Synthesis evidence

Framework Dimensional Control Boosting Charge Storage in Conjugated Coordination Polymers

Fan K., Fu C., Chen Y. et al. · Advanced Science · 2023 · 2205760

4 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

2 · Experimental section · Synthesis of 1D-CuTABQ

Metal precursorsCu(NO3)2.3H2O (241.5 mg, 1 mmol)
Linker precursorsfresh 2,3,5,6-tetraaminobenzoquinone (TABQ, 168 mg, 1 mmol)
SolventsDMSO, 30 mL for Cu salt and 30 mL for TABQ
Additivesconcentrated aqueous ammonium hydroxide, 3 mL, approx. 14 M
Atmosphereair atmosphere (main text states air and base are required)
Temperatureroom temperature; dried at 80 deg C
Time12 h stirring at 500 rpm; post-synthesis drying time not specified
Oxidant / reductantoxygen from air acts as oxidant during ligand deprotonation/oxidation
Work-upprecipitate isolated by filtration; washed with DMSO (50 mL x 2) and acetone (25 mL x 2); dried in 80 deg C oven
Activationnone beyond oven drying for characterisation
Scalability contextBatch solution precipitation with 244 mg reported yield.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCu(NO3)2.3H2O241.5 mg, 1 mmol2 · Experimental section · Synthesis of 1D-CuTABQ
Linker2,3,5,6-tetraaminobenzoquinone (TABQ)168 mg, 1 mmol2 · Experimental section · Synthesis of 1D-CuTABQ
SolventDMSO30 mL + 30 mL2 · Experimental section · Synthesis of 1D-CuTABQ
Baseconcentrated aqueous ammonium hydroxide3 mL · ~14 M2 · Experimental section · Synthesis of 1D-CuTABQ
Oxidantair/oxygenambient2 · Experimental section · Synthesis of 1D-CuTABQ
Complete recipeSource: SI

Route 2: Drop Cast

3-4 · Electrochemical Measurements

SolventsN-methyl-2-pyrrolidone (NMP)
AdditivesSuper P carbon black and PVDF binder
Atmosphereelectrochemical cells assembled in Ar-filled glove box, H2O/O2 under 1.0 ppm
Temperature120 deg C vacuum pre-drying; 80 deg C vacuum electrode drying; room-temperature cycling
Time12 h vacuum pre-drying; 12 h electrode drying
Substrate orientationAl foil current collector
Oxidant / reductantmetallic Na counter electrode in half-cell
Work-upslurry coated on Al foil with doctor blade and dried; coin cells assembled with PP and glass fibre separators
Activationactive material dried at 120 deg C under vacuum for 12 h before electrode preparation
Scalability contextStandard slurry-cast battery electrode fabrication.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Other1D-CuTABQ active material6 parts by weight3-4 · Electrochemical Measurements
AdditiveSuper P carbon black3 parts by weight3-4 · Electrochemical Measurements
AdditivePVDF1 part by weight3-4 · Electrochemical Measurements
SolventNMPnot specified3-4 · Electrochemical Measurements
ElectrolyteNaPF6 in DMEnot specified · 1 M or 4 M3-4 · Electrochemical Measurements
Complete recipeSource: Both

Route 3: Solvothermal

2 · Experimental section · Synthesis of 2D-CuTABQ

Metal precursorsCu(NO3)2.3H2O (108.7 mg, 0.45 mmol)
Linker precursorsfresh 2,3,5,6-tetraaminobenzoquinone (TABQ, 50.4 mg, 0.3 mmol)
SolventsDMSO, 12 mL for TABQ and 6 mL for Cu salt
Additivesnone; base absent
Atmospheretightly sealed vial/closed system; no added oxygen
Temperature120
Time72
Oxidant / reductantCu2+ ions/residual oxygen oxidise TABQ; TABQ reduces part of Cu2+ to Cu+ in confined space
Work-upblack precipitate obtained by vacuum filtration and washed with water
Activationnone reported for powder; electrodes later dried at 120 deg C under vacuum before electrochemical study
Scalability contextSmall sealed-vial solvothermal batch; 72 mg reported yield.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCu(NO3)2.3H2O108.7 mg, 0.45 mmol2 · Experimental section · Synthesis of 2D-CuTABQ
Linker2,3,5,6-tetraaminobenzoquinone (TABQ)50.4 mg, 0.3 mmol2 · Experimental section · Synthesis of 2D-CuTABQ
SolventDMSO12 mL + 6 mL2 · Experimental section · Synthesis of 2D-CuTABQ
Complete recipeSource: SI

Route 4: Drop Cast

3-4 · Electrochemical Measurements

SolventsN-methyl-2-pyrrolidone (NMP)
AdditivesSuper P carbon black and PVDF binder
Atmosphereelectrochemical cells assembled in Ar-filled glove box, H2O/O2 under 1.0 ppm
Temperature120 deg C vacuum pre-drying; 80 deg C vacuum electrode drying; room-temperature cycling
Time12 h vacuum pre-drying; 12 h electrode drying
Substrate orientationAl foil current collector
Oxidant / reductantmetallic Na counter electrode in half-cell
Work-upslurry coated on Al foil with doctor blade and dried; coin cells assembled with PP and glass fibre separators
Activationactive material dried at 120 deg C under vacuum for 12 h before electrode preparation
Scalability contextStandard slurry-cast battery electrode fabrication.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Other2D-CuTABQ active material6 parts by weight3-4 · Electrochemical Measurements
AdditiveSuper P carbon black3 parts by weight3-4 · Electrochemical Measurements
AdditivePVDF1 part by weight3-4 · Electrochemical Measurements
SolventNMPnot specified3-4 · Electrochemical Measurements
ElectrolyteNaPF6 in DMEnot specified · 1 M or 4 M3-4 · Electrochemical Measurements