Synthesis · Enhancing the Electrochemical Energy Storage of Metal-Organic Frameworks: Linker Engineering and Size Optimization

6 structured synthesis routes

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

Complete recipeSource: SI

Route 1: Other

S3 · Electrochemical measurements

Metal precursorsNi-tdc-bpe(0.5) positive electrode

Linker precursorsnot applicable to device fabrication

Solvents3.0 M KOH electrolyte

Additivesactive carbon negative electrode; glass fiber membrane separator

Atmosphereroom temperature electrochemical testing; assembly atmosphere not reported

Substrate orientationsandwich-like HSC device

Work-upmass ratio m+/m- determined as 3.3; typical Ni-tdc-bpe(0.5) positive-electrode loading 1.0-1.3 mg

Activationnone reported

Scalability contextDevice loading reported only for positive electrode; no larger-scale assembly details.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	Ni-tdc-bpe(0.5) positive electrode	1.0~1.3 mg typical mass loading	S3 · Electrochemical measurements
Other	active carbon (AC) negative electrode	m+/m- = 3.3	S3 · Electrochemical measurements
Electrolyte	KOH	not reported · 3.0 M	S3 · Electrochemical measurements
Other	glass fiber membrane	not reported	S3 · Electrochemical measurements

Complete recipeSource: Main

Route 2: Solvothermal

428 · Experimental Section

Metal precursorsNiCl2·6H2O (118.8 mg, 0.5 mmol) by analogy to Ni-tdc-bpe/Ni-tdc-bpy

Linker precursorsH2tdc (86 mg, 0.5 mmol by analogy); bpe (22 mg, 0.125 mmol)

SolventsDMF; wash with DMF and CH3OH by analogy to Ni-tdc-bpy

Additivesnone reported

Atmospherenot reported; sealed Teflon-lined autoclave by analogy

Temperature120

Time48

Oxidant / reductantnone reported

Work-upsame as Ni-tdc-bpy: cool, wash with DMF and CH3OH, dry at 60 °C

Activationdried at 60 °C; no additional activation reported

Scalability contextSmall-batch autoclave route; scale not discussed.

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	NiCl2·6H2O	118.8 mg, 0.5 mmol · inferred from stated similar route	428 · Experimental Section
Linker	2,5-Thiophenedicarboxylic acid (H2tdc)	86 mg, 0.5 mmol · inferred from stated similar route	428 · Experimental Section
Linker	bpe	22 mg, 0.125 mmol	428 · Experimental Section
Solvent	DMF	5 mL total · inferred from stated similar route	428 · Experimental Section
Solvent	CH3OH	wash solvent · inferred from stated similar route	428 · Experimental Section

Complete recipeSource: Main

Route 3: Solvothermal

428 · Experimental Section

Metal precursorsNiCl2·6H2O (118.8 mg, 0.5 mmol) by analogy to Ni-tdc-bpy

Linker precursorsH2tdc (86 mg, 0.5 mmol by analogy); bpe (44 mg, 0.25 mmol)

SolventsDMF; wash with DMF and CH3OH by analogy to Ni-tdc-bpy

Additivesnone reported

Atmospherenot reported; sealed Teflon-lined autoclave by analogy

Temperature120

Time48

Oxidant / reductantnone reported

Work-upsame as Ni-tdc-bpy: cool, wash with DMF and CH3OH, dry at 60 °C

Activationdried at 60 °C; no additional activation reported

Scalability contextSmall-batch autoclave route; scale not discussed.

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	NiCl2·6H2O	118.8 mg, 0.5 mmol · inferred from stated similar route	428 · Experimental Section
Linker	2,5-Thiophenedicarboxylic acid (H2tdc)	86 mg, 0.5 mmol · inferred from stated similar route	428 · Experimental Section
Linker	bpe	44 mg, 0.25 mmol	428 · Experimental Section
Solvent	DMF	5 mL total · inferred from stated similar route	428 · Experimental Section
Solvent	CH3OH	wash solvent · inferred from stated similar route	428 · Experimental Section

Complete recipeSource: Main

Route 4: Solvothermal

428 · Experimental Section

Metal precursorsNiCl2·6H2O (118.8 mg, 0.5 mmol) by analogy to Ni-tdc-bpy

Linker precursorsH2tdc (86 mg, 0.5 mmol by analogy); bpy (19.5 mg, 0.125 mmol)

SolventsDMF; wash with DMF and CH3OH by analogy to Ni-tdc-bpy

Additivesnone reported

Atmospherenot reported; sealed Teflon-lined autoclave by analogy

Temperature120

Time48

Oxidant / reductantnone reported

Work-upsame as Ni-tdc-bpy: cool, wash with DMF and CH3OH, dry at 60 °C

Activationdried at 60 °C; no additional activation reported

Scalability contextSmall-batch autoclave route; scale not discussed.

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	NiCl2·6H2O	118.8 mg, 0.5 mmol · inferred from stated similar route	428 · Experimental Section
Linker	2,5-Thiophenedicarboxylic acid (H2tdc)	86 mg, 0.5 mmol · inferred from stated similar route	428 · Experimental Section
Linker	bpy	19.5 mg, 0.125 mmol	428 · Experimental Section
Solvent	DMF	5 mL total · inferred from stated similar route	428 · Experimental Section
Solvent	CH3OH	wash solvent · inferred from stated similar route	428 · Experimental Section

Complete recipeSource: Main

Route 5: Solvothermal

428 · Experimental Section

Metal precursorsNiCl2·6H2O (118.8 mg, 0.5 mmol) in 2 mL DMF

Linker precursors2,5-thiophenedicarboxylic acid (86 mg, 0.5 mmol); bpy (39 mg, 0.25 mmol)

SolventsN,N-dimethylformamide (3 mL for linkers + 2 mL metal solution)

Additivesnone reported

Atmospherenot reported; sealed Teflon-lined autoclave

Temperature120

Time48

Oxidant / reductantnone reported

Work-upcool to room temperature; wash with DMF and CH3OH three times separately; dry at 60 °C

Activationdried at 60 °C; no additional activation reported

Scalability contextSmall-batch autoclave route; scale not discussed.

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	NiCl2·6H2O	118.8 mg, 0.5 mmol	428 · Experimental Section
Linker	2,5-Thiophenedicarboxylic acid (H2tdc)	86 mg, 0.5 mmol	428 · Experimental Section
Linker	bpy	39 mg, 0.25 mmol	428 · Experimental Section
Solvent	N,N-dimethylformamide (DMF)	5 mL total	428 · Experimental Section
Solvent	CH3OH	wash solvent	428 · Experimental Section

Complete recipeSource: SI

Route 6: Other

S3 · Electrochemical measurements

Metal precursorsactive material: Ni-tdc-bpy, Ni-tdc-bpe, Ni-tdc-bpy(0.5), or Ni-tdc-bpe(0.5)

Linker precursorsnot applicable to electrode fabrication

Solventsisopropyl alcohol used to help form slurry

Additivesacetylene black; polytetrafluoroethylene

Atmosphereroom temperature; atmosphere not reported

Substrate orientationnickel foam (~1 cm2)

Work-upslurry coated on nickel foam and pressed into thin foil at 10 MPa

Activationnone reported

Scalability contextElectrode mass loading for three-electrode tests not reported.

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	active material	80 mass parts · mass ratio 80:15:5	S3 · Electrochemical measurements
Additive	acetylene black	15 mass parts · mass ratio 80:15:5	S3 · Electrochemical measurements
Additive	polytetrafluoroethylene	5 mass parts · mass ratio 80:15:5	S3 · Electrochemical measurements
Solvent	isopropyl alcohol	not reported	S3 · Electrochemical measurements
Other	nickel foam	~1 cm2	S3 · Electrochemical measurements