Synthesis · Efficient hydrogen production from MIL-53(Fe) catalyst-modified Mo: BiVO4 photoelectrodes

10 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

2 · Preparation of nanoporous BiVO4 and 2% Mo:BiVO4 photoanodes

Metal precursorsBi(NO3)3.5H2O, 1.5 mmol; NH4VO3, 1.5 mmol

SolventsEthylene glycol

AdditivesPEG-600, 0.34 g

Atmosphereair during annealing

Temperature150 drying; 500 annealing

Time1 drying; 2.5 annealing

Substrate orientationFTO substrate, 1 x 5 cm2

Work-upDrop-cast 0.2 mL precursor solution onto FTO, dry at 150 deg C for 60 min, then anneal in muffle furnace in air at 500 deg C for 2.5 h.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Bi(NO3)3.5H2O	1.5 mmol	2 · Preparation of nanoporous BiVO4 and 2% Mo:BiVO4 photoanodes
Metal Source	NH4VO3	1.5 mmol	2 · Preparation of nanoporous BiVO4 and 2% Mo:BiVO4 photoanodes
Solvent	ethylene glycol	20 mL for each Bi and V solution; 10 mL for PEG-600 solution	2 · Preparation of nanoporous BiVO4 and 2% Mo:BiVO4 photoanodes
Additive	PEG-600	0.34 g	2 · Preparation of nanoporous BiVO4 and 2% Mo:BiVO4 photoanodes

Partial recipeSource: Both

Route 2: Other

2 · Preparation of 2% Mo:BiVO4-MIL-53(Fe) and BiVO4-MIL-53(Fe) composite materials

Metal precursorsAs-prepared MIL-53(Fe) powder, 4 mg; preformed BiVO4 film

Linker precursorsTerephthalate already incorporated in MIL-53(Fe)

SolventsEthyl alcohol, 2 mL; distilled water mentioned for ultrasonication

Atmosphereair during drying

Temperature150

Time1

Substrate orientationMIL-53(Fe) deposited on BiVO4/FTO

Work-upSpin-coat MIL-53(Fe) suspension on BiVO4 at 600 rpm for 20 s and 2000 rpm for 10 s; dry at 150 deg C for 1 h.

Show 2 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	MIL-53(Fe) powder	4 mg · 4 mg in 2 mL ethyl alcohol	2 · Preparation of 2% Mo:BiVO4-MIL-53(Fe) and BiVO4-MIL-53(Fe) composite materials
Other	BiVO4 film	one FTO-supported film	2 · Preparation of 2% Mo:BiVO4-MIL-53(Fe) and BiVO4-MIL-53(Fe) composite materials

Complete recipeSource: Main

Route 3: Other

2-3 · Preparation of 2% Mo:BiVO4-MIL-53(Fe) and BiVO4-MIL-53(Fe) composite materials; Results and discussion · Scheme 1

Metal precursorsAs-prepared MIL-53(Fe) powder, 4 mg; preformed 2% Mo:BiVO4 film

Linker precursorsTerephthalate already incorporated in MIL-53(Fe)

SolventsEthyl alcohol, 2 mL; distilled water mentioned for ultrasonication

Atmosphereair during drying

Temperature150

Time1

Substrate orientationMIL-53(Fe) deposited on 2% Mo:BiVO4/FTO

Work-upUltrasonicate MIL-53(Fe) powder in ethanol/water for 30 min; spin-coat at 600 rpm for 20 s and 2000 rpm for 10 s; dry at 150 deg C for 1 h.

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	MIL-53(Fe) powder	4 mg; 350 uL coating amount for FMBV-1 · 4 mg in 2 mL ethyl alcohol	2-3 · Preparation of 2% Mo:BiVO4-MIL-53(Fe) and BiVO4-MIL-53(Fe) composite materials; Results and discussion · Scheme 1
Solvent	ethyl alcohol	2 mL	2-3 · Preparation of 2% Mo:BiVO4-MIL-53(Fe) and BiVO4-MIL-53(Fe) composite materials; Results and discussion · Scheme 1
Other	2% Mo:BiVO4 film	one FTO-supported film	2-3 · Preparation of 2% Mo:BiVO4-MIL-53(Fe) and BiVO4-MIL-53(Fe) composite materials; Results and discussion · Scheme 1

Complete recipeSource: Main

Route 4: Other

2-3 · Preparation of 2% Mo:BiVO4-MIL-53(Fe) and BiVO4-MIL-53(Fe) composite materials; Results and discussion · Scheme 1

Metal precursorsAs-prepared MIL-53(Fe) powder, 4 mg; preformed 2% Mo:BiVO4 film

Linker precursorsTerephthalate already incorporated in MIL-53(Fe)

SolventsEthyl alcohol, 2 mL; distilled water mentioned for ultrasonication

Atmosphereair during drying

Temperature150

Time1

Substrate orientationMIL-53(Fe) deposited on 2% Mo:BiVO4/FTO

Work-upUltrasonicate MIL-53(Fe) powder in ethanol/water for 30 min; spin-coat at 600 rpm for 20 s and 2000 rpm for 10 s; dry at 150 deg C for 1 h.

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	MIL-53(Fe) powder	4 mg; 450 uL coating amount for FMBV-2 · 4 mg in 2 mL ethyl alcohol	2-3 · Preparation of 2% Mo:BiVO4-MIL-53(Fe) and BiVO4-MIL-53(Fe) composite materials; Results and discussion · Scheme 1
Solvent	ethyl alcohol	2 mL	2-3 · Preparation of 2% Mo:BiVO4-MIL-53(Fe) and BiVO4-MIL-53(Fe) composite materials; Results and discussion · Scheme 1
Other	2% Mo:BiVO4 film	one FTO-supported film	2-3 · Preparation of 2% Mo:BiVO4-MIL-53(Fe) and BiVO4-MIL-53(Fe) composite materials; Results and discussion · Scheme 1

Complete recipeSource: Main

Route 5: Other

2-3 · Preparation of 2% Mo:BiVO4-MIL-53(Fe) and BiVO4-MIL-53(Fe) composite materials; Results and discussion · Scheme 1

Metal precursorsAs-prepared MIL-53(Fe) powder, 4 mg; preformed 2% Mo:BiVO4 film

Linker precursorsTerephthalate already incorporated in MIL-53(Fe)

SolventsEthyl alcohol, 2 mL; distilled water mentioned for ultrasonication

Atmosphereair during drying

Temperature150

Time1

Substrate orientationMIL-53(Fe) deposited on 2% Mo:BiVO4/FTO

Work-upUltrasonicate MIL-53(Fe) powder in ethanol/water for 30 min; spin-coat at 600 rpm for 20 s and 2000 rpm for 10 s; dry at 150 deg C for 1 h.

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	MIL-53(Fe) powder	4 mg; 550 uL coating amount for FMBV-3 · 4 mg in 2 mL ethyl alcohol	2-3 · Preparation of 2% Mo:BiVO4-MIL-53(Fe) and BiVO4-MIL-53(Fe) composite materials; Results and discussion · Scheme 1
Solvent	ethyl alcohol	2 mL	2-3 · Preparation of 2% Mo:BiVO4-MIL-53(Fe) and BiVO4-MIL-53(Fe) composite materials; Results and discussion · Scheme 1
Other	2% Mo:BiVO4 film	one FTO-supported film	2-3 · Preparation of 2% Mo:BiVO4-MIL-53(Fe) and BiVO4-MIL-53(Fe) composite materials; Results and discussion · Scheme 1

Complete recipeSource: Main

Route 6: Other

2 · Preparation of MIL-53(Fe)

Metal precursorsFeCl3.6H2O, 4 mM

Linker precursorsTerephthalic acid, 2 mM

SolventsDMF, 40 mL; ethanol and DMF washes

Atmospherenot specified during microwave synthesis

Temperature150

Time0.5

Work-upCool to room temperature; centrifuge; wash with DMF and ethanol three times.

ActivationDried at 100 deg C under vacuum.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	FeCl3.6H2O	4 mM	2 · Preparation of MIL-53(Fe)
Linker	terephthalic acid	2 mM	2 · Preparation of MIL-53(Fe)
Solvent	DMF	40 mL	2 · Preparation of MIL-53(Fe)
Solvent	ethanol	wash solvent	2 · Preparation of MIL-53(Fe)

Complete recipeSource: Main

Route 7: Drop Cast

2 · Preparation of nanoporous BiVO4 and 2% Mo:BiVO4 photoanodes

Metal precursorsBi(NO3)3.5H2O, NH4VO3, (NH4)6.Mo7O24.4H2O

SolventsEthylene glycol

AdditivesPEG-600

Atmosphereair during annealing

Temperature150 drying; 500 annealing

Time1 drying; 2.5 annealing

Substrate orientationFTO substrate, 1 x 5 cm2

Work-upSame drop-cast/dry/anneal method as BiVO4, with Mo precursor added.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Bi(NO3)3.5H2O	as in BiVO4 route	2 · Preparation of nanoporous BiVO4 and 2% Mo:BiVO4 photoanodes
Metal Source	NH4VO3	as in BiVO4 route	2 · Preparation of nanoporous BiVO4 and 2% Mo:BiVO4 photoanodes
Metal Source	(NH4)6.Mo7O24.4H2O	Mo fraction 0.02 in Bi:V:Mo = 0.98:1:0.02	2 · Preparation of nanoporous BiVO4 and 2% Mo:BiVO4 photoanodes
Additive	PEG-600	as in BiVO4 route	2 · Preparation of nanoporous BiVO4 and 2% Mo:BiVO4 photoanodes

Complete recipeSource: SI

Route 8: Electrochemical

2 · Preparation of 2%Mo:BiVO4-FeOOH composite materials

Metal precursors0.1 M FeSO4.7H2O solution

Solventsaqueous solution

Atmospheresolution purged with nitrogen for 1 h

Time0.1667

Substrate orientation2% Mo:BiVO4 film as working electrode

Oxidant / reductantphotoelectron-deposition at 0.1 V vs SCE under 300 W Xe arc lamp with AM 1.5G filter

Show 2 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	FeSO4.7H2O	0.1 M	2 · Preparation of 2%Mo:BiVO4-FeOOH composite materials
Other	2% Mo:BiVO4 film	working electrode	2 · Preparation of 2%Mo:BiVO4-FeOOH composite materials

Complete recipeSource: SI

Route 9: Electrochemical

2 · Preparation of 2%Mo:BiVO4-FeOOH composite materials

Metal precursors0.1 M FeSO4.7H2O solution

Solventsaqueous solution

Atmospheresolution purged with nitrogen for 1 h

Time0.3333

Substrate orientation2% Mo:BiVO4 film as working electrode

Oxidant / reductantphotoelectron-deposition at 0.1 V vs SCE under 300 W Xe arc lamp with AM 1.5G filter

Show 2 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	FeSO4.7H2O	0.1 M	2 · Preparation of 2%Mo:BiVO4-FeOOH composite materials
Other	2% Mo:BiVO4 film	working electrode	2 · Preparation of 2%Mo:BiVO4-FeOOH composite materials

Complete recipeSource: SI

Route 10: Electrochemical

2 · Preparation of 2%Mo:BiVO4-FeOOH composite materials

Metal precursors0.1 M FeSO4.7H2O solution

Solventsaqueous solution

Atmospheresolution purged with nitrogen for 1 h

Time0.5

Substrate orientation2% Mo:BiVO4 film as working electrode

Oxidant / reductantphotoelectron-deposition at 0.1 V vs SCE under 300 W Xe arc lamp with AM 1.5G filter

Show 2 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	FeSO4.7H2O	0.1 M	2 · Preparation of 2%Mo:BiVO4-FeOOH composite materials
Other	2% Mo:BiVO4 film	working electrode	2 · Preparation of 2%Mo:BiVO4-FeOOH composite materials