Synthesis evidence

Self-assembly and optoelectronic properties of isoreticular MOF nanocrystals

Dawood S., Yarbrough R., Davis K. et al. · Synthetic Metals · 2019 · 107-112

6 structured synthesis routes

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

Partial recipeSource: Main

Route 1: Drop Cast

110 · 3.2. Solvents dependent self-assembly and their morphology studies · Fig. 4

Metal precursorspreformed IRMOF-8 microstructures
Solventsbutanone
Atmospherenot specified
Temperature100
Time0.0833
Substrate orientationdrop-casted substrate, not specified
Work-upAnnealed drop-casted substrate at 100 C for 5 min.
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
OtherIRMOF-8 microstructuresNot specified110 · 3.2. Solvents dependent self-assembly and their morphology studies · Fig. 4
SolventbutanoneNot specified110 · 3.2. Solvents dependent self-assembly and their morphology studies · Fig. 4
Partial recipeSource: Both

Route 2: Other

108 · 2.3. Electrical conductivity measurements · Figure S3

Metal precursorspreformed IRMOF-8 microstructures
SolventsDMF dispersion (25 mg microstructures in 500 uL DMF)
Additivessubstrate cleaning: dichloromethane, soap solution, ammonium hydroxide/hydrogen peroxide mixture
Atmospherevacuum drying under nitrogen; transferred into nitrogen filled sealed chamber after Cu deposition
Temperature50-70 during substrate NH4OH/H2O2 cleaning; room temperature not otherwise specified
Timespin coat 60 s; UV cleaning 35 min; NH4OH/H2O2 cleaning 15 min; ultrasonic water rinse 15 min
Substrate orientationITO-coated glass; Cu top electrode
Oxidant / reductanthydrogen peroxide in substrate cleaning mixture
Work-upSpin coat at 1000 rpm for 60 s; vacuum dry under nitrogen; deposit 100 nm Cu cathode by PVD e-beam.
ActivationUV/ozone cleaning of substrate before deposition; no MOF activation reported.
Scalability contextThin-film device fabrication by solution spin coating.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
OtherIRMOF-8 microstructures25 mg · 25 mg in 500 uL DMF108 · 2.3. Electrical conductivity measurements · Figure S3
SolventDMF500 uL108 · 2.3. Electrical conductivity measurements · Figure S3
OtherCopper cathode100 nm thick Cu layer108 · 2.3. Electrical conductivity measurements · Figure S3
OtherITO-coated glass substrateNot specified108 · 2.3. Electrical conductivity measurements · Figure S3
Partial recipeSource: Main

Route 3: Drop Cast

110 · 3.2. Solvents dependent self-assembly and their morphology studies · Fig. 4

Metal precursorspreformed IRMOF-8 microstructures
SolventsDMF/propanol (v/v 1:1)
Atmospherenot specified
Temperature100
Time0.0833
Substrate orientationdrop-casted substrate, not specified
Work-upAnnealed drop-casted substrate at 100 C for 5 min.
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
OtherIRMOF-8 microstructuresNot specified110 · 3.2. Solvents dependent self-assembly and their morphology studies · Fig. 4
SolventDMF/propanolv/v 1:1110 · 3.2. Solvents dependent self-assembly and their morphology studies · Fig. 4
Partial recipeSource: Main

Route 4: Other

108 · 2.1. Materials

Metal precursorspreformed IRMOF-8 microstructures
SolventsDMF dispersion
Atmospherenot specified for optical films
Substrate orientationozone/UV-treated quartz plates or ITO-coated glass substrates
Work-upSpin coating onto ozone/UV-treated substrates.
ActivationOzone/UV substrate treatment before spin coating.
Scalability contextSolution-processable pristine thin films.
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
OtherIRMOF-8 microstructuresNot specified108 · 2.1. Materials
SolventDMFNot specified108 · 2.1. Materials
Complete recipeSource: Main

Route 5: Solvothermal

108 · 2.2. General procedure for preparation of IRMOF-8 analogue · Scheme 1

Metal precursorsZinc acetate (100 mg, 0.400 mmol)
Linker precursors2,6 Naphthalene dicarboxylic acid (198 mg, 0.800 mmol)
SolventsAnhydrous DMF (2 mL)
Atmospherenot specified
Temperature260
Time0.1167
Work-upWashed with cold DMF, followed by acetone; collected as off-white powder.
ActivationNo activation step reported.
Scalability contextRapid 7 min solvothermal annealing; isolated yield 100 mg, 33 wt%.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceZinc acetate100 mg, 0.400 mmol108 · 2.2. General procedure for preparation of IRMOF-8 analogue · Scheme 1
Linker2,6 Naphthalene dicarboxylic acid198 mg, 0.800 mmol108 · 2.2. General procedure for preparation of IRMOF-8 analogue · Scheme 1
SolventAnhydrous DMF2 mL108 · 2.2. General procedure for preparation of IRMOF-8 analogue · Scheme 1
Partial recipeSource: Main

Route 6: Drop Cast

110 · 3.2. Solvents dependent self-assembly and their morphology studies · Fig. 4

Metal precursorspreformed IRMOF-8 microstructures
Solventstoluene
Atmospherenot specified
Temperature100
Time0.0833
Substrate orientationdrop-casted substrate, not specified
Work-upAnnealed drop-casted substrate at 100 C for 5 min.
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
OtherIRMOF-8 microstructuresNot specified110 · 3.2. Solvents dependent self-assembly and their morphology studies · Fig. 4
SolventtolueneNot specified110 · 3.2. Solvents dependent self-assembly and their morphology studies · Fig. 4