Synthesis evidence

Fabrication of an Active Electronic Device Using a Hetero-bimetallic Coordination Polymer

Roy S., Halder S., Drew M.G.B. et al. · ACS Omega · 2018 · 12788-12796

2 structured synthesis routes

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

Complete recipeSource: Both

Route 1: Other

2 · Experimental Section - Synthesis · Scheme 1

Metal precursorslead(II) nitrate; nickel(II) thiocyanate tetrahydrate
Linker precursorsH2L from 3-methoxysalicylaldehyde and 1,3-diaminopropane, used in situ
Solventsmethanol (20 mL ligand step; 10 mL Pb solution; 10 mL Ni solution)
Atmosphereopen atmosphere for slow evaporation; other steps not specified
Temperaturereflux for ligand step; room-temperature stirring/crystallisation after metal addition (not explicitly stated)
Timeca. 1 h reflux; 15 min after Pb addition; about 2 h after Ni addition; 3-4 days slow evaporation
Work-upLigand not isolated; solution slow-evaporated in open atmosphere; X-ray quality crystals isolated.
Scalability contextAuthors state they are working to get better yield and develop more systems based on this strategy.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Linker3-Methoxysalicylaldehyde304 mg, 2 mmol2 · Experimental Section - Synthesis · Scheme 1
Linker1,3-diaminopropane0.13 mL, 1 mmol2 · Experimental Section - Synthesis · Scheme 1
Solventmethanol20 mL for ligand step; 40 mL total including metal solutions2 · Experimental Section - Synthesis · Scheme 1
Metal Sourcelead(II) nitrate332 mg, 1 mmol2 · Experimental Section - Synthesis · Scheme 1
Metal Sourcenickel(II) thiocyanate tetrahydrate250 mg, 1 mmol2 · Experimental Section - Synthesis · Scheme 1
Complete recipeSource: Both

Route 2: Other

2 · Experimental Section - Device Fabrication · Figure S2

SolventsDMF dispersion of complex; acetone, ethanol, and distilled water for ITO cleaning
Atmosphereambient conditions for preparation/measurement; vacuum annealing and thermal evaporation under 10^-6 Torr
Temperature80 deg C annealing
Time0.5 h annealing; 4 min at 600 rpm plus 6 min at 1000 rpm spin coating
Substrate orientationITO-coated glass substrate; Al top electrode deposited through a shadow mask
Work-upUltrasonic cleaning in acetone, ethanol, and distilled water; spin coating; vacuum annealing; thermal evaporation of Al.
ActivationVacuum annealed at 80 deg C for 30 min to evaporate solvent.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Other[(NCS)Pb(H2O)LNi(NCS)]n complex20 mg mL^-1 in DMF2 · Experimental Section - Device Fabrication · Figure S2
SolventN,N-dimethylformamide (DMF)Not specified2 · Experimental Section - Device Fabrication · Figure S2
Solventacetone, ethanol, distilled watersubstrate cleaning solvents2 · Experimental Section - Device Fabrication · Figure S2
OtherITO-coated glass substrateNot specified2 · Experimental Section - Device Fabrication · Figure S2
OtherAl electrode99.99% pure Al2 · Experimental Section - Device Fabrication · Figure S2