Synthesis · Conductive Metal–Organic Framework Nanowire Array Electrodes for High-Performance Solid-State Supercapacitors

5 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

p.2, p.6 · Morphology and Structural Analysis; Experimental Section · Figure S1

Metal precursorsCopper acetate / copper acetate monohydrate; Experimental gives 8 mg, 0.04 mmol.

Linker precursorsHHTP; Experimental gives 6.5 mg, 0.02 mmol.

SolventsResults reports water/DMF v/v = 4:1 for powder; Experimental shared paragraph reports 1 mL water/DMF v:v = 1:1.

Additivesnone reported

Atmosphereoven atmosphere not specified

Temperature85

Timenot specified for isolated powder

Substrate orientationnone

Oxidant / reductantnone reported

Work-upIrregular crystallite powder collected at the bottom of the glass vial; no separate powder washing details reported.

ActivationFor sorption, samples were refluxed in methanol overnight three times and pretreated under vacuum at 100 deg C for 10 h.

Scalability contextno powder yield reported

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	copper acetate / copper acetate monohydrate	8 mg; 0.04 mmol in Experimental Section	p.2, p.6 · Morphology and Structural Analysis; Experimental Section · Figure S1
Linker	HHTP	6.5 mg; 0.02 mmol in Experimental Section	p.2, p.6 · Morphology and Structural Analysis; Experimental Section · Figure S1
Solvent	water/DMF	Results: v/v = 4:1; Experimental: 1 mL, v:v = 1:1	p.2, p.6 · Morphology and Structural Analysis; Experimental Section · Figure S1

Complete recipeSource: Main

Route 2: Solvothermal

p.6 · Experimental Section

Metal precursorsCopper acetate monohydrate (8 mg, 0.04 mmol).

Linker precursorsHHTP (6.5 mg, 0.02 mmol).

Solvents1 mL water/DMF solvent mixture; Experimental Section gives v:v = 1:1.

AdditivesCarbon fibre paper substrate; no conductive additive or binder.

Atmosphereoven atmosphere not specified

Temperature85

Time1-24; length controlled by reaction time

Substrate orientationclean carbon fibre paper immersed in reaction solution; fibre orientation not specified

Oxidant / reductantnone reported

Work-upCool to room temperature within 30 min; collect coated paper; wash with deionized water five times; freeze-dry; then wash again, perform DI-water exchange at 85 deg C for 4 h and final 15 h, methanol exchange at 65 deg C for 5 h repeated, and dry.

ActivationCarbon paper pre-cleaned in DI water/acetone/isopropanol 1:1:1 for 30 min, ethanol-washed, dried 12 h at 100 deg C; final Cu-CAT NWA papers dried under vacuum at 85 deg C for 15 h.

Scalability contextCu-CAT mass on carbon papers 0.90-4.53 mg; mass loading 0.40-2.01 mg cm-2.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Copper acetate monohydrate	8 mg; 0.04 mmol	p.6 · Experimental Section
Linker	HHTP	6.5 mg; 0.02 mmol	p.6 · Experimental Section
Solvent	water/DMF	1 mL; v:v = 1:1	p.6 · Experimental Section
Other	carbon fibre paper	immersed piece	p.6 · Experimental Section

Complete recipeSource: Main

Route 3: Other

p.6 · Fabrication of the Solid-State Supercapacitor · Figure S10

Metal precursorspreformed Cu-CAT NWA electrodes

Linker precursorspreformed Cu-CAT NWA electrodes

Solvents60 mL 3 M KCl aqueous solution

Additives6 g PVA powder; NKK TF40 separator membrane; PVA/KCl gel electrolyte

Atmosphereambient drying; assembly atmosphere not specified

Temperature85

Timeelectrodes immersed 5 min, dried 15 min, coating repeated twice, device stood 10 h

Substrate orientationtwo identical Cu-CAT NWA electrode pieces assembled face-to-face with separator between them

Oxidant / reductantnone

Work-upDissolve PVA in KCl solution until clear; immerse electrodes in gel, dry under ambient conditions, repeat coating twice, assemble symmetric device under suitable pressure and stand 10 h.

ActivationUses activated Cu-CAT NWA electrodes from water/methanol exchange and vacuum drying route.

Scalability contextelectrodes 1.5 x 1.5 cm2; mass loading 0.5-2.0 mg cm-2; usually about 2.0 mg cm-2 for performance measurements

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Electrolyte	KCl aqueous solution	60 mL · 3 M	p.6 · Fabrication of the Solid-State Supercapacitor · Figure S10
Additive	PVA powder	6 g	p.6 · Fabrication of the Solid-State Supercapacitor · Figure S10
Other	NKK TF40 separator membrane	one piece	p.6 · Fabrication of the Solid-State Supercapacitor · Figure S10
Other	Cu-CAT NWA electrodes	two pieces; 1.5 x 1.5 cm2 · mass loading 0.5-2.0 mg cm-2	p.6 · Fabrication of the Solid-State Supercapacitor · Figure S10

Complete recipeSource: Main

Route 4: Drop Cast

p.6 · Preparation of the Electrodes for Electrochemical Measurements

Metal precursorspreformed Cu-CAT crystallite powder

Linker precursorspreformed Cu-CAT crystallite powder

SolventsN-methyl-2-pyrrolidene

AdditivesPVDF binder, active material:PVDF = 80:20 w/w; no conductive carbon additive

Atmospherevacuum drying

Temperature80

Timeapproximately 12 h stirring; overnight drying

Substrate orientationslurry coated onto carbon fibre paper

Oxidant / reductantnone

Work-upStir to sticky slurry, coat onto carbon fibre paper, dry at 80 deg C overnight under vacuum.

Activationno additional activation reported

Scalability contextmass loading 0.40 mg cm-2

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	Cu-CAT crystallite powder	80 wt% of active material/binder mixture	p.6 · Preparation of the Electrodes for Electrochemical Measurements
Additive	polyvinylidene fluoride	20 wt% of active material/binder mixture	p.6 · Preparation of the Electrodes for Electrochemical Measurements
Solvent	N-methyl-2-pyrrolidene	not specified	p.6 · Preparation of the Electrodes for Electrochemical Measurements
Other	carbon fibre paper	coating substrate	p.6 · Preparation of the Electrodes for Electrochemical Measurements

Vague recipeSource: Main

Route 5: Solvothermal

p.6 · Experimental Section

Metal precursorsnot reported here

Linker precursorsnot reported here

Solventsnot reported here

Additivesnot reported here

Atmospherenot reported

Substrate orientationnone

Oxidant / reductantnot reported

Work-upnot reported

Activationnot reported for synthesis; electrode preparation uses PVDF/NMP slurry without conductive carbon additive.

Scalability contextno scale reported

Show 1 structured reagent record

Role	Reagent	Amount / concentration	Source
Other	UiO-66, ZIF-8, ZIF-67, MIL-100, and MIL-101 precursors	not reported	p.6 · Experimental Section