Synthesis · Nano UiO-66 and UiO-66-NH2 MOFs as Bifunctional Electrocatalysts for Water-Splitting: A Comparative Study

6 structured synthesis routes

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

Partial recipeSource: Main

Route 1: Drop Cast

3 · 2.4 Electrochemical studies

SolventsNMP, 40 uL added dropwise

Additivesconductive carbon black; PVDF binder

Atmospherenot specified

Substrate orientationboth sides of 1 x 2 cm2 nickel foam; 1 x 1 cm2 coated area defined by Teflon tape

Work-upGround to uniform ink, applied with micropipette to nickel foam; dried until electrode weight increased by 5-6 mg.

Show 6 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	active U sample	8 mg	3 · 2.4 Electrochemical studies
Additive	active black carbon	1 mg	3 · 2.4 Electrochemical studies
Additive	PVDF binder	1 mg	3 · 2.4 Electrochemical studies
Solvent	NMP	40 uL	3 · 2.4 Electrochemical studies
Other	nickel foam	1 x 2 cm2, half coated	3 · 2.4 Electrochemical studies
Electrolyte	KOH in deionized water	2.8 g KOH in 50 mL water · 1 M	3 · 2.4 Electrochemical studies

Complete recipeSource: Main

Route 2: Solvothermal

3 · 2.2 Synthesis

Metal precursorsZrOCl2.8H2O, 4 mmol

Linker precursorsBDC, 4 mmol

SolventsDMF, 30 mL

Atmospherenot specified

Temperature120

Time24

Work-upCentrifuged; washed three times with deionized water and three times with ethanol at 7000 RPM and room temperature; dried in oven; finely ground.

ActivationActivated in a drying oven at 100 C for 24 h.

Scalability contextIntroduction states ZrOCl2.8H2O was selected as a lower-cost precursor suitable for repeated and larger-scale studies, but no scale-up yield is reported.

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	ZrOCl2.8H2O	4 mmol	3 · 2.2 Synthesis
Linker	BDC	4 mmol	3 · 2.2 Synthesis
Solvent	DMF	30 mL	3 · 2.2 Synthesis

Partial recipeSource: SI

Route 3: Drop Cast

2 · XRD before and after the water-splitting process · Fig. S1

SolventsNMP, 10 uL

AdditivesPVDF binder

Atmospherenot specified

Time8

Substrate orientationone side of nickel foam

Work-upPaste applied to one side of nickel foam and allowed to dry for eight hours.

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	active U sample	8 mg	2 · XRD before and after the water-splitting process · Fig. S1
Additive	PVDF binder	2 mg	2 · XRD before and after the water-splitting process · Fig. S1
Solvent	NMP	10 uL	2 · XRD before and after the water-splitting process · Fig. S1

Partial recipeSource: Main

Route 4: Drop Cast

3 · 2.4 Electrochemical studies

SolventsNMP, 40 uL added dropwise

Additivesconductive carbon black; PVDF binder

Atmospherenot specified

Substrate orientationboth sides of 1 x 2 cm2 nickel foam; 1 x 1 cm2 coated area defined by Teflon tape

Work-upGround to uniform ink, applied with micropipette to nickel foam; dried until electrode weight increased by 5-6 mg.

Show 6 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	active U-N sample	8 mg	3 · 2.4 Electrochemical studies
Additive	active black carbon	1 mg	3 · 2.4 Electrochemical studies
Additive	PVDF binder	1 mg	3 · 2.4 Electrochemical studies
Solvent	NMP	40 uL	3 · 2.4 Electrochemical studies
Other	nickel foam	1 x 2 cm2, half coated	3 · 2.4 Electrochemical studies
Electrolyte	KOH in deionized water	2.8 g KOH in 50 mL water · 1 M	3 · 2.4 Electrochemical studies

Complete recipeSource: Main

Route 5: Solvothermal

3 · 2.2 Synthesis

Metal precursorsZrOCl2.8H2O, 4 mmol

Linker precursorsBDC-NH2, 4 mmol

SolventsDMF, 30 mL

Atmospherenot specified

Temperature120

Time24

Work-upCentrifuged; washed three times with deionized water and three times with ethanol at 7000 RPM and room temperature; dried in oven; finely ground.

ActivationActivated in a drying oven at 100 C for 24 h.

Scalability contextNo yield or scale-up batch mass reported.

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	ZrOCl2.8H2O	4 mmol	3 · 2.2 Synthesis
Linker	BDC-NH2	4 mmol	3 · 2.2 Synthesis
Solvent	DMF	30 mL	3 · 2.2 Synthesis

Partial recipeSource: SI

Route 6: Drop Cast

2 · XRD before and after the water-splitting process · Fig. S1

SolventsNMP, 10 uL

AdditivesPVDF binder

Atmospherenot specified

Time8

Substrate orientationone side of nickel foam

Work-upPaste applied to one side of nickel foam and allowed to dry for eight hours.

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	active U-N sample	8 mg	2 · XRD before and after the water-splitting process · Fig. S1
Additive	PVDF binder	2 mg	2 · XRD before and after the water-splitting process · Fig. S1
Solvent	NMP	10 uL	2 · XRD before and after the water-splitting process · Fig. S1