Vague recipeSource: Main
Route 1: Unknown
p007 · Experimental Section
Synthesis evidence
Quasi Solid–Liquid Reaction Strategy to In Situ Synthesize the Conductive MOF Film with Ordered Submicron Macropores for Gas Sensing
Miao M., Wang Z., Guo Z. et al. · Advanced Materials Interfaces · 2022 · 2101908
5 structured synthesis routes
Completeness describes how fully the route could be reconstructed from the main article and supporting information.
Complete recipeSource: Main
Route 2: Other
p006-p007 · Experimental Section - Synthesis of PS
Linker precursorsstyrene monomer
Solventsdeionized water; ethanol and water for purification
Additivespolyvinyl pyrrolidone (K30); 10 wt% NaOH wash
AtmosphereN2 bubbling for 30 min before polymerisation
Temperature96
Time24 after initiator addition; initial 30 min reflux before initiator
Oxidant / reductantK2S2O8 initiator
Work-upcentrifugation, repeated ethanol washing, repeated water washing, supernatant selection, final concentration dilution to 30 mg mL-1
Show 5 structured reagent records
| Role | Reagent | Amount / concentration | Source |
|---|---|---|---|
| Other | styrene | 65 mL | p006-p007 · Experimental Section - Synthesis of PS |
| Solvent | water | 500 mL | p006-p007 · Experimental Section - Synthesis of PS |
| Additive | polyvinyl pyrrolidone (K30) | 2.5 g | p006-p007 · Experimental Section - Synthesis of PS |
| Oxidant | K2S2O8 | 1 g in 50 mL aqueous solution | p006-p007 · Experimental Section - Synthesis of PS |
| Base | NaOH solution | 10 wt% | p006-p007 · Experimental Section - Synthesis of PS |
Complete recipeSource: Main
Route 3: Drop Cast
p007 · Experimental Section - Raw-Cu3(HITP)2 Film
Metal precursorsCuSO4.5H2O/Cu(NH3)4SO4 solution as for TOM film
Linker precursorsHATP ligand
Solventswater; THF/water workup as for TOM film
Additivesconcentrated ammonium hydroxide; no PS template
Atmosphereambient air for film processing; vacuum oven final drying
Temperature60 drying oven; 80 final vacuum drying
Timesame as TOM route
Substrate orientationinterdigital region of commercial ceramic-based gold IDE
Work-upsame as TOM-Cu3(HITP)2 film except PS suspension replaced with pure water
Activationvacuum oven at 80 deg C for 24 h
Show 3 structured reagent records
| Role | Reagent | Amount / concentration | Source |
|---|---|---|---|
| Linker | HATP ligand | same as TOM route · 5 mg mL-1, inferred from same route with water replacing PS suspension | p007 · Experimental Section - Raw-Cu3(HITP)2 Film |
| Metal Source | Cu(NH3)4SO4 solution | quantitative, stoichiometric ratio of Cu3(HITP)2 · 3 mg mL-1 | p007 · Experimental Section - Raw-Cu3(HITP)2 Film |
| Solvent | pure water | Not specified | p007 · Experimental Section - Raw-Cu3(HITP)2 Film |
Complete recipeSource: Main
Route 4: Drop Cast
p007 · Experimental Section - Syntheses for Spectroscopic Characterizations
Metal precursorssame as TOM-Cu3(HITP)2 on IDE
Linker precursorssame as TOM-Cu3(HITP)2 on IDE
Solventssame as TOM-Cu3(HITP)2 on IDE
AdditivesPS suspension template; concentrated ammonium hydroxide
Atmosphereambient/vacuum dry as for TOM route
Temperaturesame as TOM-Cu3(HITP)2 on IDE
Timesame as TOM-Cu3(HITP)2 on IDE
Substrate orientationquartz plate groove for XRD; glass substrate for XPS scraping
Work-upsame as TOM-Cu3(HITP)2 on IDE
Activationsame as TOM-Cu3(HITP)2 on IDE
Show 1 structured reagent record
| Role | Reagent | Amount / concentration | Source |
|---|---|---|---|
| Other | same reagents as TOM-Cu3(HITP)2 film on IDE | Not specified | p007 · Experimental Section - Syntheses for Spectroscopic Characterizations |
Complete recipeSource: Both
Route 5: Drop Cast
p007 · Experimental Section - In Situ Synthesis of the TOM-Cu3(HITP)2 Film on IDE · Scheme 1; Mechanism S1
Metal precursorsCuSO4.5H2O converted to Cu(NH3)4SO4 solution with ammonium hydroxide
Linker precursors2,3,6,7,10,11-hexaaminotriphenylene hexahydrochloride (HATP)
Solventswater; THF for PS template removal
AdditivesPS suspension template; concentrated ammonium hydroxide
Atmosphereambient air for film processing; vacuum oven final drying
Temperature60 drying oven for HATP at PS layer; 80 final vacuum drying
Time3 sealed after Cu salt addition; repeated 6 h THF and water soaks; final 24 h vacuum dry
Substrate orientationinterdigital region of commercial ceramic-based gold IDE
Work-upTHF soak/dry repeated four times to remove PS; water soak/dry repeated four times; THF soak/dry repeated three times
Activationvacuum oven at 80 deg C for 24 h
Scalability contextAuthors state direct in situ synthesis can be implemented on many substrates without transfer and template/film thickness can be adjusted.
Show 6 structured reagent records
| Role | Reagent | Amount / concentration | Source |
|---|---|---|---|
| Linker | HATP ligand | appropriate amount · 5 mg mL-1 in PS suspension | p007 · Experimental Section - In Situ Synthesis of the TOM-Cu3(HITP)2 Film on IDE · Scheme 1; Mechanism S1 |
| Additive | PS suspension | 30 mg mL-1 | p007 · Experimental Section - In Situ Synthesis of the TOM-Cu3(HITP)2 Film on IDE · Scheme 1; Mechanism S1 |
| Metal Source | CuSO4.5H2O | 33 mg | p007 · Experimental Section - In Situ Synthesis of the TOM-Cu3(HITP)2 Film on IDE · Scheme 1; Mechanism S1 |
| Base | concentrated ammonium hydroxide | 470 uL | p007 · Experimental Section - In Situ Synthesis of the TOM-Cu3(HITP)2 Film on IDE · Scheme 1; Mechanism S1 |
| Metal Source | Cu(NH3)4SO4 solution | quantitative, stoichiometric ratio of Cu3(HITP)2 · 3 mg mL-1 | p007 · Experimental Section - In Situ Synthesis of the TOM-Cu3(HITP)2 Film on IDE · Scheme 1; Mechanism S1 |
| Solvent | THF | Not specified | p007 · Experimental Section - In Situ Synthesis of the TOM-Cu3(HITP)2 Film on IDE · Scheme 1; Mechanism S1 |