Ni-N共掺杂碳气凝胶的构筑及其电催化还原CO2性能

doi:10.11949/0438-1157.20250930

摘要/Abstract

摘要：

开发高效电催化剂是提升二氧化碳还原（CO₂RR）选择性与效率、助力碳中和的关键。针对传统粉末状碳基催化剂易脱落、传质差、活性位点易被覆盖等问题，本研究提出将其稳定于三维多孔碳气凝胶载体的策略。以煤焦油沥青为前驱体，通过冷冻干燥结合热解工艺，成功制备了Ni-N共掺杂碳气凝胶催化剂（Ni-NCA）。该催化剂具有高比表面积和贯通的三维孔道网络，有效均匀分散并稳定Ni-N活性位点，同时促进CO₂吸附、电解质渗透和电子传输。将其用于CO₂RR，在-0.8 V （vs RHE）下CO法拉第效率（FE_CO）高达95.6%，且在-0.7至-1.1 V （vs RHE）的宽电位窗口内FE_CO均超过90%。50小时恒电位（-0.8 V）（vs RHE）测试中电流密度稳定，FE_CO保持在82%以上，展现出优异的催化活性和稳定性，具有良好的应用前景。

关键词: 催化剂, 电解, 二氧化碳, 碳气凝胶, 煤焦油沥青, 金属-氮-碳

Abstract:

Developing efficient electrocatalysts is crucial for enhancing the selectivity and efficiency of the electrochemical CO₂ reduction reaction (CO₂RR) and advancing carbon neutrality. To address the issues of easy detachment, poor mass transfer, and coverage of active sites inherent in traditional powdered carbon-based catalysts, this study proposes a strategy of stabilizing them within a three-dimensional (3D) porous carbon aerogel support. Using coal tar pitch as the precursor, a Ni-N co-doped carbon aerogel catalyst (Ni-NCA) was successfully synthesized via a combined freeze-drying and pyrolysis process. The catalyst possesses a high specific surface area and an interconnected 3D pore network, which effectively disperses and stabilizes Ni-N active sites while simultaneously promoting CO₂ adsorption, electrolyte penetration, and electron transport. When applied to CO₂RR, the Ni-NCA catalyst achieved a high CO Faradaic efficiency (FE_CO) of 95.6% at -0.8 V (vs RHE). Furthermore, it maintained FE_CO above 90% across a broad potential window from -0.7 V to -1.1 V (vs RHE). The current density remains stable during the 50 h potentiostatic test at -0.8 V (vs RHE)., the CO current density remained stable and FE_CO was sustained above 82%. These results demonstrate excellent catalytic activity and stability, highlighting the promising application potential of the Ni-NCA catalyst.

Key words: catalyst, electrolysis, carbon dioxide, carbon aerogel, coal tar pitch, metal-nitrogen-carbon

中图分类号:

O643.36

马明怡, 牛佳宝, 严鑫, 李然, 周高勇, 朱佳佳, 王兴宝, 何孝军, 李宏强. Ni-N共掺杂碳气凝胶的构筑及其电催化还原CO₂性能[J]. 化工学报, DOI: 10.11949/0438-1157.20250930.

Mingyi MA, Jiabao NIU, Xin YAN, Ran LI, Gaoyong ZHOU, Jiajia ZHU, Xingbao WANG, Xiaojun HE, Hongqiang LI. Construction of Ni-N co-doped carbon aerogel and its performance in electrocatalytic reduction of CO₂[J]. CIESC Journal, DOI: 10.11949/0438-1157.20250930.

图/表 16

图1 (a)Ni4-NCA催化剂的制备示意图；(b)Ni4-NCA样品的数码照片

Fig.1 (a) Schematic diagram of the synthesis process for Ni4-NCA; (b) Digital photograph of Ni4-NCA

图2 (a)前驱体的SEM图；(b-c)Ni4-NCA在不同放大倍率下的SEM图片；(d-e)Ni4-NCA在不同放大倍率下的TEM图；(f)Ni4-NCA的HR-TEM图片(插图：选取衍射图)；(g)Ni4-NCA的元素映射图

Fig.2 (a) SEM image of precursor; (b-c) SEM images of Ni4-NCA at different magnifications; (d-e) TEM images of Ni4-NCA at different magnifications; (f) HR-TEM image of Ni4-NCA (inset: SAED pattern); (g) EDS mapping images of Ni4-NCA

图3 (a-c)Ni2.5-NCA；(d-f)Ni4-NCA和(g-i)Ni4-NC在不同放大倍率下的SEM图

Fig.3 Different-magnification SEM images of Ni2.5-NCA (a-c); Ni4-NCA (d-f) and Ni4-NC (g-i)

图4 Ni4-NCA、Ni2.5-NCA、Ni4-NC 和 N-C氮气吸脱附等温曲线图(a)和孔径分布图(b)

Fig.4 (a) N2 adsorption-desorption isotherms and (b) pore size distribution of Ni4-NCA、Ni2.5-NCA、Ni4-NC and N-C

图5 (a)Ni4-NCA、Ni2.5-NCA、Ni4-NC和N-C的XRD谱图；(b)Ni4-NCA、Ni2.5-NCA和Ni4-NC的Raman光谱图

Fig.5 (a) X-ray diffraction patterns of Ni4-NCA; Ni2.5-NCA; Ni4-NC and N-C;(b) Raman spectra of Ni4-NCA, Ni2.5-NCA and Ni4-NC

图6 (a)Ni4-NCA；(b)Ni2.5-NCA; (c)Ni4-NC；(d)N-C的XPS全谱图

Fig.6 XPS survey spectra of (a) Ni4-NCA; (b) Ni2.5-NCA; (c) Ni4-NC; (d) N-C

图7 (a)Ni4-NCA;(b)Ni2.5-NCA;(c)Ni4-NC;(d)N-C的高分辨率C 1s谱图

Fig.7 High resolution C 1s spectrum of (a) Ni4-NCA; (b) Ni2.5-NCA; (c) Ni4-NC and (d) N-C.

图8 (a)Ni4-NCA、Ni2.5-NCA、Ni4-NC和N-C的高分辨率N 1s 谱图;(b)Ni4-NCA、Ni2.5-NCA和N-C的高分辨率注:Ni 2p 谱图

Fig.8 (a) High resolution N 1s of Ni4-NCA, Ni2.5-NCA, Ni4-NC and N-C; (b) High resolution Ni 2p of Ni4-NCA, Ni4-NC and N-C.

图9 Ni4-NCA、Ni2.5-NCA、Ni4-NC和N-C的不同氮物种量图

Fig.9 The content of N species for Ni4-NCA、Ni2.5-NCA、Ni4-NC and N-C

表1 XPS 测得的Ni原子含量

Table 1 XPS measurements for the atomic concentration of Ni

Catalyst

Ni (at.%)

Ni₄-NCA

Ni_2.5-NCA

Ni₄-NC

N-C

0.97%

0.17%

0.46%

0.01%

表2 ICP-OES 测得的Ni质量含量

Table 2 ICP-OES measurements for Ni weight percent.

Catalyst

Ni (wt.%)

Ni₄-NCA

Ni_2.5-NCA

Ni₄-NC

N-C

2.18%

0.96%

1.90%

0.01%

图10 样品Ni4-NCA、Ni2.5-NCA、Ni4-NC和 N-C的电化学测试(a)线性伏安扫描曲线；(b)不同电位下CO法拉第效率曲线；(c)不同电位下CO偏电流密度曲线；(d)在-0.8 V (vs RHE)条件下，样品Ni4-NCA经50小时电解稳定性测试图

Fig.10 (a) Linear sweep voltammetric (LSV) curves； (b) FEco at different potentials； (c) jco at different potentials acquired in CO2-saturated 0.5 M KHCO3 electrolytes for Ni4-NCA, Ni2.5-NCA, Ni4-NC and N-C； (d) Stability of Ni4-NCA: The FECO and current density at a potential of -0.8 V (vs RHE) during 50 h

表3 Ni4-NCA与文献报道的碳基单原子镍催化剂CO2RR性能对比

Table 3 Performance comparison of CO2RR between Ni4-NCA and literature-reported carbon-based single-atom nickel catalysts

催化剂	电解液	电压（vs RHE）/V	CO法拉第效率（%）	电流密度 (mA · cm^-2)	参考文献
Ni₄-NCA Ni-NC(HPU)	0.5 M KHCO₃ 0.5 M KHCO₃	-0.8 -0.8	95.6 91	14.85 27.1	This work ^[44]
Ni@NC SA-Ni@NC	0.5 M KHCO₃ 0.1 M KHCO₃	-0.6 ~ -1.3 -0.6	80> 86.2	16 10.1	^[45] ^[46]
Ni-N-MEGO	0.5 M KHCO₃	-0.55~ -0.7	92.1	28.6	^[47]
NiSA-NGA	0.5 M KHCO₃	-0.8	90.2	6.5	^[48]
SA-Ni/N-CS	0.5 M KHCO₃	-0.8	95.1	—	^[49]
Ni-N₃-C	0.5 M KHCO₃	-0.65	95.6	6.64	^[50]
Ni-PACN	0.5 M KHCO₃	-0.7 ~ -1.1	95	21	^[51]
Ni–N–C	0.5 M KHCO₃	-0.65	97	6.5	^[52]

图11 Ni4-NCA、Ni2.5-NCA、Ni4-NC和N-C的(a)Tafel斜率图；(b)TOF图；(c)电流密度差值∆j与扫速的关系图；(d)电化学阻抗图

Fig.11 (a) Tafel curves; (b) TOF; (c) The plot of charging current density differences Δj against the scan rate for the calculation of ECSA acquired in CO2-saturated 0.5 M KHCO3 electrolyte for Ni4-NCA, Ni2.5-NCA, Ni4-NC and N-C; (d) Electrochemical impedance spectra of Ni4-NCA、Ni2.5-NCA、Ni4-NC and N-C

图12 在5到50 mV s-1的扫描速率下(a)Ni4-NCA、(b)Ni2.5-NCA、(c)Ni4-NC、(d)N-C从-0.06 到-0.16 V (vs RHE)的循环伏安曲线；

Fig.12 (a) Cyclic voltammetry curves from -0.06 V to -0.16 V (vs RHE) at scan rates ranging from 5 to 50 mV·s-1 for (a) Ni4-NCA, (b) Ni2.5-NCA (c) Ni4-NC and (d) N-C.

图13 循环50 h后Ni4-NCA的(a)高分辨率C 1s谱图，(b)高分辨率N 1s谱图，(c)高分辨率Ni 2p谱图，(d)XRD谱图

Figure 13 (a) High-resolution C 1s, (b) N 1s, (c) Ni 2p XPS spectrum, and (d) XRD pattern of the Ni₄-NCA sample after 50 h of cycling.

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Ni-N共掺杂碳气凝胶的构筑及其电催化还原CO₂性能

Construction of Ni-N co-doped carbon aerogel and its performance in electrocatalytic reduction of CO₂

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