cMOF Evidence Base

Synthesis evidence

The Different Roles of Cobalt and Manganese in Metal-Organic Frameworks for Supercapacitors

Iqbal R., Sultan M.Q., Hussain S. et al. · Advanced Materials Technologies · 2021 · 2000941

10 structured synthesis routes

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

Partial recipeSource: Both

Route 1: Solvothermal

p008 · Experimental Section · Figure 1a

Metal precursorsCoCl2.6H2O
Linker precursorsHATP.6HCl / HITP.6HCl
SolventsWater
AdditivesConcentrated aqueous ammonia, NH4OH, 14 mol L-1
Atmospherenot specified
Temperature40
Time4
Work-upSame procedure as Mn3(HITP)2: vacuum filtration, centrifugation, water washing under reflux for 72 h with water refreshed four times, warm acetone wash.
ActivationDried under vacuum overnight at 120 degrees C.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCoCl2.6H2Onot separately stated; same procedure as Mn routep008 · Experimental Section · Figure 1a
LinkerHATP.6HCl / HITP.6HCl40 mg in the analogous procedure · 0.019 mmol in 20 mL water in the analogous procedurep008 · Experimental Section · Figure 1a
BaseNH4OH1.2 mL in the analogous procedure · 14 mol L-1p008 · Experimental Section · Figure 1a
Solventwater20 mL linker solution plus metal solution volume by same procedurep008 · Experimental Section · Figure 1a
Complete recipeSource: Main

Route 2: Other

p008 · Electrochemical Measurement

Metal precursorsCo-MOF
AdditivesActive carbon; PTFE binder
Temperature120
Time24
Substrate orientation316L stainless-steel wire mesh in 2032 coin cell
Work-upMixed in agate mortar, vacuum dried, cut into 9 mm tablets and assembled as symmetric coin cells.
ActivationVacuum drying at 120 degrees C for 24 h
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
OtherCo-MOF90 wt%p008 · Electrochemical Measurement
Additiveactive carbon5 wt% · surface area 1500 m2/g and pore volume 5 ml/g in SIp008 · Electrochemical Measurement
Additivepolytetrafluoroethylene5 wt% · 60% in water, diluted to 6% before usep008 · Electrochemical Measurement
Partial recipeSource: Main

Route 3: Other

p008 · Experimental Section

Metal precursorsCo3(HITP)2 bulk MOF
Linker precursorsHITP framework already present in Co3(HITP)2
Solventsn-hexane; ethanol suspension after washing
Additives1 M n-butyl lithium in n-hexane
Atmosphereargon
Time12
Oxidant / reductantn-butyl lithium treatment
Work-upSolid separated by filtration, washed with acetone, suspended in ethanol and centrifuged at 10000 rpm.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
OtherCo3(HITP)2not statedp008 · Experimental Section
Reductantn-butyl lithium in n-hexanenot stated · 1 Mp008 · Experimental Section
Solventethanolnot statedp008 · Experimental Section
Complete recipeSource: Main

Route 4: Other

p008 · Electrochemical Measurement

Metal precursorsCo-MOF
AdditivesPTFE binder, 60% in water diluted to 6% before use; 1 M LiTFSI electrolyte in 1,3-dioxolane/dimethoxyethane
Temperature120
Time24
Substrate orientationElectrode tablets pressed between 316L stainless-steel wire meshes; 2032 coin cell
Work-upMixed in agate mortar, dried under vacuum, cut to 9 mm circular tablets with mass about 1-2 mg, assembled with sulfonated polypropylene separator and kept overnight after pressing at 30 psi.
ActivationVacuum drying at 120 degrees C for 24 h
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
OtherCo-MOF95 wt%p008 · Electrochemical Measurement
Additivepolytetrafluoroethylene5 wt% · 60% in water, diluted to 6% before usep008 · Electrochemical Measurement
ElectrolyteLiTFSI in 1,3-dioxolane and dimethoxyethane1 mol L-1; solvent 1:1 w:wp008 · Electrochemical Measurement
Complete recipeSource: Main

Route 5: Other

p008 · Electrochemical Measurement

Metal precursorsCo-MOF
AdditivesSingle-wall carbon nanotubes; PTFE binder
Temperature120
Time24
Substrate orientation316L stainless-steel wire mesh in 2032 coin cell
Work-upMixed in agate mortar, vacuum dried, cut into 9 mm tablets and assembled as symmetric coin cells.
ActivationVacuum drying at 120 degrees C for 24 h
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
OtherCo-MOF90 wt%p008 · Electrochemical Measurement
Additivesingle-wall carbon nanotubes5 wt% · >=95%, OD <2 nm, length 5-30 micrometers in SIp008 · Electrochemical Measurement
Additivepolytetrafluoroethylene5 wt% · 60% in water, diluted to 6% before usep008 · Electrochemical Measurement
Complete recipeSource: Both

Route 6: Solvothermal

p008 · Experimental Section · Figure 1a

Metal precursorsMnCl2.6H2O
Linker precursorsHATP.6HCl / HITP.6HCl
SolventsWater
AdditivesConcentrated aqueous ammonia, NH4OH, 14 mol L-1
Atmospherenot specified
Temperature75
Time5
Work-upVacuum filtration, centrifugation, washing with water under reflux for 72 h with water refreshed 4 times, then washing with warm 200 mL acetone.
ActivationDried under vacuum overnight at 120 degrees C.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceManganese chloride hexahydrate (MnCl2.6H2O)25.6 mg · 0.028 mmol as reportedp008 · Experimental Section · Figure 1a
LinkerHATP.6HCl40 mg · 0.019 mmol in 20 mL waterp008 · Experimental Section · Figure 1a
Baseconcentrated aqueous ammonia (NH4OH)1.2 mL · 14 mol L-1p008 · Experimental Section · Figure 1a
Solventwater20 mL metal solution plus 20 mL linker solutionp008 · Experimental Section · Figure 1a
Complete recipeSource: Main

Route 7: Other

p008 · Electrochemical Measurement

Metal precursorsMn-MOF
AdditivesActive carbon; PTFE binder
Temperature120
Time24
Substrate orientation316L stainless-steel wire mesh in 2032 coin cell
Work-upMixed in agate mortar, vacuum dried, cut into 9 mm tablets and assembled as symmetric coin cells.
ActivationVacuum drying at 120 degrees C for 24 h
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
OtherMn-MOF90 wt%p008 · Electrochemical Measurement
Additiveactive carbon5 wt% · surface area 1500 m2/g and pore volume 5 ml/g in SIp008 · Electrochemical Measurement
Additivepolytetrafluoroethylene5 wt% · 60% in water, diluted to 6% before usep008 · Electrochemical Measurement
Partial recipeSource: Main

Route 8: Other

p008 · Experimental Section

Metal precursorsMn3(HITP)2 bulk MOF
Linker precursorsHITP framework already present in Mn3(HITP)2
Solventsn-hexane; ethanol suspension after washing
Additives1 M n-butyl lithium in n-hexane
Atmosphereargon
Time12
Oxidant / reductantn-butyl lithium treatment
Work-upSolid separated by filtration, washed with acetone, suspended in ethanol and centrifuged at 10000 rpm.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
OtherMn3(HITP)2not statedp008 · Experimental Section
Reductantn-butyl lithium in n-hexanenot stated · 1 Mp008 · Experimental Section
Solventethanolnot statedp008 · Experimental Section
Complete recipeSource: Main

Route 9: Other

p008 · Electrochemical Measurement

Metal precursorsMn-MOF
AdditivesPTFE binder, 60% in water diluted to 6% before use; 1 M LiTFSI electrolyte in 1,3-dioxolane/dimethoxyethane
Temperature120
Time24
Substrate orientationElectrode tablets pressed between 316L stainless-steel wire meshes; 2032 coin cell
Work-upMixed in agate mortar, dried under vacuum, cut to 9 mm circular tablets with mass about 1-2 mg, assembled with sulfonated polypropylene separator and kept overnight after pressing at 30 psi.
ActivationVacuum drying at 120 degrees C for 24 h
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
OtherMn-MOF95 wt%p008 · Electrochemical Measurement
Additivepolytetrafluoroethylene5 wt% · 60% in water, diluted to 6% before usep008 · Electrochemical Measurement
ElectrolyteLiTFSI in 1,3-dioxolane and dimethoxyethane1 mol L-1; solvent 1:1 w:wp008 · Electrochemical Measurement
Complete recipeSource: Main

Route 10: Other

p008 · Electrochemical Measurement

Metal precursorsMn-MOF
AdditivesSingle-wall carbon nanotubes; PTFE binder
Temperature120
Time24
Substrate orientation316L stainless-steel wire mesh in 2032 coin cell
Work-upMixed in agate mortar, vacuum dried, cut into 9 mm tablets and assembled as symmetric coin cells.
ActivationVacuum drying at 120 degrees C for 24 h
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
OtherMn-MOF90 wt%p008 · Electrochemical Measurement
Additivesingle-wall carbon nanotubes5 wt% · >=95%, OD <2 nm, length 5-30 micrometers in SIp008 · Electrochemical Measurement
Additivepolytetrafluoroethylene5 wt% · 60% in water, diluted to 6% before usep008 · Electrochemical Measurement