Synthesis · A Li+ conductive metal organic framework electrolyte boosts the high-temperature performance of dendrite-free lithium batteries

5 structured synthesis routes

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

Partial recipeSource: SI

Route 1: Other

SI p1 · Experimental Section - Materials/Synthesis

AdditivesLiTFSI dried at 80 deg C under vacuum for 48 h before glove-box storage

Atmosphereglove box

Work-upMix [Py13][TFSI] with LiTFSI in glove box.

ActivationLiTFSI dried at 80 deg C under vacuum for 48 h.

Show 2 structured reagent records

Role	Reagent	Amount / concentration	Source
Electrolyte	N-propyl-N-methylpyrrolidinium bis(trifluoromethylsulfonyl) imide ([Py13][TFSI])	>99%	SI p1 · Experimental Section - Materials/Synthesis
Electrolyte	lithium bis(trifluoromethylsulfonyl) imide (LiTFSI)	>99%	SI p1 · Experimental Section - Materials/Synthesis

Complete recipeSource: Both

Route 2: Other

SI p1 · Experimental Section - Synthesis

Metal precursorsZIF-67 scaffold containing Co

Linker precursorsZIF-67 imidazolate framework

Additives[Py13][TFSI]/LiTFSI ionic liquid electrolyte

AtmosphereAr-filled dry box

Time1

Work-upHigh-energy ball milling at 300 r min-1 in zirconia vial; rolled into 50-um-thick film; cut into free-standing pieces.

Scalability contextThe optimum composition is a 2:3 mass ratio of ZIF-67:ILE, equivalent to 1.0 g MOF with 1.5 g ILE.

Show 2 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	ZIF-67	2 parts by mass; main text comparison uses 1.0 g MOF	SI p1 · Experimental Section - Synthesis
Electrolyte	ILE ([Py13][TFSI] + LiTFSI)	3 parts by mass; main text optimum uses 1.5 g ILE per 1.0 g MOF	SI p1 · Experimental Section - Synthesis

Complete recipeSource: Both

Route 3: Other

9532 · Results and discussion · Fig. 1e

Metal precursorsZIF-67 scaffold containing Co

Linker precursorsZIF-67 imidazolate framework

Additives[Py13][TFSI]/LiTFSI ionic liquid electrolyte

AtmosphereAr-filled dry box for ball milling according to SI general method

Time1

Work-upHigh-energy ball milling; loading series prepared with 1.0 g MOF and 2.0, 1.5 or 1.0 g ILE.

Show 2 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	MOF (ZIF-67)	1.0 g	9532 · Results and discussion · Fig. 1e
Electrolyte	ILE	2.0 g, 1.5 g or 1.0 g	9532 · Results and discussion · Fig. 1e

Complete recipeSource: SI

Route 4: Other

SI p2 · Assembly and performance testing of LMBs

SolventsN-methyl-2-pyrrolidone (NMP) for electrode slurry

Additives10 wt% acetylene black; 10 wt% PVDF

AtmosphereAr-filled glove box for cell assembly

Temperature80

Time24

Substrate orientationslurry cast onto Al foil

Work-upCathode slurry cast onto Al foil, heated at 80 deg C for 24 h, cut into 11 mm discs, assembled with Li metal and ILE@MOF in CR2032 cell without separator.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	electrode material (LiFePO4, LiNi0.33Mn0.33Co0.33O2, LiNi0.8Mn0.1Co0.1O2 or Li4Ti5O12)	80 wt%	SI p2 · Assembly and performance testing of LMBs
Additive	acetylene black	10 wt%	SI p2 · Assembly and performance testing of LMBs
Additive	PVDF	10 wt%	SI p2 · Assembly and performance testing of LMBs
Solvent	N-methyl-2-pyrrolidone	Not specified	SI p2 · Assembly and performance testing of LMBs

Complete recipeSource: SI

Route 5: Other

SI p1 · Experimental Section - Synthesis

Metal precursorsCo(NO3)2.6H2O (8.22 g, 99.99%, J&K Chemicals)

Linker precursors2-methyl imidazole (18.5 g, 99%, J&K Chemicals)

SolventsAnhydrous methanol, 400 mL for each precursor solution

Atmospherenot specified

Temperature25

Timeovernight

Work-upSolutions mixed by peristaltic pump at 100 mL min-1; purple precipitate collected by centrifugation at 5 deg C.

ActivationDried at 60 deg C for 24 h.

Scalability contextUses 400 mL methanol solutions and pump mixing; gram-scale precursor masses reported.

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Co(NO3)2.6H2O	8.22 g	SI p1 · Experimental Section - Synthesis
Linker	2-methyl imidazole	18.5 g	SI p1 · Experimental Section - Synthesis
Solvent	anhydrous methanol	400 mL quantities for each solution	SI p1 · Experimental Section - Synthesis