Synthesis · Operando Raman and ex situ characterization of an iron-based conductive MOF as a negative electrode in Li-ion batteries

3 structured synthesis routes

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

Complete recipeSource: Main

10 · 4.3 Electrochemical measurements and operando Raman

SolventsN-methyl pyrrolidone (NMP, Sigma-Aldrich)

Additivescarbon black Super P (99+, AlfaAesar); PVDF (AlfaAesar)

Atmosphereassembled inside an Ar glovebox for cells

Temperature120

Time12

Substrate orientationcopper foil, thickness 0.012 mm

Work-upSlurry deposited onto Cu foil; dried 10 min on a hot plate; dried 12 h at 120 C under vacuum; pressed at 128 kg cm-2; 8 mm discs cut.

Scalability contextConventional slurry-cast LIB electrode preparation; average active material loading 0.56 +/- 0.28 mg cm-2 reported.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	synthesized Fe-HHTP powder	80 wt% in electrode solids	10 · 4.3 Electrochemical measurements and operando Raman
Additive	carbon black Super P (99+, AlfaAesar)	10 wt% in electrode solids	10 · 4.3 Electrochemical measurements and operando Raman
Additive	poly(vinylidene fluoride) (PVDF, AlfaAesar)	10 wt% in electrode solids	10 · 4.3 Electrochemical measurements and operando Raman
Solvent	N-methyl pyrrolidone (NMP, Sigma-Aldrich)	Not specified	10 · 4.3 Electrochemical measurements and operando Raman

Complete recipeSource: Main

10 · 4.3 Electrochemical measurements and operando Raman · Figure S11

AdditivesLiPF6 electrolyte, glass-fibre separators, lithium disc, CaF2 window

AtmosphereAr glovebox (PureLab HE, H2O and O2 <=0.1 ppm)

Substrate orientationrectangular copper-foil electrode placed with copper foil facing lithium

Oxidant / reductantlithium disc reference/counter electrode

Work-upRectangular electrode wrapped between two separators, one with a hole, with copper foil facing lithium; cell sealed with CaF2 window.

Scalability contextSpecialised operando Raman cell assembly for measurement rather than production.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Electrolyte	1 M LiPF6 in DMC : EC (1 : 1) (v : v) (Solvionic)	1 M	10 · 4.3 Electrochemical measurements and operando Raman · Figure S11
Other	lithium disc (thickness 0.38 mm, Sigma-Aldrich)	Not specified	10 · 4.3 Electrochemical measurements and operando Raman · Figure S11
Other	two fiber glass separators (Grade GF/F, Whatman glass)	two separators	10 · 4.3 Electrochemical measurements and operando Raman · Figure S11
Other	CaF2 window	Not specified	10 · 4.3 Electrochemical measurements and operando Raman · Figure S11

Complete recipeSource: Main

9 · 4.1 MOF synthesis

Metal precursors0.065 mmol iron(II) acetate (99.995%, Sigma-Aldrich)

Linker precursors0.032 mmol HHTP (>95.0%, TCI)

Solvents1.95 mL deionised water; 0.15 mL DMF (>=99.8%, Sigma-Aldrich)

Atmosphereclosed vial; atmosphere not otherwise specified

Temperature80

Time20

Work-upCentrifuged; solid washed with water, ethanol and acetone, two times with each solvent.

ActivationDried at 50 C.

Scalability contextSmall vial synthesis in a 10 mL vial; no scale-up reported.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Linker	HHTP (>95.0%, TCI)	0.032 mmol	9 · 4.1 MOF synthesis
Metal Source	iron(II) acetate (99.995%, Sigma-Aldrich)	0.065 mmol	9 · 4.1 MOF synthesis
Solvent	deionized water	1.95 mL	9 · 4.1 MOF synthesis
Solvent	dimethylformamide (DMF; >=99.8%, Sigma-Aldrich)	0.15 mL	9 · 4.1 MOF synthesis