cMOF Evidence Base

Synthesis evidence

Orientation Control of a Two-Dimensional Conductive Metal-Organic Framework Thin Film by a Pyridine Vapor-Assisted Dry Process

Chon S., Nakayama R., Iwamoto S. et al. · ACS Applied Materials and Interfaces · 2023 · 56057-56063

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: Cvd

p002 · Experimental Section · Figure 1

Metal precursorsanhydrous copper(II) acetate, Cu(OAc)2
Linker precursorsHHTP
SolventsSubstrate cleaning: acetone and isopropyl alcohol. No solvent used during IR-PLD deposition.
AdditivesSi infrared absorber mixed into Cu(OAc)2 and HHTP pellets at 20 and 30 vol %, respectively
AtmosphereVacuum deposition; base pressure 2 x 10^-6 Pa
Temperature99.85
Substrate orientationalpha-Al2O3 (001)
Oxidant / reductantNo separate oxidant/reductant added; authors suggest partially oxidized HHTP and/or vaporized Cu(OAc)2/decomposition products may oxidize/deprotonate HHTP.
Work-upSubstrate sequentially ultrasonicated in acetone, isopropyl alcohol, acetone, and isopropyl alcohol before deposition; as-deposited film transferred through ambient air for annealing experiments.
Scalability contextThin-film physical vapour deposition route; typical growth rate 1.2 nm min^-1, substrate-target distance 5 cm.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCu(OAc)2 purchased from Sigma-Aldrich8 nm per deposited layer; five cyclesp002 · Experimental Section · Figure 1
LinkerHHTP purchased from TCI10 nm per deposited layer; five cyclesp002 · Experimental Section · Figure 1
AdditiveSi infrared absorber20 vol % in Cu(OAc)2 pellet; 30 vol % in HHTP pelletp002 · Experimental Section · Figure 1
Solventacetone and isopropyl alcohol for substrate cleaningNot specifiedp002 · Experimental Section · Figure 1
Complete recipeSource: Main

Route 2: Other

p002 · Experimental Section · Figure 1

Metal precursorsas-deposited HHTP/Cu(OAc)2-derived film from IR-PLD
Linker precursorsas-deposited HHTP/Cu(OAc)2-derived film from IR-PLD
Solventspyridine vapour; no liquid contact with film
Additivespyridine, 1 uL
AtmosphereSealed gasket cell set up under air; possible moisture in pyridine
Temperature59.85
Time24
Substrate orientationalpha-Al2O3 (001)
Work-upFilm and pyridine droplets placed separately in sealed 7 mL cell to avoid direct contact.
ActivationCell cleaned with acetone/isopropyl alcohol and annealed at 433 K under vacuum before use.
Scalability contextSmall sealed-cell vapour anneal; pyridine volume varied from 1 to 5 uL.
Show 1 structured reagent record
RoleReagentAmount / concentrationSource
Additivepyridine purchased from Kanto Chemical Corporation1 uLp002 · Experimental Section · Figure 1
Complete recipeSource: Main

Route 3: Other

p002 · Experimental Section · Figure 1

Metal precursorsas-deposited HHTP/Cu(OAc)2-derived film from IR-PLD
Linker precursorsas-deposited HHTP/Cu(OAc)2-derived film from IR-PLD
Solventspyridine vapour; no liquid contact with film
Additivespyridine, 3 uL
AtmosphereSealed gasket cell set up under air; possible moisture in pyridine
Temperature59.85
Time24
Substrate orientationalpha-Al2O3 (001)
Work-upFilm and pyridine droplets placed separately in sealed 7 mL cell to avoid direct contact.
ActivationCell cleaned with acetone/isopropyl alcohol and annealed at 433 K under vacuum before use.
Scalability contextAuthors identify 3 uL pyridine annealing as producing the oriented crystalline target film.
Show 1 structured reagent record
RoleReagentAmount / concentrationSource
Additivepyridine purchased from Kanto Chemical Corporation3 uLp002 · Experimental Section · Figure 1
Complete recipeSource: Main

Route 4: Other

p003 · Results and Discussion · Figure 2

Metal precursorsas-deposited HHTP/Cu(OAc)2-derived film from IR-PLD
Linker precursorsas-deposited HHTP/Cu(OAc)2-derived film from IR-PLD
Solventspyridine vapour; no liquid contact with film
Additivespyridine, 5 uL
AtmosphereSealed gasket cell set up under air; possible moisture in pyridine
Temperature59.85
Time24
Substrate orientationalpha-Al2O3 (001)
Work-upFilm and pyridine droplets placed separately in sealed 7 mL cell to avoid direct contact.
ActivationCell cleaned with acetone/isopropyl alcohol and annealed at 433 K under vacuum before use.
Scalability contextSmall sealed-cell vapour anneal; excess pyridine was detrimental to local structure.
Show 1 structured reagent record
RoleReagentAmount / concentrationSource
Additivepyridine purchased from Kanto Chemical Corporation5 uLp003 · Results and Discussion · Figure 2