Synthesis evidence

Synthesis of a highly conductive coordination polymer film via a vapor-solid phase chemical conversion process

Li Z., Jin Y., Li C. et al. · Chemical Communications · 2024 · 8720-8723

4 structured synthesis routes

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

Partial recipeSource: SI

Route 1: Other

SI p001 · Device Fabrication

Metal precursorsPreformed Ag5BHT thin film; Au or Pt contacts
Solventsdeionised water and isopropanol cleaning solvents
Additivespiranha solution, 70/30 vol./vol. H2SO4/H2O2, for substrate cleaning
AtmosphereN2 blow-dry after cleaning
Substrate orientationheavily doped n-type Si wafer with 300 nm SiO2
Oxidant / reductantH2SO4/H2O2 piranha clean only
Work-upSubstrates cleaned with deionised water, piranha solution, deionised water, isopropanol, and blow-dried by N2; 100 nm Au or Pt source/drain electrodes evaporated.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Otherheavily doped n-type Si wafer with 300 nm SiO2Not specifiedSI p001 · Device Fabrication
AcidH2SO4/H2O2 piranha solution70/30 vol./vol.SI p001 · Device Fabrication
Solventdeionised watercleaning solventSI p001 · Device Fabrication
Solventisopropanolcleaning solventSI p001 · Device Fabrication
OtherAu or Pt source and drain electrodes100 nm thickSI p001 · Device Fabrication
Complete recipeSource: SI

Route 2: Other

SI p001 · Synthesis of Ag5BHT powder

Metal precursorssilver oxide (Ag2O), 58 mg, 0.25 mmol
Linker precursorsH6BHT, 27 mg, 0.1 mmol
Solventsdegassed isopropanol, 40 mL; water, methanol, and acetone washes
Atmosphereargon atmosphere; solvents degassed by freeze-thaw
Temperature0 deg C ultrasonic dispersion, then 50 deg C reaction
Time10 min ultrasonic dispersion; overnight heating; 24 h stirring
Oxidant / reductantAg2O metal source; no separate oxidant/reductant reported
Work-upFiltration, washed three times with water, methanol, and acetone; solvents removed under vacuum
ActivationVacuum drying/removal of solvents; no separate activation protocol reported
Scalability contextPowder yield reported as 79 mg (98%); no scale-up experiment reported.
Show 6 structured reagent records
RoleReagentAmount / concentrationSource
LinkerH6BHT27 mg, 0.1 mmolSI p001 · Synthesis of Ag5BHT powder
Metal Sourcesilver oxide (Ag2O)58 mg, 0.25 mmolSI p001 · Synthesis of Ag5BHT powder
Solventdegassed isopropanol40 mLSI p001 · Synthesis of Ag5BHT powder
Solventwaterwash solventSI p001 · Synthesis of Ag5BHT powder
Solventmethanolwash solventSI p001 · Synthesis of Ag5BHT powder
Solventacetonewash solventSI p001 · Synthesis of Ag5BHT powder
Partial recipeSource: Both

Route 3: Other

8721 · Results · Fig. S2-S4

Metal precursorsAg2O powder
Linker precursorsH6BHT powder
Solventsisopropanol vapour
Atmospheresealed reaction vessel saturated with isopropanol vapour
Temperature100
Time24
Oxidant / reductantAg2O metal source; isopropanol vapour environment
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceAg2O powderNot specified8721 · Results · Fig. S2-S4
LinkerH6BHT powderNot specified8721 · Results · Fig. S2-S4
Solventisopropanol vapoursaturated atmosphere8721 · Results · Fig. S2-S4
Partial recipeSource: Both

Route 4: Other

SI p001 · Synthesis of Ag5BHT films

Metal precursorsAg film converted to Ag2O film by plasma oxidation; example Ag2O thicknesses 50 or 100 nm
Linker precursorsH6BHT film deposited by thermal evaporation; H6BHT/Ag2O thickness ratio 1.3:1
Solventsisopropanol vapour
Atmosphereclosed container filled with an atmosphere containing vaporised isopropanol
Temperature90-120
Timeseveral days; about 48 h for 50 nm Ag2O/65 nm H6BHT and about 120 h for 100 nm Ag2O/130 nm H6BHT
Substrate orientationSi, Si/SiO2 wafer, or glass substrates; no crystallographic orientation specified
Oxidant / reductantPlasma oxidation converts Ag film to Ag2O; Ag2O reacts with H6BHT under isopropanol vapour
Work-upNo post-synthesis wash or activation reported for the films; black Ag2O/H6BHT films convert to shiny light-green Ag5BHT films.
Scalability contextThe method gives controllable 100-300 nm films and the authors describe uniform smooth films with lower energy demand; no explicit scale-up area is reported.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceAg film / Ag2O filmAg2O film examples: 50 nm or 100 nmSI p001 · Synthesis of Ag5BHT films
LinkerH6BHT film65 nm with 50 nm Ag2O; 130 nm with 100 nm Ag2O; ratio 1.3:1 relative to Ag2O thicknessSI p001 · Synthesis of Ag5BHT films
Solventisopropanol vapourclosed-container vapour atmosphereSI p001 · Synthesis of Ag5BHT films