cMOF Evidence Base

Synthesis evidence

Enhancing the energy storage performances of metal-organic frameworks by controlling microstructure

Gittins J.W., Balhatchet C.J., Fairclough S.M. et al. · Chemical Science · 2022 · 9210-9219

4 structured synthesis routes

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

Complete recipeSource: SI

Route 1: Hydrothermal

p003 · Synthesis: A-CuHHTP, C-CuHHTP

Metal precursorsCu(NO3)2.3H2O (0.127 g, 0.526 mmol, 1.65 eq)
Linker precursorsH6HHTP (0.103 g, 0.318 mmol, 1.00 eq)
Solventsdistilled water, 2 mL for Cu/modulator solution and 8.2 mL for H6HHTP dispersion
Additives35% aqueous ammonia solution, 50 eq, used as modulator
Atmospherehandled in air unless specified; stored in N2-filled glovebox after drying
Temperature80
Time24
Work-upDark blue precipitate separated by centrifugation; washed successively with water (3 x 30 mL), ethanol (3 x 30 mL), and acetone (3 x 30 mL); vacuum filtered.
ActivationDried at 80 C under dynamic vacuum for 96 h; stored in N2-filled glovebox.
Scalability context40 mL screw-top vial batch synthesis; no scale-up reported.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCu(NO3)2.3H2O0.127 g, 0.526 mmol, 1.65 eqp003 · Synthesis: A-CuHHTP, C-CuHHTP
LinkerH6HHTP0.103 g, 0.318 mmol, 1.00 eqp003 · Synthesis: A-CuHHTP, C-CuHHTP
Additive35% aqueous ammonia solution50 eq · 35%p003 · Synthesis: A-CuHHTP, C-CuHHTP
Solventdistilled water2 mL + 8.2 mLp003 · Synthesis: A-CuHHTP, C-CuHHTP
Complete recipeSource: SI

Route 2: Hydrothermal

p004 · Synthesis: B-CuHHTP

Metal precursorsCuSO4.5H2O (0.205 g, 0.820 mmol, 2.27 eq)
Linker precursorsH6HHTP (0.117 g, 0.361 mmol, 1.00 eq)
SolventsDMF (1.5 mL, 19.5 mmol, 54.0 eq) and H2O (12 mL + 9 mL distilled water)
AdditivesN,N-dimethylformamide (DMF), 54.0 eq, used as modulator and co-solvent
Atmospherehandled in air unless specified; stored in N2-filled glovebox after drying
Temperature80
Time12
Work-upDark blue precipitate separated by centrifugation; washed with water (3 x 30 mL), ethanol (3 x 30 mL), and acetone (3 x 30 mL); vacuum filtered and washed further on filter with water (250 mL), ethanol (250 mL), and acetone (250 mL).
ActivationDried at 80 C under dynamic vacuum for 96 h; stored in N2-filled glovebox.
Scalability context40 mL vial batch synthesis; no scale-up reported.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCuSO4.5H2O0.205 g, 0.820 mmol, 2.27 eqp004 · Synthesis: B-CuHHTP
LinkerH6HHTP0.117 g, 0.361 mmol, 1.00 eqp004 · Synthesis: B-CuHHTP
AdditiveN,N-dimethylformamide (DMF)1.5 mL, 19.5 mmol, 54.0 eqp004 · Synthesis: B-CuHHTP
SolventH2O / distilled water12 mL + 9 mLp004 · Synthesis: B-CuHHTP
Complete recipeSource: SI

Route 3: Hydrothermal

p003 · Synthesis: A-CuHHTP, C-CuHHTP

Metal precursorsCu(NO3)2.3H2O (0.127 g, 0.526 mmol, 1.65 eq)
Linker precursorsH6HHTP (0.103 g, 0.318 mmol, 1.00 eq)
Solventsdistilled water, 2 mL for Cu/modulator solution and 8.2 mL for H6HHTP dispersion
Additivespyridine, 50 eq, used as modulator
Atmospherehandled in air unless specified; stored in N2-filled glovebox after drying
Temperature80
Time24
Work-upDark blue precipitate separated by centrifugation; washed successively with water (3 x 30 mL), ethanol (3 x 30 mL), and acetone (3 x 30 mL); vacuum filtered.
ActivationDried at 80 C under dynamic vacuum for 96 h; stored in N2-filled glovebox.
Scalability context40 mL screw-top vial batch synthesis; no scale-up reported.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCu(NO3)2.3H2O0.127 g, 0.526 mmol, 1.65 eqp003 · Synthesis: A-CuHHTP, C-CuHHTP
LinkerH6HHTP0.103 g, 0.318 mmol, 1.00 eqp003 · Synthesis: A-CuHHTP, C-CuHHTP
Additivepyridine50 eqp003 · Synthesis: A-CuHHTP, C-CuHHTP
Solventdistilled water2 mL + 8.2 mLp003 · Synthesis: A-CuHHTP, C-CuHHTP
Partial recipeSource: SI

Route 4: Other

p005-p006 · Electrode Preparation; Supercapacitor Assembly

Metal precursorsCu3(HHTP)2 powder sample
Additivesacetylene black and PTFE
Atmosphereelectrodes dried in vacuo; cells assembled in N2-filled glovebox
Temperature80
Timeat least 24 h drying before cell assembly
Work-upFreestanding composite films cut into electrodes; assembled as symmetric CR2032 SS316 coin cells with glass microfiber separator.
ActivationElectrodes dried in vacuo at 80 C for at least 24 h; separator dried in vacuo at 100 C for 24 h.
Scalability contextFilm-making follows an existing literature method; exact mixing/shearing details are not repeated.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
OtherCu3(HHTP)2 powder85 wt% in final filmp005-p006 · Electrode Preparation; Supercapacitor Assembly
Additiveacetylene black10 wt% in final filmp005-p006 · Electrode Preparation; Supercapacitor Assembly
AdditivePTFE5 wt% in final filmp005-p006 · Electrode Preparation; Supercapacitor Assembly
Electrolyte1 M NEt4BF4/ACN or undiluted EMIM-BF410 drops from a Pasteur pipette per cell · 1 M NEt4BF4/ACN; EMIM-BF4 6.6 M in SI, 6.3 M in main textp005-p006 · Electrode Preparation; Supercapacitor Assembly