Synthesis · Sulfur vacancies enriched Nickel-Cobalt sulfides hollow spheres with high performance for All-Solid-State hybrid supercapacitor

5 structured synthesis routes

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

Partial recipeSource: Both

Route 1: Other

main p.3 · 2.6. Electrochemical performances measurements · Fig. 7a

Metal precursorsr-NiCo2S4-6 HSs positive electrode

AdditivesN/S-AC negative electrode; PVA-KOH gel electrolyte

Atmospherenot reported

Work-upAssembled as all-solid-state hybrid device; electrode mass ratio m+/m- = 0.4973.

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	r-NiCo2S4-6 HSs	positive electrode; m+/m- = 0.4973	main p.3 · 2.6. Electrochemical performances measurements · Fig. 7a
Other	N/S-AC	negative electrode	main p.3 · 2.6. Electrochemical performances measurements · Fig. 7a
Electrolyte	PVA-KOH gel electrolyte	KOH 3 M	main p.3 · 2.6. Electrochemical performances measurements · Fig. 7a

Complete recipeSource: Both

Route 2: Solvothermal

main p.2 · 2.2. Synthesis of Ni-Co CPs

Metal precursorsNi(NO3)2.6H2O (0.5 mmol); Co(NO3)2.6H2O (1 mmol)

Linker precursorsH2IPA (isophthalic acid, 1.5 mmol)

Solvents15 mL acetone and 15 mL DMF

Atmospherenot reported

Temperature160

Time4

Work-upBrown precipitates collected by centrifugation, washed with ethanol several times, and vacuum dried at 80 C.

ActivationVacuum drying at 80 C

Scalability contextBatch synthesis in 50 mL Teflon-lined stainless-steel autoclave.

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Ni(NO3)2.6H2O	0.5 mmol	main p.2 · 2.2. Synthesis of Ni-Co CPs
Metal Source	Co(NO3)2.6H2O	1 mmol	main p.2 · 2.2. Synthesis of Ni-Co CPs
Linker	H2IPA	1.5 mmol	main p.2 · 2.2. Synthesis of Ni-Co CPs
Solvent	acetone	15 mL · 99%	main p.2 · 2.2. Synthesis of Ni-Co CPs
Solvent	DMF	15 mL · 99%	main p.2 · 2.2. Synthesis of Ni-Co CPs

Partial recipeSource: Both

Route 3: Solvothermal

main p.2 · 2.3. Synthesis of NiCo2S4 HSs · Fig. S4

Metal precursorsNi-Co CPs (30 mg)

Solventsethanol (30 mL)

Additivesthioacetamide (TAA, 60 mg)

Atmospherenot reported

Temperature160

Time0.5, 1, 2, 4 or 6

Oxidant / reductantTAA sulfur source; anion exchange/sulfidation

Work-upWorkup after sulfidation not specified in this section.

Scalability context50 mL Teflon-lined stainless-steel autoclave.

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	Ni-Co CPs	30 mg	main p.2 · 2.3. Synthesis of NiCo2S4 HSs · Fig. S4
Solvent	ethanol	30 mL	main p.2 · 2.3. Synthesis of NiCo2S4 HSs · Fig. S4
Additive	thioacetamide (TAA)	60 mg	main p.2 · 2.3. Synthesis of NiCo2S4 HSs · Fig. S4

Partial recipeSource: Main

Route 4: Other

main p.2 · 2.4. Reduction of NiCo2S4 HSs

Metal precursorsNiCo2S4-6 HSs

Solventsaqueous NaBH4 solution

Atmospherenot reported

Temperatureroom temperature

Time2

Oxidant / reductantNaBH4 reductant, 0.1 M

Work-upWashed with deionised water and ethanol several times; collected and vacuum dried at 80 C for 12 h.

ActivationVacuum drying at 80 C for 12 h

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	NiCo2S4-6 HSs	not reported	main p.2 · 2.4. Reduction of NiCo2S4 HSs
Reductant	NaBH4 aqueous solution	not reported · 0.1 M	main p.2 · 2.4. Reduction of NiCo2S4 HSs
Solvent	deionised water and ethanol wash	several times	main p.2 · 2.4. Reduction of NiCo2S4 HSs

Complete recipeSource: Main

Route 5: Other

main p.3 · 2.6. Electrochemical performances measurements

Metal precursorsr-NiCo2S4-6 HSs active material

Additivesacetylene black and PTFE binder

Atmospherevacuum drying

Temperature80

Time12

Substrate orientationnickel foam, 1 x 2 cm2

Work-upPressed under 8 MPa and immersed into 3 M KOH electrolyte for 6 h before testing.

ActivationDried in vacuum at 80 C for 12 h

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	active material	8 weight parts	main p.3 · 2.6. Electrochemical performances measurements
Additive	acetylene black	1 weight part	main p.3 · 2.6. Electrochemical performances measurements
Additive	PTFE	1 weight part	main p.3 · 2.6. Electrochemical performances measurements
Electrolyte	KOH	3 M	main p.3 · 2.6. Electrochemical performances measurements