Synthesis · Pillared nickel-based metal-organic frameworks as electrode material with high electrochemical performance

4 structured synthesis routes

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

Complete recipeSource: Main

Route 1: Drop Cast

2 · 2.3 Electrochemical measurements

Solventsethanol, 1 mL

Additivescarbon black (20 wt%); PTFE (10 wt%)

Atmospherevacuum drying

Temperature110

Time12

Substrate orientationnickel foam current collector, 1 cm x 1 cm

Work-upHomogeneous slurry coated onto nickel foam; pressed under 10 MPa for 10 s after drying.

ActivationVacuum drying at 110 C for 12 h

Scalability contextActive material loading about 2-3 mg per current collector.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	synthesized active material	70 wt%	2 · 2.3 Electrochemical measurements
Additive	carbon black	20 wt%	2 · 2.3 Electrochemical measurements
Additive	polytetrafluoroethylene (PTFE)	10 wt%	2 · 2.3 Electrochemical measurements
Solvent	ethanol	1 mL	2 · 2.3 Electrochemical measurements

Partial recipeSource: Main

Route 2: Solvothermal

2 · 2.1 Synthesis of pillared Ni-based MOFs · Fig. 1

Metal precursorsNi(NO3)2.6H2O; exact Ni-only amount not explicitly stated in main text

Linker precursors1,4-benzenedicarboxylic acid (bdc); dabco

SolventsDMF; methanol and DMF washes

Atmospherenot specified

Temperature120

Time48

Work-upFiltered after natural cooling and washed using methanol and DMF for 4 days, according to shared M2(bdc)2P procedure.

ActivationVacuum drying at 110 C for 12 h, according to shared M2(bdc)2P procedure.

Scalability contextShared 50 mL autoclave method; exact Ni-only stoichiometry requires SI or author clarification.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Ni(NO3)2.6H2O	not explicitly stated for Ni-only sample	2 · 2.1 Synthesis of pillared Ni-based MOFs · Fig. 1
Linker	bdc	not explicitly stated for Ni-only sample	2 · 2.1 Synthesis of pillared Ni-based MOFs · Fig. 1
Linker	dabco	not explicitly stated for Ni-only sample	2 · 2.1 Synthesis of pillared Ni-based MOFs · Fig. 1
Solvent	DMF	not explicitly stated for Ni-only sample	2 · 2.1 Synthesis of pillared Ni-based MOFs · Fig. 1

Partial recipeSource: Main

Route 3: Solvothermal

2 · 2.1 Synthesis of pillared Ni-based MOFs

Metal precursorsZn(NO3)2.6H2O only; exact Zn-only amount not explicitly stated in main text

Linker precursors1,4-benzenedicarboxylic acid (bdc); dabco

SolventsDMF; methanol and DMF washes

Atmospherenot specified

Temperature120

Time48

Work-upSimilar procedure to mixed-metal synthesis; filtered after natural cooling and washed using methanol and DMF for 4 days.

ActivationVacuum drying at 110 C for 12 h, according to shared M2(bdc)2P procedure.

Scalability contextShared solvothermal autoclave route.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Zn(NO3)2.6H2O	not explicitly stated for Zn-only sample	2 · 2.1 Synthesis of pillared Ni-based MOFs
Linker	bdc	not explicitly stated for Zn-only sample	2 · 2.1 Synthesis of pillared Ni-based MOFs
Linker	dabco	not explicitly stated for Zn-only sample	2 · 2.1 Synthesis of pillared Ni-based MOFs
Solvent	DMF	not explicitly stated for Zn-only sample	2 · 2.1 Synthesis of pillared Ni-based MOFs

Complete recipeSource: Main

Route 4: Solvothermal

2 · 2.1 Synthesis of pillared Ni-based MOFs · Fig. 1

Metal precursorsNi(NO3)2.6H2O (1.2 mmol); Zn(NO3)2.6H2O (0.3 mmol)

Linker precursors1,4-benzenedicarboxylic acid (bdc, 1.5 mmol); dabco (0.75 mmol)

SolventsN,N-dimethylformamide (DMF), 30 mL; methanol and DMF washes

Atmospherenot specified

Temperature120

Time48

Work-upNaturally cooled to room temperature, filtered, washed with methanol and DMF for 4 days.

ActivationDried under vacuum at 110 C for 12 h to remove methanol and DMF molecules.

Scalability contextBatch scale stated as 30 mL solution in 50 mL Teflon-lined stainless-steel autoclave.

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Ni(NO3)2.6H2O	1.2 mmol	2 · 2.1 Synthesis of pillared Ni-based MOFs · Fig. 1
Metal Source	Zn(NO3)2.6H2O	0.3 mmol	2 · 2.1 Synthesis of pillared Ni-based MOFs · Fig. 1
Linker	bdc	1.5 mmol	2 · 2.1 Synthesis of pillared Ni-based MOFs · Fig. 1
Linker	dabco	0.75 mmol	2 · 2.1 Synthesis of pillared Ni-based MOFs · Fig. 1
Solvent	N,N-dimethylformamide (DMF)	30 mL	2 · 2.1 Synthesis of pillared Ni-based MOFs · Fig. 1