Synthesis evidence

Chemical Vapor Deposition of Edge-on Oriented 2D Conductive Metal-Organic Framework Thin Films

Choe M., Koo J.Y., Park I. et al. · Journal of the American Chemical Society · 2022 · 16726-16731

3 structured synthesis routes

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

Partial recipeSource: Both

Route 1: Cvd

main p002 / article page 16727 · Results · Figure S2

Metal precursorsCu(acac)2, inferred same precursor set as target CVD.
Linker precursorsTHQ, inferred same precursor set as target CVD.
SolventsNo reaction solvent.
Substrate orientationConventional CVD without the face-to-face inner tube system.
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCu(acac)2Not specifiedmain p002 / article page 16727 · Results · Figure S2
LinkerTHQNot specifiedmain p002 / article page 16727 · Results · Figure S2
Complete recipeSource: Both

Route 2: Cvd

SI S4 · Synthesis of Cu3(C6O6)2 thin film and powder by a CVD method · Table S1

Metal precursorsBis(2,4-pentanedionato)copper(II) (Cu(acac)2), >97.0%, TCI; fixed Cu(acac)2:THQ mass ratio 3:1; Cu(acac)2 amounts in Table S1 from 1.5 to 45 mg.
Linker precursorsTetrahydroxy-1,4-benzoquinone hydrate (C6H4O6.xH2O, THQ), >96.0%, TCI; THQ varied from 0.5 to 15 mg in Table S1.
SolventsNo reaction solvent; substrate pre-rinsed with deionised water, acetone, and isopropyl alcohol.
AtmosphereEvacuated to 7 mTorr, Ar purge at 100 sccm for 10 min, then Ar flow 18 sccm during reaction.
TemperatureFurnace 230; Cu(acac)2 tube position 170; THQ tube position 180
Time0.667
Substrate orientation300 nm SiO2/Si substrate, 1 cm x 1 cm, placed between two one-end-closed inner test tubes facing each other in a quartz tube.
Work-upAfter reaction, furnace cooled naturally to room temperature by turning off power and opening the lid.
Scalability contextLarge-area, highly reflective films over 1 cm x 1 cm substrates; thickness controlled by precursor amount.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal Sourcebis(2,4-pentanedionato)copper(II) (Cu(acac)2)1.5, 3, 4.5, 6, 15, 30, or 45 mg in Table S1SI S4 · Synthesis of Cu3(C6O6)2 thin film and powder by a CVD method · Table S1
Linkertetrahydroxy-1,4-benzoquinone hydrate (THQ)0.5, 1, 1.5, 2, 5, 10, or 15 mg in Table S1; SI prose also says THQ varied from 0.5 to 3 mgSI S4 · Synthesis of Cu3(C6O6)2 thin film and powder by a CVD method · Table S1
OtherAr carrier gas100 sccm purge for 10 min, then 18 sccm reaction flow · 99.999%SI S4 · Synthesis of Cu3(C6O6)2 thin film and powder by a CVD method · Table S1
OtherSiO2/Si substrate1 cm x 1 cm, 300 nm SiO2SI S4 · Synthesis of Cu3(C6O6)2 thin film and powder by a CVD method · Table S1
Complete recipeSource: SI

Route 3: Cvd

SI S4 · Synthesis of Cu3(C6O6)2 thin film and powder by a CVD method

Metal precursorsSame Cu(acac)2/THQ face-to-face CVD thin-film synthesis as route_face_to_face_cvd_film.
Linker precursorsSame THQ route as route_face_to_face_cvd_film.
SolventsNo reaction solvent.
AtmosphereSame evacuated/Ar CVD atmosphere as route_face_to_face_cvd_film.
Temperature230
Time0.667
Substrate orientationPowder generated from the thin-film product on SiO2/Si.
Work-upProduct grown on substrate was physically scraped; powder was used for TEM and pellet electrical conductivity.
Show 1 structured reagent record
RoleReagentAmount / concentrationSource
OtherCVD Cu3(C6O6)2 thin filmNot specifiedSI S4 · Synthesis of Cu3(C6O6)2 thin film and powder by a CVD method