Study of the mechanism of nitrogen doping in carbon supports on promoting electrocatalytic oxygen reduction reaction over platinum nanoparticles
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摘要: 氮掺杂碳通常被用作铂基催化剂电催化氧还原反应的功能载体，但是，掺杂的氮对分子氧在铂活性中心上的吸附和还原机理尚不清楚。本研究采用氨气热解的方法制取氮掺杂纳米碳作为载体，并采用调节氨气热解温度进而控制不同种类氮掺杂的含量，可以使铂催化剂获得较高的零价铂含量、较大的电化学活性面积、合适的铂粒径 (2.10 nm)和电子快速传输能力从而提高电催化活性。研究发现，具有最佳氮含量掺杂的Pt/Nano-NC-800催化剂显示出优异的电催化氧还原性能（例如，半波电位为0.80 V vs RHE，极限扩散电流为5.37 mA/cm2），以及强的抗甲醇和一氧化碳中毒能力。该性能优于商业铂碳催化剂（20%，JM）以及大多数沉积在碳纳米颗粒或其他载体上的铂催化剂，表现出优异的应用潜力。Abstract: Nitrogen-doped carbons (Nano-NC) are often employed as functional supports for boosting oxygen reduction reaction (ORR) over Pt-based catalysts, however, the mechanism of N doping on the adsorption and activation of molecular oxygen on Pt active sites is still not clear. Herein, Nano-NCs as the supports were prepared by a facile NH3 antipyretic method, which allowed to tune the kinds of nitrogen species in carbon matrix and their contents by adjusting the NH3 antipyretic temperatures. With such an exquisite control, the Pt nanoparticles loaded on the as-obtained Nano-NC showed an optimal Pt particle size (2.10 nm), a higher content of Pt0, a large electrochemically active surface area, and fast electron transport ability. As a consequence, the Pt/Nano-NC-800 catalyst with the optimal N-doping showed an outstanding ORR performance with half-wave potential of 0.80 V vs. RHE, limit diffusion current of 5.37 mA/cm2 and improved methanol/CO anti-poisoning, which is superior to the commercial Pt/C catalyst (20%, JM), and most of previously reported Pt-based catalysts. This work may pave a way for the design of the advanced supports for Pt-based catalysts for the ORR applications.
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Key words:
- N-doped carbon /
- nanoparticle size /
- oxygen reduction reaction /
- mechanism
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Figure 1 (a) Raman spectra of carbon nanoparticles, Nano-NC-700, Nano-NC-800, and Nano-NC-900; (b) XRD patterns of Pt/C, Pt/Nano-NC-700, Pt/Nano-NC-800, and Pt/Nano-NC-900
Figure 2 TEM images of Pt/Nano-NC-700, Pt/Nano-NC-800, and Pt/Nano-NC-900 ((a)−(c)) and the corresponding size distribution of Pt nanoparticles of ((d)−(f)) The inset of ((a)−(c)) is the HRTEM image of three catalysts
Figure 3 XPS survey spectra (a) and HR-XPS spectra of (b), (c), and (d) N 1s obtained from Pt/Nano-NC-700, Pt/Nano-NC-800, and Pt/Nano-NC-900, and HR-XPS spectra Pt 4f (e) of Pt/Nano-C, Pt/Nano-NC-700, Pt/Nano-NC-800, and Pt/Nano-NC-900 catalysts
Figure 4 (a) RDE voltammogram of the Pt/Nano-NC-800, Pt/Nano-C, and JM Pt/C catalysts recorded in O2-saturated 0.1 mol/L HClO4 electrolyte at a scan rate of 5 mV/s at 1600 r/min, (b) corresponding Tafel plots, (c) LSVs in O2-saturated 0.1 mol/L HClO4 at different RDE rotation rates of Pt/Nano-NC-800, (d) The corresponding K-L plots of Pt/Nano-NC-800
Figure 5 (a) Nyquist plots of the Pt/Nano-NC-800, Pt/Nano-C, and JM Pt/C catalysts and equivalent circuit model; (b) Endurance test of three catalysts tested at 0.756 V in O2-saturated 0.1 mol/L HClO4; (c) CO stripping experiments on three catalysts at 10 mV/s; (d) the addition of 4 mL of 3 mol/L methanol in O2-saturated solution at 1600 r/min
Table 1 Results of the fits of the N 1s XPS For each single component, the binding energy (eV) and amount (%) values are given
Sample Pyridinic-N
398.6 eVPt-N
399.4 eVPyrrolic-N
400.2 eVGraphitic-N
401.1 eVOxidized-N
402.0 eVPt/Nano-NC-700 7.4% 32.5% 19.5% 33.0% 7.6% Pt/Nano-NC-800 8.4% 31.9% 19.6% 34.6% 5.5% Pt/Nano-NC-900 17.8% 21.5% 26.4% 30.6% 3.7% 
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