电沉积制备的PtNi纳米粒子用于氧还原反应: 成核和生长机理

doi:10.1016/S1872-2067(21)63860-3

催化学报 ›› 2021, Vol. 42 ›› Issue (11): 2068-2077.DOI: 10.1016/S1872-2067(21)63860-3

电沉积制备的PtNi纳米粒子用于氧还原反应: 成核和生长机理

赵路甜^a, 郭杨格^a, 符策煌^a, 罗柳轩^a, 魏光华^b, 沈水云^a^,^#(), 章俊良^a^,^*()

^a上海交通大学机械与动力工程学院, 动力机械与工程教育部重点实验室燃料电池研究所, 上海200240
^b上海交通大学, 巴黎高科卓越工程师学院, 上海200240

收稿日期:2021-04-14 修回日期:2021-04-14 接受日期:2021-06-07 出版日期:2021-11-18 发布日期:2021-06-15
通讯作者: 沈水云,章俊良
基金资助:
国家自然科学基金(21975157);国家重点研发计划(21901247)

Electrodeposited PtNi nanoparticles towards oxygen reduction reaction: A study on nucleation and growth mechanism

Lutian Zhao^a, Yangge Guo^a, Cehuang Fu^a, Liuxuan Luo^a, Guanghua Wei^b, Shuiyun Shen^a^,^#(), Junliang Zhang^a^,^*()

^aInstitute of Fuel Cells, Key Laboratory for Power Machinery and Engineering of MOE, School of Mechanical Engineering, Shanghai Jiao Tong University, Shanghai 200240, China
^bSJTU-ParisTech Elite Institute of Technology, Shanghai Jiao Tong University, Shanghai 200240, China

Received:2021-04-14 Revised:2021-04-14 Accepted:2021-06-07 Online:2021-11-18 Published:2021-06-15
Contact: Shuiyun Shen,Junliang Zhang
About author:^#E-mail: shuiyun_shen@sjtu.edu.cn
^*E-mail: junliang.zhang@sjtu.edu.cn;
Supported by:
National Natural Science Foundation of China(21975157);National Key Research and Development Program of China(21901247)

摘要/Abstract

摘要：

质子交换膜燃料电池(PEMFCs)电堆中阴极Pt基催化剂的高用量造成其成本居高不下, 成为阻碍燃料电池汽车商业化推进的重要原因, 因此开发低Pt、高活性的Pt基催化剂势在必行. Pt合金催化剂能够有效地降低Pt用量, 并通过对合金颗粒的元素比例、晶面、粒径等实行精确调控, 显著提升氧还原(ORR)催化活性. 然而, 目前常用的制备方法由于原料与制备成本高昂、过程复杂大都难以适应规模化生产需求. 电化学方法通过控制施加的电流或电位控制晶体生长. 在水体系中该方法已得到验证, 但由于Pt化合物的热力学标准电极电位与过渡金属元素之间相差较大, 且对于过渡金属来说, 电负性大多小于铂, 因此还原电位通常负于析氢电位, 使得二者难以实现共沉积. 有机体系中电位窗口比水体系大得多, Pt与电位较负的过渡金属可实现共沉积, 采用小分子有机溶剂也可避免溶剂清洗问题, 具有应用潜力.
本文提出了一种简单的一步电沉积方法, 选择易溶于水的N,N-二甲基甲酰胺(DMF)作为溶剂, 将碳载体滴涂到玻碳电极上作为工作电极, 通过电化学方法直接将Pt-Ni合金沉积到碳载体上, 并利用物化表征与密度泛函理论(DFT)理论计算来探究共沉积机理.
透射电镜表征结果表明, 在不同的沉积电位下均可得到分散均匀、粒径适当的催化剂; 且随着电位值降低, 催化剂颗粒分散得更均匀, 颗粒粒径不断减小. 元素分布和晶面结果表明, 铂镍元素均匀分布于颗粒中. 所有样品均表现出优异的ORR性能, 最高的面积比活性达到商业催化剂的6.85倍. 将材料表征、电化学表征与DFT计算结合, 建立起了铂镍合金生长过程的模型, 并发现了有机体系中独特的成核-生长机理.
将体系中的DMF换成超纯水, 用同样的方法进行沉积, 得到的催化剂颗粒团聚严重, 说明DMF的使用能够避免颗粒团聚. 在单独铂的体系中沉积发现, 负载量极小, 表明体系中镍前驱体的添加对于催化剂的沉积过程起到重要作用. 电化学表征结果表明, 在所选用的DMF有机体系中, 镍的还原电位与铂的十分接近, 但还原动力学更慢, 趋向于先形成吸附原子后快速还原. 由此可以推测, 在二者合金的形成过程中, 镍在碳载体表面的缓慢还原而形成的吸附原子能够成为铂还原的活性位点, 从而降低了铂还原成核所需的能量, 使得载体上的成核位点大大增加, 这与DFT模拟结果一致. DFT建立了碳上镍的位点和铂的位点, 分别在上面进行铂的还原, 发现镍位点上比铂位点上更容易实现铂沉积.
本文提出了铂镍共沉积的机理: 在过电位(即还原能量)下, 铂的还原动力学较镍稍快, 于是铂先还原形成晶核, 但难以达到生长的临界半径, 于是单独铂体系中的沉积负载量很少. 载体上还原的镍为铂还原提供了大量的活性位点, 促进了铂还原, 并与镍共沉积. Pt-Ni表面则进一步促进了铂的沉积和颗粒的生长.
综上, 本文提出了一种用于制备铂合金催化剂的有机电沉积体系, 实现了单分散的碳载铂镍合金催化剂的一步制备. 随后, 本文将材料表征、电化学表征与DFT计算相结合, 建立起了有机体系中铂镍合金成核-生长过程的机理模型.

关键词: 电沉积, Pt-Ni合金纳米颗粒, 氧还原反应, 成核和生长机理, 密度泛函理论

Abstract:

In this work, highly monodispersed Pt-Ni alloy nanoparticles were directly deposited on carbon substrate through a facile electrodeposition strategy in the solvent system of N,N-dimethylformamide (DMF). A series of carbon supported Pt-Ni alloy electrocatalysts were synthesized under different applied electrode potentials. Among all as-obtained samples, the Pt-Ni/C electrocatalyst deposited at -1.73 V exhibits the optimal specific activity up to 1.850 mA cm^-2 at 0.9 V vs. RHE, which is 6.85 times higher than that of the commercial Pt/C. Comprehensive physiochemical characterizations and computational evaluations via density functional theory were conducted to unveil the nucleation and growth mechanism of PtNi alloy formation. Compared to the aqueous solution, DMF solvent molecule must not be neglected in avoiding particle agglomeration and synthesis of monodispersed nanoparticles. During the alloy co-deposition process, Ni sites produced through the reduction of Ni(II) precursor not only facilitates Pt-Ni alloy crystal nucleation but also in favor of further Pt reduction on the Ni-inserted Pt surface. As for the deposition potential, it adjusts the final particle size. This work provides a hopeful extended Pt-based catalyst layer production strategy for proton exchange membrane fuel cells and a new idea for the nucleation and growth mechanism exploration for electrodeposited Pt alloy.

Key words: Electrodeposition, PtNi alloy nanoparticles, Oxygen reduction reaction, Nucleation and growth mechanism, Density functional theory

赵路甜, 郭杨格, 符策煌, 罗柳轩, 魏光华, 沈水云, 章俊良. 电沉积制备的PtNi纳米粒子用于氧还原反应: 成核和生长机理[J]. 催化学报, 2021, 42(11): 2068-2077.

Lutian Zhao, Yangge Guo, Cehuang Fu, Liuxuan Luo, Guanghua Wei, Shuiyun Shen, Junliang Zhang. Electrodeposited PtNi nanoparticles towards oxygen reduction reaction: A study on nucleation and growth mechanism[J]. Chinese Journal of Catalysis, 2021, 42(11): 2068-2077.

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链接本文: https://www.cjcatal.com/CN/10.1016/S1872-2067(21)63860-3

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图/表 8

Fig. 1. CV curves of NC-GC WE in (a) 2 mM H2PtCl6 + 0.05 M LiClO4 + DMF; (b) (red line) 2 mM K2PtCl4 + 0.05 M LiClO4 + DMF, (black line) 0.05 M LiClO4 + DMF; (c) (red line) 0.67 mM Ni(NO3)2 + 0.05 M LiClO4 + DMF, (black line) 0.05 M LiClO4 + DMF; (d) 2 mM H2PtCl6 + 0.67 mM Ni(NO3)2 + 0.05 M LiClO4 + DMF at a scan rate of 50 mV s-1.

Fig. 2. Typical TEM images and the corresponding histogram of particle size distribution of Pt-Ni/C electrocatalysts. (a) Pt-Ni-1.60/C; (b) Pt-Ni-1.70/C; (c) Pt-Ni-1.73/C; (d) Pt-Ni-1.80/C.

Fig. 3. Electrochemical evaluation for Pt-Ni-1.60/C, Pt-Ni-1.70/C, Pt-Ni-1.73/C and Pt-Ni-1.80/C. (a) CV curves in N2-saturated 0.1 M HClO4 at a scan rate of 20 mV s-1; (b) Tafel plots with their slops at low overpotential region derived from polarization curves of the four samples and the commercial Pt/C catalysts; (c) Tafel plots comparisons of the series of electrocatalysts in the area specific activity; (d) area specific activity for the four samples and the commercial Pt/C catalysts.

Fig. 4. (a-c) Typical STEM-EDS element mapping images of Pt, Ni for Pt-Ni-1.73/C electrocatalyst; (e) corresponding line-scanning images which directions follow the red arrows in (d); (f) HRTEM image and the inset Fig. is its fast Fourier transformation (FFT) pattern.

Fig. 5. (a) CV curve in the electrolyte of 2 mM H2PtCl6 + 0.67 mM Ni(NO3)2 + 0.05 M LiClO4 + H2O (the inset is the TEM image of electrocatalyst prepared at potential of 0.1 V vs. RHE); (b) CV curves of in the electrolyte of 2 mM H2PtCl6 + 0.05 M LiClO4 + DMF (red line) and 0.05 M LiClO4 + DMF (black line) (the inset is the TEM image of as-synthesized Pt/C electrocatalyst at -1.80 V vs. Ag+/Ag). Scan rate: 50 mV s-1.

Fig. 6. (a) Structures of Pt-Graphene and Ni-graphene before (State 1) and after (State 2) the electrodeposition of Pt atoms. The gray, navy, orange and yellow represent carbon, Pt, Ni and newly-deposited Pt atom respectively; (b) Energy evolutions of Pt electrodeposition on Pt site and Ni site at U = 0.315 V vs. SHE; (c) Energy evolutions of Pt electrodeposition on Pt site and Ni site at U = 0 V vs. SHE.

Fig. 7. (a) The schematic structure diagrams of two states for the four slabs with adsorbed Pt*(the yellow color). The blue color represents deposited Pt layer, and the orange color represents located Ni; (b) The reduction potential profiles of Pt deposition on the four slabs at the electrode potential of U = 0.862 V vs. SHE; (c) The reduction energy profiles of Pt deposition on the four slabs at the electrode potential of U = 0 V vs. SHE.

Fig. 8. Schematic illustration for the growth mechanism of Pt/C and Pt-Ni/C. It is noted that the differences on radius of precursor ions and metal atoms are neglected for better presentation on the main growth process.

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电沉积制备的PtNi纳米粒子用于氧还原反应: 成核和生长机理

Electrodeposited PtNi nanoparticles towards oxygen reduction reaction: A study on nucleation and growth mechanism

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