Synthesis evidence

A two-dimensional π-d conjugated coordination polymer with extremely high electrical conductivity and ambipolar transport behaviour

Huang X., Sheng P., Tu Z. et al. · Nature Communications · 2015 · 7408

4 structured synthesis routes

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

Partial recipeSource: Main

Route 1: Other

main p.7 · Methods: Fabrication and characterization of FETs · Fig. 6

SolventsDeionized water, ethanol, acetone, methylene chloride used for substrate/film rinsing
AtmosphereDried overnight in glove box with H2O concentration <0.1 ppm
TemperatureRoom temperature device measurement; drying temperature not specified
TimeOvernight drying
Substrate orientationCu-BHT film deposited on n-type highly doped Si with 300 nm SiO2; smooth upside surface required to contact dielectric/electrodes.
Work-upSource and drain electrodes (30 nm) sputtered and patterned by lift-off; channel length 5-50 um.
ActivationNo activation reported.
Partial recipeSource: Main

Route 2: Liquid Liquid Interface

main p.6 · Methods: Synthesis of Cu-BHT thin film · Fig. 1

Metal precursorsCu(NO3)2 aqueous mixture, 5 mM
Linker precursorsBHT in degassed dichloromethane, saturated solution 0.24 mM, 20 mL
SolventsDegassed dichloromethane; degassed water; Milli-Q water
AdditivesNaBr, 1 mM in aqueous mixture
AtmosphereArgon; sealed bottle filled with argon gas; solvents degassed by freeze-thaw method
TemperatureRoom temperature implied; not explicitly stated for synthesis
Substrate orientationOil-water interface; transfer to substrates after film formation
Oxidant / reductantCu(II) nitrate acts as metal source; XPS indicates Cu(II) reduced during formation
Work-upAs-prepared film transferred onto substrate and cleaned with ethanol and acetone; device films additionally rinsed with deionized water and methylene chloride.
ActivationNo activation reported.
Scalability contextContinuous films larger than 1 cm2 were obtained.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCu(NO3)25 mMmain p.6 · Methods: Synthesis of Cu-BHT thin film · Fig. 1
LinkerBHT (benzenehexathiol)20 ml saturated solution · 0.24 mMmain p.6 · Methods: Synthesis of Cu-BHT thin film · Fig. 1
Solventdichloromethane20 ml BHT solutionmain p.6 · Methods: Synthesis of Cu-BHT thin film · Fig. 1
Solventwater20 ml degassed water layermain p.6 · Methods: Synthesis of Cu-BHT thin film · Fig. 1
AdditiveNaBr1 mMmain p.6 · Methods: Synthesis of Cu-BHT thin film · Fig. 1
Partial recipeSource: Main

Route 3: Other

main p.6 · Methods: Transfer method

SolventsCH2Cl2/aqueous interface
AtmosphereArgon inherited from reaction setup where applicable
Substrate orientationSubstrate immersed into the reaction solution and passed horizontally and slowly through the CH2Cl2/aqueous interface after film formation.
Work-upAqueous solution removed before substrate was taken out of CH2Cl2.
Partial recipeSource: Main

Route 4: Other

main p.6 · Methods: Transfer method

SolventsCH2Cl2/aqueous interface
AtmosphereArgon inherited from reaction setup where applicable
Substrate orientationSubstrate settled horizontally in reaction container before adding reaction solutions; solution surface about 10 mm higher than substrate; subphase removed so interface passes through substrate.
Work-upFilm deposited with upside-up orientation on substrate.