Synthesis · Multifunctional covalent organic framework with extended π-d conjugated structure for lithium-sulfur batteries

3 structured synthesis routes

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

Complete recipeSource: SI

Route 1: Drop Cast

p002 · Preparation of Ni-COF@PP separator

Metal precursorsNi supplied by pre-synthesised Ni-COF

Linker precursorspre-synthesised Ni-COF

SolventsNMP

AdditivesSuper P carbon; PVDF binder

Atmospherenot stated

Temperature50

Time12

Substrate orientationone side of PP separator (Celgard 2500); discs diameter 16 mm

Oxidant / reductantnone reported

Work-upslurry ground well, coated on PP separator, dried, cut into 16 mm discs

Activationdrying at 50 C for 12 h

Scalability contextDisc size 16 mm; slurry composition reported in wt% but coating loading not reported.

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	Ni-COF	40 wt%	p002 · Preparation of Ni-COF@PP separator
Additive	Super P	40 wt%	p002 · Preparation of Ni-COF@PP separator
Additive	PVDF	20 wt%	p002 · Preparation of Ni-COF@PP separator
Solvent	NMP	not specified	p002 · Preparation of Ni-COF@PP separator
Other	PP separator (Celgard 2500)	cut into 16 mm discs	p002 · Preparation of Ni-COF@PP separator

Complete recipeSource: Both

Route 2: Solvothermal

p002 · Synthesis of Ni-COF

Metal precursorsexcess nickel acetate tetrahydrate (source text: Nickel acetate tetrahydrate / NiOAc.4H2O; main text: Ni(OAc)2.4H2O)

Linker precursorsHBC (166 mg, 1 mmol); TABQ (84 mg, 0.5 mmol)

Solvents10 mL dried NMP; DMF and MeOH for washing

Additivesnone reported

Atmospheresealed Teflon-lined stainless-steel autoclave; no inert atmosphere stated for synthesis

Temperature120

Time72

Oxidant / reductantnone reported

Work-upcool to room temperature; collect black precipitate by filtration; wash with DMF and MeOH several times

Activationdried under vacuum at 80 C overnight

Scalability context25 mL glass bottle transferred into 25 mL Teflon-lined stainless-steel autoclave; batch scale HBC 1 mmol/TABQ 0.5 mmol

Show 6 structured reagent records

Role	Reagent	Amount / concentration	Source
Linker	HBC (2,5-dihydroxyterephthalaldehyde)	166 mg, 1 mmol	p002 · Synthesis of Ni-COF
Linker	TABQ (2,3,5,6-tetraaminobenzoquinone)	84 mg, 0.5 mmol	p002 · Synthesis of Ni-COF
Metal Source	nickel acetate tetrahydrate (NiOAc.4H2O / Ni(OAc)2.4H2O)	excess	p002 · Synthesis of Ni-COF
Solvent	dried NMP	10 mL	p002 · Synthesis of Ni-COF
Solvent	DMF	wash several times	p002 · Synthesis of Ni-COF
Solvent	MeOH	wash several times	p002 · Synthesis of Ni-COF

Complete recipeSource: SI

Route 3: Other

p002 · Preparation of S@SP cathode

Metal precursorsnone

Linker precursorssulfur and Super P carbon

SolventsNMP slurry solvent

AdditivesPVDF binder; additional Super P

Atmospherenot stated for melt diffusion; vacuum oven drying reported

Temperature155; then 60

Time12; then 24 plus further drying

Substrate orientationcarbon-coated Al foil; 12 mm electrode discs

Oxidant / reductantnone reported

Work-upS@SP mixed with SP and PVDF 8:1:1, ground with NMP, coated onto carbon-coated Al foil, dried, cut into discs

Activationvacuum oven at 60 C for 24 h and further dried at 60 C

Scalability contextSulfur loading approximately 1.5 mg cm-2.

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	sulfur	70 wt% in S@SP	p002 · Preparation of S@SP cathode
Additive	Super P	30 wt% in S@SP; later S@SP:SP:PVDF = 8:1:1	p002 · Preparation of S@SP cathode
Additive	PVDF	S@SP:SP:PVDF = 8:1:1	p002 · Preparation of S@SP cathode
Solvent	NMP	gradually added to form slurry	p002 · Preparation of S@SP cathode
Other	carbon-coated Al foil	substrate	p002 · Preparation of S@SP cathode