Synthesis · In situ growth of ultrathin Co-MOF nanosheets on Α-Fe2O3 hematite nanorods for efficient photoelectrochemical water oxidation

12 structured synthesis routes

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

Complete recipeSource: Main

Route 1: Hydrothermal

p002 / journal p389 · 2.1(a)

Metal precursorsFeCl3.6H2O, 0.0972 g, 0.09 M

Linker precursorsnone

Solvents4 mL aqueous solution; deionized/distilled water

AdditivesNaNO3 0.034 g (0.1 M); HCl to pH 1

Atmosphereautoclave atmosphere not stated; dried with nitrogen; annealed in air

Temperature95; then 550 and 750

Time4; then 2 and 0.25

Substrate orientationclean FTO glass placed in 10 mL beaker inside 100 mL Teflon-lined autoclave; orientation not stated

Oxidant / reductantNaNO3 additive; air annealing

Work-upcooled to room temperature; rinsed with distilled water several times; blow-dried with nitrogen

Activationannealed at 550 C for 2 h and 750 C for 15 min in air; natural cooling

Scalability contextSmall-area FTO/beaker/autoclave method; scalable area not discussed.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	FeCl3.6H2O	0.0972 g · 0.09 M	p002 / journal p389 · 2.1(a)
Additive	NaNO3	0.034 g · 0.1 M	p002 / journal p389 · 2.1(a)
Acid	HCl	pH adjusted to 1 · not reported	p002 / journal p389 · 2.1(a)
Solvent	water	4 mL · not applicable	p002 / journal p389 · 2.1(a)

Partial recipeSource: Main

Route 2: Other

p002 / journal p389 · 2.1(d)

Metal precursorsCo(NO3)2 / Co(NO3).6H2O aqueous precursor, 0.05 M

Linker precursors2-methylimidazole aqueous solution, 0.4 M

Solventswater; 4 mL 2-methylimidazole solution for immersion; Co precursor solution prepared in water

Additivesnone reported

Atmospherenot stated; heating at 70 C on hot plate/ambient implied

Temperature70

Time0.333 immersion plus 0.333 heating; Co spin-coat step 12 s inherited from Co-modified film preparation

Substrate orientationCo-modified hematite film immersed in MIm solution; orientation not stated

Oxidant / reductantnone reported

Work-upwashed with distilled water after MIm immersion

Activationheated at 70 C on a hot plate for 20 min

Scalability contextSolution immersion/spin-coating photoanode method; electrode area not stated.

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Co(NO3)2 / Co(NO3).6H2O	from Co-modified hematite spin-coat; 100 uL used for 0.1 M route · 0.05 M	p002 / journal p389 · 2.1(d)
Linker	2-methylimidazole	4 mL solution · 0.4 M	p002 / journal p389 · 2.1(d)
Solvent	water	not fully stated for all Co concentrations; MIm solution 4 mL · not applicable	p002 / journal p389 · 2.1(d)

Partial recipeSource: Main

Route 3: Other

p002 / journal p389 · 2.1(d)

Metal precursorsCo(NO3)2 / Co(NO3).6H2O aqueous precursor, 0.05 M

Linker precursors2-methylimidazole aqueous solution, 0.8 M

Solventswater; 4 mL 2-methylimidazole solution for immersion; Co precursor solution prepared in water

Additivesnone reported

Atmospherenot stated; heating at 70 C on hot plate/ambient implied

Temperature70

Time0.333 immersion plus 0.333 heating; Co spin-coat step 12 s inherited from Co-modified film preparation

Substrate orientationCo-modified hematite film immersed in MIm solution; orientation not stated

Oxidant / reductantnone reported

Work-upwashed with distilled water after MIm immersion

Activationheated at 70 C on a hot plate for 20 min

Scalability contextSolution immersion/spin-coating photoanode method; electrode area not stated.

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Co(NO3)2 / Co(NO3).6H2O	from Co-modified hematite spin-coat; 100 uL used for 0.1 M route · 0.05 M	p002 / journal p389 · 2.1(d)
Linker	2-methylimidazole	4 mL solution · 0.8 M	p002 / journal p389 · 2.1(d)
Solvent	water	not fully stated for all Co concentrations; MIm solution 4 mL · not applicable	p002 / journal p389 · 2.1(d)

Partial recipeSource: Main

Route 4: Drop Cast

p002 / journal p389 · 2.1(b)

Metal precursorsCo(NO3).6H2O, 58 mg, 0.1 M

Linker precursorsnone

Solvents2 mL deionized water

Additivesnone reported

Atmospherenot stated; heated on hot plate/ambient implied

Temperature70

Time0.0056 spin coating plus 0.333 heating

Substrate orientationbare hematite film; spin-coated at 1200 rpm

Oxidant / reductantnone reported

Work-upnot stated after Co-only heating

Activationheated at 70 C for 20 min

Scalability contextSpin-coating 100 uL precursor solution; area not stated.

Show 2 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Co(NO3).6H2O / Co(NO3)2	58 mg · 0.1 M	p002 / journal p389 · 2.1(b)
Solvent	deionized water	2 mL · not applicable	p002 / journal p389 · 2.1(b)

Partial recipeSource: Main

Route 5: Other

p002 / journal p389 · 2.1(d)

Metal precursorsCo(NO3)2 / Co(NO3).6H2O aqueous precursor, 0.1 M

Linker precursors2-methylimidazole aqueous solution, 0.4 M

Solventswater; 4 mL 2-methylimidazole solution for immersion; Co precursor solution prepared in water

Additivesnone reported

Atmospherenot stated; heating at 70 C on hot plate/ambient implied

Temperature70

Time0.333 immersion plus 0.333 heating; Co spin-coat step 12 s inherited from Co-modified film preparation

Substrate orientationCo-modified hematite film immersed in MIm solution; orientation not stated

Oxidant / reductantnone reported

Work-upwashed with distilled water after MIm immersion

Activationheated at 70 C on a hot plate for 20 min

Scalability contextSolution immersion/spin-coating photoanode method; electrode area not stated.

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Co(NO3)2 / Co(NO3).6H2O	from Co-modified hematite spin-coat; 100 uL used for 0.1 M route · 0.1 M	p002 / journal p389 · 2.1(d)
Linker	2-methylimidazole	4 mL solution · 0.4 M	p002 / journal p389 · 2.1(d)
Solvent	water	not fully stated for all Co concentrations; MIm solution 4 mL · not applicable	p002 / journal p389 · 2.1(d)

Partial recipeSource: Main

Route 6: Other

p002 / journal p389 · 2.1(d)

Metal precursorsCo(NO3)2 / Co(NO3).6H2O aqueous precursor, 0.1 M

Linker precursors2-methylimidazole aqueous solution, 0.8 M

Solventswater; 4 mL 2-methylimidazole solution for immersion; Co precursor solution prepared in water

Additivesnone reported

Atmospherenot stated; heating at 70 C on hot plate/ambient implied

Temperature70

Time0.333 immersion plus 0.333 heating; Co spin-coat step 12 s inherited from Co-modified film preparation

Substrate orientationCo-modified hematite film immersed in MIm solution; orientation not stated

Oxidant / reductantnone reported

Work-upwashed with distilled water after MIm immersion

Activationheated at 70 C on a hot plate for 20 min

Scalability contextSolution immersion/spin-coating photoanode method; electrode area not stated.

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Co(NO3)2 / Co(NO3).6H2O	from Co-modified hematite spin-coat; 100 uL used for 0.1 M route · 0.1 M	p002 / journal p389 · 2.1(d)
Linker	2-methylimidazole	4 mL solution · 0.8 M	p002 / journal p389 · 2.1(d)
Solvent	water	not fully stated for all Co concentrations; MIm solution 4 mL · not applicable	p002 / journal p389 · 2.1(d)

Partial recipeSource: Main

Route 7: Other

p002 / journal p389 · 2.1(d)

Metal precursorsCo(NO3)2 / Co(NO3).6H2O aqueous precursor, 0.1 M

Linker precursors2-methylimidazole aqueous solution, 1.6 M

Solventswater; 4 mL 2-methylimidazole solution for immersion; Co precursor solution prepared in water

Additivesnone reported

Atmospherenot stated; heating at 70 C on hot plate/ambient implied

Temperature70

Time0.333 immersion plus 0.333 heating; Co spin-coat step 12 s inherited from Co-modified film preparation

Substrate orientationCo-modified hematite film immersed in MIm solution; orientation not stated

Oxidant / reductantnone reported

Work-upwashed with distilled water after MIm immersion

Activationheated at 70 C on a hot plate for 20 min

Scalability contextSolution immersion/spin-coating photoanode method; electrode area not stated.

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Co(NO3)2 / Co(NO3).6H2O	from Co-modified hematite spin-coat; 100 uL used for 0.1 M route · 0.1 M	p002 / journal p389 · 2.1(d)
Linker	2-methylimidazole	4 mL solution · 1.6 M	p002 / journal p389 · 2.1(d)
Solvent	water	not fully stated for all Co concentrations; MIm solution 4 mL · not applicable	p002 / journal p389 · 2.1(d)

Partial recipeSource: Main

Route 8: Other

p002 / journal p389 · 2.1(d)

Metal precursorsCo(NO3)2 / Co(NO3).6H2O aqueous precursor, 0.2 M

Linker precursors2-methylimidazole aqueous solution, 0.8 M

Solventswater; 4 mL 2-methylimidazole solution for immersion; Co precursor solution prepared in water

Additivesnone reported

Atmospherenot stated; heating at 70 C on hot plate/ambient implied

Temperature70

Time0.333 immersion plus 0.333 heating; Co spin-coat step 12 s inherited from Co-modified film preparation

Substrate orientationCo-modified hematite film immersed in MIm solution; orientation not stated

Oxidant / reductantnone reported

Work-upwashed with distilled water after MIm immersion

Activationheated at 70 C on a hot plate for 20 min

Scalability contextSolution immersion/spin-coating photoanode method; electrode area not stated.

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Co(NO3)2 / Co(NO3).6H2O	from Co-modified hematite spin-coat; 100 uL used for 0.1 M route · 0.2 M	p002 / journal p389 · 2.1(d)
Linker	2-methylimidazole	4 mL solution · 0.8 M	p002 / journal p389 · 2.1(d)
Solvent	water	not fully stated for all Co concentrations; MIm solution 4 mL · not applicable	p002 / journal p389 · 2.1(d)

Partial recipeSource: Main

Route 9: Other

p002 / journal p389 · 2.1(d)

Metal precursorsCo(NO3)2 / Co(NO3).6H2O aqueous precursor, 0.2 M

Linker precursors2-methylimidazole aqueous solution, 1.6 M

Solventswater; 4 mL 2-methylimidazole solution for immersion; Co precursor solution prepared in water

Additivesnone reported

Atmospherenot stated; heating at 70 C on hot plate/ambient implied

Temperature70

Time0.333 immersion plus 0.333 heating; Co spin-coat step 12 s inherited from Co-modified film preparation

Substrate orientationCo-modified hematite film immersed in MIm solution; orientation not stated

Oxidant / reductantnone reported

Work-upwashed with distilled water after MIm immersion

Activationheated at 70 C on a hot plate for 20 min

Scalability contextSolution immersion/spin-coating photoanode method; electrode area not stated.

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Co(NO3)2 / Co(NO3).6H2O	from Co-modified hematite spin-coat; 100 uL used for 0.1 M route · 0.2 M	p002 / journal p389 · 2.1(d)
Linker	2-methylimidazole	4 mL solution · 1.6 M	p002 / journal p389 · 2.1(d)
Solvent	water	not fully stated for all Co concentrations; MIm solution 4 mL · not applicable	p002 / journal p389 · 2.1(d)

Partial recipeSource: Main

Route 10: Other

p002 / journal p389 · 2.1(d)

Metal precursorsCo(NO3)2 / Co(NO3).6H2O aqueous precursor, 0.3 M

Linker precursors2-methylimidazole aqueous solution, 2.4 M

Solventswater; 4 mL 2-methylimidazole solution for immersion; Co precursor solution prepared in water

Additivesnone reported

Atmospherenot stated; heating at 70 C on hot plate/ambient implied

Temperature70

Time0.333 immersion plus 0.333 heating; Co spin-coat step 12 s inherited from Co-modified film preparation

Substrate orientationCo-modified hematite film immersed in MIm solution; orientation not stated

Oxidant / reductantnone reported

Work-upwashed with distilled water after MIm immersion

Activationheated at 70 C on a hot plate for 20 min

Scalability contextSolution immersion/spin-coating photoanode method; electrode area not stated.

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Co(NO3)2 / Co(NO3).6H2O	from Co-modified hematite spin-coat; 100 uL used for 0.1 M route · 0.3 M	p002 / journal p389 · 2.1(d)
Linker	2-methylimidazole	4 mL solution · 2.4 M	p002 / journal p389 · 2.1(d)
Solvent	water	not fully stated for all Co concentrations; MIm solution 4 mL · not applicable	p002 / journal p389 · 2.1(d)

Partial recipeSource: Main

Route 11: Other

p002 / journal p389 · 2.1(c)

Metal precursorsbare hematite film only; no added metal precursor

Linker precursors2-methylimidazole, 0.8 M

Solventsaqueous solution, 4 mL

Additivesnone reported

Atmospherenot stated; heating ambient implied

Temperature70

Time0.333 immersion plus 0.333 heating

Substrate orientationbare hematite film immersed in solution; orientation not stated

Oxidant / reductantnone reported

Work-upwashed with distilled water

Activationheated at 70 C for 20 min

Scalability contextImmersion volume 4 mL; electrode area not stated.

Show 2 structured reagent records

Role	Reagent	Amount / concentration	Source
Linker	2-methylimidazole	4 mL solution · 0.8 M	p002 / journal p389 · 2.1(c)
Solvent	water	4 mL · not applicable	p002 / journal p389 · 2.1(c)

Partial recipeSource: Main

Route 12: Other

p004 / journal p391 · 3 Results and discussion

Metal precursors0.1 M Co2+ solution (source salt implied Co nitrate, exact salt not repeated)

Linker precursors0.8 M 2-methylimidazole solution

Solventsaqueous solutions implied from preceding routes; exact volumes not reported

Additivesnone reported

Atmospherenot stated

Temperatureroom temperature not explicitly stated

Time0.333

Substrate orientationnot applicable

Oxidant / reductantnone reported

Work-upcentrifugation and washing

Activationnone reported

Scalability contextPowder reference only; yield/scale not reported.

Show 2 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Co2+ solution	not reported · 0.1 M	p004 / journal p391 · 3 Results and discussion
Linker	2-methylimidazole	not reported · 0.8 M	p004 / journal p391 · 3 Results and discussion