Applications of low-temperature non-equilibrium plasmas in preparation and modification of high-efficiency water electrolysis catalysts

LI Yongjian; LI Guoling; LIU Xiao; ZHENG Jie

doi:10.7498/aps.74.20251363

Abstract
Hydrogen energy, as one of the most promising clean and renewable energy sources, has received much attention due to its green production technology. Electrolytic water splitting is regarded as a critical pathway for large-scale green hydrogen production due to its environmentally friendly reaction process, high product purity, and operational simplicity, However, electrocatalysts for water electrolysis commonly face challenges such as high costs and complex synthesis processes, thereby severely hindering the industrial application. Low-temperature plasma (LTP) technology, with its advantages of mild processing conditions, high reactivity, and unique electromagnetic field effects, has demonstrated remarkable potential in the surface modification of materials. This review systematically summarizes the applications of LTP in the preparation and modification of electrocatalytic materials for water splitting, focusing on the mechanism of plasma-induced enhancement in electrocatalytic efficiency. First, the physical characteristics and fundamental principle of typical non-equilibrium low-temperature plasma are elucidated. Subsequently, recent advances in plasma-assisted modification strategies for catalytic materials are categorized and critically discussed, including surface microstructure modulation, surface property regulation and interface optimization. Finally, based on the current limitations in mechanistic understanding and practical applications, future research directions for LTP technology in catalyst design are proposed.

Keywords:
plasma /

material preparation /

material modification /

electrocatalysis
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图 1 低压非平衡等离子体　(a) 直流辉光放电^[13]; (b) 电容耦合射频等离子体^[14]; (c) 介质阻挡放电等离子体^[15]

Figure 1. Low-pressure non-equilibrium plasmas: (a) Glow discharge ^[13]; (b) capacitively coupled radio-frequency plasma^[14]; (c) dielectric barrier discharge plasma^[15].

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图 2 (a) 双朗缪尔探针的I-V曲线^[32]; (b) 朗缪尔探针与非侵入式阻抗等离子体密度测量结果对比图^[33]; (c) P-Ar-H₂等离子体和Ar-CH₄等离子体的光学发光光谱^[34]; (d) 氧气气氛的光学发光光谱^[35]; (e) 不同压力下介质阻挡放电等离子体放电图像^[36]; (f) 不同压力下氮气的发射强度^[36]

Figure 2. (a) I-V curve of double Langmuir probe^[32]; (b) comparison of Langmuir probe non-invasive impedance plasma density^[33]; (c) in suit optical emission spectra of plasma of P-Ar-H₂ and Ar-CH₄^[34]; (d) optical emission spectroscopy of O₂ atmosphere^[35]; (e) discharge images of DBD at different pressures^[36]; (f) emission intensities of N₂ at different pressures^[36].

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图 3 (a), (b) L-Co纳米结构形成示意图和扫描电子显微镜图像^[37]; (c) Co₂P-Ni₂P/CC扫描电子显微镜图像^[38]; (d) 富氧NiFe-LDH的透射电子显微镜图像^[39]; (e) 富氧NiFe-LDH纳米片的比表面积和孔径分布^[39]; (f) P-Ni MOF/POM制备流程图^[40]; (g) Ni MOF/POM扫描电子显微镜图像^[40]; (h) 多孔P-Ni MOF/POM扫描电子显微镜图像^[40]; (i) Ni₃N/NF的扫描电子显微图像^[41]; (j) N₂-H₂等离子体下Ni₃N/NF合成示意图^[41]

Figure 3. (a), (b) Schematic illustration for the formation and SEM images of L-Co NSs^[37]; (c) SEM images of Co₂P-Ni₂P/CC^[38]; (d) TEM images of oxygen-enriched NiFe-LDH^[39]; (e) BET and pore diameter distribution of oxygen-enriched NiFe-LDH nanosheets^[39]; (f) schematic illustration of the fabrication process of porous P-Ni MOF/ POM^[40]; (g) SEM image of Ni MOF/POM^[40]; (h) SEM images of P-Ni MOF/ POM^[40]; (i) SEM image of Ni₃N/NF^[41]; (j) schematic illustration of the synthesis of Ni₃N/NF under N₂-H₂ plasma^[41].

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图 4 (a)—(c) NiFeP/NF合成示意图、NiFe/NF和NiFeP/NF的扫描电子显微镜图像^[44]; (d) CoPO合成示意图^[45]; (e), (f) ZIF-67和CoPO的扫描电子显微镜图像^[45]; (g), (h) 磷化前后的T-NiMoP电子显微镜图像^[46]; (i) Co₂N的扫描电子显微镜图像^[47]

Figure 4. (a)–(c) Synthesis process of NiFeP/NF and SEM images of NiFeMOF/NF and NiFeP/NF^[44]; (d) synthesis process of CoPO^[45]; (e), (f) SEM image of ZIF-67 and CoPO^[45]; (g), (h) SEM image of P-NiMoP and T-NiMoP^[46]; (i) SEM image of Co₂N^[47].

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图 5 (a), (b) NiCo-LDHs和NiCo-LDHs/Ar的扫描电子显微镜图像^[50]; (c), (d) 等离子体处理前后的氢氧化镍纳米片的扫描电子显微镜图像^[51]; (e) 等离子体处理前后MoS₂的透射电子显微镜图像^[48]; (f), (g) 等离子体剥离前后的MXene材料的扫描电子显微镜图像^[52]; (h), (i) MXene和MXene-DBD的扫描电子显微镜图像^[53]

Figure 5. (a), (b) SEM images of NiCo-LDHs and NiCo-LDHs/Ar^[50]; (c), (d) SEM images of m-Ni(OH)₂NASs and β-Ni(OH)₂/Ni NSAs^[51]; (e) TEM images of MoS₂ after plasma treatment^[48]; (f), (g) SEM images of MXene@GO and MXene@rGO^[52]; (h), (i) SEM images of MXene and MXene-DBD^[53].

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图 6 (a)—(c) 纳米颗粒晶格间距的高分辨透射电子显微镜、O 1s轨道的X射线光电子能谱、纳米颗粒的带隙测定^[58]; (d)—(f) N₂等离子体处理不同时间的电子顺磁共振光谱、O 1s轨道的X射线光电子能谱、N₂等离子体处理后的NiMoO₄的高分辨率透射电镜图像^[59]; (g) 不同条件等离子体处理的傅里叶转换光谱; (h) PBA-raw和PBA-3h-A的电子自旋共振光谱; (i) 等离子体处理后的PBA的水接触角^[60]

Figure 6. (a)–(c) HRTEM image showing lattice spacing of the nanoparticle, XPS spectra of the O 1s, bandgap determination of the nanoparticles^[58]; (d)–(f) EPR spectra by N₂ plasma for different periods, XPS spectra of the O 1s and HRTEM image of NiMoO₄ under N₂ plasma treated^[59]; (g) Fourier transform infrared spectra of plasma treated under different conditions; (h) solid electron spin resonance spectra of PBA-raw and PBA-3h-A; (i) water contact angle (WCA) of plasma treated PBA^[60].

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图 7 (a), (b) Ar/NH₃等离子体处理前后的拉曼光谱和热重曲线^[63]; (c), (d) 氧化钴异质结经氧等离子体处理前后的拉曼光谱和N₂吸附-脱附等温曲线^[64]; (e), (f) 氮掺杂纳米管经Ar等离子体处理前后的拉曼光谱和C 1s轨道的X射线光电子能谱^[65]

Figure 7. (a), (b) Raman spectra and Thermogravimetry (TGA) curves before and after Plasma treatment^[63]; (c), (d) Raman spectra and N₂ adsorption-desorptionisotherms of cobalt oxide heterojunctions before and after oxygen plasma treatment^[64]; (e), (f) Raman spectra and XPS spectra of the C 1s of nitrogen-doped nanotubes before and after Ar plasma treatment^[65].

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图 8 (a) NiFeP/NF, NiFe MOF/NF和NiFe LDH/NF的X射线衍射^[44]; (b) NiFeP/NF的高分辨率透射电镜图像^[44]; (c) CoNiP@C/NF的X射线衍射^[68]; (d) CoNiP@C和CoNiP的P 2p轨道的X射线光电子能谱^[68]; (e)—(g) N₂-H₂和纯N₂的光发射光谱、不同等离子体处理后氢氧化镍的X射线衍射、N₂-H₂等离子体处理后Ni 2p的XPS光谱^[69]; (h), (i) N₂-H₂等离子体处理NiV LDH的X射线衍射和Ni 1s轨道的X射线光电子能谱^[70]

Figure 8. (a) X-ray diffraction (XRD) of NiFeP/NF, NiFeMOF/NF, and NiFeLDH/NF^[44]; (b) HR-TEM images of NiFeP/NF^[44]; (c) XRD patterns of CoNiP@C/NF^[49]; (d) XPS spectra of P 2p of CoNiP@C and CoNiP^[68]; (e)–(g) optical emission spectra of N₂-H₂ and N₂, XRD of Ni(OH)₂ after different plasma treatment and XPS spectra of Ni 2p after N₂-H₂ plasma treatments^[69]; (h), (i) XRD pattern and Ni 1s XPS spectra of the NiV LDH after N₂-H₂ plasma treatment^[70].

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图 9 (a) Co₂P和Ni₂P的高分辨率透射电子显微图像^[71]; (b) 基于Co₂P-Ni₂P/CC中生物电化学体统(BEF)的电子转移示意图^[71]; (c) 等离子体进行磷氮掺杂的NiCo泡沫高分辨率透射电子显微镜图像^[72]; (d) CoO/Co的高分辨率透射电子显微镜图像^[73]; (e) v-CoO/Co(111), Co(111)和v-CoO的态密度和d带中心^[74]; (f) IrO₂/CoCH异质结构透射电子显微镜图像^[75]; (g) CoCH, IrO₂和IrO₂/CoCH的电子态密度^[75]; (h) Ni₁₂P₅/ZnP₂异质结构的透射电子显微镜图像^[75]; (i) N₂吸附-脱附等温线(孔径分布曲线)^[75]

Figure 9. (a) High-resolution transmission electron microscopy images of Co₂P and Ni₂P^[71]; (b) schematic diagram of electron transfer based on BEF in Co₂P-Ni₂P/CC^[71]; (c) high-resolution transmission electron microscopy images of plasma phosphorus-nitrogen doped NiCo foam^[72]; (d) the HRTEM of CoO/Co ^[73]; (e) DOS and d-band centers of -CoO/Co(111), Co(111), v-CoO^[73]; (f) the HRTEM images of heterostructure of IrO₂/CoCH^[74]; (g) the DOS of CoCH, IrO₂ and IrO₂/CoCH^[75]; (h) the TEM images of the heterostructure of Ni₁₂P₅/ZnP₂^[75]; (i) N₂ adsorption–desorption isotherms(BJH) ^[75].

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表 1 不同低温非平衡等离子体的典型参数

Table 1. Typical plasma parameters in different low temperature non-equilibrium plasma.

物理量	直流辉光放电	射频辉光放电	DBD
T_e(典型)/eV	0.5—5^[23]	1.0—3.0^[24]	1—5^[25]
n_e(典型)/cm^–3	10¹⁵—10^17[23]	10¹⁸—10^19[24]	10¹⁶—10^20[26]
IED	低压鞘层加速可达几十eV ^[27]	基底偏压或射频偏置调控几十eV^[31]	表面离子能较低, 瞬态流含高能电子^[26]
自由基	较为丰富^[28]	较为丰富^[29]	非常丰富但寿命短^[30]
典型改性	刻蚀、诱导缺陷	掺杂、诱导相变	表面改性

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