Vague recipeSource: SI
Route 1: Other
S2 · H4TTFTB Synthesis
Show 1 structured reagent record
| Role | Reagent | Amount / concentration | Source |
|---|---|---|---|
| Linker | H4TTFTB (tetrathiafulvalene tetrabenzoic acid) | Not specified | S2 · H4TTFTB Synthesis |
Synthesis evidence
A conductive metal-organic framework photoanode
Pattengale B., Freeze J.G., Guberman-Pfeffer M.J. et al. · Chemical Science · 2020 · 9593-9603
7 structured synthesis routes
Completeness describes how fully the route could be reconstructed from the main article and supporting information.
Complete recipeSource: SI
Route 2: Other
S2 · TiO2 and ZrO2 Film Preparation
Metal precursorsTiO2 (Ti-Nanoxide T/SP) nanoparticle paste; ZrO2 (Zr-Nanoxide ZT/SP) nanoparticle paste for ZrO2 controls
AdditivesScotch tape spacer layer
Atmosphereambient cooling
Temperature370 then 470
Time0.667
Substrate orientationdoctor blading on FTO or quartz substrates
Work-upcalcination; ambient cooling to room temperature
Activationcalcination at 370 C for 10 min, then 470 C for 30 min
Show 3 structured reagent records
| Role | Reagent | Amount / concentration | Source |
|---|---|---|---|
| Other | TiO2 (Ti-Nanoxide T/SP) nanoparticle paste | Not specified | S2 · TiO2 and ZrO2 Film Preparation |
| Other | ZrO2 (Zr-Nanoxide ZT/SP) nanoparticle paste | Not specified | S2 · TiO2 and ZrO2 Film Preparation |
| Other | FTO or quartz substrate | Not specified | S2 · TiO2 and ZrO2 Film Preparation |
Partial recipeSource: Both
Route 3: Solvothermal
S2 · Zn2TTFTB Film Growth
Metal precursorsZn(NO3)2·6H2O
Linker precursorsH4TTFTB
SolventsDMF and EtOH
Atmospheretightly capped vial; air not otherwise specified
Temperature40 to 75
Substrate orientationtwo cleaned FTO pieces placed back-to-back in a 20 mL glass scintillation vial
Work-upcool to room temperature; remove film from solution; rinse with DMF followed by EtOH; dry in air
Activationair drying only; no separate activation reported
Scalability contextSame procedure used for FTO, TiO2 and ZrO2 substrates.
Show 5 structured reagent records
| Role | Reagent | Amount / concentration | Source |
|---|---|---|---|
| Metal Source | Zn(NO3)2·6H2O | 37 mg (0.2 mmoles) | S2 · Zn2TTFTB Film Growth |
| Linker | H4TTFTB | 21 mg (0.03 mmoles) | S2 · Zn2TTFTB Film Growth |
| Solvent | DMF | 2.6 mL + 2.6 mL | S2 · Zn2TTFTB Film Growth |
| Solvent | ETOH | 2.6 mL + 1.5 mL | S2 · Zn2TTFTB Film Growth |
| Other | cleaned FTO substrate | two pieces | S2 · Zn2TTFTB Film Growth |
Partial recipeSource: Both
Route 4: Solvothermal
9595 · Zn2TTFTB structural characterization · Figure S2; Figure S4
Metal precursorsZn(NO3)2·6H2O
Linker precursorsH4TTFTB
SolventsDMF and EtOH; no excess H2O
Atmospheretightly capped vial; air not otherwise specified
Temperature40 to 75
Substrate orientationno substrate for powder analogue
Work-upcool to room temperature; rinse with DMF then EtOH; dry in air
Activationallowed to dry in air
Show 4 structured reagent records
| Role | Reagent | Amount / concentration | Source |
|---|---|---|---|
| Metal Source | Zn(NO3)2·6H2O | 37 mg (0.2 mmoles) | 9595 · Zn2TTFTB structural characterization · Figure S2; Figure S4 |
| Linker | H4TTFTB | 21 mg (0.03 mmoles) | 9595 · Zn2TTFTB structural characterization · Figure S2; Figure S4 |
| Solvent | DMF | 2.6 mL in metal solution; 2.6 mL in ligand solution | 9595 · Zn2TTFTB structural characterization · Figure S2; Figure S4 |
| Solvent | ETOH | 2.6 mL in metal solution; 1.5 mL in ligand solution | 9595 · Zn2TTFTB structural characterization · Figure S2; Figure S4 |
Vague recipeSource: Main
Route 5: Solvothermal
9594 · Results and discussion
Metal precursorsZn2+ ions; exact salt not repeated for standard literature synthesis
Linker precursorsH4TTFTB ligand
Solventsheated DMF/EtOH/H2O solution
Additivesexcess H2O in standard synthesis, inferred from film conditions excluding excess H2O
Show 3 structured reagent records
| Role | Reagent | Amount / concentration | Source |
|---|---|---|---|
| Metal Source | Zn2+ ions | Not specified | 9594 · Results and discussion |
| Linker | H4TTFTB ligand | Not specified | 9594 · Results and discussion |
| Solvent | DMF/ETOH/H2O | Not specified | 9594 · Results and discussion |
Partial recipeSource: Both
Route 6: Solvothermal
S2 · Zn2TTFTB Film Growth
Metal precursorsZn(NO3)2·6H2O
Linker precursorsH4TTFTB
SolventsDMF and EtOH
Atmospheretightly capped vial; air not otherwise specified
Temperature40 to 75
Substrate orientationtwo cleaned TiO2-coated substrates placed back-to-back in a 20 mL glass scintillation vial
Work-upcool to room temperature; remove film from solution; rinse with DMF followed by EtOH; dry in air
Activationair drying only; no separate activation reported
Show 5 structured reagent records
| Role | Reagent | Amount / concentration | Source |
|---|---|---|---|
| Metal Source | Zn(NO3)2·6H2O | 37 mg (0.2 mmoles) | S2 · Zn2TTFTB Film Growth |
| Linker | H4TTFTB | 21 mg (0.03 mmoles) | S2 · Zn2TTFTB Film Growth |
| Solvent | DMF | 2.6 mL + 2.6 mL | S2 · Zn2TTFTB Film Growth |
| Solvent | ETOH | 2.6 mL + 1.5 mL | S2 · Zn2TTFTB Film Growth |
| Other | TiO2-coated substrate | two pieces | S2 · Zn2TTFTB Film Growth |
Partial recipeSource: Both
Route 7: Solvothermal
S2 · Zn2TTFTB Film Growth
Metal precursorsZn(NO3)2·6H2O
Linker precursorsH4TTFTB
SolventsDMF and EtOH
Atmospheretightly capped vial; air not otherwise specified
Temperature40 to 75
Substrate orientationtwo cleaned ZrO2-coated substrates placed back-to-back in a 20 mL glass scintillation vial
Work-upcool to room temperature; remove film from solution; rinse with DMF followed by EtOH; dry in air
Activationair drying only; no separate activation reported
Show 5 structured reagent records
| Role | Reagent | Amount / concentration | Source |
|---|---|---|---|
| Metal Source | Zn(NO3)2·6H2O | 37 mg (0.2 mmoles) | S2 · Zn2TTFTB Film Growth |
| Linker | H4TTFTB | 21 mg (0.03 mmoles) | S2 · Zn2TTFTB Film Growth |
| Solvent | DMF | 2.6 mL + 2.6 mL | S2 · Zn2TTFTB Film Growth |
| Solvent | ETOH | 2.6 mL + 1.5 mL | S2 · Zn2TTFTB Film Growth |
| Other | ZrO2-coated substrate | two pieces | S2 · Zn2TTFTB Film Growth |