cMOF Evidence Base

Synthesis evidence

Semiconducting to Metallic Electronic Landscapes in Defects-Controlled 2D π-d Conjugated Coordination Polymer Thin Films

Ogle J., Lahiri N., Jaye C. et al. · Advanced Functional Materials · 2021 · 2006920

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: Cvd

10 · Experimental Section, Fabrication of Cu-BHT Thin Films · Figure S6B

Metal precursorsCuSO4.5H2O in H2O:ethanol:ethanolamine solution, spin-coated as Cu(II) precursor film on glass
Linker precursors50 mg BHT precursor in a ceramic boat
SolventsH2O:ethanol:ethanolamine = 1:1:0.025 for Cu(II) precursor coating solution
Additivesethanolamine in Cu(II) precursor coating solution
AtmosphereCu precursor spin-cast under inert atmosphere; nitrogen carrier gas 120-150 sccm; vacuum pressure <5 x 10^-3 Torr
TemperatureCu precursor film anneal 70 deg C for 10 min; BHT sublimation 140 deg C; glass substrate/Cu precursor zone 120 deg C
Substrate orientationCu(II)-precursor-coated glass substrate placed in right heating zone approximately 30 cm from tube-furnace edge; BHT boat in left zone approximately 10 cm from edge
Oxidant / reductantCu(II) precursor is reduced to Cu(I) during Cu-BHT formation; no separate reductant for framework CVD step reported
Work-upBHT vapour reacted with Cu(II) precursor to yield a dark blue/black film
Scalability contextProduces continuous large-area films over 1 inch x 1 inch glass substrates; film thickness controlled by spin-coating speed for metal salt and CVD reaction time.
Show 6 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCuSO4.5H2O85 mm · 85 mm in 1:1:0.025 H2O:ethanol:ethanolamine solution10 · Experimental Section, Fabrication of Cu-BHT Thin Films · Figure S6B
SolventH2O1 part10 · Experimental Section, Fabrication of Cu-BHT Thin Films · Figure S6B
Solventethanol1 part10 · Experimental Section, Fabrication of Cu-BHT Thin Films · Figure S6B
Additiveethanolamine0.025 part10 · Experimental Section, Fabrication of Cu-BHT Thin Films · Figure S6B
LinkerBHT precursor50 mg10 · Experimental Section, Fabrication of Cu-BHT Thin Films · Figure S6B
Othernitrogen carrier gas120-150 sccm10 · Experimental Section, Fabrication of Cu-BHT Thin Films · Figure S6B
Complete recipeSource: Both

Route 2: Cvd

10 · Experimental Section, Fabrication of Cu-BHT Thin Films · Figure S6A

Metal precursors50 mg copper(II) acetylacetonate, Cu(acac)2, in a ceramic boat
Linker precursors50 mg benzenehexathiol (BHT) precursor in a ceramic boat
Atmospherenitrogen carrier gas, 120-150 sccm; vacuum pressure <5 x 10^-3 Torr
TemperatureBHT zone 120 deg C; Cu(acac)2 zone 80 deg C
Time6
Substrate orientationglass substrates at tube centre, approximately 15-25 cm in each direction from tube centre/reaction interface
Oxidant / reductantCu(II) precursor is reduced to Cu(I) during Cu-BHT formation; no separate reductant for framework CVD step reported
Work-upRecovered glass substrates from the reaction zone where a dark blue/black film formed
Scalability contextProduces continuous large-area films over 1 inch x 1 inch glass substrates; thickness controlled by BHT and Cu(acac)2 deposition temperatures and reaction times.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
LinkerBHT precursor50 mg10 · Experimental Section, Fabrication of Cu-BHT Thin Films · Figure S6A
Metal SourceCu(acac)2 precursor50 mg10 · Experimental Section, Fabrication of Cu-BHT Thin Films · Figure S6A
Othernitrogen carrier gas120-150 sccm10 · Experimental Section, Fabrication of Cu-BHT Thin Films · Figure S6A