Synthesis · Porous field-effect transistors based on a semiconductive metal-organic framework

3 structured synthesis routes

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

Complete recipeSource: Both

Route 1: Air Liquid Interface

SI p.S2 · Synthesis of Ni3(HITP)2 membrane · Scheme S1

Metal precursorsNickel chloride hexahydrate (NiCl2.6H2O), 6.6 mg (0.028 mmol)

Linker precursorsHATP.6HCl, 10.0 mg (0.019 mmol), precursor to HITP

SolventsH2O, 20.0 mL

AdditivesTrimethylamine (Et3N), 0.2 mL

AtmosphereAir-liquid interface; no inert atmosphere reported

Temperature60

Timenot fixed; membrane visible within 1 min; ca. 3 min gives ca. 100 nm membrane

Substrate orientationFree air-liquid interface in 25.0 mL vial

Work-upFor membrane formation no isolation workup reported before transfer; membrane grows at air-liquid interface.

Scalability contextThickness controlled by reaction time; formation visible to the naked eye at the interface within 1 min.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Linker	HATP.6HCl	10.0 mg (0.019 mmol)	SI p.S2 · Synthesis of Ni3(HITP)2 membrane · Scheme S1
Metal Source	nickel chloride hexahydrate (NiCl2.6H2O)	6.6 mg (0.028 mmol)	SI p.S2 · Synthesis of Ni3(HITP)2 membrane · Scheme S1
Solvent	H2O	20.0 mL	SI p.S2 · Synthesis of Ni3(HITP)2 membrane · Scheme S1
Base	trimethylamine (Et3N)	0.2 mL	SI p.S2 · Synthesis of Ni3(HITP)2 membrane · Scheme S1

Complete recipeSource: Both

Route 2: Other

SI p.S2-S3 · Fabrication of Ni3(HITP)2-based FET · Figure S8

Metal precursorsPreformed Ni3(HITP)2 membrane; Au source/drain electrodes deposited by thermal evaporation

SolventsAcetone, ethanol and deionized water for substrate cleaning; deionized water and ethyl alcohol rinse after transfer

AtmosphereNitrogen flow for substrate drying; vacuum drying at relative vacuum degree -0.1 MPa

Temperature100

Time12 h vacuum drying after transfer; substrate cleaning 10 min in each solvent

Substrate orientationHeavily doped p-type Si substrate with 300 nm SiO2 held horizontally and stamped onto membrane; top membrane surface contacts SiO2

Work-upTransferred membrane rinsed with deionized water and ethyl alcohol to remove residual impurities.

ActivationDried at 100 deg C under -0.1 MPa relative vacuum for 12 h before Au electrode deposition.

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	preformed Ni3(HITP)2 membrane	Not specified	SI p.S2-S3 · Fabrication of Ni3(HITP)2-based FET · Figure S8
Solvent	acetone	10 minutes ultrasonic cleaning	SI p.S2-S3 · Fabrication of Ni3(HITP)2-based FET · Figure S8
Solvent	ethanol / ethyl alcohol	10 minutes ultrasonic cleaning; rinse after transfer	SI p.S2-S3 · Fabrication of Ni3(HITP)2-based FET · Figure S8
Solvent	deionized water	10 minutes ultrasonic cleaning; rinse after transfer	SI p.S2-S3 · Fabrication of Ni3(HITP)2-based FET · Figure S8
Other	Au electrodes	50 nm	SI p.S2-S3 · Fabrication of Ni3(HITP)2-based FET · Figure S8

Complete recipeSource: SI

Route 3: Other

SI p.S3 · Methods · Figure S2

Metal precursorsPreformed Ni3(HITP)2 membrane

SolventsDI water, ethanol

AtmosphereVacuum drying oven

Temperature100

TimeWater reflux 12 h repeated 3 times; ethanol treatment 3 times; final vacuum drying at 100 deg C

Work-upDried membrane gently ground; 100 mg powder mixed with 30 mL DI water, refluxed and solvent-exchanged; procedure repeated with water and ethanol.

ActivationFinal drying at 100 deg C in vacuum drying oven before surface-area measurement.

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	Ni3(HITP)2 powder	100 mg	SI p.S3 · Methods · Figure S2
Solvent	DI water	30 mL initial suspension; refreshed for repeated reflux	SI p.S3 · Methods · Figure S2
Solvent	ethanol	3 washing/reflux cycles	SI p.S3 · Methods · Figure S2