Synthesis evidence

Ultrasensitive Detection of Electrolyte Leakage from Lithium-Ion Batteries by Ionically Conductive Metal-Organic Frameworks

Lu Y., Zhang S., Dai S. et al. · Matter · 2020 · 904-919

3 structured synthesis routes

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

Complete recipeSource: Main

Route 1: Solvothermal

916-917 · Preparation of Cu-TCPP MOF Thin Films without Free Metal Ions

Metal precursorsCu(NO3)2.3H2O, 7.3 mg, 0.03 mmol
Linker precursorsH2TCPP, 7.9 mg, 0.01 mmol
Solvents18 mL N,N-diethylformamide (DMF); ethanol for colloidal nanosheet suspension
Atmospherenot specified
Temperature35 deg C then 85 deg C, cooled to 35 deg C at 5 deg C/h
Timeheat to 35 deg C over 1 h; hold 35 deg C for 10 h; heat to 85 deg C over 10 h; hold 85 deg C for 1 day
Substrate orientationdrop-cast onto quartz sheet or silicon wafer pretreated by plasma for 10 min
Work-uppurple sample dispersed in ethanol to form colloidal suspension; placed dropwise onto substrate
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
LinkerH2TCPP7.9 mg, 0.01 mmol916-917 · Preparation of Cu-TCPP MOF Thin Films without Free Metal Ions
Metal SourceCu(NO3)2.3H2O7.3 mg, 0.03 mmol916-917 · Preparation of Cu-TCPP MOF Thin Films without Free Metal Ions
SolventN,N-diethylformamide (DMF)18 mL916-917 · Preparation of Cu-TCPP MOF Thin Films without Free Metal Ions
Solventethanolcolloidal suspension916-917 · Preparation of Cu-TCPP MOF Thin Films without Free Metal Ions
Partial recipeSource: Both

Route 2: Other

907 · MOF Synthesis and Sensing Setup · Figure 1B; Figure S1

Metal precursors40 nm gold electrodes deposited after IC-MOF thin-film deposition
Substrate orientationgold electrodes on top of IC-MOF films; conductive channel length 100 um and width 1,000 um
Work-updevice placed in home-made Teflon chamber with gas inlet and outlet ports
Show 1 structured reagent record
RoleReagentAmount / concentrationSource
Othergold electrodes40 nm907 · MOF Synthesis and Sensing Setup · Figure 1B; Figure S1
Complete recipeSource: Both

Route 3: Liquid Liquid Interface

916 · Preparation of IC-MOF Thin Films by Modified Spray Liquid-Interface Process · Figure S1

Metal precursorsCopper(II) nitrate trihydrate, Cu(NO3)2.3H2O, 1 mM aqueous solution
Linker precursorsH2TCPP, 0.2 mM in toluene/EtOH
Solventstoluene/EtOH (v/v = 1:1) for ligand solution; deionized water for Cu(NO3)2.3H2O solution
Atmosphereambient/not specified
Temperatureroom temperature for spraying/drying; 80 deg C activation
Time2 h vacuum heating after natural drying
Substrate orientationquartz sheet or silicon wafer pretreated by plasma for 10 min; film deposited from water surface
Work-upresidual reaction solution removed carefully by syringe; free-standing films deposited onto substrate; natural drying
Activationheated at 80 deg C under vacuum for 2 h to remove remaining moisture
Scalability contextAuthors emphasise mild conditions, low cost, large area, good uniformity, and no specific expensive equipment.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCopper(II) nitrate trihydrate (Cu(NO3)2.3H2O)1 mM916 · Preparation of IC-MOF Thin Films by Modified Spray Liquid-Interface Process · Figure S1
LinkerH2TCPP0.2 mM916 · Preparation of IC-MOF Thin Films by Modified Spray Liquid-Interface Process · Figure S1
Solventtoluene/EtOHv/v = 1:1916 · Preparation of IC-MOF Thin Films by Modified Spray Liquid-Interface Process · Figure S1
Solventdeionized waterNot specified916 · Preparation of IC-MOF Thin Films by Modified Spray Liquid-Interface Process · Figure S1