Synthesis evidence

Oriented growth of semiconducting TCNQ@Cu3(BTC)2MOF on Cu(OH)2: crystallographic orientation and pattern formation toward semiconducting thin-film devices

Okada K., Mori K., Fukatsu A. et al. · Journal of Materials Chemistry A · 2021 · 19613-19618

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: Other

2 · Synthesis of Cu3(BTC)2 oriented film

Metal precursorsoriented Cu(OH)2 nanobelt film on substrate; Cu(OH)2 nanobelt preparation referred to prior report
Linker precursorsH3BTC (benzene-1,3,5-tricarboxylic acid), 7 mg
Solvents10 mL ethanol-water mixture (1:1 vol.%)
Atmosphereair drying; reaction atmosphere not specified
Temperatureroom temperature
Time0.1667
Substrate orientationaligned Cu(OH)2 nanobelts; longitudinal direction/a-axis used to define in-plane orientation
Work-upremoved from solution, washed with ethanol, dried under air
Scalability contextHomogeneous thin films were obtained over centimetre-scale substrates.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Metal Sourceoriented Cu(OH)2 nanobelt filmNot specified2 · Synthesis of Cu3(BTC)2 oriented film
LinkerH3BTC (Benzene-1,3,5-tricarboxylic acid)7 mg2 · Synthesis of Cu3(BTC)2 oriented film
Solventethanol (EtOH)-water (H2O), 1:1 vol.%10 mL2 · Synthesis of Cu3(BTC)2 oriented film
Partial recipeSource: Both

Route 2: Other

2 · Fabrication of oriented Cu3(BTC)2 patterns

Metal precursorsoriented Cu(OH)2 thin film deposited onto photoresist-patterned Si wafer
Linker precursorsH3BTC conversion solution as in route_oriented_cu_btc_film
Solvents2-propanol development; acetone sonication/wash; ethanol-water conversion solution
AdditivesEco UV Resin photoresist; Cr photomask
Atmosphereair drying; reaction atmosphere not specified
Temperatureroom temperature for Cu3(BTC)2 conversion
Timephotoresist spin coat 40 s; UV exposure 15 s; acetone sonication 10 min; Cu3(BTC)2 conversion 10 min
Substrate orientationSi wafer; patterned oriented Cu(OH)2 film with nanobelt a-axis aligned horizontally in images
Work-upphotoresist removed by acetone sonication, washed with acetone, dried under air, then converted using the Cu3(BTC)2 film procedure
Scalability contextMicrometre-scale patterns were demonstrated; authors state resolution up to 50 nm may be possible because Cu(OH)2 nanobelt width is ~50 nm.
Show 6 structured reagent records
RoleReagentAmount / concentrationSource
OtherSi waferNot specified2 · Fabrication of oriented Cu3(BTC)2 patterns
Additivephotoresist (Eco UV Resin, Shenzhen Anycubic Technology Co., Ltd., China)Not specified2 · Fabrication of oriented Cu3(BTC)2 patterns
Solvent2-propanolNot specified2 · Fabrication of oriented Cu3(BTC)2 patterns
SolventacetoneNot specified2 · Fabrication of oriented Cu3(BTC)2 patterns
Metal Sourceoriented Cu(OH)2 thin filmNot specified2 · Fabrication of oriented Cu3(BTC)2 patterns
LinkerH3BTC conversion solution7 mg H3BTC in 10 mL solvent, inherited from film route2 · Fabrication of oriented Cu3(BTC)2 patterns
Complete recipeSource: Both

Route 3: Other

2-3 · Infiltration of TCNQ in Cu3(BTC)2 oriented film

Metal precursorsoriented Cu3(BTC)2 film prepared on polyimide
Linker precursorspreformed Cu3(BTC)2 framework; TCNQ guest
Solventsdichloromethane saturated with TCNQ
Atmospherehigh vacuum for desolvation; N2 glove bag during transfer/immersion
Temperature180 for desolvation; room temperature during TCNQ immersion not explicitly stated
Time3 h desolvation; 72 h TCNQ immersion
Substrate orientationpolyimide substrate; underlying Cu(OH)2 nanobelt orientation chosen relative to Pt pads
Oxidant / reductantTCNQ redox-active guest molecule
Work-upwashed with dichloromethane twice, then dried under air
Activationdesolvated under high vacuum (~10^-4 Pa) at 180 C for 3 h using a Schlenk line
Scalability contextAuthors highlight substrate versatility and flexible polyimide support.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Otheroriented Cu3(BTC)2 film prepared on polyimideNot specified2-3 · Infiltration of TCNQ in Cu3(BTC)2 oriented film
AdditiveTCNQ (7,7,8,8-tetracyanoquinodimethane)saturated solution2-3 · Infiltration of TCNQ in Cu3(BTC)2 oriented film
SolventdichloromethaneNot specified2-3 · Infiltration of TCNQ in Cu3(BTC)2 oriented film