Synthesis · Novel CoS2 embedded carbon nanocages by direct sulfurizing metal-organic frameworks for dye-sensitized solar cells

6 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

11985 · 2.3 Electrode and cell fabrication

Metal precursors0.4 g product powder

Solvents4 mL anhydrous ethanol; ethyl cellulose ethanol solution

Additives2.2 mL of 10 wt% ethyl cellulose ethanol solution; 1.72 mL terpineol

Atmosphereargon during final heating

Temperature450

Time0.0083 spin coating; 0.5 heating

Substrate orientationFTO-coated glass

Work-upsonication and stirring, spin coating at 4400 rpm for 30 s

Activationheated at 450 deg C under argon for 30 min

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	product	0.4 g	11985 · 2.3 Electrode and cell fabrication
Solvent	anhydrous ethanol	4 mL	11985 · 2.3 Electrode and cell fabrication
Additive	ethyl cellulose ethanol solution	2.2 mL · 10 wt%	11985 · 2.3 Electrode and cell fabrication
Additive	terpineol	1.72 mL	11985 · 2.3 Electrode and cell fabrication

Complete recipeSource: Main

Route 2: Other

11985 · 2.2 Synthesis of CoS2 embedded carbon nanocages

Metal precursorsas-prepared ZIF-67 templates, 1.1 g

Linker precursorsZIF-67-derived 2-methylimidazolate framework

Solvents150 mL anhydrous ethanol; 150 uL DI water

Additives0.1 M thioacetamide (TAA)

AtmosphereN2 during annealing; solution sulfurisation atmosphere not specified

Temperature90 sulfurisation; 450 annealing

Time1 h sulfurisation; 1 h annealing

Oxidant / reductantthioacetamide sulfur source

Work-upcentrifuged, washed with anhydrous ethanol, dried at 60 deg C overnight

Activationannealed in N2 at 450 deg C for 1 h at 2 deg C min-1

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	as-prepared ZIF-67 templates	1.1 g	11985 · 2.2 Synthesis of CoS2 embedded carbon nanocages
Other	thioacetamide (TAA)	0.1 M	11985 · 2.2 Synthesis of CoS2 embedded carbon nanocages
Solvent	anhydrous ethanol	150 mL	11985 · 2.2 Synthesis of CoS2 embedded carbon nanocages
Solvent	DI water	150 uL	11985 · 2.2 Synthesis of CoS2 embedded carbon nanocages

Complete recipeSource: Main

Route 3: Other

11985 · 2.2 Synthesis of CoS2 embedded carbon nanocages

Metal precursorsas-prepared ZIF-67 templates, 1.1 g

Linker precursorsZIF-67-derived 2-methylimidazolate framework

Solvents150 mL anhydrous ethanol; 150 uL DI water

Additives0.1 M thioacetamide (TAA)

AtmosphereN2 during annealing; solution sulfurisation atmosphere not specified

Temperature90 sulfurisation; 450 annealing

Time2 h sulfurisation; 1 h annealing

Oxidant / reductantthioacetamide sulfur source

Work-upcentrifuged, washed with anhydrous ethanol, dried at 60 deg C overnight

Activationannealed in N2 at 450 deg C for 1 h at 2 deg C min-1

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	as-prepared ZIF-67 templates	1.1 g	11985 · 2.2 Synthesis of CoS2 embedded carbon nanocages
Other	thioacetamide (TAA)	0.1 M	11985 · 2.2 Synthesis of CoS2 embedded carbon nanocages
Solvent	anhydrous ethanol	150 mL	11985 · 2.2 Synthesis of CoS2 embedded carbon nanocages
Solvent	DI water	150 uL	11985 · 2.2 Synthesis of CoS2 embedded carbon nanocages

Complete recipeSource: Main

Route 4: Other

11985 · 2.2 Synthesis of CoS2 embedded carbon nanocages

Metal precursorsas-prepared ZIF-67 templates, 1.1 g

Linker precursorsZIF-67-derived 2-methylimidazolate framework

Solvents150 mL anhydrous ethanol; 150 uL DI water

Additives0.1 M thioacetamide (TAA)

AtmosphereN2 during annealing; solution sulfurisation atmosphere not specified

Temperature90 sulfurisation; 450 annealing

Time4 h sulfurisation; 1 h annealing

Oxidant / reductantthioacetamide sulfur source

Work-upcentrifuged, washed with anhydrous ethanol, dried at 60 deg C overnight

Activationannealed in N2 at 450 deg C for 1 h at 2 deg C min-1

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	as-prepared ZIF-67 templates	1.1 g	11985 · 2.2 Synthesis of CoS2 embedded carbon nanocages
Other	thioacetamide (TAA)	0.1 M	11985 · 2.2 Synthesis of CoS2 embedded carbon nanocages
Solvent	anhydrous ethanol	150 mL	11985 · 2.2 Synthesis of CoS2 embedded carbon nanocages
Solvent	DI water	150 uL	11985 · 2.2 Synthesis of CoS2 embedded carbon nanocages

Complete recipeSource: Main

Route 5: Other

11985 · 2.2 Synthesis of CoS2 embedded carbon nanocages

Metal precursorsas-prepared ZIF-67 templates, 1.1 g

Linker precursorsZIF-67-derived 2-methylimidazolate framework

Solvents150 mL anhydrous ethanol; 150 uL DI water

Additives0.1 M thioacetamide (TAA)

AtmosphereN2 during annealing; solution sulfurisation atmosphere not specified

Temperature90 sulfurisation; 450 annealing

Time8 h sulfurisation; 1 h annealing

Oxidant / reductantthioacetamide sulfur source

Work-upcentrifuged, washed with anhydrous ethanol, dried at 60 deg C overnight

Activationannealed in N2 at 450 deg C for 1 h at 2 deg C min-1

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	as-prepared ZIF-67 templates	1.1 g	11985 · 2.2 Synthesis of CoS2 embedded carbon nanocages
Other	thioacetamide (TAA)	0.1 M	11985 · 2.2 Synthesis of CoS2 embedded carbon nanocages
Solvent	anhydrous ethanol	150 mL	11985 · 2.2 Synthesis of CoS2 embedded carbon nanocages
Solvent	DI water	150 uL	11985 · 2.2 Synthesis of CoS2 embedded carbon nanocages

Complete recipeSource: Main

Route 6: Other

11985 · 2.1 Synthesis of ZIF-67

Metal precursorscobalt(II) chloride hexahydrate (CoCl2.6H2O), 1.5 g

Linker precursors2-methylimidazole (CH3C3H2N2H), 1.65 g

Solventsmethanol, 70 mL for each precursor solution; anhydrous ethanol wash

AdditivesPVP, 125 mg

Atmosphereambient/not specified

Temperatureroom temperature synthesis; dried at 60

Time6 h aging; dried overnight

Work-upsolid collected by centrifugation, washed with anhydrous ethanol and centrifuged several times

Activationdried at 60 deg C overnight

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	cobalt(II) chloride hexahydrate (CoCl2.6H2O)	1.5 g	11985 · 2.1 Synthesis of ZIF-67
Linker	2-methylimidazole (CH3C3H2N2H)	1.65 g	11985 · 2.1 Synthesis of ZIF-67
Additive	CH3C3H2N2H (PVP)	125 mg	11985 · 2.1 Synthesis of ZIF-67
Solvent	methanol	70 mL + 70 mL	11985 · 2.1 Synthesis of ZIF-67