Synthesis · Electrocatalytic oxygen evolution reaction at IrOx supported by Ni/Co-ZIF-67: Controlled ratio of metallic Ir and Ir3+ states

8 structured synthesis routes

Completeness describes how fully the route could be reconstructed from the main article and supporting information.

Partial recipeSource: Main

Route 1: Other

article p2 · Experimental procedure, 2.3

Metal precursors100 mg Ni/Co-ZIF-67 support; 10 mg IrCl3.3H2O

Linker precursorsNi/Co-ZIF-67 support contains imidazolate linkers

Solvents50 ml DI water for support dispersion; 50 ml ethanol for Ir precursor solution

Atmospherenot specified

Temperatureroom temperature for 48 h, then maintained at 80 deg C; results text describes 70-80 deg C ethanol synthesis

Time48 h stirring at room temperature; time at 80 deg C not specified

Oxidant / reductantIrCl3.3H2O precursor; no separate oxidant/reductant reported

Work-uprinsed with DI water and ethanol to produce final product

Activationnot specified after rinsing

Scalability contextWet-chemical surfactant-free deposition on 100 mg support; no yield reported.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	Ni/Co-ZIF-67	100 mg	article p2 · Experimental procedure, 2.3
Metal Source	IrCl3.3H2O	10 mg	article p2 · Experimental procedure, 2.3
Solvent	DI water	50 ml	article p2 · Experimental procedure, 2.3
Solvent	ethanol	50 ml	article p2 · Experimental procedure, 2.3

Partial recipeSource: Main

Route 2: Other

article p2 · Experimental procedure, 2.3

Metal precursors100 mg Ni/Co-ZIF-67 support; 20 mg IrCl3.3H2O

Linker precursorsNi/Co-ZIF-67 support contains imidazolate linkers

Solvents50 ml DI water for support dispersion; 50 ml ethanol for Ir precursor solution

Atmospherenot specified

Temperatureroom temperature for 48 h, then maintained at 80 deg C; results text describes 70-80 deg C ethanol synthesis

Time48 h stirring at room temperature; time at 80 deg C not specified

Oxidant / reductantIrCl3.3H2O precursor; no separate oxidant/reductant reported

Work-uprinsed with DI water and ethanol to produce final product

Activationnot specified after rinsing

Scalability contextWet-chemical surfactant-free deposition on 100 mg support; no yield reported.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	Ni/Co-ZIF-67	100 mg	article p2 · Experimental procedure, 2.3
Metal Source	IrCl3.3H2O	20 mg	article p2 · Experimental procedure, 2.3
Solvent	DI water	50 ml	article p2 · Experimental procedure, 2.3
Solvent	ethanol	50 ml	article p2 · Experimental procedure, 2.3

Partial recipeSource: Main

Route 3: Other

article p2 · Experimental procedure, 2.3

Metal precursors100 mg Ni/Co-ZIF-67 support; 100 mg IrCl3.3H2O

Linker precursorsNi/Co-ZIF-67 support contains imidazolate linkers

Solvents50 ml DI water for support dispersion; 50 ml ethanol for Ir precursor solution

Atmospherenot specified

Temperatureroom temperature for 48 h, then maintained at 80 deg C; results text describes 70-80 deg C ethanol synthesis

Time48 h stirring at room temperature; time at 80 deg C not specified

Oxidant / reductantIrCl3.3H2O precursor; no separate oxidant/reductant reported

Work-uprinsed with DI water and ethanol to produce final product

Activationnot specified after rinsing

Scalability contextWet-chemical surfactant-free deposition on 100 mg support; no yield reported.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	Ni/Co-ZIF-67	100 mg	article p2 · Experimental procedure, 2.3
Metal Source	IrCl3.3H2O	100 mg	article p2 · Experimental procedure, 2.3
Solvent	DI water	50 ml	article p2 · Experimental procedure, 2.3
Solvent	ethanol	50 ml	article p2 · Experimental procedure, 2.3

Partial recipeSource: Main

Route 4: Hydrothermal

article p2 · Experimental procedure, 2.2

Metal precursors1 g total Co(NO3)2.6H2O/Ni(NO3)2.6H2O mixture at 0.95:0.05 weight ratio

Linker precursors0.5 g 2-methylimidazole, inherited from ZIF-67 procedure

Solvents60 ml mixed DI water/ethanol/N,N-dimethylformamide, inherited from ZIF-67 procedure; component ratios not specified

Atmospherenot specified

Temperature160

Time12; plus 1 h stirring before autoclave and overnight drying

Work-upsame washing, filtration, and drying procedure as ZIF-67 nanosheets

Activationdried overnight at 80 deg C prior to analysis

Scalability contextBatch autoclave synthesis; no yield reported.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Co (NO3)2.6H2O	part of 1 g total; Co/Ni 0.95:0.05	article p2 · Experimental procedure, 2.2
Metal Source	Ni (NO3)2.6H2O	part of 1 g total; Co/Ni 0.95:0.05	article p2 · Experimental procedure, 2.2
Linker	2-Methylimidazole	0.5 g	article p2 · Experimental procedure, 2.2
Solvent	distilled water/ethanol/N,N-dimethylformamide	60 ml mixed solution	article p2 · Experimental procedure, 2.2

Partial recipeSource: Main

Route 5: Hydrothermal

article p2 · Experimental procedure, 2.2

Metal precursors1 g total Co(NO3)2.6H2O/Ni(NO3)2.6H2O mixture at 0.9:0.1 weight ratio

Linker precursors0.5 g 2-methylimidazole, inherited from ZIF-67 procedure

Solvents60 ml mixed DI water/ethanol/N,N-dimethylformamide, inherited from ZIF-67 procedure; component ratios not specified

Atmospherenot specified

Temperature160

Time12; plus 1 h stirring before autoclave and overnight drying

Work-upsame washing, filtration, and drying procedure as ZIF-67 nanosheets

Activationdried overnight at 80 deg C prior to analysis

Scalability contextBatch autoclave synthesis; no yield reported.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Co (NO3)2.6H2O	part of 1 g total; Co/Ni 0.9:0.1	article p2 · Experimental procedure, 2.2
Metal Source	Ni (NO3)2.6H2O	part of 1 g total; Co/Ni 0.9:0.1	article p2 · Experimental procedure, 2.2
Linker	2-Methylimidazole	0.5 g	article p2 · Experimental procedure, 2.2
Solvent	distilled water/ethanol/N,N-dimethylformamide	60 ml mixed solution	article p2 · Experimental procedure, 2.2

Partial recipeSource: Main

Route 6: Hydrothermal

article p2 · Experimental procedure, 2.2

Metal precursors1 g total Co(NO3)2.6H2O/Ni(NO3)2.6H2O mixture at 0.7:0.3 weight ratio

Linker precursors0.5 g 2-methylimidazole, inherited from ZIF-67 procedure

Solvents60 ml mixed DI water/ethanol/N,N-dimethylformamide, inherited from ZIF-67 procedure; component ratios not specified

Atmospherenot specified

Temperature160

Time12; plus 1 h stirring before autoclave and overnight drying

Work-upsame washing, filtration, and drying procedure as ZIF-67 nanosheets

Activationdried overnight at 80 deg C prior to analysis

Scalability contextBatch autoclave synthesis; no yield reported.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Co (NO3)2.6H2O	part of 1 g total; Co/Ni 0.7:0.3	article p2 · Experimental procedure, 2.2
Metal Source	Ni (NO3)2.6H2O	part of 1 g total; Co/Ni 0.7:0.3	article p2 · Experimental procedure, 2.2
Linker	2-Methylimidazole	0.5 g	article p2 · Experimental procedure, 2.2
Solvent	distilled water/ethanol/N,N-dimethylformamide	60 ml mixed solution	article p2 · Experimental procedure, 2.2

Partial recipeSource: Main

Route 7: Hydrothermal

article p2 · Experimental procedure, 2.2

Metal precursors1 g total Co(NO3)2.6H2O/Ni(NO3)2.6H2O mixture at 0.5:0.5 weight ratio

Linker precursors0.5 g 2-methylimidazole, inherited from ZIF-67 procedure

Solvents60 ml mixed DI water/ethanol/N,N-dimethylformamide, inherited from ZIF-67 procedure; component ratios not specified

Atmospherenot specified

Temperature160

Time12; plus 1 h stirring before autoclave and overnight drying

Work-upsame washing, filtration, and drying procedure as ZIF-67 nanosheets

Activationdried overnight at 80 deg C prior to analysis

Scalability contextBatch autoclave synthesis; no yield reported.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Co (NO3)2.6H2O	part of 1 g total; Co/Ni 0.5:0.5	article p2 · Experimental procedure, 2.2
Metal Source	Ni (NO3)2.6H2O	part of 1 g total; Co/Ni 0.5:0.5	article p2 · Experimental procedure, 2.2
Linker	2-Methylimidazole	0.5 g	article p2 · Experimental procedure, 2.2
Solvent	distilled water/ethanol/N,N-dimethylformamide	60 ml mixed solution	article p2 · Experimental procedure, 2.2

Partial recipeSource: Main

Route 8: Hydrothermal

article p2 · Experimental procedure, 2.1

Metal precursors1 g Co(NO3)2.6H2O

Linker precursors0.5 g 2-methylimidazole

Solvents60 ml mixed solution of distilled water, ethanol, and N,N-dimethylformamide; component ratios not specified

Atmospherenot specified

Temperature160

Time12; plus 1 h stirring before autoclave and overnight drying

Work-upcool to ambient temperature; collect purple precipitate; wash multiple times with water and ethanol; filter

Activationdried overnight at 80 deg C prior to analysis

Scalability context100 ml Teflon-lined stainless-steel autoclave batch synthesis; no yield reported.

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Co (NO3)2.6H2O	1 g	article p2 · Experimental procedure, 2.1
Linker	2-Methylimidazole	0.5 g	article p2 · Experimental procedure, 2.1
Solvent	distilled (DI) water	part of 60 ml mixed solution	article p2 · Experimental procedure, 2.1
Solvent	ethanol	part of 60 ml mixed solution	article p2 · Experimental procedure, 2.1
Solvent	N,N-dimethylformamide	part of 60 ml mixed solution	article p2 · Experimental procedure, 2.1