Synthesis · In situ construction of a dual-metal 2D conjugated metal-organic framework on carbon paper for asymmetric supercapacitors

7 structured synthesis routes

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

Complete recipeSource: Main

Route 1: Other

2 · 2.1. Carbon paper activation treatment

Solventsconcentrated nitric acid; sulfuric acid solution; acetone; anhydrous ethanol; ultrapure water

Additivespotassium dichromate in sulfuric acid solution

Atmospherenot specified

Temperature80 reflux; 70 vacuum dry

Time5 reflux; 3 soak; 12 dry

Substrate orientationhydrophobic carbon paper, 1 x 1.2 cm, 0.2 mm thick

Oxidant / reductantconcentrated nitric acid; potassium dichromate

Work-upcool; transfer to sulfuric acid solution containing potassium dichromate; rinse sequentially with acetone, anhydrous ethanol, and ultrapure water

Activationacid oxidation to hydrophilic carbon paper with oxygen-containing groups

Scalability contextReported on 1 x 1.2 cm carbon paper pieces.

Show 7 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	Toray raw carbon paper TGPH 060	1 x 1.2 cm, 0.2 mm thick	2 · 2.1. Carbon paper activation treatment
Acid	concentrated nitric acid	concentrated	2 · 2.1. Carbon paper activation treatment
Acid	sulfuric acid solution	Not specified	2 · 2.1. Carbon paper activation treatment
Oxidant	potassium dichromate	Not specified	2 · 2.1. Carbon paper activation treatment
Solvent	acetone	Not specified	2 · 2.1. Carbon paper activation treatment
Solvent	anhydrous ethanol	Not specified	2 · 2.1. Carbon paper activation treatment
Solvent	ultrapure water	Not specified	2 · 2.1. Carbon paper activation treatment

Partial recipeSource: Main

Route 2: Hydrothermal

2 · 2.2. Synthesis of M1/M2-HHTP@CP electrode materials

Metal precursorsCo and Cu acetate sources; metal ratio 1:1; exact Co/Cu@CP masses not separately specified

Linker precursorsHHTP, inferred from Co/Ni-HHTP@CP route

Solventsdeionised water, sodium acetate solution, and DMF, inferred similar to Co/Ni-HHTP@CP

Additivessodium acetate solution, inferred

Atmospherenot specified

Temperature85

Time24

Substrate orientationactivated carbon paper immersed in precursor solution

Work-upinferred wash with deionised water and acetone; vacuum dry at 60 C

Activationdry under vacuum at 60 C, inferred

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Co acetate source	not specified for @CP route	2 · 2.2. Synthesis of M1/M2-HHTP@CP electrode materials
Metal Source	Cu acetate source	not specified for @CP route	2 · 2.2. Synthesis of M1/M2-HHTP@CP electrode materials
Linker	HHTP	inferred 14 mg from Co/Ni-HHTP@CP	2 · 2.2. Synthesis of M1/M2-HHTP@CP electrode materials
Other	activated carbon paper	Not specified	2 · 2.2. Synthesis of M1/M2-HHTP@CP electrode materials

Complete recipeSource: SI

Route 3: Solvothermal

Preparation method

Metal precursors10 mg Co(OAc)2.4H2O and 7.8 mg Cu(OAc)2.2H2O; Co/Cu = 1:1

Linker precursors14 mg HHTP

Solvents4 mL deionised water; 1 mL DMF

Atmospherenot specified

Temperature85

Time24

Work-upcool to room temperature; wash sequentially with deionised water and acetone

Activationdry under vacuum at 60 C

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Co(OAc)2.4H2O	10 mg	Preparation method
Metal Source	Cu(OAc)2.2H2O	7.8 mg	Preparation method
Linker	HHTP	14 mg	Preparation method
Solvent	deionized water	4 mL	Preparation method
Solvent	DMF	1 mL	Preparation method

Complete recipeSource: Main

Route 4: Hydrothermal

2 · 2.2. Synthesis of M1/M2-HHTP@CP electrode materials

Metal precursors10 mg Co(OAc)2.4H2O and 10 mg Ni(OAc)2.4H2O; Co/Ni = 1:1

Linker precursors14 mg HHTP

Solvents4 mL deionised water; 1 mL DMF; 4 mL sodium acetate solution

Additivessodium acetate solution, 4 mol L-1

Atmospherenot specified

Temperature85

Time24

Substrate orientationactivated carbon paper immersed in the metal precursor solution

Work-upcool to room temperature; remove carbon paper; wash sequentially with deionised water and acetone

Activationdry under vacuum at 60 C

Scalability contextDirect binder-free electrode growth on 1 x 1.2 cm carbon paper.

Show 7 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Co(OAc)2.4H2O	10 mg	2 · 2.2. Synthesis of M1/M2-HHTP@CP electrode materials
Metal Source	Ni(OAc)2.4H2O	10 mg	2 · 2.2. Synthesis of M1/M2-HHTP@CP electrode materials
Linker	HHTP	14 mg	2 · 2.2. Synthesis of M1/M2-HHTP@CP electrode materials
Solvent	deionized water	4 mL	2 · 2.2. Synthesis of M1/M2-HHTP@CP electrode materials
Base	sodium acetate solution	4 mL · 4 mol L-1	2 · 2.2. Synthesis of M1/M2-HHTP@CP electrode materials
Solvent	DMF	1 mL	2 · 2.2. Synthesis of M1/M2-HHTP@CP electrode materials
Other	activated carbon paper	Not specified	2 · 2.2. Synthesis of M1/M2-HHTP@CP electrode materials

Complete recipeSource: SI

Route 5: Solvothermal

Preparation method

Metal precursors10 mg Co(OAc)2.4H2O and 10 mg Ni(OAc)2.4H2O; Co/Ni = 1:1

Linker precursors14 mg HHTP

Solvents5.5 mL deionised water; 0.15 mL DMF

Atmospherenot specified

Temperature85

Time24

Work-upcool to room temperature; wash sequentially with deionised water and acetone

Activationdry under vacuum at 60 C

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Co(OAc)2.4H2O	10 mg	Preparation method
Metal Source	Ni(OAc)2.4H2O	10 mg	Preparation method
Linker	HHTP	14 mg	Preparation method
Solvent	deionized water	5.5 mL	Preparation method
Solvent	DMF	0.15 mL	Preparation method

Partial recipeSource: Main

Route 6: Hydrothermal

2 · 2.2. Synthesis of M1/M2-HHTP@CP electrode materials

Metal precursorsCu and Ni acetate sources; metal ratio 1:1; exact Cu/Ni@CP masses not separately specified

Linker precursorsHHTP, inferred from Co/Ni-HHTP@CP route

Solventsdeionised water, sodium acetate solution, and DMF, inferred similar to Co/Ni-HHTP@CP

Additivessodium acetate solution, inferred

Atmospherenot specified

Temperature85

Time24

Substrate orientationactivated carbon paper immersed in precursor solution

Work-upinferred wash with deionised water and acetone; vacuum dry at 60 C

Activationdry under vacuum at 60 C, inferred

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Cu acetate source	not specified for @CP route	2 · 2.2. Synthesis of M1/M2-HHTP@CP electrode materials
Metal Source	Ni acetate source	not specified for @CP route	2 · 2.2. Synthesis of M1/M2-HHTP@CP electrode materials
Linker	HHTP	inferred 14 mg from Co/Ni-HHTP@CP	2 · 2.2. Synthesis of M1/M2-HHTP@CP electrode materials
Other	activated carbon paper	Not specified	2 · 2.2. Synthesis of M1/M2-HHTP@CP electrode materials

Complete recipeSource: SI

Route 7: Solvothermal

Preparation method

Metal precursors10 mg Ni(OAc)2.4H2O and 7.8 mg Cu(OAc)2.2H2O; Cu/Ni = 1:1

Linker precursors14 mg HHTP

Solvents4 mL deionised water; 1 mL DMF

Atmospherenot specified

Temperature85

Time24

Work-upcool to room temperature; wash sequentially with deionised water and acetone

Activationdry under vacuum at 60 C

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Ni(OAc)2.4H2O	10 mg	Preparation method
Metal Source	Cu(OAc)2.2H2O	7.8 mg	Preparation method
Linker	HHTP	14 mg	Preparation method
Solvent	deionized water	4 mL	Preparation method
Solvent	DMF	1 mL	Preparation method