Synthesis evidence

The Origins of Ion Conductivity in MOF-Ionic Liquids Hybrid Solid Electrolytes

Zettl R., Hanzu I. · Frontiers in Energy Research · 2021 · 714698

6 structured synthesis routes

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

Partial recipeSource: Main

Route 1: Unknown

2 · 2 Materials and Methods

Metal precursorsaluminium metal source not specified in main text
Linker precursors1,2,4,5-benzenetetracarboxylic acid / pyromellitic acid
Activationall samples activated at 300 deg C at 1e-3 mbar for 24 h before soaking electrolyte was added
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
Metal Sourcealuminium metal centres; exact precursor not specifiedNot specified2 · 2 Materials and Methods
Linker1,2,4,5-benzenetetracarboxylic acid / pyromellitic acidNot specified2 · 2 Materials and Methods
Partial recipeSource: Main

Route 2: Other

3 · Table 1 · Table 1

Metal precursorsMIL-121 (no Li)
SolventsEMIM-TFSI ionic liquid
AdditivesLiTFSI
Atmosphereclosed container in drying oven
Timeat least 24 h rest after mixing
Work-upvigorous mixing to homogenise powder; rest in closed drying oven container; powder pressed into pellets at 0.3 tons; Au blocking electrodes sputtered for impedance tests
ActivationMIL-121 activated at 300 deg C and 1e-3 mbar for 24 h before soaking electrolyte addition
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
OtherMIL-121 (no Li)77 wt% of final sample3 · Table 1 · Table 1
ElectrolyteLiTFSI in EMIM-TFSI23 wt% of final sample · 0.4 M LiTFSI3 · Table 1 · Table 1
Partial recipeSource: Main

Route 3: Other

3 · Table 1 · Table 1

Metal precursorsMIL-121 (no Li)
AdditivesEMIM-TFSI ionic liquid
Atmosphereclosed container in drying oven
Timeat least 24 h rest after mixing
Work-upvigorous mixing to homogenise powder; rest in closed drying oven container; powder pressed into pellets at 0.3 tons; Au blocking electrodes sputtered for impedance tests
ActivationMIL-121 activated at 300 deg C and 1e-3 mbar for 24 h before ionic-liquid addition
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
OtherMIL-121 (no Li)77 wt% of final sample3 · Table 1 · Table 1
ElectrolyteEMIM-TFSI ionic liquid23 wt% of final sample3 · Table 1 · Table 1
Partial recipeSource: Main

Route 4: Other

2 · 2 Materials and Methods

Metal precursorsMIL-121/Li
SolventsEMIM-TFSI ionic liquid
AdditivesLiTFSI
Atmosphereclosed container in drying oven
Timeat least 24 h rest after mixing
Work-upvigorous mixing to homogenise powder; rest in closed drying oven container; powder pressed into pellets at 0.3 tons; Au blocking electrodes sputtered for impedance tests
ActivationMIL-121/Li activated at 300 deg C and 1e-3 mbar for 24 h before soaking electrolyte addition
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
OtherMIL-121/Li powder77 wt% of final sample2 · 2 Materials and Methods
ElectrolyteLiTFSI in EMIM-TFSI23 wt% of final sample · 0.4 M LiTFSI2 · 2 Materials and Methods
Partial recipeSource: Main

Route 5: Other

2 · 2 Materials and Methods

Metal precursorsMIL-121/Li
AdditivesEMIM-TFSI ionic liquid
Atmosphereclosed container in drying oven
Timeat least 24 h rest after mixing
Work-upvigorous mixing to homogenise powder; rest in closed drying oven container; powder pressed into pellets at 0.3 tons; Au blocking electrodes sputtered for impedance tests
ActivationMIL-121/Li activated at 300 deg C and 1e-3 mbar for 24 h before ionic-liquid addition
Scalability contextsample kept a true solid appearance, was not waxy and could be pressed into pellets
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
OtherMIL-121/Li powder77 wt% of final sample2 · 2 Materials and Methods
ElectrolyteEMIM-TFSI ionic liquid23 wt% of final sample2 · 2 Materials and Methods
Partial recipeSource: Main

Route 6: Other

2 · 2 Materials and Methods

Metal precursorsMIL-121
Additiveslithium acetate (LiAc)
Atmosphereclosed container; samples kept free from moisture and air for subsequent measurements
Timeovernight stirring; activation 24 h
Work-uprinsed and dried MIL-121/Li sample mentioned for ICPMS aliquot; detailed rinse/dry conditions not specified in supplied main text
Activation300 deg C at 1e-3 mbar for 24 h before soaking electrolyte addition
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
OtherMIL-121Not specified2 · 2 Materials and Methods
Additivelithium acetate (LiAc)Not specified2 · 2 Materials and Methods