Synthesis evidence

Conjugated Copper–Catecholate Framework Electrodes for Efficient Energy Storage

Liu J., Zhou Y., Xie Z. et al. · Angewandte Chemie - International Edition · 2020 · 1081-1086

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: Other

S4 · Preparation the free-standing Cu-DBC film electrode · Scheme S2

SolventsSmall amount of ethanol; PTFE binder solution in water
AdditivesCarbon black and PTFE binder
AtmosphereVacuum drying
Temperature70
TimeOvernight drying
Work-upGround Cu-DBC/carbon black, added PTFE binder and ethanol, kneaded into paste, rolled into free-standing film.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
OtherCu-DBC powder10 mgS4 · Preparation the free-standing Cu-DBC film electrode · Scheme S2
Additivecarbon black2 mgS4 · Preparation the free-standing Cu-DBC film electrode · Scheme S2
AdditivePTFE binder solution16 uL · 10 wt% in H2OS4 · Preparation the free-standing Cu-DBC film electrode · Scheme S2
Solventethanolsmall amountS4 · Preparation the free-standing Cu-DBC film electrode · Scheme S2
Complete recipeSource: SI

Route 2: Drop Cast

S4 · Standard three-electrode system measurements

Solvents0.3 mL isopropanol vehicle
Additives0.3 mg carbon black; 30 uL 5% Nafion solution
AtmosphereAir drying
TimeAt least 1 h drying before measurement
Substrate orientationPre-polished glassy carbon electrode, 0.0707 cm2
Work-upUltrasonically mixed for 30 min; 5 uL slurry pipetted and spread onto GCE; dried in air.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Otheras-prepared Cu-DBC powder3.0 mgS4 · Standard three-electrode system measurements
Additivecarbon black0.3 mgS4 · Standard three-electrode system measurements
AdditiveNafion solution30 uL · 5%S4 · Standard three-electrode system measurements
Solventisopropanol0.3 mLS4 · Standard three-electrode system measurements
Complete recipeSource: Both

Route 3: Solvothermal

S3 · Section 2. Synthetic Procedures · Scheme S1

Metal precursorsCu(OAc)2.H2O
Linker precursors8OH-DBC ligand
SolventsDegassed N,N-dimethylformamide and degassed deionized water; SI recipe 500 uL DMF plus 2 mL water, main text v/v = 1:4.
AtmosphereMain text: argon atmosphere; SI: degassed solvents.
Temperature85
Time72
Work-upWashed with water and acetone several times; dried overnight under vacuum at room temperature.
ActivationFor gas sorption, samples were activated at 120 C for 12 h under vacuum (10-5 bar).
Scalability contextSmall-vial microcrystal synthesis; no scale-up study reported.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Linker8OH-DBC ligand8.6 mgS3 · Section 2. Synthetic Procedures · Scheme S1
Metal SourceCu(OAc)2.H2O6 mgS3 · Section 2. Synthetic Procedures · Scheme S1
Solventdegassed dimethyformamide (DMF)500 uLS3 · Section 2. Synthetic Procedures · Scheme S1
Solventdegassed deionized water2 mLS3 · Section 2. Synthetic Procedures · Scheme S1
Complete recipeSource: SI

Route 4: Other

S4 · Preparation Two-electrode symmetrical Solid-State cell · Scheme S2

Solvents30 uL 1 mol L-1 NaCl aqueous electrolyte
AdditivesNKK-MPF30AC-100 membrane separator
Substrate orientationTwo identical 3 x 3 mm2 free-standing Cu-DBC film pieces
Work-upFilm cut into small slices and assembled with separator/electrolyte in a coin-shaped symmetric cell.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Otherfreestanding Cu-DBC filmstwo pieces; 3 x 3 mm2; active mass about 2.22 mg cm-2S4 · Preparation Two-electrode symmetrical Solid-State cell · Scheme S2
AdditiveNKK-MPF30AC-100 membraneNot specifiedS4 · Preparation Two-electrode symmetrical Solid-State cell · Scheme S2
ElectrolyteNaCl aqueous solution30 uL · 1 mol L-1S4 · Preparation Two-electrode symmetrical Solid-State cell · Scheme S2