Synthesis · 1D Conductive Metal-Organic Framework-Enabled Dual-Parameter MEMS Gas Sensor for Thermal Runaway Monitoring

6 structured synthesis routes

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

Complete recipeSource: Main

Route 1: Air Liquid Interface

p.12 · Experimental Section, Synthesis of MBTA MOF Film · Figure 3b

Metal precursors1.0 mg CuCl2.2H2O corresponding metal chloride salt

Linker precursors1.0 mg BTA.4HCl

Solvents100.0 uL DI water; 100.0 uL glycerol additive/viscosity modifier; DI water and ethanol rinses

Additives14 mol L^-1 ammonia solution placed around the device in Petri dish; glycerol added to precursor solution

AtmosphereCovered Petri dish with ammonia vapour diffusion into precursor droplet; ambient gas-liquid interface assembly.

Temperatureroom temperature reaction; 60 drying

Time12 reaction; ammonia replenished every 4 h; 12 drying

Substrate orientationPrecursor solution dispensed by 0.1 mm inner-diameter capillary onto MEMS IDEs.

Oxidant / reductantAmmonia vapour catalysis; ambient oxygen likely participates analogously to powder synthesis.

Work-upRepeated DI water and ethanol rinsing; ultrasonic cleaning avoided to protect cantilever structures.

ActivationVacuum dried at 60 deg C for 12 h.

Scalability contextDirect on-device growth on four-channel MEMS IDEs, suitable for integrated microsensor fabrication.

Show 6 structured reagent records

Role	Reagent	Amount / concentration	Source
Linker	BTA.4HCl	1.0 mg · in 100.0 uL DI water with metal salt	p.12 · Experimental Section, Synthesis of MBTA MOF Film · Figure 3b
Metal Source	CuCl2.2H2O	1.0 mg · corresponding metal chloride salt in 100.0 uL DI water	p.12 · Experimental Section, Synthesis of MBTA MOF Film · Figure 3b
Additive	glycerol	100.0 uL · AR	p.12 · Experimental Section, Synthesis of MBTA MOF Film · Figure 3b
Base	ammonia aqueous solution	small amount around Petri dish, replenished every 4 h · 14 mol L^-1	p.12 · Experimental Section, Synthesis of MBTA MOF Film · Figure 3b
Solvent	DI water	100.0 uL precursor solvent plus rinses	p.12 · Experimental Section, Synthesis of MBTA MOF Film · Figure 3b
Solvent	ethanol	rinse solvent · AR	p.12 · Experimental Section, Synthesis of MBTA MOF Film · Figure 3b

Partial recipeSource: Main

Route 2: Other

p.8 · Results and Discussion, 2.4 · Figure 6a

Metal precursorsPreformed in-situ CuBTA MEMS film

Linker precursorsPreformed CuBTA framework

AdditivesPDMS precursor solution

AtmosphereAmbient thermal curing; gas-impermeable PDMS membrane formed on MEMS channel.

Temperature80

Time12

Substrate orientationPDMS precursor applied to Sens. 3 using capillary drop-coating on 4-channel MEMS device.

Work-upThermal curing to form uniform PDMS encapsulation layer.

Scalability contextOn-chip post-processing step for decoupled gas and temperature channels.

Show 2 structured reagent records

Role	Reagent	Amount / concentration	Source
Additive	PDMS precursor solution	not reported · not reported	p.8 · Results and Discussion, 2.4 · Figure 6a
Other	CuBTA MEMS film	Sens. 3	p.8 · Results and Discussion, 2.4 · Figure 6a

Complete recipeSource: Main

Route 3: Other

p.12 · Experimental Section, Synthesis of MBTA MOF Powder

Metal precursors17.0 mg CuCl2.2H2O (0.1 mmol) in 5.0 mL DI water

Linker precursors28.4 mg BTA.4HCl (0.1 mmol) in 5.0 mL DI water

SolventsDI water; ethanol used in washing

Additives1.0 mL 14 mol L^-1 ammonia solution

AtmosphereVial capped but not fully tightened to allow limited air exposure; O2 from air participates in ligand oxidation.

Temperature25 for reaction; 60 for vacuum drying

Time12 reaction; 24 drying

Oxidant / reductantO2 from air oxidises -NH2 to -NH- during coordination polymerisation.

Work-upCentrifuge at 8000 rpm; wash three times alternately with DI water and ethanol.

ActivationVacuum oven drying at 60 deg C for 24 h; no separate activation reported.

Scalability contextRoom-temperature wet-chemical route in a 20 mL vial; no scale-up demonstrated.

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Linker	BTA.4HCl	28.4 mg · 0.1 mmol in 5.0 mL DI water	p.12 · Experimental Section, Synthesis of MBTA MOF Powder
Metal Source	CuCl2.2H2O	17.0 mg · 0.1 mmol in 5.0 mL DI water	p.12 · Experimental Section, Synthesis of MBTA MOF Powder
Base	ammonia aqueous solution (NH3.H2O)	1.0 mL · 14 mol L^-1	p.12 · Experimental Section, Synthesis of MBTA MOF Powder
Solvent	DI water	10.0 mL total before ammonia · 18.1 Mohm cm resistivity	p.12 · Experimental Section, Synthesis of MBTA MOF Powder
Solvent	ethanol	washing solvent · AR	p.12 · Experimental Section, Synthesis of MBTA MOF Powder

Complete recipeSource: Main

Route 4: Air Liquid Interface

p.12 · Experimental Section, Synthesis of MBTA MOF Film · Figure 3b

Metal precursors1.0 mg NiCl2.6H2O corresponding metal chloride salt

Linker precursors1.0 mg BTA.4HCl

Solvents100.0 uL DI water; 100.0 uL glycerol additive/viscosity modifier; DI water and ethanol rinses

Additives14 mol L^-1 ammonia solution placed around the device in Petri dish; glycerol added to precursor solution

AtmosphereCovered Petri dish with ammonia vapour diffusion into precursor droplet; ambient gas-liquid interface assembly.

Temperatureroom temperature reaction; 60 drying

Time12 reaction; ammonia replenished every 4 h; 12 drying

Substrate orientationPrecursor solution dispensed by 0.1 mm inner-diameter capillary onto MEMS IDEs.

Oxidant / reductantAmmonia vapour catalysis; ambient oxygen likely participates analogously to powder synthesis.

Work-upRepeated DI water and ethanol rinsing; ultrasonic cleaning avoided to protect cantilever structures.

ActivationVacuum dried at 60 deg C for 12 h.

Scalability contextDirect on-device growth on four-channel MEMS IDEs, suitable for integrated microsensor fabrication.

Show 6 structured reagent records

Role	Reagent	Amount / concentration	Source
Linker	BTA.4HCl	1.0 mg · in 100.0 uL DI water with metal salt	p.12 · Experimental Section, Synthesis of MBTA MOF Film · Figure 3b
Metal Source	NiCl2.6H2O	1.0 mg · corresponding metal chloride salt in 100.0 uL DI water	p.12 · Experimental Section, Synthesis of MBTA MOF Film · Figure 3b
Additive	glycerol	100.0 uL · AR	p.12 · Experimental Section, Synthesis of MBTA MOF Film · Figure 3b
Base	ammonia aqueous solution	small amount around Petri dish, replenished every 4 h · 14 mol L^-1	p.12 · Experimental Section, Synthesis of MBTA MOF Film · Figure 3b
Solvent	DI water	100.0 uL precursor solvent plus rinses	p.12 · Experimental Section, Synthesis of MBTA MOF Film · Figure 3b
Solvent	ethanol	rinse solvent · AR	p.12 · Experimental Section, Synthesis of MBTA MOF Film · Figure 3b

Partial recipeSource: Main

Route 5: Other

p.8 · Results and Discussion, 2.4 · Figure 6a

Metal precursorsPreformed in-situ NiBTA MEMS film

Linker precursorsPreformed NiBTA framework

AdditivesPDMS precursor solution

AtmosphereAmbient thermal curing; gas-impermeable PDMS membrane formed on MEMS channel.

Temperature80

Time12

Substrate orientationPDMS precursor applied to Sens. 4 using capillary drop-coating on 4-channel MEMS device.

Work-upThermal curing to form uniform PDMS encapsulation layer.

Scalability contextOn-chip post-processing step for decoupled gas and temperature channels.

Show 2 structured reagent records

Role	Reagent	Amount / concentration	Source
Additive	PDMS precursor solution	not reported · not reported	p.8 · Results and Discussion, 2.4 · Figure 6a
Other	NiBTA MEMS film	Sens. 4	p.8 · Results and Discussion, 2.4 · Figure 6a

Complete recipeSource: Main

Route 6: Other

p.12 · Experimental Section, Synthesis of MBTA MOF Powder

Metal precursors23.8 mg NiCl2.6H2O (0.1 mmol) in 5.0 mL DI water

Linker precursors28.4 mg BTA.4HCl (0.1 mmol) in 5.0 mL DI water

SolventsDI water; ethanol used in washing

Additives1.0 mL 14 mol L^-1 ammonia solution

AtmosphereVial capped but not fully tightened to allow limited air exposure; O2 from air participates in ligand oxidation.

Temperature25 for reaction; 60 for vacuum drying

Time12 reaction; 24 drying

Oxidant / reductantO2 from air oxidises -NH2 to -NH- during coordination polymerisation.

Work-upCentrifuge at 8000 rpm; wash three times alternately with DI water and ethanol.

ActivationVacuum oven drying at 60 deg C for 24 h; no separate activation reported.

Scalability contextRoom-temperature wet-chemical route in a 20 mL vial; no scale-up demonstrated.

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Linker	BTA.4HCl	28.4 mg · 0.1 mmol in 5.0 mL DI water	p.12 · Experimental Section, Synthesis of MBTA MOF Powder
Metal Source	NiCl2.6H2O	23.8 mg · 0.1 mmol in 5.0 mL DI water	p.12 · Experimental Section, Synthesis of MBTA MOF Powder
Base	ammonia aqueous solution (NH3.H2O)	1.0 mL · 14 mol L^-1	p.12 · Experimental Section, Synthesis of MBTA MOF Powder
Solvent	DI water	10.0 mL total before ammonia · 18.1 Mohm cm resistivity	p.12 · Experimental Section, Synthesis of MBTA MOF Powder
Solvent	ethanol	washing solvent · AR	p.12 · Experimental Section, Synthesis of MBTA MOF Powder