NH4Cl辅助热解制备镍-氮-碳纳米管催化剂及其电还原CO2性能

doi:10.11949/0438-1157.20220507

化工学报 ›› 2022, Vol. 73 ›› Issue (10): 4484-4497.DOI: 10.11949/0438-1157.20220507

• 催化、动力学与反应器 • 上一篇下一篇

NH₄Cl辅助热解制备镍-氮-碳纳米管催化剂及其电还原CO₂性能

吴诗德¹^,²(), 易峰², 平丹²(), 张逸飞², 郝健³, 刘国际¹(), 方少明²

^1.郑州大学化工学院，河南郑州 450001
^2.郑州轻工业大学材料与化学工程学院，河南郑州 450002
^3.省部共建煤炭高效利用与绿色化工国家重点实验室，宁夏银川 750021

收稿日期:2022-04-07 修回日期:2022-09-28 出版日期:2022-10-05 发布日期:2022-11-02
通讯作者: 平丹,刘国际
作者简介:吴诗德（1979—），男，博士研究生，副教授，wushide@zzuli.edu.cn
基金资助:
郑州轻工业大学星空众创空间孵化项目(2020ZCKJ218);郑州轻工业大学博士基金项目(2018BSJJ024);河南省自然科学基金项目(212300410299);省部共建煤炭高效利用与绿色化工国家重点实验室开放课题项目(2022-K14);国家自然科学基金-河南联合基金重点项目(U1704256)

NH₄Cl assisted preparation of Ni-N-CNTs catalyst and its performance for electrochemical CO₂ reduction

Shide WU¹^,²(), Feng YI², Dan PING²(), Yifei ZHANG², Jian HAO³, Guoji LIU¹(), Shaoming FANG²

^1.School of Chemical Engineering, Zhengzhou University, Zhengzhou 450001，Henan, China
^2.School of Material and Chemical Engineering, Zhengzhou University of Light Industry, Zhengzhou 450002, Henan, China
^3.State Key Laboratory of High-efficiency Utilization of Coal and Green Chemical Engineering, Yinchuan 750021, Ningxia, China

Received:2022-04-07 Revised:2022-09-28 Online:2022-10-05 Published:2022-11-02
Contact: Dan PING, Guoji LIU

摘要/Abstract

摘要：

二氧化碳（CO₂）的资源化利用是实现“碳达峰，碳中和”的重要手段。在众多CO₂转化技术当中，电催化CO₂还原反应因反应条件温和、工艺过程简单等优点，被认为是极具应用前景的减碳技术之一，其关键在于高效、高稳定性电催化剂的开发。过渡金属-氮-碳（M-N-C）材料是电还原CO₂生成CO的有效催化剂，针对其高温热解制备过程中活性金属原子容易聚集且氮原子流失严重，进而使得活性位密度降低，催化性能下降等问题，本文提出以双氰胺（DCDA）为碳源和氮源，以乙酰丙酮镍（Ni（acac）₂）为金属源，以氯化铵（NH₄Cl）为第二氮源和造孔剂，采用简单的NH₄Cl辅助热解-酸刻蚀的方法制备得到镍-氮-碳纳米管（Ni-N-CNTs）电还原CO₂催化剂，并详细考察NH₄Cl添加量对催化剂结构和催化性能的影响。表征结果表明：NH₄Cl的加入有利于催化剂纳米管状形貌和多级孔结构的生成，同时有利于催化剂中Ni-Nx （1.6%，摩尔分数）和pyridinic-N （1.75%，摩尔分数）物种含量的增加。一系列性能测试结果表明：催化剂的活性中心为Ni-Nx，同时pyridinic-N的存在也有利于催化性能的提高，当前体中NH₄Cl加入量与氮源和金属源总质量比为1∶1时，所得Ni-N-CNTs-1催化剂催化性能最好，在电压为-0.65 V （vs RHE）时，CO法拉第效率最高达92%，此时CO部分电流密度为8 mA·cm^-2。此外，该催化剂还表现出良好的催化稳定性，连续恒电位电解12 h，催化性能基本不变。该催化剂制备工艺简单，制备条件可控，研究结果可为高效M-N-C电还原CO₂催化剂的设计和制备提供一种切实有效的研究思路和方法。

关键词: 热解, 氮掺杂碳纳米管, 电还原二氧化碳

Abstract:

The resource utilization of carbon dioxide (CO₂) is an important means to achieve “carbon peak, carbon neutrality”. Among various CO₂ conversion technologies, electrochemical CO₂ reduction is considered to be one of the most promising carbon reduction technologies due to its mild reaction conditions and simple process. The key lies in the development of high-efficiency and high-stability electrocatalysts. Transition metal-nitrogen-carbon (M-N-C) material is an effective catalyst for electrochemical CO₂reduction to CO. However, the inevitable aggregation of active metal atoms and the serious N loss during the pyrolysis preparation usually lead to the reduction of active sites density and then the degradation of catalytic performance. Herein, this paper proposes the construction of Ni-N-carbon nanotubes (Ni-N-CNTs) catalysts for electrochemical CO₂reduction via NH₄Cl-assisted pyrolysis and associated acid leaching method. The catalysts are prepared by using dicyandiamide as carbon and nitrogen sources, the nickel acetylacetonate as metal source and the NH₄Cl as additional nitrogen source and pore-forming agent. The influence of NH₄Cl addition on the structure and catalytic performance of catalysts is investigated in detail. The characterization results show that the addition of NH₄Cl is beneficial to the formation of nanotube-like morphology and hierarchical pore structure of the catalyst. At the same time, it is beneficial to increase the content of Ni-Nx (1.6%, mole fraction) and pyridinic-N (1.75%, mole fraction) species in the catalyst. A series of catalytic performance results indicate that the catalyst active site is the atomic Ni-Nx, and the presence of pyridinic-N species also contribute to an enhanced catalytic performance. When the mass ratio of NH₄Cl to the total mass of nitrogen and metal sources is 1∶1, the derived Ni-N-CNTs-1 catalyst exhibits the best catalytic performance. The CO Faradaic efficiency is as high as 92% with a large CO partial current density of 8 mA·cm^-2 at a low potential of -0.65 V (vs RHE). In addition, this catalyst also shows good operation stability for 12 h without obvious performance decay. The catalyst preparation process is simple and the preparation conditions are controllable. This work will provide a practical and feasible approach to build highly efficient M-N-C catalyst for CO₂electroreduction.

Key words: pyrolysis, N doped carbon nanotubes, electrochemical CO₂ reduction

中图分类号:

TQ151

吴诗德, 易峰, 平丹, 张逸飞, 郝健, 刘国际, 方少明. NH₄Cl辅助热解制备镍-氮-碳纳米管催化剂及其电还原CO₂性能[J]. 化工学报, 2022, 73(10): 4484-4497.

Shide WU, Feng YI, Dan PING, Yifei ZHANG, Jian HAO, Guoji LIU, Shaoming FANG. NH₄Cl assisted preparation of Ni-N-CNTs catalyst and its performance for electrochemical CO₂ reduction[J]. CIESC Journal, 2022, 73(10): 4484-4497.

图/表 13

图1 Ni-N-CNTs-x催化剂制备流程

Fig.1 The fabrication scheme of Ni-N-CNTs-x catalyst

图2 所制备催化剂的XRD谱图

Fig.2 XRD patterns of prepared catalysts

图3 所制备催化剂的Raman光谱图

Fig.3 Raman spectra of the prepared catalysts

图4 Ni-N-CNTs催化剂的FE-SEM图，Ni-N-CNTs-1催化剂的FE-SEM图、TEM图、HR-TEM图、SAED图和TEM-EDS图

Fig.4 The FE-SEM image of the Ni-N-CNTs catalyst, and the FE-SEM, TEM, HR-TEM, SAED and TEM-EDS mapping images of the Ni-N-CNTs-1 catalyst

图5 所制备催化剂的N2吸附/脱附曲线和孔径分布

Fig.5 N2 adsorption/desorption curves and pore size distributions of prepared catalysts

表1 所制备催化剂的比表面积和孔结构特性

Table1 The specific surface areas and textural properties of prepared catalysts

样品	比表面积/ (m²·g^-1)	孔隙体积/ (cm³·g^-1)	孔隙直径/nm
Ni-N-CNTs	448.24	0.97	8.35
Ni-N-CNTs-1/3	320.10	0.58	6.79
Ni-N-CNTs-1	333.48	1.00	11.07
Ni-N-CNTs-3	272.88	0.24	4.05

图6 所制备催化剂的 XPS总谱图、Ni 2p的XPS谱图、 N 1s的XPS谱图和各类含氮物种的含量对比

Fig.6 The full-scale XPS spectra, Ni 2p XPS spectra, N 1s XPS spectra, and the contents of various N-containing species of prepared catalysts

表2 所制备催化剂中各物种的定量分析结果

Table 2 Summary contents of various species in the prepared catalysts

样品	XPS								Ni(ICP-OES)/% (mass)
	C/%(mol(mass))	N/%(mol(mass))	Ni/%(mol(mass))	N/%(mol)				Ni ⁿ⁺/Ni⁰
	C/%(mol(mass))	N/%(mol(mass))	Ni/%(mol(mass))	Ni-Nx	Graphitic-N	Pyrrolic-N	Pyridinic-N	Ni ⁿ⁺/Ni⁰
Ni-N-CNTs	84.36(77.99)	6.17(6.65)	1.12(5.06)	1.09	2.31	2.23	1.15	0.97	18.12
Ni-N-CNTs-1/3	87.32(82.56)	6.5(7.08)	0.87(3.97)	1.18	2.06	1.65	1.65	1.42	13.82
Ni-N-CNTs-1	87.44(81.58)	7.86(8.56)	1.21(5.11)	1.60	2.46	2.06	1.75	1.59	16.1
Ni-N-CNTs-3	87.19(81.04)	7.45(8.08)	1.08(4.91)	1.43	2.03	2.00	2.01	1.22	10.8

图7 所制备催化剂的LSV图、FECO和jCO以及Ni-N-CNTs-1催化剂在-0.65 V（vs RHE）下的稳定性测试结果和稳定性测试前后的LSV图

Fig.7 The LSV curves, FECO and jCO of prepared catalysts, the stability test of Ni-N-CNTs-1 at -0.65 V（vs RHE）and the LSV curves of Ni-N-CNT-1 before and after the stability test

表3 文献报道的CO2RR催化剂的性能比较

Table 3 Performance comparison of CO2RR catalysts reported in recent years

Electrocatalyst	Cathode material	Electrolyte(pH)	FE_CO/%	Potential (vs RHE)/V	$j C O$ / (mA·cm^-2)	Ref.
Meso NC-Fe	glassy carbon	0.5 mol·L^-1 KHCO₃ (7.2)	85.0	-0.73	3.7	[36]
SA-Ni@NC	glassy carbon	0.5 mol·L^-1 KHCO₃(7.2)	86.2	-0.60	1.78	[37]
NiSA-N-CNTs	carbon paper	0.5 mol·L^-1 KHCO₃ (7.2)	92	-0.70	23.5	[38]
Ni SAs/N-C	carbon paper	0.5 mol·L^-1 KHCO₃(7.2)	70.3	-1.00	7.37	[39]
Fe-N/O-C (MZ)	carbon paper	0.1 mol·L^-1 KHCO₃(6.8)	95.5	-0.57	5.6	[40]
FeMn-N-C	glassy carbon plate	0.1 mol·L^-1 KHCO₃ (6.8)	84.0	-0.51	1.8	[41]
CATpyr/CNT	glassy carbon plate	0.5 mol·L^-1 KHCO₃(7.2)	93	-0.59	0.24	[42]
CoPc@HCS-9	carbon fiber paper	0.5 mol·L^-1 KHCO₃ (7.2)	88	-0.87	6.5	[43]
Ni-N-CNTs-1	glassy carbon	0.5 mol·L^-1 KHCO₃(7.2)	92.0	-0.65	8.0	this work

表3 文献报道的CO2RR催化剂的性能比较

Table 3 Performance comparison of CO2RR catalysts reported in recent years

Electrocatalyst	Cathode material	Electrolyte(pH)	FE_CO/%	Potential (vs RHE)/V	$j C O$ / (mA·cm^-2)	Ref.
Meso NC-Fe	glassy carbon	0.5 mol·L^-1 KHCO₃ (7.2)	85.0	-0.73	3.7	[36]
SA-Ni@NC	glassy carbon	0.5 mol·L^-1 KHCO₃(7.2)	86.2	-0.60	1.78	[37]
NiSA-N-CNTs	carbon paper	0.5 mol·L^-1 KHCO₃ (7.2)	92	-0.70	23.5	[38]
Ni SAs/N-C	carbon paper	0.5 mol·L^-1 KHCO₃(7.2)	70.3	-1.00	7.37	[39]
Fe-N/O-C (MZ)	carbon paper	0.1 mol·L^-1 KHCO₃(6.8)	95.5	-0.57	5.6	[40]
FeMn-N-C	glassy carbon plate	0.1 mol·L^-1 KHCO₃ (6.8)	84.0	-0.51	1.8	[41]
CATpyr/CNT	glassy carbon plate	0.5 mol·L^-1 KHCO₃(7.2)	93	-0.59	0.24	[42]
CoPc@HCS-9	carbon fiber paper	0.5 mol·L^-1 KHCO₃ (7.2)	88	-0.87	6.5	[43]
Ni-N-CNTs-1	glassy carbon	0.5 mol·L^-1 KHCO₃(7.2)	92.0	-0.65	8.0	this work

图8 所制备催化剂在不同扫速下的CV曲线图、在-0.07 V （vs RHE）时电流密度差与扫速关系及Tafel曲线

Fig.8 CV curves of prepared catalysts at different scan rates, the capacitive current (Δj) against the scan rate at -0.07 V (vs RHE) and the Tafel plots

图9 Ni-N-CNTs-1，Ni-N-CNTs-1-12h，Ni-N-CNTs-1-24h和Ni NPs/N-CNTs-1样品的XRD谱图和性能对比

Fig.9 XRD patterns and performances of Ni-N-CNTs-1, Ni-N-CNTs-1-12h, Ni-N-CNTs-1-24h and Ni NPs/N-CNTs-1 samples

图10 Ni-N-CNTs-1催化剂经KSCN处理前后和经2 mol·L-1 H3PO4溶液浸泡不同时间后的FECO和jCO,所制备催化剂上Ni-Nx和pyridinic-N含量与FECO的对应关系以及CO2RR生成CO可能的机理

Fig.10 The catalytic performance of Ni-N-CNTs-1 electrocatalyst with or without KSCN treatment, and after soaking in 2 mol·L-1 H3PO4 for different time, the relationship between the contents of Ni-Nx and pyridinic-N with FECO, and the proposed mechanism for CO2RR to CO on prepared electrocatalysts

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NH₄Cl辅助热解制备镍-氮-碳纳米管催化剂及其电还原CO₂性能

NH₄Cl assisted preparation of Ni-N-CNTs catalyst and its performance for electrochemical CO₂ reduction

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