cMOF Evidence Base

Synthesis evidence

Metal-Organic Framework Assembled on Oriented Nanofiber Arrays for Field-Effect Transistor and Gas Sensor-Based Applications

Mu J., Zhong X., Dai W. et al. · Molecules · 2022 · 2131

5 structured synthesis routes

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

Partial recipeSource: Both

Route 1: Other

S3 · Section S2. Chemical Synthesis

Metal precursorsCu centres in PDMS-PCDA/Cu template; CuSO4.5H2O in distilled water/concentrated ammonia
Linker precursorsHATP.6HCl in distilled water, forming HITP-derived framework linker under ammonia conditions
Solventsaqueous ammonia; distilled water
Additivesconcentrated aqueous ammonia
Atmosphereair
Temperatureroom temperature for CuSO4.5H2O/ammonia step
Time1 h aqueous ammonia pre-immersion; 1 h HATP.6HCl step; 1 h CuSO4.5H2O/ammonia step per cycle; 20 cycles
Substrate orientationoriented PDMS-PCDA/Cu NFAs on (n++) Si; precursor arrays prepared at 300, 400 or 500 r/min
Oxidant / reductantaqueous ammonia oxidises o-phenylenediamine link to radical anion form according to authors
Work-upwashed by distilled water and dried after HATP.6HCl exposure and after CuSO4.5H2O/ammonia exposure
Scalability contextAuthors describe the LBL method as enabling rapid production of Cu3(HITP)2 NFAs.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
OtherPDMS-PCDA/Cu NFAs on the (n++) Si substrateNot specifiedS3 · Section S2. Chemical Synthesis
Baseaqueous ammoniasolution; first immersion for 1 hS3 · Section S2. Chemical Synthesis
LinkerHATP.6HClsolution in distilled waterS3 · Section S2. Chemical Synthesis
Metal SourceCuSO4.5H2Osolution in distilled waterS3 · Section S2. Chemical Synthesis
Baseconcentrated aqueous ammoniawith CuSO4.5H2O at room temperatureS3 · Section S2. Chemical Synthesis
Vague recipeSource: SI

Route 2: Unknown

S3 · Section S2. Chemical Synthesis

Partial recipeSource: Both

Route 3: Other

S3 · Section S2. Chemical Synthesis

Metal precursorsPDMS-PCDA/Cu precursor
Linker precursorsPDMS-PCDA/Cu precursor
Solventstetrahydrofuran (THF); dimethylformamide (DMF)
Additivespolymethyl methacrylate (PMMA)
Time8 h PMMA in THF stirring; 5 h after PDMS-PCDA/Cu addition; 2 h after DMF addition; 10 h vacuum drying after collection
Substrate orientation(n++) Si substrate fixed on drum; drum speed 300, 400, or 500 r/min
Work-upelectrostatic spinning at 18 kV, 15 cm acceptance distance, 0.2 mL/h propulsion speed; vacuum drying line for 10 h
Scalability contextMain text describes electrospinning as simple, inexpensive and suitable for large-scale nanofibre preparation.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
AdditivePMMA0.2 gS3 · Section S2. Chemical Synthesis
Solventtetrahydrofuran (THF)4 mlS3 · Section S2. Chemical Synthesis
OtherPDMS-PCDA/CuNot specifiedS3 · Section S2. Chemical Synthesis
Solventdimethylformamide (DMF)4 mlS3 · Section S2. Chemical Synthesis
Other(n++) Si substratefixed on drumS3 · Section S2. Chemical Synthesis
Partial recipeSource: Both

Route 4: Other

S3 · Section S2. Chemical Synthesis

Metal precursorscopper sulfate pentahydrate in methanol
Linker precursorsPDMS-PCDA ligand
Solventsmethylene chloride; methanol
Atmospheresealed glass bottle then air
Temperature80 during vacuum drying
Timetwo days sealed magnetic stirring; 24 h in air; 24 h vacuum drying
Work-upvacuum drying at 80 C; repeated dissolution with dichloromethane and methanol to remove uncoordinated copper ions
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
LinkerPDMS-PCDA0.8 gS3 · Section S2. Chemical Synthesis
Solventmethylene chloride2 mlS3 · Section S2. Chemical Synthesis
Metal Sourcecopper sulfate pentahydratea certain amount by calculation · in methanolS3 · Section S2. Chemical Synthesis
SolventmethanolNot specifiedS3 · Section S2. Chemical Synthesis
Solventdichloromethaneworkup dissolutionS3 · Section S2. Chemical Synthesis
Partial recipeSource: SI

Route 5: Other

S2-S3 · Section S2. Chemical Synthesis

Linker precursorsH2N-PDMS-NH2 (Mn = 6000); 2,6-pyridinedicarbonyl dichloride
Solventsanhydrous CH2Cl2; MeOH quench
Additivestriethylamine (Et3N)
Atmosphereargon
Temperature0 then room temperature
Time2 h after Et3N addition; 2 h after acyl chloride addition at 0 C; two days at room temperature
Work-upMeOH quench; vacuum evaporation to remove solvent and trace Et3N
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
LinkerH2N-PDMS-NH2 (Mn = 6000)solution in anhydrous CH2Cl2S2-S3 · Section S2. Chemical Synthesis
Linker2,6-pyridinedicarbonyl dichloridesolution in CH2Cl2S2-S3 · Section S2. Chemical Synthesis
Basetriethylamine (Et3N)Not specifiedS2-S3 · Section S2. Chemical Synthesis
Solventanhydrous CH2Cl2Not specifiedS2-S3 · Section S2. Chemical Synthesis
SolventMeOHquenchS2-S3 · Section S2. Chemical Synthesis