cMOF Evidence Base

Synthesis evidence

In Situ Growth of Lithiophilic MOF Layer Enabling Dendrite-free Lithium Deposition

Yin D., Wang Z., Li Q. et al. · iScience · 2020 · 101869

7 structured synthesis routes

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

Complete recipeSource: Both

Route 1: Other

p015 / SI p.3 · Transparent Methods - In situ synthesis

Metal precursorsCu foil substrate, 4 cm x 4 cm
Linker precursors7,7,8,8-tetracyanoquinodimethane (TCNQ), 0.05 mg ml^-1
SolventsMethanol; acetone cleaning solvent
Additives1 M HCl used for Cu foil cleaning
AtmosphereN2 drying after cleaning and final rinse; immersion at room temperature
Temperatureroom temperature
Time24
Substrate orientationCu foil, no crystal orientation reported
Oxidant / reductantCu foil acts as Cu source; no separate oxidant/reductant reported
Work-upRemove from solution, rinse with methanol several times, dry with N2
ActivationNone reported
Scalability contextLonger growth creates a thick/bulged Cu-MOF layer and is less favourable for long-term Li cycling.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCopper foil4 cm x 4 cmp015 / SI p.3 · Transparent Methods - In situ synthesis
Linker7,7,8,8-Tetracyanoquinodimethane (TCNQ)0.05 mg ml-1p015 / SI p.3 · Transparent Methods - In situ synthesis
SolventMethanolNot specifiedp015 / SI p.3 · Transparent Methods - In situ synthesis
AcidHydrochloric acid10 min dipping · 1 Mp015 / SI p.3 · Transparent Methods - In situ synthesis
SolventAcetone10 min dippingp015 / SI p.3 · Transparent Methods - In situ synthesis
Complete recipeSource: Both

Route 2: Other

p015 / SI p.3 · Transparent Methods - In situ synthesis

Metal precursorsCu foil substrate, 4 cm x 4 cm
Linker precursors7,7,8,8-tetracyanoquinodimethane (TCNQ), 0.05 mg ml^-1
SolventsMethanol; acetone cleaning solvent
Additives1 M HCl used for Cu foil cleaning
AtmosphereN2 drying after cleaning and final rinse; immersion at room temperature
Temperatureroom temperature
Time0.5
Substrate orientationCu foil, no crystal orientation reported
Oxidant / reductantCu foil acts as Cu source; no separate oxidant/reductant reported
Work-upRemove from solution, rinse with methanol several times, dry with N2
ActivationNone reported
Scalability contextMain text states the immersion method is easy for large-scale production.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCopper foil4 cm x 4 cmp015 / SI p.3 · Transparent Methods - In situ synthesis
Linker7,7,8,8-Tetracyanoquinodimethane (TCNQ)0.05 mg ml-1p015 / SI p.3 · Transparent Methods - In situ synthesis
SolventMethanolNot specifiedp015 / SI p.3 · Transparent Methods - In situ synthesis
AcidHydrochloric acid10 min dipping · 1 Mp015 / SI p.3 · Transparent Methods - In situ synthesis
SolventAcetone10 min dippingp015 / SI p.3 · Transparent Methods - In situ synthesis
Complete recipeSource: SI

Route 3: Other

p023 / SI p.11 · Supplemental Figure S5 caption · Figure S5D

Metal precursorsCu foil substrate
Linker precursorsTCNQ, concentration follows methanol procedure where specified
Solventsn-Butanol; acetone cleaning solvent
Additives1 M HCl used for Cu foil cleaning
AtmosphereN2 drying; room-temperature immersion
Temperatureroom temperature
Time0.5
Substrate orientationCu foil, no crystal orientation reported
Oxidant / reductantCu foil acts as Cu source; no separate oxidant/reductant reported
Work-upFollowing above procedures; rinse and N2 dry
ActivationNone reported
Scalability contextDemonstrates extension of synthesis to n-butanol.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCopper foilNot specifiedp023 / SI p.11 · Supplemental Figure S5 caption · Figure S5D
LinkerTCNQ0.05 mg ml-1 by same procedurep023 / SI p.11 · Supplemental Figure S5 caption · Figure S5D
Solventn-ButanolNot specifiedp023 / SI p.11 · Supplemental Figure S5 caption · Figure S5D
AcidHydrochloric acid10 min dipping · 1 Mp023 / SI p.11 · Supplemental Figure S5 caption · Figure S5D
SolventAcetone10 min dippingp023 / SI p.11 · Supplemental Figure S5 caption · Figure S5D
Complete recipeSource: SI

Route 4: Other

p023 / SI p.11 · Supplemental Figure S5 caption · Figure S5E

Metal precursorsCu foil substrate
Linker precursorsTCNQ, concentration follows methanol procedure where specified
SolventsDiethyl ether; acetone cleaning solvent
Additives1 M HCl used for Cu foil cleaning
AtmosphereN2 drying; room-temperature immersion
Temperatureroom temperature
Time0.5
Substrate orientationCu foil, no crystal orientation reported
Oxidant / reductantCu foil acts as Cu source; no separate oxidant/reductant reported
Work-upFollowing above procedures; rinse and N2 dry
ActivationNone reported
Scalability contextDemonstrates extension of synthesis to diethyl ether.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCopper foilNot specifiedp023 / SI p.11 · Supplemental Figure S5 caption · Figure S5E
LinkerTCNQ0.05 mg ml-1 by same procedurep023 / SI p.11 · Supplemental Figure S5 caption · Figure S5E
SolventDiethyl etherNot specifiedp023 / SI p.11 · Supplemental Figure S5 caption · Figure S5E
AcidHydrochloric acid10 min dipping · 1 Mp023 / SI p.11 · Supplemental Figure S5 caption · Figure S5E
SolventAcetone10 min dippingp023 / SI p.11 · Supplemental Figure S5 caption · Figure S5E
Complete recipeSource: SI

Route 5: Other

p023 / SI p.11 · Supplemental Figure S5 caption · Figure S5C

Metal precursorsCu foil substrate
Linker precursorsTCNQ, concentration follows methanol procedure where specified
SolventsEthanol; acetone cleaning solvent
Additives1 M HCl used for Cu foil cleaning
AtmosphereN2 drying; room-temperature immersion
Temperatureroom temperature
Time0.5
Substrate orientationCu foil, no crystal orientation reported
Oxidant / reductantCu foil acts as Cu source; no separate oxidant/reductant reported
Work-upFollowing above procedures; rinse and N2 dry
ActivationNone reported
Scalability contextDemonstrates extension of synthesis to ethanol.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCopper foilNot specifiedp023 / SI p.11 · Supplemental Figure S5 caption · Figure S5C
LinkerTCNQ0.05 mg ml-1 by same procedurep023 / SI p.11 · Supplemental Figure S5 caption · Figure S5C
SolventEthanolNot specifiedp023 / SI p.11 · Supplemental Figure S5 caption · Figure S5C
AcidHydrochloric acid10 min dipping · 1 Mp023 / SI p.11 · Supplemental Figure S5 caption · Figure S5C
SolventAcetone10 min dippingp023 / SI p.11 · Supplemental Figure S5 caption · Figure S5C
Complete recipeSource: SI

Route 6: Drop Cast

p016 / SI p.4 · Transparent Methods - Electrochemical measurements

Metal precursorsCommercial LiFePO4
SolventsN-methyl-2-pyrrolidone
AdditivesCarbon black; poly(vinylidene difluoride)
AtmosphereVacuum drying
Temperature60
Timeovernight
Substrate orientationAl foil
Work-upPunch into 12 mm disks
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
OtherCommercial LFPmass ratio 8p016 / SI p.4 · Transparent Methods - Electrochemical measurements
OtherCarbon blackmass ratio 1p016 / SI p.4 · Transparent Methods - Electrochemical measurements
OtherPoly(vinylidene difluoride)mass ratio 1p016 / SI p.4 · Transparent Methods - Electrochemical measurements
SolventN-methyl-2-pyrrolidoneNot specifiedp016 / SI p.4 · Transparent Methods - Electrochemical measurements
Complete recipeSource: SI

Route 7: Electrochemical

p016 / SI p.4 · Transparent Methods - Electrochemical measurements

Metal precursorsCu-MOF-30 min current collector and Li metal counter electrode
Solvents1,3-dioxolane (DOL) / dimethoxyethane (DME), 1:1 v/v
Additives0.1 M LiNO3
AtmosphereCoin-cell electrochemical deposition at room temperature
Temperatureroom temperature
Oxidant / reductantElectrochemical Li plating
Work-upLi@Cu-MOF electrode assembled into symmetrical cells
ActivationCells cycled at 50 uA between 0.01-1.00 V for five cycles to form stable SEI before Li deposition
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
ElectrolyteLiTFSI in DOL/DME100 uL · 1 M; DOL:DME 1:1 v/vp016 / SI p.4 · Transparent Methods - Electrochemical measurements
AdditiveLiNO30.1 Mp016 / SI p.4 · Transparent Methods - Electrochemical measurements
OtherMetallic lithium foilNot specifiedp016 / SI p.4 · Transparent Methods - Electrochemical measurements