Synthesis · Construction of sulfur vacancies enriched hollow zinc cobalt bimetallic sulfides for high-performance supercapacitors

6 structured synthesis routes

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

Partial recipeSource: Main

Route 1: Solvothermal

p002 · 2.2. Synthesis of ZnxCo3-xS4

Metal precursorsCo-MOF

Solventsethanol

Additivesthioacetamide

Atmospherenot reported

Temperature120

Time4

Oxidant / reductantthioacetamide as sulphur source/vulcanisation reagent

Work-upWashed with ethanol several times.

ActivationDried in vacuum at 60 deg C overnight.

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	Co-MOF	not separately stated; same experimental procedure as 80 mg ZnxCo3-x-MOF route	p002 · 2.2. Synthesis of ZnxCo3-xS4
Solvent	ethanol	not separately stated; same procedure as ZnxCo3-xS4	p002 · 2.2. Synthesis of ZnxCo3-xS4
Additive	thioacetamide	not separately stated; same procedure as ZnxCo3-xS4	p002 · 2.2. Synthesis of ZnxCo3-xS4

Partial recipeSource: Main

Route 2: Other

p002 · 2.1. Synthesis of ZnxCo3-x-MOF

Metal precursorsCo(NO3)2.6H2O; no Zn(NO3)2.6H2O

Linker precursors2-methylimidazole

Solventsmethanol; DI water and methanol washing

Atmospherenot reported

Temperatureroom temperature

Timesimilar to ZnxCo3-x-MOF route; 4 h stirring plus 24 h standing inferred from same conditions

Work-upCollected by centrifugation and washed as for ZnxCo3-x-MOF.

ActivationDried overnight in vacuum at 60 deg C.

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Co(NO3)2.6H2O	not separately stated; prepared under similar conditions	p002 · 2.1. Synthesis of ZnxCo3-x-MOF
Linker	2-methylimidazole	not separately stated; parent route uses 12 mmol	p002 · 2.1. Synthesis of ZnxCo3-x-MOF
Solvent	methanol	not separately stated; parent route uses 30 mL + 20 mL	p002 · 2.1. Synthesis of ZnxCo3-x-MOF

Partial recipeSource: Main

Route 3: Other

p002 · 2.4. Electrochemical measurements

Metal precursorsZn0.3Co2.7S4 positive electrode

Additivesactivated carbon negative electrode; 3 M KOH electrolyte

Atmospherenot reported

Work-upAssembled asymmetric aqueous HSC with charge balance based on positive and negative electrode capacitances.

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	Zn0.3Co2.7S4 positive electrode	active material loading about 2 mg	p002 · 2.4. Electrochemical measurements
Other	activated carbon negative electrode	mass loading determined by charge balance m+/m- = Cs-/Cs+	p002 · 2.4. Electrochemical measurements
Electrolyte	KOH	3 M	p002 · 2.4. Electrochemical measurements

Partial recipeSource: Main

Route 4: Drop Cast

p002 · 2.4. Electrochemical measurements

Metal precursorsresultant ZnxCo3-xS4 active material

Solventsnot reported for slurry

Additivesacetylene black; PTFE binder

Atmospherenot reported

Temperature60

Timeovernight drying

Substrate orientation1 x 2 cm precleaned nickel foam

Work-upSlurry coated onto nickel foam; dried at 60 deg C overnight; pressed under 10 MPa.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	ZnxCo3-xS4	80 wt% of electrode solids	p002 · 2.4. Electrochemical measurements
Additive	acetylene black	10 wt% of electrode solids	p002 · 2.4. Electrochemical measurements
Additive	polytetrafluoroethylene (PTFE) binder	10 wt% of electrode solids	p002 · 2.4. Electrochemical measurements
Other	nickel foam	1 x 2 cm; active material loading about 2-5 mg cm-2	p002 · 2.4. Electrochemical measurements

Partial recipeSource: Main

Route 5: Other

p002 · 2.1. Synthesis of ZnxCo3-x-MOF

Metal precursorsZn(NO3)2.6H2O and Co(NO3)2.6H2O; total Zn2+ + Co2+ amount 3 mmol; molar ratio varied for x = 0, 0.15, 0.3 and 0.45

Linker precursors2-methylimidazole, 12 mmol

Solventsmethanol, 30 mL for metal solution plus 20 mL for linker solution

Atmospherenot reported

Temperatureroom temperature

Time4 h stirring plus 24 h standing

Work-upPurple precipitate collected by centrifugation; washed with methanol and DI water several times.

ActivationDried overnight in vacuum at 60 deg C.

Scalability contextConclusion describes the coprecipitation method as scalable, but no batch-size scaling data are supplied.

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Zn(NO3)2.6H2O	variable; total Zn2+ + Co2+ = 3 mmol	p002 · 2.1. Synthesis of ZnxCo3-x-MOF
Metal Source	Co(NO3)2.6H2O	variable; total Zn2+ + Co2+ = 3 mmol	p002 · 2.1. Synthesis of ZnxCo3-x-MOF
Linker	2-methylimidazole	12 mmol	p002 · 2.1. Synthesis of ZnxCo3-x-MOF
Solvent	methanol	30 mL + 20 mL	p002 · 2.1. Synthesis of ZnxCo3-x-MOF
Solvent	DI water	wash solvent	p002 · 2.1. Synthesis of ZnxCo3-x-MOF

Partial recipeSource: Main

Route 6: Solvothermal

p002 · 2.2. Synthesis of ZnxCo3-xS4

Metal precursorsas-obtained ZnxCo3-x-MOF, 80 mg

Solventsethanol, 40 mL

Additivesthioacetamide (CH3CSNH2), 1.6 mmol

Atmospherenot reported

Temperature120

Time4

Oxidant / reductantthioacetamide as sulphur source/vulcanisation reagent

Work-upCooled to room temperature; product washed with ethanol several times.

ActivationDried in vacuum at 60 deg C overnight.

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	ZnxCo3-x-MOF	80 mg	p002 · 2.2. Synthesis of ZnxCo3-xS4
Solvent	ethanol	40 mL	p002 · 2.2. Synthesis of ZnxCo3-xS4
Additive	thioacetamide (CH3CSNH2)	1.6 mmol	p002 · 2.2. Synthesis of ZnxCo3-xS4