cMOF Evidence Base

Synthesis evidence

A Triptycene-Based Layered/Flower-Like 2D Conductive Metal–Organic Framework with 3D Extension as an Electrode for Efficient Li Storage

Liu X., Yu M., Liu J. et al. · Small · 2024 · 2306159

6 structured synthesis routes

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

Complete recipeSource: Both

Route 1: Solvothermal

p003 · 2.1 Preparation of M-DBH

Metal precursorsCobalt(II) acetate tetrahydrate, Co(OAc)2.4H2O, 0.72 mM
Linker precursors6OH-DBH, 0.032 mM in 1 mL degassed DMF
Solvents4 mL degassed DMF, 5 mL degassed deionized water, plus 1 mL degassed DMF for ligand
Additives100 uL NH4OH (25-28%)
AtmosphereDegassed solvents; round pressure bottle; atmosphere not otherwise specified
Temperature80
Time5
Work-upWashed with water and acetone several times; dried overnight in vacuum at room temperature.
ActivationNo separate activation reported for pristine powder.
Scalability contextSmall-volume pressure-bottle reaction; no scale-up data reported.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCobalt(II) acetate tetrahydrate (Co(OAc)2.4H2O)0.72 mMp003 · 2.1 Preparation of M-DBH
Linker6OH-DBH0.032 mMp003 · 2.1 Preparation of M-DBH
Solventdegassed DMF4 mL + 1 mLp003 · 2.1 Preparation of M-DBH
Solventdegassed deionized water5 mLp003 · 2.1 Preparation of M-DBH
BaseNH4OH100 uL · 25-28%p003 · 2.1 Preparation of M-DBH
Partial recipeSource: SI

Route 2: Other

p004 · 2.5 Electrochemical Characterization

Metal precursorsPreformed M-DBH active material
Linker precursorsPreformed M-DBH active material
SolventsSlurry solvent not reported
AdditivesSuper P carbon black and PVDF binder
AtmosphereAir/inert atmosphere not specified for slurry coating
Temperature50
Time24
Substrate orientationAluminium foil
Work-upSlurry coated onto aluminium foil and dried.
ActivationCells activated three times at 0.1 C before long-cycle testing.
Scalability contextCoin-cell electrode fabrication only.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
OtherM-DBH active material70 wt.%p004 · 2.5 Electrochemical Characterization
AdditiveSuper P carbon black20 wt.%p004 · 2.5 Electrochemical Characterization
AdditivePVDF10 wt.%p004 · 2.5 Electrochemical Characterization
Complete recipeSource: Both

Route 3: Solvothermal

p002 · Results and Discussion 2.1

Metal precursorsManganese acetate tetrahydrate, Mn(OAc)2.4H2O, 0.72 mM
Linker precursors6OH-DBH, 0.032 mM in 1 mL degassed DMF
Solvents4 mL degassed DMF, 5 mL degassed deionized water, plus 1 mL degassed DMF for ligand
Additives100 uL NH4OH (25-28%)
AtmosphereDegassed solvents; round pressure bottle; atmosphere not otherwise specified
Temperature80
Time5
Work-upWashed with water and acetone several times; dried overnight in vacuum at room temperature.
ActivationNo separate activation reported for pristine powder.
Scalability contextSmall-volume pressure-bottle reaction; no scale-up data reported.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceManganese acetate tetrahydrate (Mn(OAc)2.4H2O)0.72 mMp002 · Results and Discussion 2.1
Linker6OH-DBH0.032 mMp002 · Results and Discussion 2.1
Solventdegassed DMF4 mL + 1 mLp002 · Results and Discussion 2.1
Solventdegassed deionized water5 mLp002 · Results and Discussion 2.1
BaseNH4OH100 uL · 25-28%p002 · Results and Discussion 2.1
Complete recipeSource: Both

Route 4: Solvothermal

p003 · 2.1 Preparation of M-DBH

Metal precursorsNickel acetate tetrahydrate, Ni(OAc)2.4H2O, 0.72 mM
Linker precursors6OH-DBH, 0.032 mM in 1 mL degassed DMF
Solvents4 mL degassed DMF, 5 mL degassed deionized water, plus 1 mL degassed DMF for ligand
Additives100 uL NH4OH (25-28%)
AtmosphereDegassed solvents; round pressure bottle; atmosphere not otherwise specified
Temperature80
Time5
Work-upWashed with water and acetone several times; dried overnight in vacuum at room temperature.
ActivationNo separate activation reported for pristine powder.
Scalability contextSmall-volume pressure-bottle reaction; no scale-up data reported.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceNickel acetate tetrahydrate (Ni(OAc)2.4H2O)0.72 mMp003 · 2.1 Preparation of M-DBH
Linker6OH-DBH0.032 mMp003 · 2.1 Preparation of M-DBH
Solventdegassed DMF4 mL + 1 mLp003 · 2.1 Preparation of M-DBH
Solventdegassed deionized water5 mLp003 · 2.1 Preparation of M-DBH
BaseNH4OH100 uL · 25-28%p003 · 2.1 Preparation of M-DBH
Complete recipeSource: SI

Route 5: Other

p003 · 2.2 Preparation of S@ M-DBH

Metal precursorsPreformed M-DBH (M = Ni, Mn, Co)
Linker precursorsPreformed 6OH-DBH-based framework
SolventsNone reported for sulfur loading
AdditivesSublimed sulfur
AtmosphereArgon; sealed glass tube
Temperature155
Time12
Work-upDry ball milling before heating; ball-milled again before slurry preparation.
ActivationThermal sulfur infusion/coheating at 155 deg C under argon.
Scalability contextNo scale-up data reported.
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
OtherM-DBH powder3 parts by weightp003 · 2.2 Preparation of S@ M-DBH
Additivesublimed sulfur7 parts by weightp003 · 2.2 Preparation of S@ M-DBH
Partial recipeSource: Both

Route 6: Other

p006 · Results and Discussion 2.3

Metal precursorsPreformed S@M-DBH active material
Linker precursorsPreformed S@M-DBH active material
SolventsSlurry solvent not reported
AdditivesSuper P carbon black and PVDF binder
AtmosphereAir/inert atmosphere not specified for slurry coating
Temperature50
Time24
Substrate orientationAluminium foil
Work-upSlurry coated onto aluminium foil and dried.
ActivationCells activated three times at 0.1 C before long-cycle testing.
Scalability contextCoin-cell electrode fabrication only.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
OtherS@M-DBH active material70 wt.%p006 · Results and Discussion 2.3
AdditiveSuper P carbon black20 wt.%p006 · Results and Discussion 2.3
AdditivePVDF10 wt.%p006 · Results and Discussion 2.3