cMOF Evidence Base

Synthesis evidence

Probing the electronic and ionic transport in topologically distinct redox-active metal-organic frameworks in aqueous electrolytes

Shen C.-H., Chen Y.-H., Wang Y.-C. et al. · Physical Chemistry Chemical Physics · 2022 · 9855-9865

8 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

9857 · Experimental - Synthesis of Zr-MOFs

Metal precursors105 mg zirconium(IV) oxychloride octahydrate
Linker precursors32.8 mg H4TCPB
Solvents8 mL DMF; 10 mL DMF in HCl/DMF activation; acetone exchange
Additives2.7 g benzoic acid modulator; 0.5 mL 8 M HCl(aq)
Atmosphereair/not specified; activation condition same as MOF-808/UiO-66
Temperature80 C pre-heating; 120 C crystal growth; 100 C HCl/DMF benzoate-removal step; 80 C activation
Time2 h pre-heating; 20 min sonication after H4TCPB; 48 h growth; 24 h HCl/DMF treatment; activation time same as MOF-808/UiO-66
Work-upWashed with DMF three times; HCl/DMF treatment to remove coordinated benzoate; washed with 10 mL DMF three times; acetone exchange.
ActivationSolvent exchange with acetone and activation similar to MOF-808 and UiO-66; SI confirms HCl/DMF activation removes benzoate.
Scalability contextScintillation-vial batch.
Show 6 structured reagent records
RoleReagentAmount / concentrationSource
Metal Sourcezirconium(IV) oxychloride octahydrate105 mg9857 · Experimental - Synthesis of Zr-MOFs
LinkerH4TCPB32.8 mg9857 · Experimental - Synthesis of Zr-MOFs
SolventDMF8 mL + 10 mL in HCl/DMF step9857 · Experimental - Synthesis of Zr-MOFs
Acidbenzoic acid2.7 g9857 · Experimental - Synthesis of Zr-MOFs
AcidHCl(aq)0.5 mL · 8 M9857 · Experimental - Synthesis of Zr-MOFs
Solventacetonenot specified; exchange as MOF-808/UiO-669857 · Experimental - Synthesis of Zr-MOFs
Complete recipeSource: Main

Route 2: Drop Cast

9857 · Experimental - Fabrication of pellets and thin films

Solventsacetone suspension
Atmospheresubstrate dried under nitrogen flow; ambient drop-casting not otherwise specified
Temperatureroom temperature
Time5 min substrate sonication in each solvent; 10 min suspension sonication
Substrate orientationFTO conducting substrate; exposed 0.25 cm2 area defined by insulating polyamide tape
Work-upFTO cleaned sequentially with water, ethanol and acetone; dried with nitrogen; MOF suspension drop-cast five times.
Scalability contextSmall-area drop-cast electrodes for three-electrode electrochemistry.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
OtherMOF solid6 mg · 6 mg in 0.5 mL acetone9857 · Experimental - Fabrication of pellets and thin films
Solventacetone0.5 mL suspension; cleaning solvent9857 · Experimental - Fabrication of pellets and thin films
Solventwatercleaning solvent9857 · Experimental - Fabrication of pellets and thin films
Solventethanolcleaning solvent9857 · Experimental - Fabrication of pellets and thin films
OtherFTO substrate3 cm x 1.5 cm; 0.25 cm2 exposed · 7 ohm sq^-19857 · Experimental - Fabrication of pellets and thin films
Complete recipeSource: Main

Route 3: Solvothermal

9857 · Experimental - Installation of manganese sites in Zr-MOFs

Metal precursors47.1 mg manganese(II) acetate tetrahydrate
Linker precursorsCAU-24 framework precursor containing TCPB linkers
Solvents6 mL DMF for Mn installation; DMF washes; acetone exchange
Atmosphereair/not specified
Temperatureroom temperature SIM installation; 80 C activation
Time18 h SIM installation; activation time same as Zr-MOFs
Work-upSame SIM procedure as Mn-UiO-66, replacing UiO-66 with 37.1 mg CAU-24; DMF wash and acetone exchange.
ActivationActivated at 80 C after acetone exchange.
Scalability context37.1 mg CAU-24 batch.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal Sourcemanganese(II) acetate tetrahydrate47.1 mg9857 · Experimental - Installation of manganese sites in Zr-MOFs
OtherCAU-2437.1 mg9857 · Experimental - Installation of manganese sites in Zr-MOFs
SolventDMF6 mL for reaction plus wash9857 · Experimental - Installation of manganese sites in Zr-MOFs
Solventacetone6 mL three times9857 · Experimental - Installation of manganese sites in Zr-MOFs
Complete recipeSource: Main

Route 4: Solvothermal

9857 · Experimental - Installation of manganese sites in Zr-MOFs

Metal precursors47.1 mg manganese(II) acetate tetrahydrate
Linker precursorsMOF-808 framework precursor containing BTC linkers
Solvents6 mL DMF for Mn installation; DMF washes; acetone exchange
Atmosphereair/not specified
Temperatureroom temperature SIM installation; 80 C activation
Time18 h SIM installation; activation time same as Zr-MOFs
Work-upSame SIM procedure as Mn-UiO-66, replacing UiO-66 with 26.7 mg MOF-808; DMF wash and acetone exchange.
ActivationActivated at 80 C after acetone exchange.
Scalability context26.7 mg MOF-808 batch.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal Sourcemanganese(II) acetate tetrahydrate47.1 mg9857 · Experimental - Installation of manganese sites in Zr-MOFs
OtherMOF-80826.7 mg9857 · Experimental - Installation of manganese sites in Zr-MOFs
SolventDMF6 mL for reaction plus wash9857 · Experimental - Installation of manganese sites in Zr-MOFs
Solventacetone6 mL three times9857 · Experimental - Installation of manganese sites in Zr-MOFs
Complete recipeSource: Main

Route 5: Other

9857 · Experimental - Fabrication of pellets and thin films

Solventsacetone wetting
Atmospherevacuum oven drying
Temperature80 C drying
Timeovernight drying
Work-upSequentially pelletised in a mini pellet press with 7 mm die set and 0.5 ton load; sandwiched between titanium foils.
ActivationDried in a vacuum oven at 80 C overnight before conductivity measurement.
Scalability contextPellet preparation for conductivity testing only.
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
Solventacetonewetting amount not reported9857 · Experimental - Fabrication of pellets and thin films
OtherMn-MOF-808, Mn-UiO-66, or Mn-CAU-24 powdernot reported9857 · Experimental - Fabrication of pellets and thin films
Complete recipeSource: Main

Route 6: Solvothermal

9857 · Experimental - Installation of manganese sites in Zr-MOFs

Metal precursors47.1 mg manganese(II) acetate tetrahydrate
Linker precursorsDefective UiO-66 framework precursor containing BDC linkers
Solvents6 mL DMF for Mn installation; 6 mL DMF washes; 6 mL acetone solvent exchange
Atmosphereair/not specified
Temperatureroom temperature SIM installation; 80 C activation
Time18 h SIM installation; activation time same as Zr-MOFs
Work-upWashed with 6 mL DMF three times by centrifugation; solvent exchange with 6 mL acetone three times.
ActivationActivated at 80 C after acetone exchange.
Scalability context30 mg UiO-66 batch.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal Sourcemanganese(II) acetate tetrahydrate47.1 mg9857 · Experimental - Installation of manganese sites in Zr-MOFs
Otherdefective UiO-6630 mg9857 · Experimental - Installation of manganese sites in Zr-MOFs
SolventDMF6 mL for reaction plus wash9857 · Experimental - Installation of manganese sites in Zr-MOFs
Solventacetone6 mL three times9857 · Experimental - Installation of manganese sites in Zr-MOFs
Complete recipeSource: Main

Route 7: Solvothermal

9857 · Experimental - Synthesis of Zr-MOFs

Metal precursors160 mg zirconium(IV) oxychloride octahydrate
Linker precursors110 mg H3BTC
Solvents20 mL DMF; 20 mL formic acid; HCl/DMF post-treatment; acetone exchange
Additivesformic acid; concentrated HCl
Atmosphereair/not specified; activation under vacuum
Temperature120 C synthesis; 120 C HCl/DMF treatment; 80 C activation
Time48 h synthesis; overnight HCl/DMF treatment; 2 h/overnight/2 h acetone exchange; overnight activation
Work-upWashed with DMF three times by centrifugation; HCl/DMF treatment; washed with DMF; acetone solvent exchange.
ActivationActivated under vacuum at 80 C overnight.
Scalability contextBatch powder synthesis in 100 mL DURAN bottle.
Show 6 structured reagent records
RoleReagentAmount / concentrationSource
Metal Sourcezirconium(IV) oxychloride octahydrate160 mg9857 · Experimental - Synthesis of Zr-MOFs
LinkerH3BTC110 mg9857 · Experimental - Synthesis of Zr-MOFs
SolventDMF20 mL + 20 mL in HCl/DMF step9857 · Experimental - Synthesis of Zr-MOFs
Acidformic acid20 mL9857 · Experimental - Synthesis of Zr-MOFs
Acidconcentrated HCl0.5 mL · 36.5-38.0% source reagent9857 · Experimental - Synthesis of Zr-MOFs
Solventacetonenot specified; three exchanges9857 · Experimental - Synthesis of Zr-MOFs
Complete recipeSource: Main

Route 8: Solvothermal

9857 · Experimental - Synthesis of Zr-MOFs

Metal precursors43 uL zirconium(IV) propoxide solution
Linker precursors45 mg H2BDC
Solvents4.2 mL DMF; acetone exchange
Additives2.4 mL acetic acid
Atmosphereair/not specified; activation under vacuum
Temperature130 C pre-treatment; room temperature linker addition/stirring; 80 C activation
Time2 h pre-treatment; 20 h stirring after H2BDC addition; solvent exchange/activation as MOF-808
Work-upWashed with 10 mL DMF three times by centrifugation; solvent exchange and activation same as MOF-808.
ActivationSame as MOF-808: acetone exchange followed by vacuum activation at 80 C overnight.
Scalability context20 mL scintillation-vial batch.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Metal Sourcezirconium(IV) propoxide solution43 uL · 70 wt% in 1-propanol9857 · Experimental - Synthesis of Zr-MOFs
LinkerH2BDC45 mg9857 · Experimental - Synthesis of Zr-MOFs
SolventDMF4.2 mL9857 · Experimental - Synthesis of Zr-MOFs
Acidacetic acid2.4 mL9857 · Experimental - Synthesis of Zr-MOFs
Solventacetonenot specified; exchange as MOF-8089857 · Experimental - Synthesis of Zr-MOFs