Synthesis evidence

Charge-transfer interface of insulating metal-organic frameworks with metallic conduction

Sindhu P., Ananthram K.S., Jain A. et al. · Nature Communications · 2022 · 7665

4 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

8 · Methods/Fabrication of pristine Cu-BPyDC thin film

Metal precursors1 mM Cu(OAc)2.H2O in DMF
Linker precursors1 mM BPyDC solution in DMF
SolventsDMF; FTO cleaning in acetone, ethanol and water
AdditivesFTO functionalisation: conc. KOH (2 mmol) aqueous solution and 30% H2O2, 3:1 volume ratio
AtmosphereN2 drying stream
Temperature56.85
Time10
Substrate orientationfunctionalised FTO coated glass substrate
Oxidant / reductantH2O2/KOH used only for FTO functionalisation
Work-upwashed with DMF between steps to remove uncoordinated metal ions; dried with N2 gas
Scalability contextLayer-by-layer thin-film recipe; no scale-up data reported.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCu(OAc)2.H2O1 mM8 · Methods/Fabrication of pristine Cu-BPyDC thin film
LinkerBPyDC solution1 mM8 · Methods/Fabrication of pristine Cu-BPyDC thin film
SolventDMFNot specified8 · Methods/Fabrication of pristine Cu-BPyDC thin film
AdditiveKOH aqueous solution and H2O2 for FTO functionalisationKOH 2 mmol; KOH:H2O2 volume ratio 3:1 · H2O2 30%8 · Methods/Fabrication of pristine Cu-BPyDC thin film
Complete recipeSource: Main

Route 2: Other

8 · Methods/Fabrication of pristine Cu-TCNQ thin film

Metal precursors1 mM ethanolic Cu(OAc)2.H2O
Linker precursors1 mM ethanolic TCNQ
Solventsethanol; FTO cleaning in acetone, ethanol and water
AdditivesFTO functionalisation: conc. KOH (2 mmol) aqueous solution and 30% H2O2, 3:1 volume ratio
AtmosphereN2 drying stream
Temperature56.85
Time10
Substrate orientationFTO coated glass substrate
Oxidant / reductantinterfacial reduction of Cu(II) to Cu(I) during Cu-TCNQ formation; H2O2/KOH used only for FTO functionalisation
Work-upwashed with ethanol between steps; dried with N2 gas
Scalability contextLayer-by-layer thin-film recipe; no scale-up data reported.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCu(OAc)2.H2O1 mM8 · Methods/Fabrication of pristine Cu-TCNQ thin film
LinkerTCNQ1 mM8 · Methods/Fabrication of pristine Cu-TCNQ thin film
SolventethanolNot specified8 · Methods/Fabrication of pristine Cu-TCNQ thin film
Complete recipeSource: Main

Route 3: Other

8 · Methods/Fabrication of Cu-TCNQ/Cu-BPyDC hetero-structured thin film

Metal precursorsCu(OAc)2.H2O ethanolic solution used during Cu-TCNQ growth on prefabricated Cu-BPyDC
Linker precursorsTCNQ ethanolic solution; prefabricated Cu-BPyDC thin film
Solventsethanol; Cu-BPyDC base film prepared in DMF
AtmosphereN2 drying stream
Time8.333
Substrate orientationprefabricated Cu-BPyDC thin film on FTO; Cu-TCNQ grown on top
Oxidant / reductantinterfacial reduction reaction (IRR) forms Cu(I)-TCNQ from Cu(II) precursor
Work-upwashed with ethanol between dips; dried with N2 gas
Scalability contextLayer-by-layer heterostructure recipe; no scale-up data reported.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCu(OAc)2.H2ONot specified8 · Methods/Fabrication of Cu-TCNQ/Cu-BPyDC hetero-structured thin film
LinkerTCNQNot specified8 · Methods/Fabrication of Cu-TCNQ/Cu-BPyDC hetero-structured thin film
SolventethanolNot specified8 · Methods/Fabrication of Cu-TCNQ/Cu-BPyDC hetero-structured thin film
Otherprefabricated pristine Cu-BPyDC thin filmNot specified8 · Methods/Fabrication of Cu-TCNQ/Cu-BPyDC hetero-structured thin film
Complete recipeSource: Main

Route 4: Other

8 · Methods/Fabrication of TCNQ@Cu-BPyDC thin film

Metal precursorsprefabricated pristine Cu-BPyDC thin film
Linker precursorsTCNQ guest/dopant
Solventsethanol
AtmosphereN2 drying stream
Time48
Substrate orientationprefabricated Cu-BPyDC thin film on FTO
Work-upwashed with ethanol to remove surface adsorbed TCNQ and dried under N2
Scalability contextGuest-loading comparison route; no scale-up data reported.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
LinkerTCNQsaturated ethanolic solution8 · Methods/Fabrication of TCNQ@Cu-BPyDC thin film
SolventethanolNot specified8 · Methods/Fabrication of TCNQ@Cu-BPyDC thin film
Otherprefabricated pristine Cu-BPyDC thin filmNot specified8 · Methods/Fabrication of TCNQ@Cu-BPyDC thin film