新型多孔三聚氰胺负载MnCe用于高选择性电催化CO2产甲酸

doi:10.6023/A23120529

摘要/Abstract

本研究提出了一种尚未见报道的CO₂还原电催化剂及其构造, 由MnCe作为活性位点, 三聚氰胺泡沫(MS)作为载体前驱体的新型电极材料——MnCe-CMS(碳化MS)和MnCe-GOMS(氧化石墨烯活化MS), 用于电催化CO₂还原研究. 结果发现, MnCe-MS具有较宽的电位范围(–0.2~–3 V vs. RHE)及较好的产甲酸能力. 对比以常用的碳布(CC)为载体的MnCe-CC, MnCe-CMS和MnCe-GOMS的甲酸生成速率分别提高到2.3、2.8倍, 法拉第效率分别提高到2.3、2.5倍(MnCe-CC的最佳电位–0.4 V条件下), 并且MnCe-GOMS在–0.6 V表现出最佳甲酸法拉第效率(75.72%). 这归因于MS材料丰富的孔隙结构、较大的电化学表面积、易形成碳缺陷的特点, 分析表明GO的掺入可以进一步增大这些优势; 此外, 在Mn、Ce共同作用下, 有效促进电子传输、抑制析氢竞争反应、形成氧空位, 有利于CO₂的吸附、活化与转化, 从而促进甲酸生成.

关键词: 电催化CO₂还原技术, 甲酸, Mn, Ce, 三聚氰胺泡沫(MS), 氧化石墨烯活化, 高温碳化

A previously unreported CO₂ reduction electrocatalyst consisting of MnCe as the active site and melamine foam (MS) as the carrier precursor is proposed. The MS were prepared into carbonized melamine foam (CMS) and graphene oxide- activated melamine foam (GOMS) by activation, respectively. And Mn and Ce were impregnated on the above substrates to synthesize MnCe-CMS and MnCe-GOMS catalysts for the electrocatalytic CO₂ reduction to formic acid. It was found that MnCe-MS (MnCe-CMS and MnCe-GOMS) had a wide potential range (–0.2~–3 V vs. RHE) and better formic acid production ability. Among them, the Faraday efficiency of formic acid (FE_f) on MnCe-CMS was 63.04% at –0.4 V, and the yield rate of formic acid (Y_f) was 470.89 μg•h^–1•cm^–2 at –3.0 V. MnCe-GOMS showed better electrocatalytic activity, with a FE_f of 75.72% at –0.6 V (when the Y_f=661.99 μg•h^–1•cm^–2), and optimal Y_f of 746.9 μg•h^–1•cm^–2 at –0.8 V. In addition, no other products (e.g., acetic acid, methanol, ethanol, CO, methane) were detected during the reaction, suggesting that MnCe-MS has a good formic acid selectivity. Compared with the MnCe-CC, which are based on the commonly used carbon cloth (CC) as a carrier, the Y_f of MnCe-CMS and MnCe-GOMS were increased to 2.3 and 2.8 times, and the FE_f were increased to 2.3 and 2.5 times, respectively, at the optimal potential of MnCe-CC of –0.4 V. This is attributed to the rich pore structure and large electrochemical surface area of the MS material, which can easily form carbon defects during the preparation, thus favoring the adsorption of CO₂. Moreover, under the joint action of Mn and Ce, it effectively promotes electron transport, inhibits the competition reaction of hydrogen precipitation, and forms oxygen vacancies, which is conducive to the adsorption, activation and conversion of CO₂, thus promoting the formation of formic acid.

Key words: electrocatalytic CO₂ reduction reaction, formic acid, Mn, Ce, melamine foam, graphene oxide activation, high temperature carbonization

引用此文

雷雅茹, 熊廷楷, 于湘涛, 黄秀兵, 唐晓龙, 易红宏, 周远松, 赵顺征, 孙龙, 高凤雨. 新型多孔三聚氰胺负载MnCe用于高选择性电催化CO₂产甲酸[J]. 化学学报, 2024, 82(4): 396-408.

Yaru Lei, Tingkai Xiong, Xiangtao Yu, Xiubing Huang, Xiaolong Tang, Honghong Yi, Yuansong Zhou, Shunzheng Zhao, Long Sun, Fengyu Gao. Novel Porous Melamine Foam Loaded with MnCe for Highly Selective Electrocatalytic CO₂ to Formic Acid[J]. Acta Chimica Sinica, 2024, 82(4): 396-408.

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图/表 17

Catalysts	Onset potential (V vs. RHE)	exit potential (V vs. RHE)	Selection of experimental sites (V vs. RHE)	Maximum yield rate/ (μg•h^–1•cm^–2)	Optimum FE_f/%
MnCe-GOMS	–0.06	–2.99	–0.2, –0.4, –0,5, –0.6, –0.8, –1.0, –2.0, –2.5	746.92 (–0.8 V)	75.72 (–0.6 V)
MnCe-CMS	–0.13	–3.1	–0.2, –0.4, –1.0, –2.0, –3.0	470.89 (–3.0 V)	63.04 (–0.4 V)
MnCe-CC	0.58	–1.06	0.0, –0.2, –0.4, –0.8, –1.0	78.69 (–0.4 V)	64.14 (0 V)
MnCe-CF	0.65	–0.23	0.0, –0.1, –0.2	489.62 (–0.2 V)	11.67 (0 V)
MnCe-NF	0.43	–0.74	–0.4, –0.5, –0.6, –0.7	542.69 (–0.4 V)	41.47 (–0.4 V)

表1. 不同载体负载MnCe材料电催化CO2还原产甲酸的性能

Table 1. Performance of different carrier-loaded MnCe materials for electrocatalytic CO2 reduction to formic acid

图1. 不同载体上负载MnCe的材料电催化CO2还原为甲酸的(a)生成速率和(b)法拉第效率

Figure 1. (a) Yield and (b) Faraday efficiency of formic acid on different carriers loaded with MnCe materials

图2. (a, d) MnCe-GOMS、(b, e) MnCe-CMS和(c, f) MnCe-CC在不同放大倍数下的SEM图; (g~k) MnCe-GOMS催化剂上C、N、Mn、Ce、O的EDS图像

Figure 2. SEM images of (a, d) MnCe-GOMS, (b, e) MnCe-CMS, and (c, f) MnCe-CC at different magnifications; (g~k) EDS images of C, N, Mn, Ce, and O on MnCe-GOMS catalysts

图3. MnCe-GOMS、MnCe-CMS和MnCe-CC的(a) XRD图和(b)拉曼图谱

Figure 3. (a) XRD and (b) Raman spectra of MnCe-GOMS, MnCe-CMS and MnCe-CC

图4. MnCe-GOMS、MnCe-CMS及MnCe-CC的固体红外(FTIR)光谱

Figure 4. Solid-state infrared (FTIR) spectra of MnCe-GOMS, MnCe-CMS and MnCe-CC

Adsorption site types		Weak adsorption		Medium adsorption		Strong adsorption	Amount
Adsorption site types		1# (30~180 ℃)	2# (180~350 ℃)	3# (350~430 ℃)	4# (400~600 ℃)	5# (600~800 ℃)	Amount
MnCe-CMS	Area	34.45	14.98	3.10	35.42	95.67	183.62
MnCe-CMS	Proportion%	18.76	8.16	1.69	19.29	52.10	100
MnCe-GOMS	Area	9.28	28.01	94.40	101.29	24.48	248.18
MnCe-GOMS	Proportion%	3.60	10.88	36.67	39.34	9.51	100

表2. MnCe-CMS和MnCe-GOMS的CO2吸附位点及其占比

Table 2. CO2 adsorption sites and the percentage of each fraction of MnCe-CMS and MnCe-GOMS.

图5. (a) MnCe-CMS和(b) MnCe-GOMS的CO2-TPD曲线; (c~g) CO2的五种吸附类型, 经参考文献[39]许可重绘

Figure 5. CO2-TPD curves of (a) MnCe-CMS and (b) MnCe-GOMS; (c~g) five types of CO2 adsorption on the catalyst surface, redrawn with permission from ref.[39]

Catalysts	Element content/%					Atomic ratio/%
Catalysts	C	N	O	Mn	Ce	Mn³⁺/Mn	Ce³⁺/Ce	O_α/O	O_β/O
MnCe-CC	60.10	0.37	30.33	3.60	5.57	30.75	9.30	46.81	53.19
MnCe-CMS	38.00	1.20	46.55	8.67	5.58	32.29	11.09	37.69	26.81
MnCe-GOMS	55.87	4.49	33.22	4.68	4.49	40.45	24.92	48.62	11.76

表3. C 1s, N 1s, O 1s, Mn 2p, Ce 3d元素各价态的拟合峰面积及比例

Table 3. Fitted peak areas and ratios for each valence state of C 1s, N 1s, O 1s, Mn 2p, Ce 3d elements

图6. MnCe-GOMS、MnCe-CMS和MnCe-CC的XPS图: (a) Mn 2p; (b) Ce 3d; (c) C 1s; (d) O 1s

Figure 6. XPS spectra of MnCe-GOMS, MnCe-CMS and MnCe-CC: (a) Mn 2p; (b) Ce 3d; (c) C 1s; (d) O 1s

图7. MnCe-GOMS、MnCe-CMS及MnCe-CC的(a) CV曲线和(b) LSV曲线; MnCe-GOMS分别在通N2和CO2条件下的(c) CV和(d) LSV曲线

Figure 7. (a) CV and (b) LSV curves of MnCe-GOMS, MnCe-CMS, and MnCe-CC; (c) CV and (d) LSV curves of MnCe-GOMS in N2 and CO2, respectively

图8. (a~c) MnCe-CC、MnCe-CMS及MnCe-GOMS材料在电压窗口为0.69~0.85 V间、不同扫速(20~120 mV/s)下的CV曲线; (d) ECSA计算结果, 电流密度与扫速的线性关系

Figure 8. (a~c) CV curves of MnCe-CC, MnCe-CMS and MnCe-GOMS in the voltage window of 0.69~0.85 V with different sweep rates (20~120 mV/s); (d) linear relationship between current density and sweep rates (ECSA)

图9. MnCe-GOMS、MnCe-CMS及MnCe-CC的EIS曲线

Figure 9. EIS curves of MnCe-GOMS, MnCe-CMS and MnCe-CC

图10. MnCe-GOMS、MnCe-CMS及MnCe-CC的Tafel曲线

Figure 10. Tafel curves of MnCe-GOMS, MnCe-CMS and MnCe-CC

Parameters	MnCe-CC	MnCe-CMS	MnCe-GOMS
b/(mV•dec^–1)	–396	–1750	–1169
i₀/(mA•cm^–2)	0.042	0.783	0.575
k⁰/(cm•s^–1)	7.0×10^–6	1.23×10^–5	9.1×10^–6
α	–0.149	–0.034	–0.051

表4. MnCe-GOMS、MnCe-CMS及MnCe-CC动力学参数

Table 4. Kinetic fitting parameters for MnCe-GOMS, MnCe-CMS and MnCe-CC

Catalysts	Carrier	Advantages	Disadvantages	Potentiostatic properties
MnCe-CMS	Melamine foam (MS)	High FE, high yield and low cost	Low conductivity and poor stability	Wider potential range (–0.2~–3 V)
MnCe-GOMS	Melamine foam (MS)	High FE, high yield and low cost	Low conductivity and poor stability	Wider potential range (–0.2~–3 V)
MnCe-CC	Carbon cloth (CC)	Higher FE	Low yield	Narrower potential range (0~–1 V)
MnCe-CF	Metal foams	High conductivity and higher yield	Low FE, severe HER competitive response and poor reproducibility	Narrow potential range (<–0.7 V)
MnCe-NF	Metal foams	High conductivity and higher yield		Narrow potential range (<–0.7 V)

表5. 不同基底上负载MnCe材料的性能对比

Table 5. Performance comparison of MnCe materials loaded on different substrates

图11. (a) MnCe-GOMS、MnCe-CMS及MnCe-CC性能对比; (b) MnCe-GOMS材料在–1.0 V外加电压下的稳定性测试

Figure 11. (a) Comparison of MnCe-GOMS, MnCe-CMS and MnCe-CC materials; (b) stability test of MnCe-GOMS at –1.0 V

图12. (a) MnCe-GOMS和MnCe-CMS的制备过程; (b) MnCe-GOMS电催化CO2还原生成甲酸示意图

Figure 12. (a) Preparation of MnCe-GOMS and MnCe-CMS; (b) schematic diagram of electrocatalytic CO2 reduction to formic acid by MnCe-GOMS

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新型多孔三聚氰胺负载MnCe用于高选择性电催化CO₂产甲酸

Novel Porous Melamine Foam Loaded with MnCe for Highly Selective Electrocatalytic CO₂ to Formic Acid

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