Synthesis · Polythiophene hybrid film with zirconium–porphyrin metal–organic framework for improved charge carrier transport and NO2 gas sensing

3 structured synthesis routes

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

Partial recipeSource: Main

2 · 2.2 Preparation of PCN-222/P3HT blend films and transistor-type gas sensors

Metal precursorspre-synthesised PCN-222 powder

Linker precursorsP3HT polymer; PCN-222 contains Fe-TCPP-Cl

Solventschloroform for P3HT solution

AdditivesHMDS surface modifier on SiO2

Atmospherenot specified

Temperature50 C sonication; room temperature stirring

Time1 h sonication at 50 C; 12 h stirring at room temperature

Substrate orientationHMDS-coated Si/SiO2 substrate; top-contact bottom-gate OTFT

Work-upPCN-222 added to cooled P3HT solution; blend solution sonicated and stirred; spin-coated at 1500 rpm for 60 s.

Scalability contextSolution-processable spin coating enabled blend film fabrication for OTFT-type gas sensors.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	synthesized PCN-222	different weight ratios; 10, 20, 30, 50, and 100 wt% shown	2 · 2.2 Preparation of PCN-222/P3HT blend films and transistor-type gas sensors
Other	P3HT	10 mg mL-1 in chloroform	2 · 2.2 Preparation of PCN-222/P3HT blend films and transistor-type gas sensors
Solvent	chloroform	Not specified	2 · 2.2 Preparation of PCN-222/P3HT blend films and transistor-type gas sensors
Additive	HMDS	Not specified	2 · 2.2 Preparation of PCN-222/P3HT blend films and transistor-type gas sensors

Complete recipeSource: Main

2 · 2.1 Synthesis of PCN-222

Metal precursorsZrOCl2.8H2O (37.5 mg, 0.116 mmol)

Linker precursors5,10,15,20-tetrakis-(4-carboxyphenyl)-porphine-Fe(III) chloride (7.2 mg, 0.0082 mmol)

SolventsDMF (16.25 mL initially; 12 mL for acid treatment)

Additivesdichloroacetic acid (0.25 mL); 8 M HCl (0.5 mL in 12 mL DMF)

Atmospherenot specified

Temperature130 C synthesis; 100 C acid treatment; 120 C vacuum activation

Time18 h synthesis; 24 h acid treatment; activation until vacuum level reached

Work-upCentrifugation; washed with fresh DMF three times; acid-treated in DMF/HCl; supernatant decanted; washed three times with DMF and acetone.

ActivationDynamic vacuum at 120 C until a vacuum level of <=0.002 mmHg min-1 was reached.

Scalability contextBatch synthesis in a 6-dram vial; no yield or scale-up data reported.

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	ZrOCl2.8H2O	37.5 mg, 0.116 mmol	2 · 2.1 Synthesis of PCN-222
Linker	5,10,15,20-Tetrakis-(4-carboxyphenyl)-porphine-Fe(III) chloride	7.2 mg, 0.0082 mmol	2 · 2.1 Synthesis of PCN-222
Solvent	dimethylformamide (DMF)	16.25 mL; later 12 mL	2 · 2.1 Synthesis of PCN-222
Acid	dichloroacetic acid	0.25 mL	2 · 2.1 Synthesis of PCN-222
Acid	HCl	0.5 mL · 8 M	2 · 2.1 Synthesis of PCN-222

Partial recipeSource: Main

2 · 2.2 Preparation of PCN-222/P3HT blend films and transistor-type gas sensors

Solventschloroform

Additiveshexamethyldisilazane (HMDS) surface modifier

Atmospherenot specified

Temperature50 C solution stirring; room temperature aging

Time2 h stirring at 50 C; 3 h at room temperature

Substrate orientationHMDS-coated Si/SiO2 substrate; top-contact bottom-gate OTFT

Work-upP3HT dissolved in chloroform, stirred, cooled, left at room temperature, then spin-coated.

Scalability contextSpin coating at 1500 rpm for 60 s; device channel length 100 um and width 2000 um.

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	P3HT	10 mg mL-1	2 · 2.2 Preparation of PCN-222/P3HT blend films and transistor-type gas sensors
Solvent	chloroform	Not specified	2 · 2.2 Preparation of PCN-222/P3HT blend films and transistor-type gas sensors
Additive	hexamethyldisilazane (HMDS)	Not specified	2 · 2.2 Preparation of PCN-222/P3HT blend films and transistor-type gas sensors