Synthesis · A conductive anionic Co-MOF cage with zeolite framework for 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

main p.2 · Experimental/synthesis description

Metal precursors0.3 mmol Co(NO3)2.6H2O; Ni2+ from Ni foam dissolution

Linker precursors0.05 mmol H6TATAT

SolventsDMF/H2O, v/v = 6/1; methanol exchange after synthesis

AdditivesCTAB at CTAB:H6TATAT molar ratio 1:1

Atmospherenot reported

Temperature70

Time36

Substrate orientationNi foam discs added after CTAB addition

Work-upsame as typical synthesis: washed with DMF and CH3OH; methanol exchange for 2 days

Activationhigh vacuum (<10^-8 bar) at 70 C; pressed at 10 MPa

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Co(NO3)2.6H2O	0.3 mmol	main p.2 · Experimental/synthesis description
Linker	H6TATAT	0.05 mmol	main p.2 · Experimental/synthesis description
Solvent	DMF and H2O	v/v = 6/1	main p.2 · Experimental/synthesis description
Additive	cetyltrimethylammonium bromide (CTAB)	CTAB:H6TATAT = 1:1	main p.2 · Experimental/synthesis description
Other	Ni foam	12 mm diameter pieces	main p.2 · Experimental/synthesis description

Partial recipeSource: Main

Route 2: Solvothermal

main p.2 · Experimental/synthesis description

Metal precursors0.3 mmol Co(NO3)2.6H2O; Ni2+ from Ni foam dissolution

Linker precursors0.05 mmol H6TATAT

SolventsDMF/H2O, v/v = 6/1; methanol exchange after synthesis

AdditivesCTAB at CTAB:H6TATAT molar ratio 2:1

Atmospherenot reported

Temperature70

Time36

Substrate orientationNi foam discs added after CTAB addition

Work-upsame as typical synthesis

Activationhigh vacuum (<10^-8 bar) at 70 C; pressed at 10 MPa

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Co(NO3)2.6H2O	0.3 mmol	main p.2 · Experimental/synthesis description
Linker	H6TATAT	0.05 mmol	main p.2 · Experimental/synthesis description
Solvent	DMF and H2O	v/v = 6/1	main p.2 · Experimental/synthesis description
Additive	cetyltrimethylammonium bromide (CTAB)	CTAB:H6TATAT = 2:1	main p.2 · Experimental/synthesis description
Other	Ni foam	12 mm diameter pieces	main p.2 · Experimental/synthesis description

Partial recipeSource: Main

Route 3: Solvothermal

main p.2 · Experimental/synthesis description

Metal precursors0.3 mmol Co(NO3)2.6H2O; Ni2+ from Ni foam dissolution

Linker precursors0.05 mmol H6TATAT

SolventsDMF/H2O, v/v = 6/1; methanol exchange after synthesis

AdditivesCTAB at CTAB:H6TATAT molar ratio 4:1

Atmospherenot reported

Temperature70

Time36

Substrate orientationNi foam discs added after CTAB addition

Work-upsame as typical synthesis

Activationhigh vacuum (<10^-8 bar) at 70 C; pressed at 10 MPa

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Co(NO3)2.6H2O	0.3 mmol	main p.2 · Experimental/synthesis description
Linker	H6TATAT	0.05 mmol	main p.2 · Experimental/synthesis description
Solvent	DMF and H2O	v/v = 6/1	main p.2 · Experimental/synthesis description
Additive	cetyltrimethylammonium bromide (CTAB)	CTAB:H6TATAT = 4:1	main p.2 · Experimental/synthesis description
Other	Ni foam	12 mm diameter pieces	main p.2 · Experimental/synthesis description

Partial recipeSource: Main

Route 4: Solvothermal

main p.5 · Summary · Fig. 6, Fig. 7

Metal precursors0.3 mmol Co(NO3)2.6H2O; Ni2+ from Ni foam dissolution

Linker precursors0.05 mmol H6TATAT

SolventsDMF/H2O, v/v = 6/1; methanol exchange after synthesis

AdditivesCTAB at CTAB:H6TATAT molar ratio 6:1

Atmospherenot reported

Temperature70

Time36

Substrate orientationNi foam discs added after CTAB addition

Work-upsame as typical synthesis

Activationhigh vacuum (<10^-8 bar) at 70 C; pressed at 10 MPa

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Co(NO3)2.6H2O	0.3 mmol	main p.5 · Summary · Fig. 6, Fig. 7
Linker	H6TATAT	0.05 mmol	main p.5 · Summary · Fig. 6, Fig. 7
Solvent	DMF and H2O	v/v = 6/1	main p.5 · Summary · Fig. 6, Fig. 7
Additive	cetyltrimethylammonium bromide (CTAB)	CTAB:H6TATAT = 6:1	main p.5 · Summary · Fig. 6, Fig. 7
Other	Ni foam	12 mm diameter pieces	main p.5 · Summary · Fig. 6, Fig. 7

Partial recipeSource: Main

Route 5: Solvothermal

main p.4 · Results and discussion · Fig. 5

Metal precursors0.3 mmol Co(NO3)2.6H2O; Ni2+ from Ni foam dissolution

Linker precursors0.05 mmol H6TATAT

SolventsDMF/H2O, v/v = 6/1; methanol exchange after synthesis

AdditivesCTAB at CTAB:H6TATAT molar ratio 8:1

Atmospherenot reported

Temperature70

Time36

Substrate orientationNi foam discs added after CTAB addition

Work-upsame as typical synthesis

Activationhigh vacuum (<10^-8 bar) at 70 C; pressed at 10 MPa

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Co(NO3)2.6H2O	0.3 mmol	main p.4 · Results and discussion · Fig. 5
Linker	H6TATAT	0.05 mmol	main p.4 · Results and discussion · Fig. 5
Solvent	DMF and H2O	v/v = 6/1	main p.4 · Results and discussion · Fig. 5
Additive	cetyltrimethylammonium bromide (CTAB)	CTAB:H6TATAT = 8:1	main p.4 · Results and discussion · Fig. 5
Other	Ni foam	12 mm diameter pieces	main p.4 · Results and discussion · Fig. 5

Partial recipeSource: Main

Route 6: Solvothermal

main p.2 · Experimental/synthesis description

Metal precursors0.3 mmol Co(NO3)2.6H2O; Ni2+ additionally derived in situ from partial dissolution of Ni foam

Linker precursors0.05 mmol H6TATAT

SolventsDMF/H2O mixed solvent, v/v = 6/1; methanol exchange after synthesis

Atmospherenot reported

Temperature70

Time36

Substrate orientationtwo 12 mm diameter cut-out Ni foam pieces with same mass placed in 23 mL Teflon-lined stainless-steel vessel

Work-upcooled to room temperature; washed with DMF and CH3OH; immersed in methanol for 2 days with fresh solvent exchanged every 24 h

Activationmethanol removed under high vacuum (<10^-8 bar) at 70 C; pressed at 10 MPa before use as working electrodes

Scalability contextBatch used two Ni foam discs in a 23 mL vessel; active material loading typically 4-6 mg.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Co(NO3)2.6H2O	0.3 mmol	main p.2 · Experimental/synthesis description
Linker	H6TATAT	0.05 mmol	main p.2 · Experimental/synthesis description
Solvent	DMF and H2O	v/v = 6/1	main p.2 · Experimental/synthesis description
Other	Ni foam	two cut-out pieces, 12 mm diameter, same mass	main p.2 · Experimental/synthesis description