Synthesis evidence

In-Plane Oriented Two-Dimensional Conjugated Metal-Organic Framework Films for High-Performance Humidity Sensing

Park S., Zhang Z., Qi H. et al. · ACS Materials Letters · 2022 · 1146-1153

4 structured synthesis routes

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

Complete recipeSource: SI

Route 1: Other

5 · Synthesis of HAB-Cu

Metal precursorscopper acetate, 2.04 mg (11.25 umol)
Linker precursorsHAB, 2.09 mg (7.5 umol)
Solvents3 ml deoxygenated deionized water
Atmospherenitrogen atmosphere; excess nitrogen flow; glovebox workup; air-free conditions
Temperatureroom temperature
Time72 h drying plus 12 h final nitrogen drying
Oxidant / reductantair-free, prior to oxidation
Work-upgrey precipitate washed several times with anhydrous ethanol in glovebox
Activationdried again under excess nitrogen flow for 12 hours
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Metal Sourcecopper acetate2.04 mg (11.25 umol)5 · Synthesis of HAB-Cu
LinkerHAB2.09 mg (7.5 umol)5 · Synthesis of HAB-Cu
Solventdeoxygenated, deionized water3 ml5 · Synthesis of HAB-Cu
Complete recipeSource: SI

Route 2: Other

5 · Synthesis of HAB-Cu/SDS

Metal precursorscopper acetate, 2.04 mg (11.25 umol)
Linker precursorsHAB, 2.09 mg (7.5 umol)
Solvents3 ml deoxygenated deionized water
AdditivesSDS, 0.75 mg (2.6 umol)
Atmospherenitrogen atmosphere; excess nitrogen flow; glovebox workup; air-free conditions
Temperatureroom temperature
Time72 h drying plus 12 h final nitrogen drying
Oxidant / reductantair-free, prior to oxidation
Work-uplight grey precipitate washed several times with anhydrous ethanol in glovebox
Activationdried again under excess nitrogen flow for 12 hours
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal Sourcecopper acetate2.04 mg (11.25 umol)5 · Synthesis of HAB-Cu/SDS
LinkerHAB2.09 mg (7.5 umol)5 · Synthesis of HAB-Cu/SDS
AdditiveSDS0.75 mg (2.6 umol)5 · Synthesis of HAB-Cu/SDS
Solventdeoxygenated, deionized water3 ml5 · Synthesis of HAB-Cu/SDS
Complete recipeSource: Both

Route 3: Air Liquid Interface

4 · Synthesis of HIB-Cu film

Metal precursorscopper acetate, 2.04 mg (11.25 umol); tunable 5.625-16.875 umol
Linker precursorsHAB, 2.09 mg (7.5 umol); tunable 3.75-11.25 umol
Solvents3 ml deoxygenated deionized water
Additivessodium carbonate 0.64 mg (6 umol); SDS 0.75 mg (2.6 umol)
Atmosphereinitially nitrogen atmosphere; then air exposure/air treatment at interface
Temperature50
Time12
Substrate orientationfilm formed at air-water interface; transferred by vertical deposition to Si/SiO2, TEM grid, or quartz substrate
Oxidant / reductantair/oxygen-triggered oxidation at the air-water interface
Work-upsolid-supported film gently rinsed with water and ethanol
Activationdried under nitrogen atmosphere at 80 C for 1 day
Scalability contextfree-standing films transferable to several substrates; thickness controlled by copper acetate and HAB concentration.
Show 6 structured reagent records
RoleReagentAmount / concentrationSource
Metal Sourcecopper acetate2.04 mg (11.25 umol)4 · Synthesis of HIB-Cu film
LinkerHAB2.09 mg (7.5 umol)4 · Synthesis of HIB-Cu film
Basesodium carbonate0.64 mg (6 umol)4 · Synthesis of HIB-Cu film
AdditiveSDS0.75 mg (2.6 umol)4 · Synthesis of HIB-Cu film
Solventdeoxygenated, deionized water3 ml4 · Synthesis of HIB-Cu film
OxidantairNot specified4 · Synthesis of HIB-Cu film
Complete recipeSource: Both

Route 4: Air Liquid Interface

4 · Synthesis of HITP-Cu film

Metal precursorscopper acetate, 0.51 mg (2.81 umol)
Linker precursorsHATP, 1.01 mg (1.88 umol)
Solvents3 ml deoxygenated deionized water
Additivessodium carbonate 2.56 mg (24 umol); SDS 0.75 mg (2.6 umol)
Atmospheresealed under nitrogen during dispersion; opened to air at room temperature
Temperatureroom temperature
Time24
Substrate orientationfilm formed at air-water interface; transferred by vertical deposition to Si/SiO2, TEM grid, or quartz substrate
Oxidant / reductantair-triggered oxidation at the air-water interface
Work-upsolid-supported film gently rinsed with ethanol
Activationdried under nitrogen atmosphere for 1 day
Scalability contextfree-standing mechanically stable film transferable to supports.
Show 6 structured reagent records
RoleReagentAmount / concentrationSource
Metal Sourcecopper acetate0.51 mg (2.81 umol)4 · Synthesis of HITP-Cu film
LinkerHATP1.01 mg (1.88 umol)4 · Synthesis of HITP-Cu film
Basesodium carbonate2.56 mg (24 umol)4 · Synthesis of HITP-Cu film
AdditiveSDS0.75 mg (2.6 umol)4 · Synthesis of HITP-Cu film
Solventdeoxygenated, deionized water3 ml4 · Synthesis of HITP-Cu film
OxidantairNot specified4 · Synthesis of HITP-Cu film