铱基催化剂在酸性析氧反应中的研究进展

doi:10.1016/S1872-2067(20)63722-6

催化学报 ›› 2021, Vol. 42 ›› Issue (7): 1054-1077.DOI: 10.1016/S1872-2067(20)63722-6

铱基催化剂在酸性析氧反应中的研究进展

刘一蒲^a, 梁宵^a, 陈辉^a, 高瑞芹^a^,^b, 石磊^a, 杨岚^a, 邹晓新^a^,^*()

^a吉林大学化学学院, 无机合成与制备化学国家重点实验室, 吉林长春130012
^b宁波理工学院, 生物与化学工程学院, 浙江宁波315100

收稿日期:2020-08-27 接受日期:2020-10-13 出版日期:2021-07-18 发布日期:2020-12-10
通讯作者: 邹晓新
作者简介:^* 电话/传真: (0431)85168221; 电子信箱: xxzou@jlu.edu.cn
基金资助:
国家自然科学基金(21922507);国家自然科学基金(21771079);国家自然科学基金(22005116);国家自然科学基金(21621001);霍英东青年教师奖励基金(161011);博士后国际交流计划派出项目(20190054);111引智计划(B17020)

Iridium-containing water-oxidation catalysts in acidic electrolyte

Yipu Liu^a, Xiao Liang^a, Hui Chen^a, Ruiqin Gao^a^,^b, Lei Shi^a, Lan Yang^a, Xiaoxin Zou^a^,^*()

^aState Key Laboratory of Inorganic Synthesis and Preparative Chemistry, College of Chemistry, Jilin University, Changchun 130012, Jilin, China
^bSchool of Biological and Chemical Engineering, NingboTech University, Ningbo 315100, Zhejiang, China

Received:2020-08-27 Accepted:2020-10-13 Online:2021-07-18 Published:2020-12-10
Contact: Xiaoxin Zou
Supported by:
National Natural Science Foundation of China(21922507);National Natural Science Foundation of China(21771079);National Natural Science Foundation of China(22005116);National Natural Science Foundation of China(21621001);Fok Ying Tung Education Foundation(161011);International Postdoctoral Exchange Fellowship Program(20190054);111 Project(B17020)

摘要/Abstract

摘要：

降低对化石能源依赖, 实现无碳能源需要构建以可再生能源(如太阳能、风能等)为主体的能源框架. 氢气是无碳能源框架下的一种较为理想的能源载体, 而电解水制氢技术能够有效制备环境友好的高纯氢气. 其中, 质子交换膜基(PEM)电解水技术相较碱性电解技术能够实现更高的质子导电性、电解效率、响应速度以及产物气体分离能力, 展现出较高的应用价值. 然而, 由于PEM电解技术工作环境为高腐蚀性的强酸条件, 极大限制了催化材料的选择范围. 同时, 由于PEM电解池的阳极端析氧反应效率远远低于阴极端析氢反应, 因此析氧反应作为瓶颈反应决定了PEM电解池的总体工作效率. 由于其催化条件同时具有强酸性和强氧化性, 目前只有铱基催化剂能够保持较长时间催化活性. 二氧化铱(IrO₂)是PEM电解水技术商用析氧催化剂. 然而由于铱元素在地球上储量极低(0.001 ppm), 因此铱基催化剂的使用严重限制了PEM电解池的大规模应用. 为发展PEM电解技术, 亟需研制出高活性、高稳定性的新型低铱催化剂来替代IrO₂.
本文首先总结了酸性析氧反应的催化机理, 并给出了衡量材料催化性能的普适方法. 其次, 总结了多个课题组利用原位表征技术获得的晶化IrO₂以及无定形IrO_x在不同催化条件下的结构变化, 以期了解材料的共性催化特征及影响结构变化的可能因素. 再次, 进一步重点描述了三类常见低铱催化剂, 包括异原子掺杂IrO₂(IrO_x)基催化剂、钙钛矿型铱基催化剂及烧绿石型铱基催化剂, 并尝试关联材料结构特征与催化本征性能. 最后, 介绍了该领域尚未解决的问题与挑战, 以期在酸性析氧反应条件下进一步平衡催化材料的催化活性和催化稳定性.

关键词: 电催化, 析氧反应, 水裂解, 铱, 质子交换膜电解池

Abstract:

With the goal of constructing a carbon-free energy cycle, proton-exchange membrane (PEM) water electrolysis is a promising technology that can be integrated effectively with renewable energy resources to produce high-purity hydrogen. IrO₂, as a commercial electrocatalyst for the anode side of a PEM water electrolyzer, can both overcome the high corrosion conditions and exhibit efficient catalytic performance. However, the high consumption of Ir species cannot meet the sustainable development and economic requirements of this technology. Accordingly, it is necessary to understand the OER catalytic mechanisms for Ir species, further designing new types of low-iridium catalysts with high activity and stability to replace IrO₂. In this review, we first summarize the related catalytic mechanisms of the acidic oxygen evolution reaction (OER), and then provide general methods for measuring the catalytic performance of materials. Second, we present the structural evolution results of crystalline IrO₂ and amorphous IrO_x using in situ characterization techniques under catalytic conditions to understand the common catalytic characteristics of the materials and the possible factors affecting the structural evolution characteristics. Furthermore, we focus on three types of common low-iridium catalysts, including heteroatom-doped IrO₂ (IrO_x)-based catalysts, perovskite-type iridium-based catalysts, and pyrochlore-type iridium-based catalysts, and try to correlate the structural features with the intrinsic catalytic performance of materials. Finally, at the end of the review, we present the unresolved problems and challenges in this field in an attempt to develop effective strategies to further balance the catalytic activity and stability of materials under acidic OER catalytic conditions.

Key words: Electrocatalysis, Oxygen evolution reaction, Water splitting, Iridium, Proton exchange membrane electrolyzer

刘一蒲, 梁宵, 陈辉, 高瑞芹, 石磊, 杨岚, 邹晓新. 铱基催化剂在酸性析氧反应中的研究进展[J]. 催化学报, 2021, 42(7): 1054-1077.

Yipu Liu, Xiao Liang, Hui Chen, Ruiqin Gao, Lei Shi, Lan Yang, Xiaoxin Zou. Iridium-containing water-oxidation catalysts in acidic electrolyte[J]. Chinese Journal of Catalysis, 2021, 42(7): 1054-1077.

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图/表 12

Fig. 1. Schematic illustration of the electrolyzer as a key part for constructing future hydrogen energy systems.

Fig. 2. Schematic illustration of (a) typical AEM scheme, (b) scaling relationship among M-OH, M-O and M-OOH, (c) a volcano plot using descriptor to represent the catalytic activity trend. (d) The volcano plot between catalytic activities and ΔGO - ΔGOH. Reproduced with permission [36]. Copyright 2011, Wiley-VCH. (e) The volcano plot between catalytic activities and eg electron. Reproduced with permission [38]. Copyright 2011, American Association for the Advancement of Science. (f) The relationship between p-state center and oxygen adsorption energy for cubic ABO3 oxides. Reproduced with permission. Copyright 2018, Royal Society of Chemistry [39].

Fig. 3. (a) Schematic illustration of three possible LOM schemes. (b) APT data of the near-surface region of hydrous Ir16Ox. (c) Local mass spectrum of oxide cluster in (b). (b,c) Reproduced with permission [42]. Copyright 2019, Royal Society of Chemistry. (d) Colored HRTEM image of La2LiIrO6 after 50 CV measurements. (e) XAS spectra of pristine La2LiIrO6, La2LiIrO6 after oxidation and IrO2. (d,e) Reproduced with permission [43]. Copyright 2017, Nature Publishing Group.

Fig. 4. (a) A polarization curve for OER. η10 is the overpotential at 10 mA/cm2. (b) A Tafel plot converted from (a). The red dashed line depicts the least potential deviation for determining the linear region. (c) Schematic diagrams of Tafel plot analysis for two specific catalysts. (d) CV plots with different scan rates under the non-Faradic range. (e) A linear trend conducted from the difference of ?j against different scan rates. (f) CV plot of SrZrO3-SrIrO3 solid solution at a potential region of 0.4-1.4 V vs. RHE.

Fig. 5. (a) The inverse relationship between the stabilities of monometallic oxides and their reactivities for OER. Reproduced with permission [56]. Copyright 2014, American Chemical Society. (b) Stability number presented for iridium containing catalysts in thin film or powder form. (c) Stability number plotted versus mass specific current density for some iridium containing powder catalysts. (b,c) Reproduced with permission [60]. Copyright 2018, Nature Publishing Group. (d) The activity stability factor (ASF) for Ir-poly and dft-Ir25Os75. Reproduced under the terms of the Creative Commons Attribution License.

Fig. 6. Iridium dissolution profiles for (a) Ir black (red), electrochemically oxidized iridium (blue) and (b) thermally prepared IrO2 when cycling the catalysts from 0.05 to 1.2 V. (a,b) Reproduced with permission [62]. Copyright 2017, American Chemical Society. (c) CV curves (left axis) and Ir oxidation state value at applied potentials (right axis) of EIROF. Reproduced with permission [65]. Copyright 2014, Royal Society of Chemistry. Ir 4f (d) and O 1s (e) XPS spectrum under open circuit and oxygen evolution conditions. (d,e) Reproduced with permission [66]. Copyright 2014, Wiley-VCH.

Fig. 7. (a) O K-edge spectra of IrO2 and amorphous IrOx. Reproduced with permission [67]. Copyright 2016, Royal Society of Chemistry. (b) O K-edge spectra of Ir-coated PEM during and after OER. (c) O K-edge spectra of Ir-coated PEM at successively applied potentials. (b,c) Reproduced with permission [69]. Copyright 2017, Royal Society of Chemistry.

Fig. 8. Dissolved Ru and Ir for (a) Ru@IrOx and (b) RuIrOx at different times. Reproduced with permission [71]. Copyright 2019, Elsevier. (c) Mass activity comparison between Ir0.7Ru0.3Ox (EC) and Ir0.7Ru0.3O2 (TT). Reproduced with permission [74]. Copyright 2017, Elsevier. (d) Schematic illustration of the Ni leaching from the surface of Ir-Ni mixed oxides. Reproduced with permission [75]. Copyright 2015, American Chemical Society. (e) Schematic illustration of catalytic sites in IrNiOx nanoparticles. Reproduced with permission [76]. Copyright 2018, Nature Publishing Group.

Fig. 9. (a) Crystal structure of 6H-SrIrO3. Reproduced with permission [87]. Copyright 2018, Nature Publishing Group. (b) Crystal structure of Ba3M’M’’2O9 triple perovskites. (c) XRD patterns of Ba3M’Ir2O9. (b,c) Reproduced with permission [91]. Copyright 2020, American Chemical Society. (d) The crystal structure and (e) electron location function (ELF) of 12L-perovskites (Ba4MIr3O12). (d,e) Reproduced with permission [90]. Copyright 2020, Elsevier. (f) The structure of Ruddlesden-Popper (RP) phases with (ABO3)n=1/(AO) formula. Reproduced with permission [93]. Copyright 2014, American Chemical Society. (g) Specific OER activity of Sr iridates in 0.1 M HClO4. Reproduced with permission [94]. Copyright 2017, American Chemical Society.

Table 1 List of structure information, measurement parameters and catalytic performances of complex iridium-based oxides.

Catalyst	Structural information	Electrolyte solution	Mass loading (mg/cm²)	η at j_geo=10 mA/cm_geo²(mV)	Specific activity	Mass fraction of dissolved ions	Ref.
IrO_x/SrIrO₃	Orthorhombic perovskite	0.5 M H₂SO₄	—	270-290 (AFM normalized)	1.53 V ~12 mA/cm_AFM²	CV @30 min (ICP) Sr-30%-50%	[79]
Ba₂PrIrO₆	Cubic perovskite	0.1 M HClO₄	0.95	~400 (~425 @1 h)	1.53 V ~1 mA/cm_ECSA²	1.55 V @1 h (ICP) Ba-14.2% Ir-0.8% Pr-11.3%	[82]
Pr₃IrO₇	Fluorite	0.1 M HClO₄	0.95	—	1.53 V ~0.1 mA/cm_ECSA²	—	[82]
SrCo_0.9Ir_0.1O_3-_δ	Orthorhombic perovskite	0.1 M HClO₄	0.255	~330	1.53 V ~10 mA/cm_BET²	10k cycles CV (ICP) Sr-64.11% Co-67.08% Ir-35.5%	[83]
Ir doped SrTiO₃	Cubic perovskite	0.1 M HClO₄	0.21	247	1.525 V 820 A/g_Ir 0.125 mA/cm_ECSA² 0.455 mA/cm_BET²	—	[84]
SrZrO₃-SrIrO₃ solid solution	Orthorhombic perovskite	0.1 M HClO₄	0.13	240	1.53 V 1540 A/g_Ir 0.22 mA/cm_ECSA² 1.2 mA/cm_BET²1.35 A/C	10 mA/cm_geo² @10h (ICP) Sr-12% Ir-1%	[53]
3C-SrIrO₃	Orthorhombic perovskite-3C	0.5 M H₂SO₄	0.9	270	1.525 V 38 A/g_Ir	10 mA/cm_geo² @30h (ICP) Sr-24%	[87]
6H-SrIrO₃	Monoclinic perovskite-6H	0.5 M H₂SO₄	0.9	248	1.525 V 76 A/g_Ir	10 mA/cm_geo² @30h (ICP) Sr-1%	[87]
Co-doped SrIrO₃ (6H)	Monoclinic perovskite-6H	0.1 M HClO₄	0.45	235	1.525 V 286.7 A/g_Ir	10 mA/cm_geo² @1h (ICP) Sr-12% Co-0.5% Ir-0.1%	[104]
BaIrO₃ polycrystalline particles	Monoclinic perovskite	0.5 M H₂SO₄	0.5	—	1.58 V 90 A/g_oxide ~4 A/F_ECSA	100-cycle CV (EDS) Ba-100%	[105]
La₂LiIrO₆	Monoclinic perovskite	0.1 M H₂SO₄	0.25	~300	1.53V ~40 A/g_oxide ~2.5 mA/cm_BET²	1.65 V @10 min (XPS) Ir-26.7% La-94.5% Li-100%	[43]
Ba₄PrIr₃O₁₂	Monoclinic perovskite-12L	0.1 M HClO₄	0.562	278	1.55 V 145 A/g_Ir 2.63 mA/cm_ECSA²	10 mA/cm_geo² @10 h (ICP) Ba-32% Pr-32% Ir-1.18%	[90]
Ba₃TiIr₂O₉	Hexagonal perovskite	0.1 M HClO₄	0.281	275	1.53 V 0.89 mA/cm_ECSA² 250 A/g_Ir	10 mA/cm_geo² @10 h (ICP) Ba-2.1% Ti-1.6%	[91]
Sr₂IrO₄	Tetragonal perovskite	0.1 M HClO₄	0.08 mg_Ir/cm²	286	1.55 V 394 A/g_Ir 6.1 mA/cm_BET²	10 mA/cm_geo² @6h (ICP) Sr-74% Ir-4%	[94]
Sr₄IrO₆	Hexagonal perovskite	0.1 M HClO₄	0.08 mg_Ir/cm²	287	1.55 V 274 A/g_Ir 0.7 mA/cm_BET²	10 mA/cm_geo² @6h (ICP) Sr-90% Ir-30%	[94]
Ca₂IrO₄	Hexagonal perovskite	0.1 M HClO₄	0.20	370	—	—	[95]
H_3.6IrO₄·3.7H₂O	Tetragonal perovskite	0.1 M HClO₄	0.255	—	1.53 V ~3.5 mA/cm_BET²	1 mA/cm_geo² @1 h (ICP) Ir-0.08%	[85]
Sr₂CoIrO₆	Orthorhombic perovskite	0.1 M HClO₄	0.255	330 (BET normalized)	1.55 V 3.5 mA/cm_BET²	1 mA/cm_BET² @24 h (ICP) Sr-5% Co-4% Ir-2.8%	[106]
Sr₂FeIrO₆	Triclinic perovskite	0.1 M HClO₄	0.255	420 (BET normalized)	1.55 V 1.8 mA/cm_BET²	1 mA/cm_oxide² @24 h (ICP) Sr-7% Fe-6% Ir-3%	[106]
Sr₂Fe_0.5Ir_0.5O₄	Tetragonal perovskite	0.1 M HClO₄	0.255	410 (BET normalized)	1.55 V 2.5 mA/cm_BET²	1 mA/cm_oxide² @24 h (ICP) Sr-4% Fe-6% Ir-8%	[106]
Pb₂Ir₂O_6.5	Cubic pyrochlore	0.1 M HClO₄	0.2	~470	1.55 V ~150 A/g_Ircm^-2	—	[98]
Bi₂Ir₂O₇	Cubic pyrochlore	0.1 M HClO₄	0.2		1.6 V ~30 A/g_Ircm^-2	—	[98]
Pr₂Ir₂O₇	Cubic pyrochlore	0.1 M HClO₄	0.285	~290	1.53 V 424.5 A/g_Ir	—	[99]
K_x_≈0.25IrO₂	Monoclinic hollandite	0.1 M HClO₄	0.2	350	1.53 V 12.2 A/g_Ir	—	[107]
CaIrO₃	Cubic perovskite	0.1 M HClO₄	0.2	—	1.55 V 30 A/g_Ir	—	[108]
β-H₂IrO₃	Orthorhombic	0.1 M H₂SO₄	0.5	345	1.53 V 1.0 mA/cm_BET²	50 h@1.55 V Ir-0.2 %	[109]

Table 1 List of structure information, measurement parameters and catalytic performances of complex iridium-based oxides.

Catalyst	Structural information	Electrolyte solution	Mass loading (mg/cm²)	η at j_geo=10 mA/cm_geo²(mV)	Specific activity	Mass fraction of dissolved ions	Ref.
IrO_x/SrIrO₃	Orthorhombic perovskite	0.5 M H₂SO₄	—	270-290 (AFM normalized)	1.53 V ~12 mA/cm_AFM²	CV @30 min (ICP) Sr-30%-50%	[79]
Ba₂PrIrO₆	Cubic perovskite	0.1 M HClO₄	0.95	~400 (~425 @1 h)	1.53 V ~1 mA/cm_ECSA²	1.55 V @1 h (ICP) Ba-14.2% Ir-0.8% Pr-11.3%	[82]
Pr₃IrO₇	Fluorite	0.1 M HClO₄	0.95	—	1.53 V ~0.1 mA/cm_ECSA²	—	[82]
SrCo_0.9Ir_0.1O_3-_δ	Orthorhombic perovskite	0.1 M HClO₄	0.255	~330	1.53 V ~10 mA/cm_BET²	10k cycles CV (ICP) Sr-64.11% Co-67.08% Ir-35.5%	[83]
Ir doped SrTiO₃	Cubic perovskite	0.1 M HClO₄	0.21	247	1.525 V 820 A/g_Ir 0.125 mA/cm_ECSA² 0.455 mA/cm_BET²	—	[84]
SrZrO₃-SrIrO₃ solid solution	Orthorhombic perovskite	0.1 M HClO₄	0.13	240	1.53 V 1540 A/g_Ir 0.22 mA/cm_ECSA² 1.2 mA/cm_BET²1.35 A/C	10 mA/cm_geo² @10h (ICP) Sr-12% Ir-1%	[53]
3C-SrIrO₃	Orthorhombic perovskite-3C	0.5 M H₂SO₄	0.9	270	1.525 V 38 A/g_Ir	10 mA/cm_geo² @30h (ICP) Sr-24%	[87]
6H-SrIrO₃	Monoclinic perovskite-6H	0.5 M H₂SO₄	0.9	248	1.525 V 76 A/g_Ir	10 mA/cm_geo² @30h (ICP) Sr-1%	[87]
Co-doped SrIrO₃ (6H)	Monoclinic perovskite-6H	0.1 M HClO₄	0.45	235	1.525 V 286.7 A/g_Ir	10 mA/cm_geo² @1h (ICP) Sr-12% Co-0.5% Ir-0.1%	[104]
BaIrO₃ polycrystalline particles	Monoclinic perovskite	0.5 M H₂SO₄	0.5	—	1.58 V 90 A/g_oxide ~4 A/F_ECSA	100-cycle CV (EDS) Ba-100%	[105]
La₂LiIrO₆	Monoclinic perovskite	0.1 M H₂SO₄	0.25	~300	1.53V ~40 A/g_oxide ~2.5 mA/cm_BET²	1.65 V @10 min (XPS) Ir-26.7% La-94.5% Li-100%	[43]
Ba₄PrIr₃O₁₂	Monoclinic perovskite-12L	0.1 M HClO₄	0.562	278	1.55 V 145 A/g_Ir 2.63 mA/cm_ECSA²	10 mA/cm_geo² @10 h (ICP) Ba-32% Pr-32% Ir-1.18%	[90]
Ba₃TiIr₂O₉	Hexagonal perovskite	0.1 M HClO₄	0.281	275	1.53 V 0.89 mA/cm_ECSA² 250 A/g_Ir	10 mA/cm_geo² @10 h (ICP) Ba-2.1% Ti-1.6%	[91]
Sr₂IrO₄	Tetragonal perovskite	0.1 M HClO₄	0.08 mg_Ir/cm²	286	1.55 V 394 A/g_Ir 6.1 mA/cm_BET²	10 mA/cm_geo² @6h (ICP) Sr-74% Ir-4%	[94]
Sr₄IrO₆	Hexagonal perovskite	0.1 M HClO₄	0.08 mg_Ir/cm²	287	1.55 V 274 A/g_Ir 0.7 mA/cm_BET²	10 mA/cm_geo² @6h (ICP) Sr-90% Ir-30%	[94]
Ca₂IrO₄	Hexagonal perovskite	0.1 M HClO₄	0.20	370	—	—	[95]
H_3.6IrO₄·3.7H₂O	Tetragonal perovskite	0.1 M HClO₄	0.255	—	1.53 V ~3.5 mA/cm_BET²	1 mA/cm_geo² @1 h (ICP) Ir-0.08%	[85]
Sr₂CoIrO₆	Orthorhombic perovskite	0.1 M HClO₄	0.255	330 (BET normalized)	1.55 V 3.5 mA/cm_BET²	1 mA/cm_BET² @24 h (ICP) Sr-5% Co-4% Ir-2.8%	[106]
Sr₂FeIrO₆	Triclinic perovskite	0.1 M HClO₄	0.255	420 (BET normalized)	1.55 V 1.8 mA/cm_BET²	1 mA/cm_oxide² @24 h (ICP) Sr-7% Fe-6% Ir-3%	[106]
Sr₂Fe_0.5Ir_0.5O₄	Tetragonal perovskite	0.1 M HClO₄	0.255	410 (BET normalized)	1.55 V 2.5 mA/cm_BET²	1 mA/cm_oxide² @24 h (ICP) Sr-4% Fe-6% Ir-8%	[106]
Pb₂Ir₂O_6.5	Cubic pyrochlore	0.1 M HClO₄	0.2	~470	1.55 V ~150 A/g_Ircm^-2	—	[98]
Bi₂Ir₂O₇	Cubic pyrochlore	0.1 M HClO₄	0.2		1.6 V ~30 A/g_Ircm^-2	—	[98]
Pr₂Ir₂O₇	Cubic pyrochlore	0.1 M HClO₄	0.285	~290	1.53 V 424.5 A/g_Ir	—	[99]
K_x_≈0.25IrO₂	Monoclinic hollandite	0.1 M HClO₄	0.2	350	1.53 V 12.2 A/g_Ir	—	[107]
CaIrO₃	Cubic perovskite	0.1 M HClO₄	0.2	—	1.55 V 30 A/g_Ir	—	[108]
β-H₂IrO₃	Orthorhombic	0.1 M H₂SO₄	0.5	345	1.53 V 1.0 mA/cm_BET²	50 h@1.55 V Ir-0.2 %	[109]

Fig. 10. (a) The crystal structure of pyrochlore. Reproduced with permission [97]. Copyright 2017, American Chemical Society. (b) Valence band spectra of Pb-Ir, Bi-Ir pyrochlores and IrO2. (c) Schematic illustration of the broadening Ir-5d band induced by the distortion of octahedra. (b,c) Reproduced with permission [98]. Copyright 2016, Nature Publishing Group. (d) Electronic phase diagram and corresponding band structure of Ir 5d orbitals. (e) O K-edge XAS of different pyrochlores. (d,e) Reproduced with permission [99]. Copyright 2018, Wiley-VCH. (f) Geometric current density and iridium mass activity of the different pyrochlores. Reproduced with permission [100]. Copyright 2019, American Chemical Society.

Fig. 11. Important perspectives for balancing the activity and stability of catalysts under acidic OER condition.

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铱基催化剂在酸性析氧反应中的研究进展

Iridium-containing water-oxidation catalysts in acidic electrolyte

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