Synthesis · Exposing {001} Crystal Plane on Hexagonal Ni-MOF with Surface-Grown Cross-Linked Mesh-Structures for Electrochemical Energy Storage

5 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

5 · 1.4 Electrochemical measurements

Additivesactivated carbon; acetylene black; polytetrafluoroethylene

Atmosphereroom temperature electrochemical testing; atmosphere not specified

Substrate orientationfoamed nickel foam substrate, approx. 1 cm2

Work-uppositive and negative electrode slurries coated on nickel foam and pressed at 10 MPa

Scalability contextPositive/negative active material mass ratio 1:4.

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	hexagonal Ni-MOF	positive electrode active material	5 · 1.4 Electrochemical measurements
Other	activated carbon	negative electrode active material	5 · 1.4 Electrochemical measurements
Additive	acetylene black	15 wt parts in 80:15:5 electrode mixture	5 · 1.4 Electrochemical measurements
Additive	polytetrafluoroethylene	5 wt parts in 80:15:5 electrode mixture	5 · 1.4 Electrochemical measurements
Electrolyte	KOH aqueous solution	3.0 M	5 · 1.4 Electrochemical measurements

Partial recipeSource: Main

Route 2: Solvothermal

2 · Results and Discussion · Scheme S1

Metal precursorsnickel nitrate hexahydrate, amount scaled in growth study

Linker precursorsH3BTC and 4,4'-bipy, amount scaled in growth study

SolventsDMF

Atmospherenot specified

Temperature80

Time18

Work-upnot separately stated for amount-series samples

Scalability contextReactant amount was varied over 0.375, 0.75, and 1.5 mmol to probe growth.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	nickel nitrate hexahydrate	0.375, 0.75, or 1.5 mmol in growth study	2 · Results and Discussion · Scheme S1
Linker	H3BTC	0.375, 0.75, or 1.5 mmol in growth study	2 · Results and Discussion · Scheme S1
Linker	4,4'-bipy	0.375, 0.75, or 1.5 mmol in growth study	2 · Results and Discussion · Scheme S1
Solvent	DMF	Not specified	2 · Results and Discussion · Scheme S1

Complete recipeSource: SI

Route 3: Other

5 · 1.4 Electrochemical measurements

Additivesacetylene black; polytetrafluoroethylene

Atmosphereroom temperature electrochemical preparation/testing; atmosphere not specified

Substrate orientationfoamed nickel foam substrate, approx. 1 cm2

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

Scalability contextTypical active material mass loading 1.0 mg.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	hexagonal Ni-MOF	80 wt parts in 80:15:5 mixture	5 · 1.4 Electrochemical measurements
Additive	acetylene black	15 wt parts in 80:15:5 mixture	5 · 1.4 Electrochemical measurements
Additive	polytetrafluoroethylene	5 wt parts in 80:15:5 mixture	5 · 1.4 Electrochemical measurements
Other	foamed nickel foam	approx. 1 cm2 piece	5 · 1.4 Electrochemical measurements

Partial recipeSource: Both

Route 4: Solvothermal

3 · Results and Discussion · Figure 1

Metal precursorsnickel nitrate hexahydrate

Linker precursorsH3BTC and 4,4'-bipy

SolventsDMF

Atmospherenot specified

Temperature80

Time6, 12, 24, and 30 for Y1, Y2, Y4, and Y5; Y3 is 18 h

Work-uppresumed as base SI workup; not separately stated for each time variant

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	nickel nitrate hexahydrate	Not specified	3 · Results and Discussion · Figure 1
Linker	H3BTC	Not specified	3 · Results and Discussion · Figure 1
Linker	4,4'-bipy	Not specified	3 · Results and Discussion · Figure 1
Solvent	DMF	Not specified	3 · Results and Discussion · Figure 1

Complete recipeSource: Both

Route 5: Solvothermal

4 · 1.2 Synthesis of the hexagonal Ni-MOF

Metal precursorsNi(NO3)2.6H2O (0.4362 g, 1.5 mmol)

Linker precursorsH3BTC (0.3165 g, 1.5 mmol); 4,4'-bipy (0.288 g, 1.5 mmol)

Solvents60 mL DMF

Atmospherenot specified

Temperature80

Time18

Work-upcooled to room temperature; washed thoroughly with DMF and ethanol; dried in air naturally

Scalability context100 mL Teflon-lined autoclave; batch solvothermal reaction.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Ni(NO3)2.6H2O	0.4362 g, 1.5 mmol	4 · 1.2 Synthesis of the hexagonal Ni-MOF
Linker	H3BTC	0.3165 g, 1.5 mmol	4 · 1.2 Synthesis of the hexagonal Ni-MOF
Linker	4,4'-bipy	0.288 g, 1.5 mmol	4 · 1.2 Synthesis of the hexagonal Ni-MOF
Solvent	DMF	60 mL	4 · 1.2 Synthesis of the hexagonal Ni-MOF