Synthesis · Hierarchical 3D micro-nanostructures based on in situ deposited bimetallic metal-organic structures on carbon fabric for supercapacitor applications

5 structured synthesis routes

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

Partial recipeSource: Both

Route 1: Solvothermal

p002 / article p6032 · Methods

Metal precursorsnickel(II) nitrate hexahydrate; amount follows same procedure but is not restated for NMF

Linker precursorsBTC/trimesic acid; amount follows same procedure but is not restated for NMF

SolventsDI water/DMF/ethanol, same as NZMF route

Additivesnone stated

Atmospherenot stated

Temperature170

Time6

Substrate orientationnot applicable

Oxidant / reductantnone stated

Work-upsame as NZMF route: centrifuge, DI water/ethanol wash, dry at 100 C for 10 h

Activationdrying at 100 C for 10 h; no separate activation stated

Scalability contextnone stated for NMF control

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	nickel(II) nitrate hexahydrate	same as NZMF procedure; exact amount for NMF not separately restated	p002 / article p6032 · Methods
Linker	BTC / trimesic acid	same as NZMF procedure; exact amount for NMF not separately restated	p002 / article p6032 · Methods
Solvent	DI water/DMF/ethanol	same as NZMF procedure	p002 / article p6032 · Methods

Complete recipeSource: Both

Route 2: Solvothermal

p002 / article p6032 · Methods

Metal precursors137 mg nickel(II) nitrate hexahydrate and 137 mg zinc nitrate hexahydrate

Linker precursors103 mg BTC/trimesic acid

SolventsDI water/DMF/ethanol, 70:70:70 mL total 210 mL; 130 mL solution A, 80 mL solution B

Additivescarbon fabric substrate added to solution B

Atmospherenot stated

Temperature170

Time6

Substrate orientationCF added to solution B before dropwise addition of solution A; orientation not stated

Oxidant / reductantnone stated

Work-upcentrifugation at 8000 rpm, washing with DI water and ethanol, drying at 100 C for 10 h

Activationdrying at 100 C for 10 h; no separate activation stated

Scalability contextDirect in situ growth on CF is described as binder-free and scalable; actual substrate mass/loading not fully reported.

Show 7 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	nickel(II) nitrate hexahydrate	137 mg	p002 / article p6032 · Methods
Metal Source	zinc nitrate hexahydrate	137 mg	p002 / article p6032 · Methods
Linker	BTC / trimesic acid	103 mg	p002 / article p6032 · Methods
Solvent	DI water	70 mL in 210 mL solvent mixture	p002 / article p6032 · Methods
Solvent	DMF	70 mL in 210 mL solvent mixture	p002 / article p6032 · Methods
Solvent	ethanol	70 mL in 210 mL solvent mixture	p002 / article p6032 · Methods
Additive	carbon fabric	amount not stated	p002 / article p6032 · Methods

Complete recipeSource: SI

Route 3: Drop Cast

SI · 1.3 Electrochemical measurements

Metal precursorspre-synthesised NZMF active material

Linker precursorspre-synthesised NZMF active material

Solventsethanol 10 uL; cleaned CF sonicated in DI water, ethanol, and acetone

AdditivesNafion 2.5 uL binder

Atmosphereair/oven atmosphere not stated

Temperature90

Time12

Substrate orientationcarbon fabric 2 x 3 cm, 0.3 mm thick; slurry covered onto cleaned CF

Oxidant / reductantnone stated

Work-upsequential ultrasonic cleaning of CF in DI water, ethanol and acetone for 1 h; slurry drop casting; oven drying

Activationoven drying at 90 C for 12 h

Scalability contextcontrol electrode preparation only

Show 6 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	NZMF active material	1.5 mg	SI · 1.3 Electrochemical measurements
Additive	Nafion	2.5 uL	SI · 1.3 Electrochemical measurements
Solvent	ethanol	10 uL	SI · 1.3 Electrochemical measurements
Other	carbon fabric	2 x 3 cm, 0.3 mm thickness	SI · 1.3 Electrochemical measurements
Solvent	DI water	cleaning solvent	SI · 1.3 Electrochemical measurements
Solvent	acetone	cleaning solvent	SI · 1.3 Electrochemical measurements

Complete recipeSource: Both

Route 4: Solvothermal

p002 / article p6032 · Methods

Metal precursors137 mg nickel(II) nitrate hexahydrate and 137 mg zinc nitrate hexahydrate

Linker precursors103 mg BTC/trimesic acid

SolventsDI water/DMF/ethanol, 70:70:70 mL total 210 mL; 130 mL used for solution A and 80 mL for solution B

Additivesnone stated

Atmospherenot stated

Temperature170

Time6

Substrate orientationnot applicable; no CF for powder NZMF

Oxidant / reductantnone stated

Work-upcentrifuged at 8000 rpm; washed several times with DI water and ethanol; dried at 100 C for 10 h

Activationdrying at 100 C for 10 h; no separate activation stated

Scalability contextAuthors call the synthesis scalable for growth of NZMF on CF; no batch scale beyond stated masses/volumes.

Show 6 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	nickel(II) nitrate hexahydrate	137 mg	p002 / article p6032 · Methods
Metal Source	zinc nitrate hexahydrate	137 mg	p002 / article p6032 · Methods
Linker	BTC / trimesic acid	103 mg	p002 / article p6032 · Methods
Solvent	DI water	70 mL in 210 mL solvent mixture	p002 / article p6032 · Methods
Solvent	DMF	70 mL in 210 mL solvent mixture	p002 / article p6032 · Methods
Solvent	ethanol	70 mL in 210 mL solvent mixture	p002 / article p6032 · Methods

Partial recipeSource: SI

Route 5: Other

SI · 1.4 Preparation of gel electrolyte

Metal precursorsNZMF/CF positive electrode

Linker precursorsNZMF/CF positive electrode contains BTC linker

SolventsDI water for PVA/KOH gel preparation; slurry solvent not fully stated for AC/PVDF/Nafion negative electrode

AdditivesPVA/KOH gel electrolyte, activated carbon, PVDF, Nafion, filter paper separator

Atmospherenot stated

Temperature90

Time1

Substrate orientation12 mm diameter NZMF/CF working electrode; activated carbon/PVDF/Nafion slurry on nickel foam negative electrode

Oxidant / reductantKOH electrolyte

Work-upPVA dissolved in water at 90 C; KOH solution dropped into PVA with stirring; cooled to room temperature; device assembled with filter paper separator

Activationgel electrolyte cooled to room temperature before use

Scalability contextdevice fabrication described for 12 mm electrode only

Show 9 structured reagent records

Role	Reagent	Amount / concentration	Source
Electrolyte	polyvinyl alcohol	3 g	SI · 1.4 Preparation of gel electrolyte
Electrolyte	KOH	3 g	SI · 1.4 Preparation of gel electrolyte
Solvent	DI water	24 mL for PVA plus 6 mL for KOH	SI · 1.4 Preparation of gel electrolyte
Other	NZMF/CF	12 mm diameter electrode	SI · 1.4 Preparation of gel electrolyte
Other	activated carbon	95:5 with PVDF	SI · 1.4 Preparation of gel electrolyte
Additive	PVDF	95:5 with activated carbon	SI · 1.4 Preparation of gel electrolyte
Additive	Nafion	3 uL	SI · 1.4 Preparation of gel electrolyte
Other	nickel foam	negative electrode substrate	SI · 1.4 Preparation of gel electrolyte
Other	filter paper	separator	SI · 1.4 Preparation of gel electrolyte