Synthesis · Molecular-Level Pore Tuning in 2D Conductive Metal-Organic Frameworks for Advanced Supercapacitor Performance

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: Other

S4 · Fabrication of free-standing electrode

SolventsA few drops of ethanol; PTFE dispersion in H2O

AdditivesAcetylene black; PTFE binder

AtmosphereDried under dynamic vacuum; stored in Ar-filled glovebox

Temperature80

Time24

Substrate orientationFree-standing rolled film; 5 mm punched electrodes

Work-upGround MOF and acetylene black, mixed with PTFE dispersion and ethanol into paste, kneaded, rolled into film, punched into electrodes.

ActivationDried under dynamic vacuum at 80 C for 24 h to remove residual solvent.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	Cu3(HHTATP)2	85 wt% of film	S4 · Fabrication of free-standing electrode
Additive	acetylene black (99.9+%, Alfa Aesar)	10 wt% by SI; 15 wt% stated in main text	S4 · Fabrication of free-standing electrode
Additive	PTFE (60 wt% PTFE dispersion in H2O, Aldrich)	5 wt% of film · 60 wt% dispersion	S4 · Fabrication of free-standing electrode
Solvent	ethanol (EtOH, 99.5%, Samchun)	a few drops	S4 · Fabrication of free-standing electrode

Complete recipeSource: SI

Route 2: Other

S4 · Fabrication of free-standing electrode

SolventsA few drops of ethanol; PTFE dispersion in H2O

AdditivesAcetylene black; PTFE binder

AtmosphereDried under dynamic vacuum; stored in Ar-filled glovebox

Temperature80

Time24

Substrate orientationFree-standing rolled film; 5 mm punched electrodes

Work-upSame composite film fabrication method as Cu3(HHTATP)2 control electrodes.

ActivationDried under dynamic vacuum at 80 C for 24 h.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	Cu3(HHTP)2	85 wt% of film	S4 · Fabrication of free-standing electrode
Additive	acetylene black	10 wt% by SI electrode recipe	S4 · Fabrication of free-standing electrode
Additive	PTFE dispersion	5 wt% of film · 60 wt% PTFE in H2O	S4 · Fabrication of free-standing electrode
Solvent	ethanol	a few drops	S4 · Fabrication of free-standing electrode

Complete recipeSource: Both

Route 3: Solvothermal

S4 · Synthesis of Cu3(HHTATP)2

Metal precursorsCu(NO3)2*3H2O (63.5 mg, 0.239 mmol)

Linker precursorsHHTATP*3HBr (97.3 mg, 0.159 mmol) in 4.2 mL aqueous solution

SolventsDI water; washing with DI water, DMF, acetone

Additives0.414 mL of 28% aqueous ammonia solution

AtmosphereAmbient during mixing; capped vial; product stored in N2-filled glovebox

Temperature65

Time24

Work-upSlow cool to room temperature over 3 h; centrifuge; wash with DI water (35 mL x 3), DMF (20 mL x 2), acetone (20 mL x 2).

ActivationDried at 80 C under dynamic vacuum; porosity samples activated separately at 120 C under dynamic vacuum (4 umHg) for 12 h.

Scalability contextOptimized synthesis scale yielded approximately 120 mg per 20 mL vial.

Show 6 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	*Copper(II) nitrate trihydrate (Cu(NO3)23H2O, 99.5%, Strem)**	63.5 mg, 0.239 mmol	S4 · Synthesis of Cu3(HHTATP)2
Linker	*HHTATP3HBr**	97.3 mg, 0.159 mmol	S4 · Synthesis of Cu3(HHTATP)2
Base	aqueous ammonia solution (28%, JUNSEI)	0.414 mL · 28%	S4 · Synthesis of Cu3(HHTATP)2
Solvent	DI water	1 mL for Cu solution; 4.2 mL linker solution	S4 · Synthesis of Cu3(HHTATP)2
Solvent	DMF wash	20 mL x 2	S4 · Synthesis of Cu3(HHTATP)2
Solvent	acetone wash	20 mL x 2	S4 · Synthesis of Cu3(HHTATP)2

Vague recipeSource: SI

Route 4: Unknown

S4 · Materials

Linker precursorsHHTP (>95.0%, TCI)

Show 1 structured reagent record

Role	Reagent	Amount / concentration	Source
Linker	2,3,6,7,10,11-hexahydroxytriphenylene (HHTP, >95.0%, TCI)	Not specified	S4 · Materials