Synthesis · Nickel(II) Cluster-Based Pillar-Layered Metal-Organic Frameworks for High-Performance Supercapacitors

4 structured synthesis routes

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

Complete recipeSource: Both

Route 1: Drop Cast

main p.2 (journal p.17279) · 2.7. Electrochemical Measurements

Metal precursorsNi-mba-Na or Ni-mba-K active material

Linker precursorsnot applicable

Solventsabsolute ethanol

Additivesacetylene black (10 wt%) and PTFE (10 wt%)

Atmosphereair oven; atmosphere not specified

Temperature60

Time12

Substrate orientationnickel foam, 1 x 1 cm2

Work-upSlurry coated on nickel foam and oven dried.

Activationnone reported

Scalability contextActive material loading approximately 2.5 mg cm-2.

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	Ni MOF active material	80 wt%	main p.2 (journal p.17279) · 2.7. Electrochemical Measurements
Additive	acetylene black	10 wt%	main p.2 (journal p.17279) · 2.7. Electrochemical Measurements
Additive	PTFE	10 wt%	main p.2 (journal p.17279) · 2.7. Electrochemical Measurements
Solvent	absolute ethanol	not reported	main p.2 (journal p.17279) · 2.7. Electrochemical Measurements
Other	nickel foam	1 x 1 cm2	main p.2 (journal p.17279) · 2.7. Electrochemical Measurements

Complete recipeSource: Both

Route 2: Other

main p.2 (journal p.17279) · 2.4. Synthesis of Nitrogen-Doped Porous Carbon (NDC)

Metal precursorszinc nitrate hexahydrate (0.25 mmol)

Linker precursorsbptp (0.5 mmol)

SolventsDMF (10 mL), deionised water (10 mL plus 5 mL), anhydrous ethanol (20 mL)

AdditivesKOH (25 mmol)

AtmosphereN2 during carbonisation

Temperature700

Time2

Oxidant / reductantKOH activation/base treatment

Work-upWash three times with 2 M HCl, deionised water and anhydrous ethanol; dry in electric blast oven at 80 deg C.

Activationcarbonisation/activation at 700 deg C under N2

Scalability contextYield about 21 wt% based on bptp; no scale-up discussed.

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Linker	bptp	0.5 mmol	main p.2 (journal p.17279) · 2.4. Synthesis of Nitrogen-Doped Porous Carbon (NDC)
Solvent	DMF	10 mL	main p.2 (journal p.17279) · 2.4. Synthesis of Nitrogen-Doped Porous Carbon (NDC)
Metal Source	zinc nitrate hexahydrate	0.25 mmol · in 10 mL deionised water	main p.2 (journal p.17279) · 2.4. Synthesis of Nitrogen-Doped Porous Carbon (NDC)
Base	KOH	25 mmol · in 20 mL ethanol + 5 mL water	main p.2 (journal p.17279) · 2.4. Synthesis of Nitrogen-Doped Porous Carbon (NDC)
Acid	HCl	three washes · 2 M	main p.2 (journal p.17279) · 2.4. Synthesis of Nitrogen-Doped Porous Carbon (NDC)

Complete recipeSource: Both

Route 3: Solvothermal

main p.2 (journal p.17279) · 2.3. Synthesis of Ni MOFs

Metal precursorsnickel chloride hexahydrate (NiCl2.6H2O, 3 mmol) in 10 mL water, inferred same as Na route

Linker precursors2-mercaptobenzoic acid / mba (6 mmol), inferred same as Na route

Solventsanhydrous ethanol (20 mL) plus 10 mL aqueous nickel chloride solution, inferred same as Na route

Additivespotassium hydroxide equimolar to NaOH (3 mmol)

Atmospheresealed 50 mL Teflon-lined stainless-steel reactor; atmosphere not otherwise specified

Temperature120

Time96

Work-upInferred same as Na route: cool to 25 deg C; wash with deionised water, anhydrous ethanol and dilute hydrochloric acid; dry at 90 deg C for 12 h.

Activationnone reported beyond drying

Scalability contextYield about 23 wt%; no scale-up discussed.

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Base	potassium hydroxide	equimolar to NaOH (3 mmol)	main p.2 (journal p.17279) · 2.3. Synthesis of Ni MOFs
Linker	mba / 2-mercaptobenzoic acid	6 mmol, inferred from Na route	main p.2 (journal p.17279) · 2.3. Synthesis of Ni MOFs
Solvent	anhydrous ethanol	20 mL, inferred from Na route	main p.2 (journal p.17279) · 2.3. Synthesis of Ni MOFs
Metal Source	nickel chloride hexahydrate	3 mmol in 10 mL aqueous solution, inferred from Na route	main p.2 (journal p.17279) · 2.3. Synthesis of Ni MOFs
Acid	dilute hydrochloric acid	several washes, inferred from Na route · dilute	main p.2 (journal p.17279) · 2.3. Synthesis of Ni MOFs

Complete recipeSource: Both

Route 4: Solvothermal

main p.2 (journal p.17279) · 2.3. Synthesis of Ni MOFs

Metal precursorsnickel chloride hexahydrate (NiCl2.6H2O, 3 mmol) in 10 mL water

Linker precursors2-mercaptobenzoic acid / mba (6 mmol)

Solventsanhydrous ethanol (20 mL) plus 10 mL aqueous nickel chloride solution

Additivessodium hydroxide (3 mmol)

Atmospheresealed 50 mL Teflon-lined stainless-steel reactor; atmosphere not otherwise specified

Temperature120

Time96

Work-upCool to 25 deg C; wash several times with deionised water, anhydrous ethanol and dilute hydrochloric acid; dry in electric blast oven at 90 deg C for 12 h.

Activationnone reported beyond drying

Scalability context50 mL Teflon-lined reactor; yield about 18 wt% based on NiCl2.6H2O, mba and NaOH; no scale-up discussed.

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Base	sodium hydroxide	3 mmol	main p.2 (journal p.17279) · 2.3. Synthesis of Ni MOFs
Linker	mba / 2-mercaptobenzoic acid	6 mmol	main p.2 (journal p.17279) · 2.3. Synthesis of Ni MOFs
Solvent	anhydrous ethanol	20 mL	main p.2 (journal p.17279) · 2.3. Synthesis of Ni MOFs
Metal Source	nickel chloride hexahydrate	3 mmol in 10 mL aqueous solution	main p.2 (journal p.17279) · 2.3. Synthesis of Ni MOFs
Acid	dilute hydrochloric acid	several washes · dilute	main p.2 (journal p.17279) · 2.3. Synthesis of Ni MOFs