Preparation of NiCoFe electrodes for electrochemical deoxidation by one-step electrodeposition

doi:10.19965/j.cnki.iwt.2023-0551

Abstract

Abstract:

Aiming at the high cost and poor effect of catalytic materials for cathodic oxygen reduction reaction(ORR) in electrochemical deoxygenation, NiCoFe ternary alloy was efficiently prepared by electrodeposition under different current densities, and the morphology and structure of the alloy material were characterized and analyzed, which showed that NiCoFe alloy had a fluffy cauliflower-like surface morphology and alloy crystalline structure. The ORR performance of the NiCoFe alloy was tested in a three-electrode system at different current densities. When the electrodeposition current density was 1.0 A/cm², the alloy was obtained with a half-wave potential of 0.782 V, an onset potential of 0.936 V, and a limiting current density of 2.9 mA/cm². The rotating ring disk electrode(RRDE) test showed that the number of transferred electrons of the alloywas 3.52, which was close to that of the four-electron transfer of commercial Pt/C catalysts. An electrochemical deoxidation test equipment was designed to investigate the removal effect of NiCoFe alloy as a cathode electrode on dissolved oxygen in simulated industrial water. The results showed that the deoxidation rate of NiCoFe cathode was over 99%, making it an excellent ORR electrocatalyst material.

Key words: electrochemistry, deoxidation, electrocatalyst, oxygen reduction reaction, NiCoFe

摘要：

针对电化学脱氧中阴极氧还原反应（ORR）所用催化材料成本高、效果差的问题，在不同电流密度下通过电沉积法高效制备NiCoFe三元合金，并对合金材料的形貌和结构进行表征和分析，结果表明所制备NiCoFe合金有着蓬松的花椰菜状表面形貌和合金晶型结构。在三电极体系中对不同电流密度下制备的NiCoFe合金进行ORR性能测试，结果表明，当电沉积电流密度为1.0 A/cm²时，NiCoFe合金的半波电位为0.782 V，起始电位为0.936 V，极限电流密度为2.9 mA/cm²，盘环电极（RRDE）测试显示合金的转移电子数为3.52，接近于商用Pt/C催化剂的四电子转移。设计电化学脱氧小试设备用于考察NiCoFe合金作为阴极电极时对于模拟工业水中溶解氧的去除效果，结果表明NiCoFe阴极的脱氧率达99%以上，是一种性能优异的ORR电催化材料。

关键词: 电化学, 脱氧, 电催化剂, 氧还原反应, NiCoFe

CLC Number:

X703.1

Ximin WANG, Deze YU, Chenxin XIE, Tianzhen ZHU, Guanglei QIAN, Guangyuan YAO. Preparation of NiCoFe electrodes for electrochemical deoxidation by one-step electrodeposition[J]. Industrial Water Treatment, 2024, 44(6): 127-134.

王锡民, 于德泽, 谢陈鑫, 朱田震, 钱光磊, 姚光源. 一步电沉积法制备NiCoFe电极用于电化学脱氧的研究[J]. 工业水处理, 2024, 44(6): 127-134.

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URL: https://gyscl.magtechjournal.com/EN/10.19965/j.cnki.iwt.2023-0551

https://gyscl.magtechjournal.com/EN/Y2024/V44/I6/127

Figures/Tables 13

Fig.1 Schematic diagram of electrochemical deoxidation device

Fig.2 SEM of NiCoFe alloys electrodeposition at different current densities

Fig.3 XRD patterns of electrodeposited NiCoFe alloys at different current densities

Table 1 The elemental composition of electrodeposited NiCoFe alloys at different current densities

电流密度/（A·cm^-2）	原子数分数/%
电流密度/（A·cm^-2）	Fe	Co	Ni
0.3	6.4	31.1	62.5
0.5	9.3	31.6	59.1
1.0	22.1	32.7	45.2
1.5	10.8	32.0	57.2

Fig.4 Distribution of Fe，Co and Ni elements in NiCoFe alloy

Fig.5 CV diagrams of different metallic materials（a） and NiCoFe alloys（b） prepared under different current densities

Fig.6 LSV curves of NiCoFe alloys prepared under different current densities

Fig.7 EIS patterns of different metallic materials（a） and NiCoFe alloys（b） prepared under different current densities

Fig.8 Stability test curves of electrodeposited NiCoFe alloys at different current densities

Fig.9 Disk ring current density of NiCoFe alloy obtained by RRDE test

Table 2 Oxygen removal properties of different metal materials

材料	电流/A	电压/V	阴极进水流量/（L·h^-1）	阳极进水流量/（L·h^-1）	出水溶解氧/（μg·L^-1）
铜片	0.3	5.10	9.0	3.6	2 300
不锈钢片	0.3	5.00	9.0	3.6	3 600
钛片	0.3	5.30	9.0	3.6	5 400
NiCoFe	0.3	5.10	9.0	3.6	400

Fig.10 Deoxidation performance of electrodeposited NiCoFe alloys at different current densities for different time periods

Table 3 Oxygen removal properties of NiCoFe alloys at different current

电流/A	电压/V	阴极进水流量/（L·h^-1）	阳极进水流量/（L·h^-1）	出水溶解氧/（μg·L^-1）
0.053（理论）	2.15	1.5	0.6	90
0.106（2倍）	3.10	1.5	0.6	35
0.161（3倍）	3.95	1.5	0.6	38
0.212（4倍）	4.30	1.5	0.6	40

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