Synthesis · From 0D to 2D: Microwave-assisted synthesis of electrically conductive metal-organic frameworks with controlled morphologies

9 structured synthesis routes

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

Complete recipeSource: SI

Route 1: Other

SI p.S3 · Synthesis of Cu-HHTP

Metal precursorsCu(NO3)2.2.5H2O (0.0355 g, 0.15 mmol).

Linker precursorsHHTP ligand (0.0259 g, 0.08 mmol).

SolventsDMF (10 mL); wash solvents acetone, H2O, DMF and ethanol.

AdditivesTemperature-controlled ultrasonication with ice bath.

AtmosphereNot specified for synthesis; drying under reduced pressure.

Temperature0 deg C ultrasonication bath for 1 h; microwave at 100 deg C for 15 min; dry at 70 deg C.

Time1 h ultrasonication plus 0.25 h microwave reaction.

Work-upBlack precipitate isolated by centrifugation; washed with acetone (35 mL), H2O (2 x 15 mL), DMF (2 x 15 mL), ethanol (2 x 15 mL).

ActivationDried in a 70 deg C oven under reduced pressure for further characterization.

Scalability contextYield after solvent removal was 0.0055 g (16%).

Show 7 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Cu(NO3)2.2.5H2O	0.0355 g, 0.15 mmol	SI p.S3 · Synthesis of Cu-HHTP
Linker	HHTP ligand	0.0259 g, 0.08 mmol	SI p.S3 · Synthesis of Cu-HHTP
Solvent	DMF	10 mL	SI p.S3 · Synthesis of Cu-HHTP
Solvent	acetone wash	35 mL	SI p.S3 · Synthesis of Cu-HHTP
Solvent	H2O wash	2 x 15 mL	SI p.S3 · Synthesis of Cu-HHTP
Solvent	DMF wash	2 x 15 mL	SI p.S3 · Synthesis of Cu-HHTP
Solvent	ethanol wash	2 x 15 mL	SI p.S3 · Synthesis of Cu-HHTP

Complete recipeSource: SI

Route 2: Other

SI p.S3 · Synthesis of Cu-HHTP

Metal precursorsCu(NO3)2.2.5H2O (0.0355 g, 0.15 mmol).

Linker precursorsHHTP ligand (0.0259 g, 0.08 mmol).

SolventsDMF (10 mL); wash solvents acetone, H2O, DMF and ethanol.

AdditivesBrief sonication to dissolve reactants; no additional modulator reported.

AtmosphereNot specified for synthesis; drying under reduced pressure.

TemperatureMicrowave at 100 deg C for 15 min; dry at 70 deg C.

Time0.25 h microwave reaction.

Work-upBlack precipitate isolated by centrifugation; washed with acetone (35 mL), H2O (2 x 15 mL), DMF (2 x 15 mL), ethanol (2 x 15 mL).

ActivationDried in a 70 deg C oven under reduced pressure for further characterization.

Scalability contextYield after solvent removal was 0.0062 g (19%).

Show 7 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Cu(NO3)2.2.5H2O	0.0355 g, 0.15 mmol	SI p.S3 · Synthesis of Cu-HHTP
Linker	HHTP ligand	0.0259 g, 0.08 mmol	SI p.S3 · Synthesis of Cu-HHTP
Solvent	N,N-Dimethylformamide (DMF)	10 mL	SI p.S3 · Synthesis of Cu-HHTP
Solvent	acetone wash	35 mL	SI p.S3 · Synthesis of Cu-HHTP
Solvent	H2O wash	2 x 15 mL	SI p.S3 · Synthesis of Cu-HHTP
Solvent	DMF wash	2 x 15 mL	SI p.S3 · Synthesis of Cu-HHTP
Solvent	ethanol wash	2 x 15 mL	SI p.S3 · Synthesis of Cu-HHTP

Complete recipeSource: SI

Route 3: Other

SI p.S3 · Synthesis of Cu-HHTP

Metal precursorsCu(NO3)2.2.5H2O (0.0355 g, 0.15 mmol).

Linker precursorsHHTP ligand (0.0259 g, 0.08 mmol).

SolventsDMF (4 mL) plus H2O (2 mL) for HHTP; H2O (4 mL) plus NH4OH (0.6 mL) for copper source; wash solvents H2O, DMF and ethanol.

AdditivesNH4OH (0.6 mL).

AtmosphereNot specified for synthesis; drying under reduced pressure.

TemperatureMicrowave at 100 deg C for 15 min; dry at 70 deg C.

Time0.25 h microwave reaction.

Work-upBlack precipitate isolated by centrifugation; washed with H2O (2 x 15 mL), DMF (2 x 15 mL), and ethanol (2 x 10 mL).

ActivationDried in a 70 deg C oven under reduced pressure for further characterization.

Scalability contextYield after solvent removal was 0.0245 g (74%).

Show 9 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Cu(NO3)2.2.5H2O	0.0355 g, 0.15 mmol	SI p.S3 · Synthesis of Cu-HHTP
Linker	HHTP ligand	0.0259 g, 0.08 mmol	SI p.S3 · Synthesis of Cu-HHTP
Solvent	DMF	4 mL	SI p.S3 · Synthesis of Cu-HHTP
Solvent	H2O for HHTP solution	2 mL	SI p.S3 · Synthesis of Cu-HHTP
Solvent	H2O for Cu solution	4 mL	SI p.S3 · Synthesis of Cu-HHTP
Base	NH4OH	0.6 mL	SI p.S3 · Synthesis of Cu-HHTP
Solvent	H2O wash	2 x 15 mL	SI p.S3 · Synthesis of Cu-HHTP
Solvent	DMF wash	2 x 15 mL	SI p.S3 · Synthesis of Cu-HHTP
Solvent	ethanol wash	2 x 10 mL	SI p.S3 · Synthesis of Cu-HHTP

Complete recipeSource: SI

Route 4: Drop Cast

SI p.S2 · Electrochemical Measurements

SolventsIPA (2 mL) for slurry; 0.5 M Na2SO4 aqueous electrolyte.

AdditivesNafion (5 wt%, 5 uL).

AtmosphereNa2SO4 electrolyte prepared in degassed water.

Time30 min sonication of slurry.

Substrate orientation1 cm x 2 cm ITO glass electrode, back-illuminated through ITO.

Work-up0.05 g MOF powder ground with Nafion, mixed with IPA under sonication, then drop-cast on ITO glass.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	MOF powders	0.05 g	SI p.S2 · Electrochemical Measurements
Additive	Nafion	5 uL · 5 wt%	SI p.S2 · Electrochemical Measurements
Solvent	IPA	2 mL	SI p.S2 · Electrochemical Measurements
Electrolyte	Na2SO4	7.10 g in 100 mL degassed water · 0.5 M	SI p.S2 · Electrochemical Measurements

Complete recipeSource: SI

Route 5: Drop Cast

SI p.S2 · Electrochemical Measurements

SolventsIPA (2 mL) for slurry; 0.5 M Na2SO4 aqueous electrolyte.

AdditivesNafion (5 wt%, 5 uL).

AtmosphereNa2SO4 electrolyte prepared in degassed water.

Time30 min sonication of slurry.

Substrate orientation1 cm x 2 cm ITO glass electrode, back-illuminated through ITO.

Work-up0.05 g MOF powder ground with Nafion, mixed with IPA under sonication, then drop-cast on ITO glass.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	MOF powders	0.05 g	SI p.S2 · Electrochemical Measurements
Additive	Nafion	5 uL · 5 wt%	SI p.S2 · Electrochemical Measurements
Solvent	IPA	2 mL	SI p.S2 · Electrochemical Measurements
Electrolyte	Na2SO4	7.10 g in 100 mL degassed water · 0.5 M	SI p.S2 · Electrochemical Measurements

Complete recipeSource: SI

Route 6: Drop Cast

SI p.S2 · Electrochemical Measurements

SolventsIPA (2 mL) for slurry; 0.5 M Na2SO4 aqueous electrolyte.

AdditivesNafion (5 wt%, 5 uL).

AtmosphereNa2SO4 electrolyte prepared in degassed water.

Time30 min sonication of slurry.

Substrate orientation1 cm x 2 cm ITO glass electrode, back-illuminated through ITO.

Work-up0.05 g MOF powder ground with Nafion, mixed with IPA under sonication, then drop-cast on ITO glass.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	MOF powders	0.05 g	SI p.S2 · Electrochemical Measurements
Additive	Nafion	5 uL · 5 wt%	SI p.S2 · Electrochemical Measurements
Solvent	IPA	2 mL	SI p.S2 · Electrochemical Measurements
Electrolyte	Na2SO4	7.10 g in 100 mL degassed water · 0.5 M	SI p.S2 · Electrochemical Measurements

Complete recipeSource: SI

Route 7: Drop Cast

SI p.S2 · Electrochemical Measurements

Solvents0.1 M TEBF4 in acetonitrile used as electrolyte for electrochemical measurements.

AdditivesPTFE binder solution (60 wt% in H2O).

AtmosphereElectrolyte degassed for 10 min with nitrogen before measurements.

Substrate orientationGlassy carbon working electrode.

Work-upInk composed of 80 wt% MOF powder and 20 wt% PTFE binder was drop-cast on glassy carbon.

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	MOF powders	80 wt% of ink	SI p.S2 · Electrochemical Measurements
Additive	PTFE binder solution	20 wt% of ink · 60 wt% in H2O	SI p.S2 · Electrochemical Measurements
Electrolyte	tetraethylammonium tetrafluoroborate (TEBF4)	4.34 g in 200 mL acetonitrile · 0.1 M	SI p.S2 · Electrochemical Measurements

Complete recipeSource: SI

Route 8: Drop Cast

SI p.S2 · Electrochemical Measurements

Solvents0.1 M TEBF4 in acetonitrile used as electrolyte for electrochemical measurements.

AdditivesPTFE binder solution (60 wt% in H2O).

AtmosphereElectrolyte degassed for 10 min with nitrogen before measurements.

Substrate orientationGlassy carbon working electrode.

Work-upInk composed of 80 wt% MOF powder and 20 wt% PTFE binder was drop-cast on glassy carbon.

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	MOF powders	80 wt% of ink	SI p.S2 · Electrochemical Measurements
Additive	PTFE binder solution	20 wt% of ink · 60 wt% in H2O	SI p.S2 · Electrochemical Measurements
Electrolyte	tetraethylammonium tetrafluoroborate (TEBF4)	4.34 g in 200 mL acetonitrile · 0.1 M	SI p.S2 · Electrochemical Measurements

Complete recipeSource: SI

Route 9: Drop Cast

SI p.S2 · Electrochemical Measurements

Solvents0.1 M TEBF4 in acetonitrile used as electrolyte for electrochemical measurements.

AdditivesPTFE binder solution (60 wt% in H2O).

AtmosphereElectrolyte degassed for 10 min with nitrogen before measurements.

Substrate orientationGlassy carbon working electrode.

Work-upInk composed of 80 wt% MOF powder and 20 wt% PTFE binder was drop-cast on glassy carbon.

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	MOF powders	80 wt% of ink	SI p.S2 · Electrochemical Measurements
Additive	PTFE binder solution	20 wt% of ink · 60 wt% in H2O	SI p.S2 · Electrochemical Measurements
Electrolyte	tetraethylammonium tetrafluoroborate (TEBF4)	4.34 g in 200 mL acetonitrile · 0.1 M	SI p.S2 · Electrochemical Measurements