导电共聚物衍化新策略制备硫、氮共掺杂碳纳米管及其对改善PtCu纳米晶分散性与甲醇电催化氧化的促进作用

doi:10.1016/S1872-2067(20)63748-2

催化学报 ›› 2021, Vol. 42 ›› Issue (7): 1205-1215.DOI: 10.1016/S1872-2067(20)63748-2

导电共聚物衍化新策略制备硫、氮共掺杂碳纳米管及其对改善PtCu纳米晶分散性与甲醇电催化氧化的促进作用

钟静萍^a^,^d^,†, 黄科薪^a^,†, 许文涛^a, 唐华果^a, Muhammad Waqas^a, 樊友军^a^,^*(), 王睿翔^a, 陈卫^a^,^#(), 王沂轩^b^,^c^,^$()

^a广西师范大学化学与药学院, 广西低碳能源材料重点实验室, 广西桂林541004, 中国
^b美国奥尔巴尼州立大学化学与法医学系, 奥尔巴尼, GA 31705, 美国
^c齐鲁工业大学(山东科学院), 山东省分子工程重点实验室, 山东济南250010, 中国
^d广西医科大学生命科学研究院, 广西组织器官再生生物医学材料工程中心, 广西南宁530021, 中国

收稿日期:2020-10-22 接受日期:2020-11-27 出版日期:2021-07-18 发布日期:2020-12-10
通讯作者: 樊友军,陈卫,王沂轩
作者简介:^$ 电子信箱: yixuan.wamg@asurams.edu
^# 电子信箱: weichen@mailbox.gxnu.edu.cn;
^* 电子信箱: youjunfan@mailbox.gxnu.edu.cn;
^†共同第一作者.
基金资助:
国家自然科学基金(21463007);广西自然科学基金(2017GXNSFDA198031);广西自然科学基金(2019GXNSFGA245003)

New strategy of S,N co-doping of conductive-copolymer-derived carbon nanotubes to effectively improve the dispersion of PtCu nanocrystals for boosting the electrocatalytic oxidation of methanol

Jingping Zhong^a^,^d^,†, Kexin Huang^a^,†, Wentao Xu^a, Huaguo Tang^a, Muhammad Waqas^a, Youjun Fan^a^,^*(), Ruixiang Wang^a, Wei Chen^a^,^#(), Yixuan Wang^b^,^c^,^$()

^aGuangxi Key Laboratory of Low Carbon Energy Materials, School of Chemistry and Pharmaceutical Sciences, Guangxi Normal University, Guilin 541004, Guangxi, China
^bDepartment of Chemistry and Forensic Science, Albany State University, Albany, GA 31705, USA
^cProvincial Key Laboratory of Molecular Engineering, Qilu University of Technology (Shandong Academy of Sciences), Jinan 250010, Shandong, China
^dGuangxi Engineering Center in Biomedical Material for Tissue and Organ Regeneration, Life Sciences Institute, Guangxi Medical University, Nanning 530021, Guangxi, China

Received:2020-10-22 Accepted:2020-11-27 Online:2021-07-18 Published:2020-12-10
Contact: Youjun Fan,Wei Chen,Yixuan Wang
About author:^$ E-mail: yixuan.wamg@asurams.edu
^# E-mail: weichen@mailbox.gxnu.edu.cn;
^* E-mail: youjunfan@mailbox.gxnu.edu.cn;
^† These authors contributed equally to this work.
Supported by:
National Natural Science Foundation of China(21463007);Natural Science Foundation of Guangxi Province(2017GXNSFDA198031);Natural Science Foundation of Guangxi Province(2019GXNSFGA245003)

摘要/Abstract

摘要：

有效调控碳纳米材料的几何和电子结构的协同效应和缺陷是获得优良电化学性能的关键. 然而, 如何设计一种具有优势结构的杂化材料及对其电催化机理的认识尚不清楚. 本文提出了一种聚(3,4-乙撑二氧噻吩)/聚苯胺导电共聚物热解策略来制备S和N共掺杂多壁碳纳米管(MWCNTs), 发现改变前驱体溶液中两种单体的比例可以调控掺杂MWCNTs中S和N原子的含量与表面活性位结构. S和N的共掺杂明显增大了碳纳米管表面的缺陷程度并暴露出更丰富的活性位点, 从而有利于超细Pt和PtCu纳米颗粒的均匀分布和沉积. 透射电镜和扫描透射电镜结果表明, 所制备S和N共掺杂MWCNTs(SN-MWCNTs)负载的催化剂中Pt和PtCu纳米颗粒以及掺杂的S和N原子都均匀地分布在MWCNTs上, 且沉积的Pt和PtCu纳米颗粒的平均尺寸仅分别为2.30和2.87 nm. X射线光电子能谱结果表明, S和N共掺杂MWCNTs与负载的Pt基纳米颗粒之间存在强烈的电荷转移相互作用, 明显改变了贵金属Pt的表面电子结构. 电化学测试结果表明, 与Pt/SN-MWCNTs, Pt/N-MWCNTs, Pt/S-MWCNTs和商业Pt/C催化剂相比, Pt₁Cu₂/SN-MWCNTs表现出更大的电化学活性表面积(148.85 m² g^-1), 更高的甲醇氧化质量活性(1589.9 mA mg_Pt^-1)、电化学稳定性和抗CO毒化能力. 密度泛函理论研究表明, S和N共掺杂导致碳纳米管极大地变形, 同时极化和激活了相邻的C原子. 因此, 增强了Pt₁Cu₂纳米颗粒在SN-MWCNTs上的吸附以及随后甲醇分子的吸附. 此外, Pt₁Cu₂/SN-MWCNTs对甲醇氧化的电催化活性均在热力学和动力学上优于相应的CNTs和N-CNTs基材料. 本文提供了一种新颖的在碳基材料上构建高度分散且稳定的Pt基纳米颗粒高性能燃料电池电催化剂的方法.

关键词: 甲醇氧化, 导电共聚物, 双掺杂碳纳米管, Pt基纳米颗粒, 密度泛函理论计算

Abstract:

Efficacious regulation of the geometric and electronic structures of carbon nanomaterials via the introduction of defects and their synergy is essential to achieving good electrochemical performance. However, the guidelines for designing hybrid materials with advantageous structures and the fundamental understanding of their electrocatalytic mechanisms remain unclear. Herein, superfine Pt and PtCu nanoparticles supported by novel S,N-co-doped multi-walled CNT (MWCNTs) were prepared through the innovative pyrolysis of a poly(3,4-ethylenedioxythiophene)/polyaniline copolymer as a source of S and N. The uniform wrapping of the copolymer around the MWCNTs provides a high density of evenly distributed defects on the surface after the pyrolysis treatment, facilitating the uniform distribution of ultrafine Pt and PtCu nanoparticles. Remarkably, the Pt₁Cu₂/SN-MWCNTs show an obviously larger electroactive surface area and higher mass activity, stability, and CO poisoning resistance in methanol oxidation compared to Pt/SN-MWCNTs, Pt/S-MWCNTs, Pt/N-MWCNTs, and commercial Pt/C. Density functional theory studies confirm that the co-doping of S and N considerably deforms the CNTs and polarizes the adjacent C atoms. Consequently, both the adsorption of Pt₁Cu₂ onto the SN-MWCNTs and the subsequent adsorption of methanol are enhanced; in addition, the catalytic activity of Pt₁Cu₂/SN-MWCNTs for methanol oxidation is thermodynamically and kinetically more favorable than that of its CNT and N-CNT counterparts. This work provides a novel method to fabricate high-performance fuel cell electrocatalysts with highly dispersed and stable Pt-based nanoparticles on a carbon substrate.

Key words: Methanol oxidation, Conductive copolymers, Dual-doped carbon nanotubes, Pt-based nanoparticles, DFT calculation

钟静萍, 黄科薪, 许文涛, 唐华果, Muhammad Waqas, 樊友军, 王睿翔, 陈卫, 王沂轩. 导电共聚物衍化新策略制备硫、氮共掺杂碳纳米管及其对改善PtCu纳米晶分散性与甲醇电催化氧化的促进作用[J]. 催化学报, 2021, 42(7): 1205-1215.

Jingping Zhong, Kexin Huang, Wentao Xu, Huaguo Tang, Muhammad Waqas, Youjun Fan, Ruixiang Wang, Wei Chen, Yixuan Wang. New strategy of S,N co-doping of conductive-copolymer-derived carbon nanotubes to effectively improve the dispersion of PtCu nanocrystals for boosting the electrocatalytic oxidation of methanol[J]. Chinese Journal of Catalysis, 2021, 42(7): 1205-1215.

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图/表 7

Fig. 1. (a) FTIR spectra for AO-MWCNTs, PEDOT-PANI/MWCNTs and SN-MWCNTs. (b) Raman spectra of AO-MWCNTs, PEDOT-PANI/MWCNTs and SN-MWCNTs. (c) XRD spectra of Pt/SN-MWCNTs, Pt/N-MWCNTs and Pt/S-MWCNTs. (d) XRD spectra for Pt1Cu3/SN-MWCNTs, Pt1Cu2/SN-MWCNTs, Pt1Cu1/SN-MWCNTs, Pt1Cu0.4/SN-MWCNTs and Pt/SN-MWCNTs.

Fig. 2. (a,b) TEM images of Pt1Cu2/SN-MWCNTs. The insets in (a) and (b) show the corresponding HRTEM images and size distribution histograms, respectively. (c) HAADF-STEM image of Pt1Cu2/SN-MWCNTs. (d-h) Element mappings for C, N, S, Pt and Cu.

Fig. 3. (a) XPS survey spectra for Pt1Cu2/SN-MWCNTs (1), Pt/SN-MWCNTs (2), Pt/N-MWCNTs (3) and Pt/S-MWCNTs (4). (b) Cu 2p high-resolution spectrum for Pt1Cu2/SN-MWCNTs. Pt 4f high-resolution spectra for Pt1Cu2/SN-MWCNTs (c) and Pt/SN-MWCNTs (d).

Fig. 4. Cyclic voltammograms for Pt1Cu2/SN-MWCNTs (1), Pt/SN-MWCNTs (2), Pt/N-MWCNTs (3), Pt/S-MWCNTs (4) and commercial Pt/C (5) catalysts in 0.5 M H2SO4 (a) and 0.5 M CH3OH + 0.5 M H2SO4 (b) solutions measured at a scan rate of 50 mV s-1; (c) CO stripping voltammograms for Pt1Cu2/SN-MWCNTs (1), Pt/SN-MWCNTs (2), Pt/N-MWCNTs (3), Pt/S-MWCNTs (4) and commercial Pt/C (5) catalysts in 0.5 M H2SO4 solution measured at a scan rate of 50 mV s-1; (d) Current-time curves measured at 0.6 V for methanol oxidation on different catalysts in 0.5 M CH3OH + 0.5 M H2SO4 solution.

Fig. 5. TEM images of Pt1Cu2/SN-MWCNTs (a,b), Pt/SN-MWCNTs (c,d) and commercial Pt/C (e,f) before and after 7200 s chronoamperometry tests in 0.5 M CH3OH + 0.5 M H2SO4 solution at a test potential of 0.6 V.

Fig. 6. HOMO of (5,5) CNT (a) and (5,5) S,N-CNT (b) with B3PW91 (isosurface = 0.004).

Fig. 7. Gibbs free energy profile (ΔG) for the electro-oxidation of CH3OH (CH3OH + H2O → CO2 + 6H+ + 6e-) catalyzed by bimetallic Pt1Cu2 supported on Gr (green, top), N-Gr (red, middle) and S,N-Gr (black, bottom).

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导电共聚物衍化新策略制备硫、氮共掺杂碳纳米管及其对改善PtCu纳米晶分散性与甲醇电催化氧化的促进作用

New strategy of S,N co-doping of conductive-copolymer-derived carbon nanotubes to effectively improve the dispersion of PtCu nanocrystals for boosting the electrocatalytic oxidation of methanol

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