Synthesis · Adjustable Synthesis of Ni-Based Metal-Organic Framework Membranes and Their Field-Effect Transistor Sensors for Mercury Detection

7 structured synthesis routes

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

Complete recipeSource: Both

Route 1: Hydrothermal

623 · 2.3. In Situ Synthesis of Ni3(HITP)2 Membranes · Figure S3

Metal precursors7 mg NiCl2.6H2O in 5 mL deionized water

Linker precursors10 mg HATP.6HCl in 5 mL deionized water

Solventsdeionized water; additional NH3.H2O/H2O mixture with total volume 300 uL

Additives25-28% ammonia, ammonia/water volume ratio 1/5; pH 9.9

Atmospheresealed beaker in air; sealed to prevent ammonia volatilisation

Temperature65

Time1

Substrate orientationFET device put upside down on the mixed solution surface and suspended by surface tension, creating a liquid-solid interface

Work-upDevice removed after 1 h, rinsed with a little deionized water, and dried in a vacuum oven at 100 deg C for 2 h.

ActivationVacuum drying at 100 deg C for 2 h.

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Linker	HATP.6HCl	10 mg · in 5 mL deionized water	623 · 2.3. In Situ Synthesis of Ni3(HITP)2 Membranes · Figure S3
Metal Source	NiCl2.6H2O	7 mg · in 5 mL deionized water	623 · 2.3. In Situ Synthesis of Ni3(HITP)2 Membranes · Figure S3
Base	NH3.H2O, 25-28% ammonia	about 50 uL within 300 uL NH3.H2O/H2O mixture for 1/5 ratio	623 · 2.3. In Situ Synthesis of Ni3(HITP)2 Membranes · Figure S3
Solvent	deionized water	5 mL + 5 mL + about 250 uL in ratio mixture	623 · 2.3. In Situ Synthesis of Ni3(HITP)2 Membranes · Figure S3
Other	Si/SiO2 FET device with patterned Au electrodes	one device	623 · 2.3. In Situ Synthesis of Ni3(HITP)2 Membranes · Figure S3

Complete recipeSource: Both

Route 2: Hydrothermal

623 · 2.3. In Situ Synthesis of Ni3(HITP)2 Membranes

Metal precursors7 mg NiCl2.6H2O in 5 mL deionized water

Linker precursors10 mg HATP.6HCl in 5 mL deionized water

Solventsdeionized water; additional NH3.H2O/H2O mixture with total volume 300 uL

Additives25-28% ammonia, ammonia/water volume ratio 1/2; pH 10.2

Atmospheresealed beaker in air; sealed to prevent ammonia volatilisation

Temperature65

Time1

Substrate orientationFET device upside down on solution surface at the liquid-solid interface

Work-upRinsed with a little deionized water and dried in a vacuum oven at 100 deg C for 2 h.

ActivationVacuum drying at 100 deg C for 2 h.

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Linker	HATP.6HCl	10 mg · in 5 mL deionized water	623 · 2.3. In Situ Synthesis of Ni3(HITP)2 Membranes
Metal Source	NiCl2.6H2O	7 mg · in 5 mL deionized water	623 · 2.3. In Situ Synthesis of Ni3(HITP)2 Membranes
Base	NH3.H2O, 25-28% ammonia	about 100 uL within 300 uL NH3.H2O/H2O mixture for 1/2 ratio	623 · 2.3. In Situ Synthesis of Ni3(HITP)2 Membranes
Solvent	deionized water	5 mL + 5 mL + about 200 uL in ratio mixture	623 · 2.3. In Situ Synthesis of Ni3(HITP)2 Membranes
Other	Si/SiO2 FET device with patterned Au electrodes	one device	623 · 2.3. In Situ Synthesis of Ni3(HITP)2 Membranes

Complete recipeSource: Both

Route 3: Hydrothermal

623 · 2.3. In Situ Synthesis of Ni3(HITP)2 Membranes

Metal precursors7 mg NiCl2.6H2O in 5 mL deionized water

Linker precursors10 mg HATP.6HCl in 5 mL deionized water

Solventsdeionized water; additional NH3.H2O/H2O mixture with total volume 300 uL

Additives25-28% ammonia, ammonia/water volume ratio 2/1; pH 10.6

Atmospheresealed beaker in air; sealed to prevent ammonia volatilisation

Temperature65

Time1

Substrate orientationFET device upside down on solution surface at the liquid-solid interface

Work-upRinsed with a little deionized water and dried in a vacuum oven at 100 deg C for 2 h.

ActivationVacuum drying at 100 deg C for 2 h.

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Linker	HATP.6HCl	10 mg · in 5 mL deionized water	623 · 2.3. In Situ Synthesis of Ni3(HITP)2 Membranes
Metal Source	NiCl2.6H2O	7 mg · in 5 mL deionized water	623 · 2.3. In Situ Synthesis of Ni3(HITP)2 Membranes
Base	NH3.H2O, 25-28% ammonia	about 200 uL within 300 uL NH3.H2O/H2O mixture for 2/1 ratio	623 · 2.3. In Situ Synthesis of Ni3(HITP)2 Membranes
Solvent	deionized water	5 mL + 5 mL + about 100 uL in ratio mixture	623 · 2.3. In Situ Synthesis of Ni3(HITP)2 Membranes
Other	Si/SiO2 FET device with patterned Au electrodes	one device	623 · 2.3. In Situ Synthesis of Ni3(HITP)2 Membranes

Partial recipeSource: Main

Route 4: Other

627 · 3.2. Hg2+ Sensing Performance · Figure S9

Metal precursorsS4 Ni3(HITP)2 membrane on FET device

Linker precursorsHITP framework already present; DNA probe 5'-NH2-TTG-TTG-TTT-CCT-TTC-GTT-TT-3'

Solvents1x TE buffer solution; 1x PBS rinse

Additives10 uM DNA solution

Atmospherelow-temperature incubation at 0-4 deg C

Temperature0-4

Time12

Substrate orientationsilicon rubber liquid cell on FET channel region

Work-upDevice rinsed with PBS solution after incubation.

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Additive	DNA probe, 5'-NH2-TTG-TTG-TTT-CCT-TTC-GTT-TT-3'	10 uM in 1x TE buffer	627 · 3.2. Hg2+ Sensing Performance · Figure S9
Solvent	1x TE buffer solution	EDTA, pH 7.4	627 · 3.2. Hg2+ Sensing Performance · Figure S9
Electrolyte	1x PBS solution	rinse solution · pH 7.4	627 · 3.2. Hg2+ Sensing Performance · Figure S9

Partial recipeSource: Main

Route 5: Other

627 · 3.2. Hg2+ Sensing Performance · Figure S9

Metal precursorsS4 Ni3(HITP)2 membrane on FET device

Linker precursorsHITP framework already present

Solvents1x PBS solution

Additives20 uL of 0.25% glutaraldehyde solution

Atmosphereroom temperature

Temperatureroom temperature

Time1

Substrate orientationsilicon rubber liquid cell on FET channel region

Work-upGA solution removed and device rinsed with 1x PBS solution.

Show 2 structured reagent records

Role	Reagent	Amount / concentration	Source
Additive	glutaraldehyde (GA) solution	20 uL · 0.25%	627 · 3.2. Hg2+ Sensing Performance · Figure S9
Electrolyte	1x PBS solution	rinse solution · pH 7.4	627 · 3.2. Hg2+ Sensing Performance · Figure S9

Complete recipeSource: Main

Route 6: Other

623 · 2.4. Sensor Fabrication

Metal precursorsS4 Ni3(HITP)2 membrane on FET device

Linker precursorsHITP framework already present; DNA probe 5'-NH2-TTG-TTG-TTT-CCT-TTC-GTT-TT-3'

Solvents1x PBS solution; 1x TE buffer solution

Additives20 uL of 0.25% glutaraldehyde solution; 10 uM DNA solution

Atmosphereroom-temperature liquid-cell treatment, then low-temperature incubation at 0-4 deg C

Temperatureroom temperature for GA; 0-4 for DNA incubation

Time1 h GA treatment; 12 h DNA incubation

Substrate orientationsilicon rubber liquid cell on FET channel region

Work-upGA solution removed, device rinsed with 1x PBS; after DNA incubation, device rinsed with PBS again.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Additive	glutaraldehyde (GA) solution	20 uL · 0.25%	623 · 2.4. Sensor Fabrication
Additive	DNA probe, 5'-NH2-TTG-TTG-TTT-CCT-TTC-GTT-TT-3'	10 uM in 1x TE buffer	623 · 2.4. Sensor Fabrication
Electrolyte	1x PBS solution	rinse solution · pH 7.4	623 · 2.4. Sensor Fabrication
Solvent	1x TE buffer solution	EDTA, pH 7.4	623 · 2.4. Sensor Fabrication

Complete recipeSource: Both

Route 7: Hydrothermal

623 · 2.3. In Situ Synthesis of Ni3(HITP)2 Membranes · Figure S3

Metal precursors7 mg NiCl2.6H2O in 5 mL deionized water

Linker precursors10 mg HATP.6HCl in 5 mL deionized water

Solventsdeionized water; additional NH3.H2O/H2O mixture with total volume 300 uL

Additives25-28% ammonia, ammonia/water volume ratio 3/0; pH 11.1

Atmospheresealed beaker in air; sealed to prevent ammonia volatilisation

Temperature65

Time1

Substrate orientationFET device upside down on solution surface at the liquid-solid interface

Work-upRinsed with a little deionized water and dried in a vacuum oven at 100 deg C for 2 h.

ActivationVacuum drying at 100 deg C for 2 h.

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Linker	HATP.6HCl	10 mg · in 5 mL deionized water	623 · 2.3. In Situ Synthesis of Ni3(HITP)2 Membranes · Figure S3
Metal Source	NiCl2.6H2O	7 mg · in 5 mL deionized water	623 · 2.3. In Situ Synthesis of Ni3(HITP)2 Membranes · Figure S3
Base	NH3.H2O, 25-28% ammonia	300 uL for 3/0 ammonia/water ratio	623 · 2.3. In Situ Synthesis of Ni3(HITP)2 Membranes · Figure S3
Solvent	deionized water	5 mL + 5 mL	623 · 2.3. In Situ Synthesis of Ni3(HITP)2 Membranes · Figure S3
Other	Si/SiO2 FET device with patterned Au electrodes	one device	623 · 2.3. In Situ Synthesis of Ni3(HITP)2 Membranes · Figure S3