Synthesis · Self-assembled Mo doped Ni-MOF nanosheets based electrode material for high performance battery-supercapacitor hybrid device

10 structured synthesis routes

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

Partial recipeSource: SI

Route 1: Other

SI text p.1 · Electrochemical Measurements

AdditivesAcetylene black and PTFE binder; same electrode sheet method as positive electrode.

AtmosphereNot specified; electrochemical tests at room temperature in 3 M KOH.

Temperatureroom temperature electrode fabrication/test; no drying temperature reported for coated electrode

Timenot reported

Substrate orientationNickel foam current collector.

Work-upPrepare activated-carbon electrode sheet by the same method as the positive electrode.

ActivationNo electrode activation step reported before testing.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	activated carbon (AC)	1.7 mg active material mass	SI text p.1 · Electrochemical Measurements
Additive	acetylene black	same 8:1.5:0.5 electrode-sheet method as positive electrode	SI text p.1 · Electrochemical Measurements
Additive	poly(tetrafluoroethylene) (PTFE)	same 8:1.5:0.5 electrode-sheet method as positive electrode	SI text p.1 · Electrochemical Measurements
Other	nickel foam current collector	not separately specified for AC electrode	SI text p.1 · Electrochemical Measurements

Partial recipeSource: Both

Route 2: Other

main p.8, article p.20827 · Battery-supercapacitor hybrid device · Fig. 7

Metal precursorsM-NMN-1 positive electrode from hydrothermal Mo-doped Ni-MOF route.

Linker precursors4,4-bipyridine present in M-NMN-1 positive electrode component.

Solvents3 M KOH aqueous electrolyte.

AdditivesActivated carbon negative electrode; charge-balanced positive/negative mass ratio R = 0.47.

AtmosphereNot specified; device tested at room temperature.

Temperatureroom temperature test; assembly temperature not reported

Timenot reported

Substrate orientationTwo-electrode battery-supercapacitor hybrid device; separator/current-collector stack not described.

Work-upAssemble M-NMN-1 positive electrode with AC negative electrode using charge balance; test in 3 M KOH.

ActivationNo separate activation step reported; main text notes capacitance retention slightly increases before 5000 cycles due to electrode activation during cycling.

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	M-NMN-1 positive electrode	mass ratio R positive:negative = 0.47	main p.8, article p.20827 · Battery-supercapacitor hybrid device · Fig. 7
Other	activated carbon negative electrode	negative active material mass 1.7 mg reported in SI	main p.8, article p.20827 · Battery-supercapacitor hybrid device · Fig. 7
Electrolyte	KOH aqueous electrolyte	not reported · 3 M	main p.8, article p.20827 · Battery-supercapacitor hybrid device · Fig. 7

Partial recipeSource: SI

Route 3: Other

SI text p.1 · Electrochemical Measurements

Metal precursorsHydrothermally synthesised M-NMN-1 active material from the corresponding Ni-MOF/M-NMN route.

AdditivesAcetylene black and poly(tetrafluoroethylene) (PTFE) binder; active material:acetylene black:PTFE = 8:1.5:0.5.

AtmosphereNot specified; electrochemical tests at room temperature in 3 M KOH.

Temperatureroom temperature electrode fabrication/test; no drying temperature reported for coated electrode

Timenot reported

Substrate orientationNickel foam current collector, 1 x 2 cm2; coating area 1 x 1 cm2.

Work-upMix active material with acetylene black and PTFE, coat on nickel foam current collector.

ActivationNo electrode activation step reported before testing.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	M-NMN-1	0.8 mg active substance on electrode	SI text p.1 · Electrochemical Measurements
Additive	acetylene black	1.5 parts by mass relative to 8 parts active material	SI text p.1 · Electrochemical Measurements
Additive	poly(tetrafluoroethylene) (PTFE)	0.5 parts by mass relative to 8 parts active material	SI text p.1 · Electrochemical Measurements
Other	nickel foam current collector	1 x 2 cm2; coating area 1 x 1 cm2	SI text p.1 · Electrochemical Measurements

Partial recipeSource: Both

Route 4: Hydrothermal

main p.2, article p.20821 · Experimental section

Metal precursorsNiCl2.6H2O and Na2MoO4.2H2O; Ni:Mo feed ratio 1:1.

Linker precursors4,4'-bipyridine, 1.56 g.

Solvents100 mL deionized water; ethanol and water washes.

AtmosphereNot specified.

Temperature150 reaction; 65 drying

Time72 reaction; drying time not specified

Work-upCool to room temperature, collect by suction filtration, wash with ethanol and water.

ActivationDried at 65 C.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	NiCl2.6H2O	not reported	main p.2, article p.20821 · Experimental section
Metal Source	Na2MoO4.2H2O	not reported; Ni:Mo = 1:1 feed	main p.2, article p.20821 · Experimental section
Linker	4,4'-bipyridine	1.56 g	main p.2, article p.20821 · Experimental section
Solvent	deionized water	100 mL	main p.2, article p.20821 · Experimental section

Partial recipeSource: SI

Route 5: Other

SI text p.1 · Electrochemical Measurements

Metal precursorsHydrothermally synthesised M-NMN-2 active material from the corresponding Ni-MOF/M-NMN route.

AdditivesAcetylene black and poly(tetrafluoroethylene) (PTFE) binder; active material:acetylene black:PTFE = 8:1.5:0.5.

AtmosphereNot specified; electrochemical tests at room temperature in 3 M KOH.

Temperatureroom temperature electrode fabrication/test; no drying temperature reported for coated electrode

Timenot reported

Substrate orientationNickel foam current collector, 1 x 2 cm2; coating area 1 x 1 cm2.

Work-upMix active material with acetylene black and PTFE, coat on nickel foam current collector.

ActivationNo electrode activation step reported before testing.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	M-NMN-2	0.8 mg active substance on electrode	SI text p.1 · Electrochemical Measurements
Additive	acetylene black	1.5 parts by mass relative to 8 parts active material	SI text p.1 · Electrochemical Measurements
Additive	poly(tetrafluoroethylene) (PTFE)	0.5 parts by mass relative to 8 parts active material	SI text p.1 · Electrochemical Measurements
Other	nickel foam current collector	1 x 2 cm2; coating area 1 x 1 cm2	SI text p.1 · Electrochemical Measurements

Partial recipeSource: Both

Route 6: Hydrothermal

main p.2, article p.20821 · Experimental section

Metal precursorsNiCl2.6H2O and Na2MoO4.2H2O; Ni:Mo feed ratio 1:2.

Linker precursors4,4'-bipyridine, 1.56 g.

Solvents100 mL deionized water; ethanol and water washes.

AtmosphereNot specified.

Temperature150 reaction; 65 drying

Time72 reaction; drying time not specified

Work-upCool to room temperature, collect by suction filtration, wash with ethanol and water.

ActivationDried at 65 C.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	NiCl2.6H2O	not reported	main p.2, article p.20821 · Experimental section
Metal Source	Na2MoO4.2H2O	not reported; Ni:Mo = 1:2 feed	main p.2, article p.20821 · Experimental section
Linker	4,4'-bipyridine	1.56 g	main p.2, article p.20821 · Experimental section
Solvent	deionized water	100 mL	main p.2, article p.20821 · Experimental section

Partial recipeSource: SI

Route 7: Other

SI text p.1 · Electrochemical Measurements

Metal precursorsHydrothermally synthesised M-NMN-3 active material from the corresponding Ni-MOF/M-NMN route.

AdditivesAcetylene black and poly(tetrafluoroethylene) (PTFE) binder; active material:acetylene black:PTFE = 8:1.5:0.5.

AtmosphereNot specified; electrochemical tests at room temperature in 3 M KOH.

Temperatureroom temperature electrode fabrication/test; no drying temperature reported for coated electrode

Timenot reported

Substrate orientationNickel foam current collector, 1 x 2 cm2; coating area 1 x 1 cm2.

Work-upMix active material with acetylene black and PTFE, coat on nickel foam current collector.

ActivationNo electrode activation step reported before testing.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	M-NMN-3	0.8 mg active substance on electrode	SI text p.1 · Electrochemical Measurements
Additive	acetylene black	1.5 parts by mass relative to 8 parts active material	SI text p.1 · Electrochemical Measurements
Additive	poly(tetrafluoroethylene) (PTFE)	0.5 parts by mass relative to 8 parts active material	SI text p.1 · Electrochemical Measurements
Other	nickel foam current collector	1 x 2 cm2; coating area 1 x 1 cm2	SI text p.1 · Electrochemical Measurements

Partial recipeSource: Both

Route 8: Hydrothermal

main p.2, article p.20821 · Experimental section

Metal precursorsNiCl2.6H2O and Na2MoO4.2H2O; Ni:Mo feed ratio 1:3.

Linker precursors4,4'-bipyridine, 1.56 g.

Solvents100 mL deionized water; ethanol and water washes.

AtmosphereNot specified.

Temperature150 reaction; 65 drying

Time72 reaction; drying time not specified

Work-upCool to room temperature, collect by suction filtration, wash with ethanol and water.

ActivationDried at 65 C.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	NiCl2.6H2O	not reported	main p.2, article p.20821 · Experimental section
Metal Source	Na2MoO4.2H2O	not reported; Ni:Mo = 1:3 feed	main p.2, article p.20821 · Experimental section
Linker	4,4'-bipyridine	1.56 g	main p.2, article p.20821 · Experimental section
Solvent	deionized water	100 mL	main p.2, article p.20821 · Experimental section

Partial recipeSource: SI

Route 9: Other

SI text p.1 · Electrochemical Measurements

Metal precursorsHydrothermally synthesised Ni-MOF active material from the corresponding Ni-MOF/M-NMN route.

AdditivesAcetylene black and poly(tetrafluoroethylene) (PTFE) binder; active material:acetylene black:PTFE = 8:1.5:0.5.

AtmosphereNot specified; electrochemical tests at room temperature in 3 M KOH.

Temperatureroom temperature electrode fabrication/test; no drying temperature reported for coated electrode

Timenot reported

Substrate orientationNickel foam current collector, 1 x 2 cm2; coating area 1 x 1 cm2.

Work-upMix active material with acetylene black and PTFE, coat on nickel foam current collector.

ActivationNo electrode activation step reported before testing.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	Ni-MOF	0.8 mg active substance on electrode	SI text p.1 · Electrochemical Measurements
Additive	acetylene black	1.5 parts by mass relative to 8 parts active material	SI text p.1 · Electrochemical Measurements
Additive	poly(tetrafluoroethylene) (PTFE)	0.5 parts by mass relative to 8 parts active material	SI text p.1 · Electrochemical Measurements
Other	nickel foam current collector	1 x 2 cm2; coating area 1 x 1 cm2	SI text p.1 · Electrochemical Measurements

Partial recipeSource: Both

Route 10: Hydrothermal

main p.2, article p.20821 · Experimental section · Scheme 1

Metal precursorsNiCl2.6H2O; Ni:Mo feed ratio 1:0.

Linker precursors4,4'-bipyridine, 1.56 g.

Solvents100 mL deionized water; ethanol and water washes.

AtmosphereNot specified.

Temperature150 reaction; 65 drying

Time72 reaction; drying time not specified

Work-upCool to room temperature, collect by suction filtration, wash with ethanol and water.

ActivationDried at 65 C.

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	NiCl2.6H2O	not reported	main p.2, article p.20821 · Experimental section · Scheme 1
Linker	4,4'-bipyridine	1.56 g	main p.2, article p.20821 · Experimental section · Scheme 1
Solvent	deionized water	100 mL	main p.2, article p.20821 · Experimental section · Scheme 1