硫代硫酸钠辅助合成高Pt含量燃料电池金属间电催化剂

doi:10.1016/S1872-2067(24)60127-0

催化学报 ›› 2024, Vol. 66: 292-301.DOI: 10.1016/S1872-2067(24)60127-0

• 论文 • 上一篇

硫代硫酸钠辅助合成高Pt含量燃料电池金属间电催化剂

殷诗怡^a, 许实龙^b^,^*(), 李子睿^a, 李帅^a, 薛锟泽^a, 张万群^a, 储胜启^c^,^*(), 梁海伟^a^,^*()

^a中国科学技术大学化学系, 合肥国家微尺度物理科学研究中心, 安徽合肥 230026
^b安徽建筑大学安徽省先进建材工程实验室, 安徽合肥 230601
^c中国科学院高能物理研究所, 北京 100049

收稿日期:2024-08-07 接受日期:2024-08-30 出版日期:2024-11-18 发布日期:2024-11-10
通讯作者: *电子信箱: hwliang@ustc.edu.cn (梁海伟),xslong@ahjzu.edu.cn (许实龙),chusq@ihep.ac.cn (储胜启).
基金资助:
国家自然科学基金(22325903);国家自然科学基金(22221003);国家自然科学基金(22071225);中国博士后面上基金(2022M712179);安徽省科技重大专项计划(202203a0520013);安徽省科技重大专项计划(2021d05050006);中国科大“双一流”项目科研经费(YD2060002032)

Sodium thiosulfate-assisted synthesis of high-Pt-content intermetallic electrocatalysts for fuel cells

Shi-Yi Yin^a, Shi-Long Xu^b^,^*(), Zi-Rui Li^a, Shuai Li^a, Kun-Ze Xue^a, Wanqun Zhang^a, Sheng-Qi Chu^c^,^*(), Hai-Wei Liang^a^,^*()

^aHefei National Research Center for Physical Sciences at the Microscale, Department of Chemistry, University of Science and Technology of China, Hefei 230026, Anhui, China
^bAnhui Advanced Building Materials Engineering Laboratory, Anhui Jianzhu University, Hefei 230601, Anhui, China
^cInstitute of High Energy Physics, Chinese Academy of Sciences, Beijing 100049, China

Received:2024-08-07 Accepted:2024-08-30 Online:2024-11-18 Published:2024-11-10
Contact: *E-mail: hwliang@ustc.edu.cn (H.-W. Liang),xslong@ahjzu.edu.cn (S.-L. Xu),chusq@ihep.ac.cn (S.-Q. Chu).
Supported by:
National Natural Science Foundation of China(22325903);National Natural Science Foundation of China(22221003);National Natural Science Foundation of China(22071225);fellowship of China Postdoctoral Science Foundation(2022M712179);Plan for Anhui Major Provincial Science & Technology Project(202203a0520013);Plan for Anhui Major Provincial Science & Technology Project(2021d05050006);USTC Research Funds of the Double First-Class Initiative(YD2060002032)

摘要/Abstract

摘要：

质子交换膜燃料电池(PEMFCs)是一种前景广阔的绿色能源技术, 但其商业化发展受到阴极氧还原反应(ORR)动力学缓慢、Pt/C催化剂成本高以及稳定性差等因素的制约. 通过将Pt与非贵金属(如Co、Fe)合金化,可以减少Pt用量并提高ORR活性. 相比无序固溶体合金, 有序结构的Pt基金属间化合物(IMCs)由于更强的应变和配体效应, 能进一步提升ORR活性, 并通过3d-5d轨道电子相互作用抑制非贵金属浸出, 增强耐久性. Pt基IMCs催化剂的合成通常需要在高温退火(> 700 °C)下进行, 以促进合金化并克服无序向有序转变的动力学阻碍. 然而, 高温退火通常会导致烧结、晶粒增大、电化学表面积减少, 催化活性降低, 尤其在高Pt含量催化剂中更明显. 为解决上述问题, 提出了碳包覆、金属有机框架限制、强锚定等策略, 但高Pt含量下难以控制晶粒尺寸或过程复杂, 不利于规模化生产.

本文提出了一种硫代硫酸钠辅助浸渍的策略, 用于合成高Pt载量(达到44.5 wt%)且小尺寸、高有序度的PtM-S IMCs (M = Co, Fe, Ni)催化剂. 在浸渍过程中, 硫代硫酸盐将H₂PtCl₆还原为均匀分散的Pt胶体, 并沉积在碳载体上, 从而防止了Pt在低温退火阶段团聚. 在高温热解过程中, 含S物质被掺杂进碳晶格中, 形成稳定的噻吩硫结构, Pt和S的强相互作用有效抑制了颗粒的烧结, 确保了在高温退火阶段形成小尺寸、高有序度的PtM-S IMCs的催化剂. 由于硫代硫酸钠辅助浸渍策略的便捷性和可扩展性, 成功合成了高有序度且小尺寸(3-5 nm)的PtM-S (M = Co, Fe, Ni) IMCs催化剂. 此外, 采用冷冻干燥技术, 实现了2.5 g高有序度(67.2%)的L10 PtCo-S IMCs催化剂的克级一批次合成. 随着Pt金属负载含量从27.2 wt%增加到44.5 wt%, 催化剂没有出现任何聚集和严重烧结现象, 且仍保持高有序度. 优化后的PtCo-S IMCs催化剂在单电池测试中表现出较好的电催化性能, 质量活性达到0.72 A mgPt^-1, 并在0.65 V, H₂/Air条件下实现了1.17 W cm^-2的高功率密度, 性能优于商业催化剂TKK-Pt/C. PtCo-S催化剂ORR性能的提升, 归因于PtCo@Pt核壳结构表面Pt的压缩应变, 使得d带中心下移, 从而减弱了对含氧中间体的吸附强度. 此外, PtCo-S催化剂在加速应力测试后, 仍保留74%的质量活性, 耐久性显著优于商业催化剂TKK-Pt/C. PtCo-S催化剂的核壳结构显著提高了催化剂的稳定性, 抑制了Co从内核的进一步浸出. 同时, 3d-5d轨道间的强电子相互作用也有效阻碍了Co的浸出.

综上, 硫代硫酸钠辅助合成策略可以有效地抑制金属烧结和相分离, 从而制备出高Pt含量、小尺寸且高有序度的PtM-S IMCs (M = Co, Fe, Ni)催化剂. 同时, 该策略的便捷性、可扩展性和经济性使规模化的生产成为可能. 合成的PtM-S IMCs (M = Co, Fe, Ni)催化剂在燃料电池单电池测试中表现出高活性与稳定性, 为设计高性能质子交换膜燃料电池阴极催化剂提供了新思路.

关键词: 硫代硫酸钠, 小尺寸, Pt基金属间化合物, 高Pt含量, 质子交换膜燃料电池

Abstract:

Carbon supported Pt-based intermetallic compounds (IMCs) with high activity and durability are the most competitive cathode catalysts for the commercialization of proton exchange membrane fuel cells (PEMFCs). The synthesis of Pt-based intermetallics with a good balance between small size and high metal loading remains challenging because of the high-temperature annealing that is generally required to form intermetallic phases. We developed a sodium thiosulfate-assisted impregnation strategy to synthesize small-sized and highly ordered PtM IMCs catalysts (M = Co, Fe, Ni) with high-Pt-content (up to 44.5 wt%). During the impregnation process, thiosulfate could reduce H₂PtCl₆ to form uniformly dispersed Pt colloid on carbon supports, which in turn prevents the aggregation of Pt at the low-temperature annealing stage. Additionally, the strong interaction between Pt and S inhibits particle sintering, ensuring the formation of small-sized and uniform PtM intermetallic catalysts at the high-temperature annealing stage. The optimized intermetallic PtCo catalyst delivered a high mass activity of 0.72 A mg_Pt^-1 and a large power performance of 1.17 W cm^-2 at 0.65 V under H₂-air conditions, along with 74% mass activity retention after the accelerated stress test.

Key words: Sodium thiosulfate, Small-sized, Pt-based intermetallic compound, High-Pt-content, Proton exchange membrane fuel cells

殷诗怡, 许实龙, 李子睿, 李帅, 薛锟泽, 张万群, 储胜启, 梁海伟. 硫代硫酸钠辅助合成高Pt含量燃料电池金属间电催化剂[J]. 催化学报, 2024, 66: 292-301.

Shi-Yi Yin, Shi-Long Xu, Zi-Rui Li, Shuai Li, Kun-Ze Xue, Wanqun Zhang, Sheng-Qi Chu, Hai-Wei Liang. Sodium thiosulfate-assisted synthesis of high-Pt-content intermetallic electrocatalysts for fuel cells[J]. Chinese Journal of Catalysis, 2024, 66: 292-301.

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图/表 6

Fig. 1. Schematic illustration of the Pt-M (M = Co, Fe, and Ni) IMCs catalysts formation with or without Na2S2O3 by an industrially relevant impregnation-reduction approach.

Fig. 2. XRD patterns of PtM-S and PtM (M = Co, Fe, and Ni). XRD patterns of PtCo (a), PtFe (b), and PtNi (c) prepared with or without Na2S2O3. Asterisks marked in (a-c) are the characteristic super-lattice peaks of ordered intermetallic structures. (d-f) The (111) diffraction peaks originate from the magnified region in the red box of (a-c). The insets show the particle size and distribution estimation by XRD results (order from left to right: dark blue represents Pt-rich phase, purple represents M-rich phase, and light blue represents single M phase).

Fig. 3. HAADF-STEM images and particle size distributions of PtM-S and PtM (M = Co, Fe, and Ni). HAADF-STEM images and particle size distribution of PtCo (a), PtFe (b), PtNi (c), PtCo-S (d), PtFe-S (e), and PtNi-S (f). (g) Violin plots of number-average particle size distributions for between PtM-S and PtM catalysts (M = Co, Fe, and Ni). (h) Violin plots of number-average particle size distributions for PtCo-S and PtCo catalysts with various Pt loading from 27.1 wt% to 44.5 wt%. (i) Comparison of Pt-based intermetallic size between our work and the state-of-art in the literature. The red shaded areas represent the size distribution range of PtCo-S IMCs with different loadings prepared in our work.

Fig. 4. Formation mechanism of PtCo-S IMCs. (a) UV-vis spectra of the H2PtCl6·6H2O solution, Na2S2O3 solution, and the mixture solution of H2PtCl6·6H2O and Na2S2O3. The photographs showed the color change of Na2S2O3 with H2PtCl6 after 24 hours. (b) Comparison of XPS results of the Pt 42f of PtCo-S/C precursor powder and PtCo/C precursor powder. (c) XANES spectra of PtCo-S/C precursor powder, PtCo/C precursor powder, PtS2 and Pt foil. XRD patterns of Pt/C (d), Pt-S/C (e), and PtCo-S/C (f) were prepared under elevated temperatures. (g) EXAFS spectra at Pt L3-edge for PtCo-S/C catalysts at 300 and 900 °C, referenced PtO2, PtS2 and Pt foil. XPS spectra of Pt 4f (h) and S 2p (i) for PtCo-S catalysts from 300 to 900 °C.

Fig. 5. Structure evolution of PtCo-S catalyst after post-treatment with H2O2 oxidation, H2SO4 etching and H2 reduction treatment. (a) Schematic illustration of structure evolution of PtM-S (M = Co, Fe, Ni) IMC catalyst from L10-Pt1M1 to Pt1M1@Pt core-shell structure. (b) Comparison of XRD patterns of PtCo-S IMC catalyst after post-treatment. (c) The change of ordering degree and atom ratio of Pt/Co for PtCo-S IMC catalyst after post-treatment. Atomic-resolution HAADF-STEM image (d) and corresponding line-profile (e) taken from red region of (d), and EDS line scanning (f) of Pt1Co1@Pt core-shell structure.

Fig. 6. MEA performance. H2-air single-cell polarization curves and power density plots of the PtCo-S (a) and TKK-Pt/C (b) cathodes under beginning-of-life (BOL) and end-of-life (EOL) after 30000 AST. Test conditions: cathode loading of 0.1 mgPt cm-2, 80 °C, 100% relative humidity, 150 kPaabs; H2 and air flow rates were fixed at 0.5 and 2.0 L min-1, respectively. Current density and power density of PtCo-S (c) and TKK-Pt/C (d) cathodes at BOL and EOL. (e) MA at 0.9?V in H2-O2 fuel cells and the voltage at 0.8 A?cm-2 in H2-air fuel cells at BOL and EOL. (f) ECSA was measured by CO stripping at BOL and EOL.

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硫代硫酸钠辅助合成高Pt含量燃料电池金属间电催化剂

Sodium thiosulfate-assisted synthesis of high-Pt-content intermetallic electrocatalysts for fuel cells

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