Synthesis · 2D Tetrathiafulvalene-Based Metal–Organic Framework Linked by Hydrogen Bonding for Boosting Long-Cycle Stability of Lithium-Ion Batteries

2 structured synthesis routes

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

Partial recipeSource: Main

Route 1: Other

main p.6 · Electrochemical Tests

SolventsElectrolyte and washing solvents as reported in methods: NaClO4 in 1:1 propylene carbonate/ethylene carbonate with 5 vol% fluoroethylene carbonate; DMC and acetone for washing recycled battery.

AdditivesSuper P conductive agent is discussed as causing partial irreversible capacity; PVDF and NMP appear in SI reagent table, but active-material/carbon/binder ratio is not reported.

AtmosphereGlovebox filled with high-purity argon (99.99%), H2O < 0.05 ppm and O2 < 0.05 ppm.

Temperature80

Time10

Work-upDried for 10 h in vacuum at 80 C, assembled in glovebox, rested for 10 h before constant-current charge-discharge; recycled battery washed with DMC and acetone.

ActivationPrelithiation for full-cell test: half cell cycled at 1 A g^-1 for three cycles.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Electrolyte	NaClO4	1.0 M	main p.6 · Electrochemical Tests
Solvent	propylene carbonate (PC) and ethylene carbonate (EC)	1:1 by volume	main p.6 · Electrochemical Tests
Additive	fluoroethylene carbonate (FEC)	5 vol%	main p.6 · Electrochemical Tests
Other	glass fiber separator (Whatman GF/D)	Not specified	main p.6 · Electrochemical Tests

Complete recipeSource: Both

Route 2: Solvothermal

main p.2 · 2.1. Synthesis · SI Table S1

Metal precursorsCo(NO3)2*6H2O (8.70 mg, 0.03 mmol) in H2O (0.5 mL).

Linker precursorsH4TTFTB / m-H4-TTFTB (6.80 mg, 0.01 mmol) in DMF (0.8 mL); ligand prepared according to reported method and checked by NMR in SI Figures S1-S2.

SolventsDMF (0.8 mL), H2O (0.5 mL), ethanol (0.26 mL).

AdditivesEthanol added after combining H4TTFTB/DMF and Co(NO3)2*6H2O/H2O solutions.

AtmosphereAir/ambient atmosphere not explicitly specified for the sealed/heated synthesis; dried in air after washing.

Temperature75

Time96

Work-upOven power turned off and mixture naturally cooled to room temperature; red-black crystals filtered, washed with DMF and ethanol, and dried in air.

ActivationSeparate PXRD stability test used activation at 200 C for 2 h.

Scalability contextSmall-batch recipe: 0.01 mmol linker; yield about 56.0% calculated from Co.

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Linker	H4TTFTB / m-H4-TTFTB	6.80 mg, 0.01 mmol	main p.2 · 2.1. Synthesis · SI Table S1
Metal Source	*Co(NO3)26H2O**	8.70 mg, 0.03 mmol	main p.2 · 2.1. Synthesis · SI Table S1
Solvent	N,N-dimethylformamide (DMF)	0.8 mL	main p.2 · 2.1. Synthesis · SI Table S1
Solvent	H2O	0.5 mL	main p.2 · 2.1. Synthesis · SI Table S1
Solvent	ethanol	0.26 mL	main p.2 · 2.1. Synthesis · SI Table S1