Synthesis · Ionic Liquid-Laden Zn-MOF-74-Based Solid-State Electrolyte for Sodium Batteries

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: Other

p004 / journal page 4 · 2.2.3 Insertion of Na[EMIm][TFSI] into Zn-MOF-74

Metal precursorspreformed Zn-MOF-74

Linker precursorspreformed Zn-MOF-74 linker

SolventsNa-enriched [EMIm][TFSI] ionic liquid

AdditivesNaTFSI within [EMIm][TFSI]

Atmospherenot specified for loading; Ar-filled glove box used for Na/IL0.5@MOF/Na and Na/IL0.5@MOF/SS cell assembly

Temperature100 deg C MOF activation; 80 deg C loading distribution

Timeat least 6 h activation; 1 h at 80 deg C

Work-upmixture heated for better distribution into MOF porosity

ActivationMOF water removed by heating at 100 deg C for at least 6 h before loading

Show 2 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	activated Zn-MOF-74	1 mass part	p004 / journal page 4 · 2.2.3 Insertion of Na[EMIm][TFSI] into Zn-MOF-74
Electrolyte	Na-enriched [EMIm][TFSI]	0.5 mass part · 0.91 M NaTFSI in [EMIm][TFSI]	p004 / journal page 4 · 2.2.3 Insertion of Na[EMIm][TFSI] into Zn-MOF-74

Partial recipeSource: Main

Route 2: Other

p004 / journal page 4 · 2.2.3 Insertion of Na[EMIm][TFSI] into Zn-MOF-74

Metal precursorspreformed Zn-MOF-74

Linker precursorspreformed Zn-MOF-74 linker

SolventsNa-enriched [EMIm][TFSI] ionic liquid

AdditivesNaTFSI within [EMIm][TFSI]

Atmospherenot specified

Temperature100 deg C MOF activation; 80 deg C loading distribution

Timeat least 6 h activation; 1 h at 80 deg C

Work-upmixture heated for better distribution into MOF porosity

ActivationMOF water removed by heating at 100 deg C for at least 6 h before loading

Show 2 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	activated Zn-MOF-74	1 mass part	p004 / journal page 4 · 2.2.3 Insertion of Na[EMIm][TFSI] into Zn-MOF-74
Electrolyte	Na-enriched [EMIm][TFSI]	0.6 mass part · 0.91 M NaTFSI in [EMIm][TFSI]	p004 / journal page 4 · 2.2.3 Insertion of Na[EMIm][TFSI] into Zn-MOF-74

Partial recipeSource: Main

Route 3: Other

p004 / journal page 4 · 2.2.3 Insertion of Na[EMIm][TFSI] into Zn-MOF-74

Metal precursorspreformed Zn-MOF-74

Linker precursorspreformed Zn-MOF-74 linker

SolventsNa-enriched [EMIm][TFSI] ionic liquid

AdditivesNaTFSI within [EMIm][TFSI]

Atmospherenot specified

Temperature100 deg C MOF activation; 80 deg C loading distribution

Timeat least 6 h activation; 1 h at 80 deg C

Work-upmixture heated for better distribution into MOF porosity

ActivationMOF water removed by heating at 100 deg C for at least 6 h before loading

Show 2 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	activated Zn-MOF-74	1 mass part	p004 / journal page 4 · 2.2.3 Insertion of Na[EMIm][TFSI] into Zn-MOF-74
Electrolyte	Na-enriched [EMIm][TFSI]	0.8 mass part · 0.91 M NaTFSI in [EMIm][TFSI]	p004 / journal page 4 · 2.2.3 Insertion of Na[EMIm][TFSI] into Zn-MOF-74

Partial recipeSource: Main

Route 4: Other

p004 / journal page 4 · 2.2.3 Insertion of Na[EMIm][TFSI] into Zn-MOF-74

Metal precursorspreformed Zn-MOF-74

Linker precursorspreformed Zn-MOF-74 linker

SolventsNa-enriched [EMIm][TFSI] ionic liquid

AdditivesNaTFSI within [EMIm][TFSI]

Atmospherenot specified for loading; Ar-filled glove box used later for Na cells

Temperature100 deg C MOF activation; 80 deg C loading distribution

Timeat least 6 h activation; 1 h at 80 deg C

Work-upmixture heated for better distribution into MOF porosity

ActivationMOF water removed by heating at 100 deg C for at least 6 h before loading

Show 2 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	activated Zn-MOF-74	1 mass part	p004 / journal page 4 · 2.2.3 Insertion of Na[EMIm][TFSI] into Zn-MOF-74
Electrolyte	Na-enriched [EMIm][TFSI]	1 mass part · 0.91 M NaTFSI in [EMIm][TFSI]	p004 / journal page 4 · 2.2.3 Insertion of Na[EMIm][TFSI] into Zn-MOF-74

Partial recipeSource: Main

Route 5: Other

p003 / journal page 3 · 2.2.2 Sodium Enrichment of the Ionic Liquid [EMIm][TFSI]

Metal precursorsNaTFSI sodium salt

Solvents[EMIm][TFSI] ionic liquid

AdditivesNaTFSI

Atmosphereambient / not specified

Temperatureroom temperature sonication; dried at 100

Time5 min ultrasonic bath; 24 h drying

Work-updry in oven at 100 deg C for 24 h to remove remaining moisture

Show 2 structured reagent records

Role	Reagent	Amount / concentration	Source
Electrolyte	1-ethyl-3-methylimidazolium bis(trifluoromethylsulfonyl)imide (EMIm TFSI, 99%)	Not specified	p003 / journal page 3 · 2.2.2 Sodium Enrichment of the Ionic Liquid [EMIm][TFSI]
Electrolyte	bis(trifluoromethane)sulfonimide sodium salt (NaTFSI, 99%)	saturated in ionic liquid · final concentration 0.91 M	p003 / journal page 3 · 2.2.2 Sodium Enrichment of the Ionic Liquid [EMIm][TFSI]

Complete recipeSource: Main

Route 6: Other

p003 / journal page 3 · 2.2.1 Synthesis of Zn-MOF-74

Metal precursors(ZnOAc)2.2H2O, 1.145 g in 15 mL distilled water

Linker precursors2,5-dihydroxyteraphthalic acid (DBCO), 0.3417 g in 15 mL 0.46 M NaOH

Solventsdistilled water; aqueous 0.46 M NaOH

AdditivesNaOH base, 0.46 M; 100 mL prepared

Atmosphereambient / not specified

Temperatureroom temperature; dried at 100

Time24 h stirring; drying time not specified

Work-upyellow product washed with distilled water and filtered

Activationdried at 100 deg C; later heated at 100 deg C for at least 6 h before ionic-liquid insertion

Scalability contextAuthors state Zn-MOF-74 synthesis is fast, simple, reproducible on a larger scale and environmentally friendly because no toxic solvents are used.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	(ZnOAc)2.2H2O	1.145 g · in 15 mL distilled water	p003 / journal page 3 · 2.2.1 Synthesis of Zn-MOF-74
Linker	2,5-dihydroxyteraphthalic acid (DBCO, 98%)	0.3417 g · dissolved in 15 mL 0.46 M NaOH	p003 / journal page 3 · 2.2.1 Synthesis of Zn-MOF-74
Base	NaOH	100 mL solution prepared; 15 mL used for DBCO solution · 0.46 M	p003 / journal page 3 · 2.2.1 Synthesis of Zn-MOF-74
Solvent	distilled water	15 mL for zinc solution plus wash solvent	p003 / journal page 3 · 2.2.1 Synthesis of Zn-MOF-74