Synthesis · Tailoring of electrocatalytic oxygen evolution reaction performance of 2D conductive Co-catecholate metal-organic frameworks

4 structured synthesis routes

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

Complete recipeSource: Main

Route 1: Drop Cast

3 · 2.4. Electrocatalytic measurements

Solvents0.5 mL DI water

Additives10 uL of 5% Nafion

Atmospherenot reported; dried under vacuum

Temperatureroom temperature

Time1 h sonication plus 30 min vacuum drying

Substrate orientationglassy carbon electrode

Work-upSonicated to homogeneous ink; 5 uL deposited on GCE; vacuum dried for 30 min.

ActivationElectrochemical CV activation was applied in some tests as 25 cycles between 0.9 and 1.6 V vs RHE at 10 mV/s.

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	Co-CAT-W electrocatalyst	1.5 mg	3 · 2.4. Electrocatalytic measurements
Additive	Nafion	10 uL · 5%	3 · 2.4. Electrocatalytic measurements
Solvent	DI water	0.5 mL	3 · 2.4. Electrocatalytic measurements

Complete recipeSource: Main

Route 2: Hydrothermal

3 · 2.2. Synthesis of Co-CAT · Scheme 2b

Metal precursorsCo(OAc)2.4H2O (0.4 mmol)

Linker precursorsHHTP (0.21 mmol)

Solvents30 mL deionised water; 2 mL NMP

AdditivesN-methyl-2-pyrrolidone (NMP), 2 mL

Atmospherenot reported

Temperature85

Time0.5

Work-upSame Co-CAT-WO procedure: microwave treatment, centrifugation at 4000 rpm for 10 min, water/acetone washing, room-temperature drying, grinding.

Activationnone reported

Scalability contextMicrowave-assisted method described as rapid, low-reaction-time synthesis; no scale-up yield reported.

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Co(OAc)2.4H2O	0.4 mmol	3 · 2.2. Synthesis of Co-CAT · Scheme 2b
Linker	HHTP	0.21 mmol	3 · 2.2. Synthesis of Co-CAT · Scheme 2b
Solvent	DI water	30 mL	3 · 2.2. Synthesis of Co-CAT · Scheme 2b
Additive	N-Methyl-2-pyrrolidone (NMP)	2 mL	3 · 2.2. Synthesis of Co-CAT · Scheme 2b
Solvent	acetone	several washes	3 · 2.2. Synthesis of Co-CAT · Scheme 2b

Complete recipeSource: Main

Route 3: Drop Cast

3 · 2.4. Electrocatalytic measurements

Solvents0.5 mL DI water

Additives10 uL of 5% Nafion

Atmospherenot reported; dried under vacuum

Temperatureroom temperature

Time1 h sonication plus 30 min vacuum drying

Substrate orientationglassy carbon electrode

Work-upSonicated to homogeneous ink; 5 uL deposited on GCE; vacuum dried for 30 min.

ActivationElectrochemical CV activation was applied in some tests as 25 cycles between 0.9 and 1.6 V vs RHE at 10 mV/s.

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	Co-CAT-WO electrocatalyst	1.5 mg	3 · 2.4. Electrocatalytic measurements
Additive	Nafion	10 uL · 5%	3 · 2.4. Electrocatalytic measurements
Solvent	DI water	0.5 mL	3 · 2.4. Electrocatalytic measurements

Complete recipeSource: Main

Route 4: Hydrothermal

3 · 2.2. Synthesis of Co-CAT · Scheme 2a

Metal precursorsCo(OAc)2.4H2O (0.4 mmol)

Linker precursorsHHTP (0.21 mmol)

Solvents30 mL deionised water

Atmospherenot reported

Temperature85

Time0.5

Work-upCentrifuged at 4000 rpm for 10 min; washed with water and acetone several times; dried at room temperature; ground.

Activationnone reported

Scalability contextMicrowave-assisted method described as rapid, low-reaction-time synthesis; no scale-up yield reported.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Co(OAc)2.4H2O	0.4 mmol	3 · 2.2. Synthesis of Co-CAT · Scheme 2a
Linker	2,3,6,7,10,11-hexahydroxytriphenylene (HHTP)	0.21 mmol	3 · 2.2. Synthesis of Co-CAT · Scheme 2a
Solvent	DI water	30 mL	3 · 2.2. Synthesis of Co-CAT · Scheme 2a
Solvent	acetone	several washes	3 · 2.2. Synthesis of Co-CAT · Scheme 2a