cMOF Evidence Base

Synthesis evidence

Insights into the electric double-layer capacitance of two-dimensional electrically conductive metal-organic frameworks

Gittins J.W., Balhatchet C.J., Chen Y. et al. · Journal of Materials Chemistry A · 2021 · 16006-16015

6 structured synthesis routes

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

Complete recipeSource: Main

Route 1: Other

p007 · Electrode film preparation

Solventsethanol ca. 1.5 mL plus a few drops
Additivesacetylene black; PTFE dispersion (60 wt% in water)
AtmosphereGrinding/slurry processing under ambient conditions; EDLC electrode cutting later in N2-filled glovebox.
Temperature75
Time>=48
Substrate orientationfreestanding film rolled on glass surface
Work-upLightly grind Cu3(HHTP)2 powder and acetylene black; add ethanol slurry; sonicate 15 min; add to PTFE dispersion; stir by hand 40 min; dry gradually; knead 20 min; roll with aluminium rolling pin.
ActivationDry in vacuo at 75 C for at least 48 h.
Scalability contextAdapted standard activated-carbon film fabrication method.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
OtherCu3(HHTP)2 powder85 wt% final filmp007 · Electrode film preparation
Additiveacetylene black10 wt% final filmp007 · Electrode film preparation
AdditivePTFE dispersion5 wt% final film as PTFE · 60 wt% in waterp007 · Electrode film preparation
Solventethanolca. 1.5 mL plus dropsp007 · Electrode film preparation
Partial recipeSource: Main

Route 2: Other

p007 · Electrode film preparation

Solventsethanol
AdditivesPTFE dispersion (60 wt% in water); no conductive carbon additive
AtmosphereFilm preparation by same technique; atmosphere not otherwise specified.
Temperature75
Time>=48
Substrate orientationfreestanding film
Work-upSame freestanding-film technique as composite electrodes, excluding conductive additive.
ActivationDry in vacuo at 75 C for at least 48 h.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
OtherCu3(HHTP)2 powder95 wt% final filmp007 · Electrode film preparation
AdditivePTFE5 wt% final filmp007 · Electrode film preparation
SolventethanolNot specifiedp007 · Electrode film preparation
Complete recipeSource: Main

Route 3: Hydrothermal

p006 · Synthesis of Cu3(HHTP)2

Metal precursorsCu(NO3)2.3H2O (0.127 g, 0.526 mmol, 1.65 eq.)
Linker precursors2,3,6,7,10,11-hexahydroxytriphenylene hydrate, H6HHTP.xH2O (0.103 g, 0.318 mmol, 1.00 eq.)
Solventsdistilled water: 2 mL for Cu/ammonia solution plus 8.4 mL for linker dispersion
Additivesaqueous ammonia (35%) solution (0.829 mL, 15.0 mmol, 47 eq.)
AtmosphereProduct stored in N2-filled glovebox; synthesis atmosphere not specified.
Temperature80
Time24
Work-upCentrifuge; discard supernatant; wash with water (3 x 30 mL), ethanol (4 x 30 mL), acetone (4 x 30 mL), centrifuging 15-30 min each wash; vacuum filter.
ActivationDry at 75 C under dynamic vacuum for 72 h; rapid washing/activation completed in ca. 5 h to minimise air exposure.
Scalability contextAuthors note all starting materials are commercially available.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCu(NO3)2.3H2O0.127 g, 0.526 mmol, 1.65 eq.p006 · Synthesis of Cu3(HHTP)2
Baseaqueous ammonia (35%) solution0.829 mL, 15.0 mmol, 47 eq. · 35%p006 · Synthesis of Cu3(HHTP)2
Solventdistilled water2 mL + 8.4 mLp006 · Synthesis of Cu3(HHTP)2
Linker2,3,6,7,10,11-hexahydroxytriphenylene hydrate, H6HHTP.xH2O0.103 g, 0.318 mmol, 1.00 eq.p006 · Synthesis of Cu3(HHTP)2
Complete recipeSource: Main

Route 4: Other

p007 · Conductivity measurements

Time0.083
Substrate orientation13 mm pellet die
Work-upPress Cu3(HHTP)2 powder in 13 mm evacuable pellet die at 3 ton-force cm-2 for 5 min.
Show 1 structured reagent record
RoleReagentAmount / concentrationSource
OtherCu3(HHTP)2 powderareal mass loading approximately 50 mg cm-2p007 · Conductivity measurements
Complete recipeSource: Main

Route 5: Other

p007 · EDLC assembly

Solventsanhydrous acetonitrile
Additives1 M NEt4BF4 electrolyte; GF/A separator
AtmosphereElectrode cutting and electrolyte preparation in N2-filled glovebox; separator dried before use.
Substrate orientationSwagelok PFA-820-6 union tube fitting
Work-upCut electrodes from freestanding films in N2-filled glovebox; assemble symmetric EDLCs with stainless-steel plugs/current collectors and dried GF/A separator; hand-seal air-tight.
ActivationGF/A separator dried in vacuo at 100 C for 24 h; acetonitrile purged with N2 and dried over activated 3 A molecular sieves.
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
ElectrolyteNEt4BF4 in anhydrous acetonitrileexcess · 1 Mp007 · EDLC assembly
OtherWhatman glass microfiber filter (GF/A)separatorp007 · EDLC assembly
Complete recipeSource: Main

Route 6: Other

p007 · EDLC assembly

Solventsanhydrous acetonitrile for electrolyte
AdditivesPTFE binder; 1 M NEt4BF4 electrolyte
AtmosphereN2-filled glovebox for assembly; electrodes dried before assembly.
Temperature100
Time>=24
Substrate orientationCR2032 SS316 coin cell cases
Work-upPrepare 95 wt% YP50F/5 wt% PTFE freestanding film using same technique; cut electrodes with 10-15 mg cm-2 areal mass loadings; assemble coin cells.
ActivationElectrodes and GF/A separator dried in vacuo at 100 C for at least 24 h before assembly.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
OtherYP50F activated carbon95 wt% electroactive material in filmp007 · EDLC assembly
AdditivePTFE5 wt% in filmp007 · EDLC assembly
ElectrolyteNEt4BF4 in anhydrous acetonitrile1 Mp007 · EDLC assembly