Synthesis · Rational design of sulfur vacancy-rich NiCo2S4/C nanostructure for high-performance hybrid supercapacitors

9 structured synthesis routes

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

Complete recipeSource: Main

Route 1: Other

2 · 2.2

Metal precursorsNaOH

Linker precursorstrimesic acid (1,3,5-benzenetricarboxylic acid, H3BTC)

Solventsethanol

Atmospherenot specified

Temperature60

Time2 h stirring; dried overnight at 60 deg C

Work-upvacuum filtration

Activationdried at 60 deg C overnight

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Base	NaOH	1.2 g	2 · 2.2
Linker	trimesic acid	2.1 g	2 · 2.2
Solvent	ethanol	400 mL	2 · 2.2

Partial recipeSource: Main

Route 2: Other

3 · 2.4

Metal precursorsNi1Co1-BTC nanorods

Linker precursorsBTC in Ni1Co1-BTC precursor

Atmospherenot specified; muffle furnace

Temperature500

Time2

Oxidant / reductantthermal oxidation in muffle furnace

Work-upcooled to room temperature

Scalability contextHeating rate 5 deg C min-1.

Show 1 structured reagent record

Role	Reagent	Amount / concentration	Source
Other	Ni1Co1-BTC nanorods	Not specified	3 · 2.4

Complete recipeSource: Main

Route 3: Other

4 · 2.5

Metal precursorsNiCo2O4@NiO (NCO)

Additivessulfur powder, same way as NCSC

Atmospherenitrogen

Temperature500

Time2

Oxidant / reductantsulfur powder as sulfurising agent

Activationtube furnace; heating rate 5 deg C min-1

Show 2 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	NCO	same way	4 · 2.5
Additive	sulfur powder	same way	4 · 2.5

Complete recipeSource: Main

Route 4: Other

4 · 2.5 · Fig. 1

Metal precursorsNi1Co1-BTC nanorods

Linker precursorsBTC in Ni1Co1-BTC precursor

Additivessulfur powder, precursor:sulfur mass ratio 1:2

Atmospherenitrogen

Temperature500

Time2

Oxidant / reductantsulfur powder as sulfurising agent; carbonization-vulcanization

Activationtube furnace; heating rate 5 deg C min-1

Show 2 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	Ni1Co1-BTC nanorods	mass ratio 1 part	4 · 2.5 · Fig. 1
Additive	sulfur powder	mass ratio 2 parts	4 · 2.5 · Fig. 1

Partial recipeSource: Main

Route 5: Other

5 · 2.7

Metal precursorsNCSC positive electrode

Additivesactivated carbon negative electrode

Atmospherenot specified

Work-upassembled as hybrid supercapacitor; positive/negative mass ratio determined by charge balance

Show 2 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	NCSC positive electrode	charge-balanced	5 · 2.7
Other	activated carbon negative electrode	charge-balanced	5 · 2.7

Complete recipeSource: Main

Route 6: Other

4 · 2.5

Metal precursorsNi1Co1-BTC nanorods

Linker precursorsBTC in Ni1Co1-BTC precursor

Additivessulfur powder, precursor:sulfur mass ratio 1:2

Atmospherenitrogen

Temperature500

Time0.5, 1.0, or 1.5

Oxidant / reductantsulfur powder as sulfurising agent; carbonization-vulcanization

Activationtube furnace; heating rate 5 deg C min-1

Show 2 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	Ni1Co1-BTC nanorods	mass ratio 1 part	4 · 2.5
Additive	sulfur powder	mass ratio 2 parts	4 · 2.5

Complete recipeSource: Main

Route 7: Other

2-3 · 2.3

Metal precursors45 mg Ni(NO3)2.6H2O and 45 mg Co(NO3)2.6H2O

Linker precursors45 mg Na-BTC

SolventsDI water:ethanol = 1:1 v/v; 10 mL for solution A and 10 mL for solution B

Atmosphereair/not specified

Temperatureroom temperature ageing; vacuum dried at 60

Time10 min stirring; 6 h ageing; 12 h drying

Work-upcentrifuged; washed repeatedly with ethanol

Activationvacuum oven at 60 deg C for 12 h

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Ni(NO3)2.6H2O	45 mg	2-3 · 2.3
Metal Source	Co(NO3)2.6H2O	45 mg	2-3 · 2.3
Linker	Na-BTC	45 mg	2-3 · 2.3
Solvent	DI water:ethanol = 1:1 v/v	20 mL total	2-3 · 2.3

Partial recipeSource: Main

Route 8: Other

3 · 2.3

Metal precursorsnickel nitrate and cobalt nitrate solutions varied to Ni/Co mass ratios 0:1, 1:0, and 1:2

Linker precursorsNa-BTC

SolventsDI water:ethanol = 1:1 v/v

Atmosphereair/not specified

Temperatureroom temperature ageing; vacuum dried at 60

Time10 min stirring; 6 h ageing; 12 h drying

Work-upcentrifuged; washed repeatedly with ethanol

Activationvacuum oven at 60 deg C for 12 h

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	nickel nitrate solution	varied	3 · 2.3
Metal Source	cobalt nitrate solution	varied	3 · 2.3
Linker	Na-BTC	same procedure	3 · 2.3
Solvent	DI water:ethanol = 1:1 v/v	same procedure	3 · 2.3

Complete recipeSource: Main

Route 9: Drop Cast

4 · 2.7

Metal precursorsNCSC, NCS, or NCO active material

Solventsethanol

Additivesacetylene black; polytetrafluoroethylene

Atmospherenot specified

Temperature60

Timeovernight drying

Substrate orientationnickel foam, 1.0 cm x 1.0 cm

Work-upuniform slurry coating on nickel foam

Activationvacuum dried overnight at 60 deg C

Scalability contextMass loading 1 mg cm-2.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	active material	8 mass parts	4 · 2.7
Additive	acetylene black	1 mass part	4 · 2.7
Additive	polytetrafluoroethylene	1 mass part	4 · 2.7
Solvent	ethanol	Not specified	4 · 2.7