Synthesis · In-situ growth of electrically conductive MOFs in wood cellulose scaffold for flexible, robust and hydrophobic membranes with improved electrochemical performance

6 structured synthesis routes

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

Blocked Missing Si recipeSource: Missing SI

Route 1: Hydrothermal

p002 / journal page 2 · 2.3 Preparation of NiCAT@TOW composite membrane

Metal precursorsCu(NO3)2.H2O pretreatment and Cu(CH3COO)2.H2O growth salt likely from materials list and same-as statement

Linker precursorsHHTP

SolventsDMF and water likely from same-as NiCAT@TOW statement

Atmospherenot reported

Temperature85 likely by same-as statement

Timenot fully specified locally

Substrate orientationTOW scaffold

Scalability contextCuCAT@TOW was used to test generality of the EC-MOF@wood strategy.

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Cu(NO3)2.H2O	listed in materials; control concentration not locally specified	p002 / journal page 2 · 2.3 Preparation of NiCAT@TOW composite membrane
Metal Source	Cu(CH3COO)2.H2O	listed in materials; growth amount not locally specified	p002 / journal page 2 · 2.3 Preparation of NiCAT@TOW composite membrane
Linker	HHTP	same-as NiCAT route implied but not SI-verified	p002 / journal page 2 · 2.3 Preparation of NiCAT@TOW composite membrane

Partial recipeSource: Main

Route 2: Hydrothermal

p008 / journal page 8 · 3.3 Electrochemical properties of EC-MOF@TOW membrane · Fig. 6b

Metal precursors50 wt% Ni2+ treatment

Linker precursorsHHTP assumed from NiCAT growth protocol

SolventsDMF and water assumed from NiCAT growth protocol

Atmospherenot reported

Temperature85 assumed from NiCAT@TOW protocol

Timenot fully specified for control

Substrate orientationdelignified wood without TEMPO oxidation

Partial recipeSource: Main

Route 3: Other

p009 / journal page 9 · 3.3 Electrochemical properties of EC-MOF@TOW membrane

Additivespolymer binder

Substrate orientationcarbon paper current collector

Work-upcoated onto carbon paper

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	NiCAT powder	Not specified	p009 / journal page 9 · 3.3 Electrochemical properties of EC-MOF@TOW membrane
Additive	polymer binder	Not specified	p009 / journal page 9 · 3.3 Electrochemical properties of EC-MOF@TOW membrane
Other	carbon paper	Not specified	p009 / journal page 9 · 3.3 Electrochemical properties of EC-MOF@TOW membrane

Blocked Missing Si recipeSource: Missing SI

Route 4: Hydrothermal

p005 / journal page 5 · 3.1 Preparation of EC-MOF@TOW membrane · Fig. 2f

Metal precursorsnot specified in main text

Linker precursorsnot specified in main text; HHTP is the NiCAT linker in the material

Solventsnot specified in main text

Partial recipeSource: Main

Route 5: Hydrothermal

p002 / journal page 2 · 2.3 Preparation of NiCAT@TOW composite membrane

Metal precursors50 wt% Ni(NO3)2.6H2O pretreatment; Ni(CH3COO)2.4H2O growth salt

Linker precursorsHHTP

SolventsDMF and deionized water

Atmospherenot reported

Temperature85

Time6 h Ni2+ pretreatment; 24 h EC-MOF growth; 48 h humidification; 48 h pressing

Substrate orientationTOW scaffold, 20 mm x 15 mm x 1 mm original oxidised wood pieces, fibre-aligned wood scaffold

Work-upwash TOW-Ni2+-A% with deionized water to remove nitrate ions; wash A%-NiCAT@TOW bulk with water and acetone in turn

Activation98% relative humidity for 48 h followed by 10 MPa room-temperature pressing for 48 h

Scalability contextFacile in-situ growth on wood scaffold followed by room-temperature compression; same method used for 1%, 5%, 10% and 50% Ni salt series.

Show 6 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Ni(NO3)2.6H2O	50 wt% aqueous metallic salt solution	p002 / journal page 2 · 2.3 Preparation of NiCAT@TOW composite membrane
Linker	HHTP	0.4 mmol	p002 / journal page 2 · 2.3 Preparation of NiCAT@TOW composite membrane
Solvent	DMF	2 mL	p002 / journal page 2 · 2.3 Preparation of NiCAT@TOW composite membrane
Solvent	deionized water	8 mL for HHTP solution; 10 mL for Ni acetate solution	p002 / journal page 2 · 2.3 Preparation of NiCAT@TOW composite membrane
Metal Source	Ni(CH3COO)2.4H2O	0.8 mmol	p002 / journal page 2 · 2.3 Preparation of NiCAT@TOW composite membrane
Solvent	water and acetone	wash solvents	p002 / journal page 2 · 2.3 Preparation of NiCAT@TOW composite membrane

Partial recipeSource: Main

Route 6: Other

p002 / journal page 2 · 2.2 Preparation of TEMPO oxidized Balsa wood substrate (TOW)

Solventswater; absolute ethanol

AdditivesNaClO2/acetate buffer; TEMPO; NaBr; NaOH

Temperature80 for delignification; vacuum freeze-drying after oxidation

Time9 h delignification; 6 h TEMPO oxidation

Substrate orientationbalsa wood samples cut to 20 mm x 15 mm x 1 mm

Oxidant / reductantNaClO2 for delignification; NaClO/TEMPO/NaBr oxidation system

Work-upstored in absolute ethanol; oxidised samples washed with deionized water three times and vacuum freeze-dried

Activationnone reported

Scalability contextUses top-down balsa wood scaffold processing and simple aqueous oxidation.

Show 8 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	balsa wood (Ochroma pyramidale)	20 mm x 15 mm x 1 mm DW samples	p002 / journal page 2 · 2.2 Preparation of TEMPO oxidized Balsa wood substrate (TOW)
Oxidant	sodium chlorite (NaClO2)	1 wt% in acetate buffer, pH 4.6	p002 / journal page 2 · 2.2 Preparation of TEMPO oxidized Balsa wood substrate (TOW)
Additive	TEMPO	0.032 g	p002 / journal page 2 · 2.2 Preparation of TEMPO oxidized Balsa wood substrate (TOW)
Additive	NaBr	0.2 g	p002 / journal page 2 · 2.2 Preparation of TEMPO oxidized Balsa wood substrate (TOW)
Solvent	deionized water	200 mL	p002 / journal page 2 · 2.2 Preparation of TEMPO oxidized Balsa wood substrate (TOW)
Base	NaOH	pH adjusted/maintained at 10 · 0.1 mol L-1 for adjustment; 1 mol L-1 added during oxidation	p002 / journal page 2 · 2.2 Preparation of TEMPO oxidized Balsa wood substrate (TOW)
Oxidant	NaClO	20 mmol · 10% available chlorine reagent	p002 / journal page 2 · 2.2 Preparation of TEMPO oxidized Balsa wood substrate (TOW)
Other	absolute ethanol	added to stop oxidation	p002 / journal page 2 · 2.2 Preparation of TEMPO oxidized Balsa wood substrate (TOW)