate electron accumulation and depletion. (b) 2D charge difference isosurface based on DFT analysis, red is the electron-rich area while blue is the deficient area. (c) The PDOS of Pd 4d in Vp-Pd3P@C, Pd3P@C and Pd@C (each d-band center is marked by a dashed line). (d) Hydrogen binding energy on Vp-Pd3P@C, Pd3P@C, and Pd@C models. (e) Hydroxyl binding energy on Vp-Pd3P@C, Pd3P@C, and Pd@C models. (f) The reaction pathways of Vp-Pd3P@C, Pd3P@C, and Pd@C for alkaline HOR. (g) Schematic illustration of HOR catalysis on the Vp-Pd3P@C.

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构筑富含磷空位缺陷的磷化钯催化剂实现高效和抗CO毒化的碱性氢氧化反应

Uleashing efficient and CO-resilient alkaline hydrogen oxidation of Pd₃P through phosphorus vacancy defect engineering

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构筑富含磷空位缺陷的磷化钯催化剂实现高效和抗CO毒化的碱性氢氧化反应

Uleashing efficient and CO-resilient alkaline hydrogen oxidation of Pd3P through phosphorus vacancy defect engineering

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Uleashing efficient and CO-resilient alkaline hydrogen oxidation of Pd₃P through phosphorus vacancy defect engineering