cMOF Evidence Base

Synthesis evidence

Conductive Metal-Organic Framework Thin Film Hybrids by Electropolymerization of Monosubstituted Acetylenes

Klyatskaya S., Kanj A.B., Molina-Jiron C. et al. · ACS Applied Materials and Interfaces · 2020 · 30972-30979

4 structured synthesis routes

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

Complete recipeSource: Both

Route 1: Electrochemical

SI p.S-2 · 1-Hexyne loading and Electropolymerization · Figure S6

Metal precursors1-hexyne-loaded Cu(BDC) SURMOF-2 cathode
Solventsdichloromethane
Additives0.1 M tetrabutylammonium hexafluorophosphate (TBAHFP) supporting electrolyte
Atmosphereargon used during loading; electrochemical solution described as dichloromethane/TBAHFP
Temperatureroom temperature
Time0.25 h
Substrate orientationtwo-compartment cell; SURMOF substrate as cathode; Ag-strip anode, S about 3 cm2
Oxidant / reductantCathodic reduction/electroinitiated polymerisation under negative DC voltage
Work-upNo isolation required for in situ I-V; separate MALDI workup dissolved film in ethanolic acetic acid.
ActivationImmediate use after loading and dichloromethane rinse.
Scalability contextConstant-voltage two-electrode setup used to overcome low currents through the pristine SURMOF cathode.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
ElectrolyteTBAHFP15 ml solution in both compartments · 0.1 MSI p.S-2 · 1-Hexyne loading and Electropolymerization · Figure S6
Solventdichloromethane15 mlSI p.S-2 · 1-Hexyne loading and Electropolymerization · Figure S6
OtherAg-strip electrodeS about 3 cm2SI p.S-2 · 1-Hexyne loading and Electropolymerization · Figure S6
Partial recipeSource: Both

Route 2: Other

SI p.S-1 · Sample preparation

Metal precursorsCu2(CH3COO)4.H2O, 1 mM ethanolic solution (raw SI formula)
Linker precursors1,4-benzenedicarboxylic acid (BDC), 0.2 mM ethanolic solution
SolventsEthanol
Additives16-mercaptohexadecanoic acid (MHDA) self-assembled monolayer on Au
Atmospherenot specified for spray growth
Temperatureroom temperature
Substrate orientation150 nm Au / 5 nm Ti on Si wafer; MHDA-functionalised Au surface; oriented SURMOF layer
Work-upAfter synthesis all samples were characterised with XRD.
Scalability contextSI describes a high-throughput spray method and the main text cites layer-by-layer growth of monolithic oriented films.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCu2(CH3COO)4.H2O1 mM in ethanolSI p.S-1 · Sample preparation
Linker1,4-benzenedicarboxylic acid (BDC)0.2 mM in ethanolSI p.S-1 · Sample preparation
Additive16-mercaptohexadecanoic acid (MHDA)self-assembled monolayer on AuSI p.S-1 · Sample preparation
SolventethanolNot specifiedSI p.S-1 · Sample preparation
Complete recipeSource: Both

Route 3: Other

SI p.S-1 · 1-Hexyne loading and Electropolymerization

Metal precursorspreformed Cu(BDC) SURMOF-2 thin film
Solventsdry dichloromethane
Atmosphereargon
Temperatureambient temperature for loading; 80 C for activation
Timeabout 45 h loading; 1 h activation
Substrate orientationactivated SURMOF-2 samples with area about 1 cm2
Work-upRinsed with fresh dichloromethane and immediately used as cathode.
ActivationHeated under argon at 80 C for 60 min to evaporate excess synthesis solvent; stability verified by XRD.
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
Other1-Hexyne (C6H10)2 ml solution · 20 mMSI p.S-1 · 1-Hexyne loading and Electropolymerization
Solventdry dichloromethaneNot specifiedSI p.S-1 · 1-Hexyne loading and Electropolymerization
Complete recipeSource: SI

Route 4: Other

SI p.S-2 · MALDI-ToF Analysis

Metal precursorsBPA@Cu(BDC)-SURMOF-2 thin film after EP
Solventsethanol, acetic acid, dichloromethane
Additives3,5-dimethoxy-4-hydroxycinnamic acid (sinapinic acid) MALDI matrix
Atmosphereair dried before MALDI
Substrate orientationSURMOF-2 thin film substrate about 2 x 0.5 cm2
Work-upFilm dissolved by immersion in acetic acid/ethanol; aliquot mixed with matrix solution and spotted onto MALDI target.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Acidacetic acid250 uLSI p.S-2 · MALDI-ToF Analysis
Solventethanol0.2 mLSI p.S-2 · MALDI-ToF Analysis
Additivesinapinic acid5 mg in 1 mL dichloromethane; 0.5 uL matrix mixed with 0.5 uL sample · 5 mg/mLSI p.S-2 · MALDI-ToF Analysis