cMOF Evidence Base

Synthesis evidence

Microscopic Origin of Electrochemical Capacitance in Metal-Organic Frameworks

Shin S.-J., Gittins J.W., Golomb M.J. et al. · Journal of the American Chemical Society · 2023 · 14529-14538

2 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

14535 · Material Synthesis

Metal precursorsCu3(HHTP)2 powder
Solventsethanol ca. 1.5 mL plus a few drops during PTFE addition
Additivesacetylene black; PTFE dispersion (60 wt% in water)
Atmosphereambient conditions for stirring; in vacuo drying
Temperature100
Time0.25 sonication; 0.667 hand stirring; 0.333 kneading; at least 48 drying
Substrate orientationfreestanding film rolled with homemade aluminium rolling pin
Work-upElectroactive components ground, slurried in ethanol, sonicated, mixed with PTFE dispersion, dried, kneaded and rolled.
ActivationDried in vacuo at 100 deg C for at least 48 h to remove ethanol.
Scalability contextAll final film mass fractions and thickness are reported, but exact component masses are not given.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
OtherCu3(HHTP)2 powder85 wt% in final film14535 · Material Synthesis
Additiveacetylene black10 wt% in final film · measured BET area = 62 m2 g^-114535 · Material Synthesis
AdditivePTFE dispersion5 wt% PTFE in final film · 60 wt% in water14535 · Material Synthesis
Solventethanolca. 1.5 mL plus a few drops14535 · Material Synthesis
Complete recipeSource: Both

Route 2: Other

14535 · Material Synthesis

Metal precursorsCu(NO3)2.3H2O (0.127 g, 0.526 mmol, 1.65 equiv)
Linker precursorsHHTP (0.103 g, 0.318 mmol, 1.00 equiv)
Solventsdistilled water; metal/ammonia solution in 2 mL water; HHTP dispersion in 8.2 mL water
Additivesaqueous ammonia (35%, 0.883 mL, 50 equiv)
Atmospherestored in N2-filled glovebox after drying; synthesis atmosphere not otherwise specified
Temperature80
Time24 reaction; 96 drying
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.
ActivationDried at 80 deg C under dynamic vacuum for 96 h.
Scalability contextPreviously published procedure used; batch amounts are reported.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCu(NO3)2.3H2O0.127 g; 0.526 mmol; 1.65 eq14535 · Material Synthesis
Baseaqueous ammonia0.883 mL; 50 equiv · 35%14535 · Material Synthesis
Solventdistilled water2 mL for Cu/ammonia solution; 8.2 mL for HHTP dispersion14535 · Material Synthesis
LinkerHHTP0.103 g; 0.318 mmol; 1.00 equiv14535 · Material Synthesis