Synthesis · A Humidity-Induced Large Electronic Conductivity Change of 107 on a Metal-Organic Framework for Highly Sensitive Water Detection

6 structured synthesis routes

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

Complete recipeSource: SI

Route 1: Solvothermal

3 · S1.2 Materials and Synthetic Procedures

Metal precursorstetrabutyl titanate, Ti(OC4H9)4, 0.105 mL

Linker precursorsNH2-BDC 0.163 g; (NH2)2-BDC 0.02 g

SolventsDMF 8 mL; dry methanol 2 mL

Atmospherenot specified

Temperature150 reaction; 150 drying

Time72 h reaction; overnight drying

Work-upcooled, centrifuged, washed with DMF/methanol

Activationdried in an oven at 150 C overnight

Scalability context20 mL Teflon-lined autoclave batch synthesis.

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Linker	NH2-BDC	0.163 g	3 · S1.2 Materials and Synthetic Procedures
Linker	(NH2)2-BDC	0.02 g	3 · S1.2 Materials and Synthetic Procedures
Metal Source	tetrabutyl titanate	0.105 mL	3 · S1.2 Materials and Synthetic Procedures
Solvent	DMF	8 mL	3 · S1.2 Materials and Synthetic Procedures
Solvent	dry methanol	2 mL	3 · S1.2 Materials and Synthetic Procedures

Complete recipeSource: SI

Route 2: Other

3 · S1.2 Materials and Synthetic Procedures

Metal precursorspreformed (NH2)2-MIL-125 powder

Linker precursorspreformed (NH2)2-MIL-125

Solventsmethanol 10 mL

AdditivesH2SO4, 0.2 mL, 1 M

Atmospherenot specified

Temperature80 drying

Timeovernight drying; H2SO4 injection rate 4 microL min-1

Work-upvigorous stirring during H2SO4 injection; product obtained and dried

Activationdried at 80 C overnight

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	(NH2)2-MIL-125 powder	500 mg	3 · S1.2 Materials and Synthetic Procedures
Solvent	methanol solution	10 mL	3 · S1.2 Materials and Synthetic Procedures
Acid	H2SO4	0.2 mL · 1 M	3 · S1.2 Materials and Synthetic Procedures

Complete recipeSource: Both

Route 3: Drop Cast

4 · S1.4 Evaluation of Sensing Performance · Figures S10-S11

Metal precursorsH2SO4@(NH2)2-MIL-125 powder

Solventsmethanol 1 mL

Atmosphereroom temperature stirring; dried in air/unspecified atmosphere

Temperature80 drying

Time12 h stirring

Substrate orientationAd-Pd interdigital electrodes on Al2O3; electrode width and gap 0.15 mm

Work-up20 microL suspension drop coated onto interdigital electrodes

Activationdried at 80 C

Scalability contextConvenient drop-coating fabrication; no film thickness reported.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	H2SO4@(NH2)2-MIL-125	20 mg	4 · S1.4 Evaluation of Sensing Performance · Figures S10-S11
Solvent	methanol	1 mL	4 · S1.4 Evaluation of Sensing Performance · Figures S10-S11
Other	drop-coated suspension	20 microL	4 · S1.4 Evaluation of Sensing Performance · Figures S10-S11
Other	Ad-Pd interdigital electrodes	Not specified	4 · S1.4 Evaluation of Sensing Performance · Figures S10-S11

Partial recipeSource: Both

Route 4: Other

4 · S1.5 Measurements of electronic conduction contribution · Figure S5

Metal precursorsH2SO4@(NH2)2-MIL-125 powder

AdditivesPt wires/electrodes

Atmosphere0-100 percent RH during measurement

Temperature25 measurement

Substrate orientationPt ion-blocking electrodes attached to membrane/thick film

Work-uppowder particles prepared into a thick film/membrane

Show 2 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	H2SO4@(NH2)2-MIL-125 powder	Not specified	4 · S1.5 Measurements of electronic conduction contribution · Figure S5
Other	Pt electrodes	Not specified	4 · S1.5 Measurements of electronic conduction contribution · Figure S5

Complete recipeSource: SI

Route 5: Solvothermal

3 · S1.2 Materials and Synthetic Procedures

Metal precursorstetrabutyl titanate, Ti(OC4H9)4, 0.21 mL

Linker precursorsterephthalic acid, H2-BDC, 0.25 g

SolventsDMF 4.5 mL; methanol 0.5 mL

Atmospherenot specified

Temperature105 pre-treatment; 150 solvothermal reaction; 150 drying

Time4 h pre-treatment; 72 h solvothermal; overnight drying

Work-upcooled, centrifuged, washed with DMF/methanol

Activationdried in an oven at 150 C overnight

Scalability context20 mL Teflon-lined autoclave batch synthesis.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Linker	H2-BDC	0.25 g	3 · S1.2 Materials and Synthetic Procedures
Metal Source	tetrabutyl titanate	0.21 mL	3 · S1.2 Materials and Synthetic Procedures
Solvent	DMF	4.5 mL	3 · S1.2 Materials and Synthetic Procedures
Solvent	methanol	0.5 mL	3 · S1.2 Materials and Synthetic Procedures

Complete recipeSource: SI

Route 6: Solvothermal

3 · S1.2 Materials and Synthetic Procedures

Metal precursorstetrabutyl titanate, Ti(OC4H9)4, 0.105 mL

Linker precursors2-amino terephthalic acid, NH2-BDC, 0.2172 g

SolventsDMF 9 mL; dry methanol 1 mL

Atmospherenot specified

Temperature150 reaction; 150 drying

Time72 h reaction; overnight drying

Work-upcooled, centrifuged, washed with DMF/methanol

Activationdried in an oven at 150 C overnight

Scalability context20 mL Teflon-lined autoclave batch synthesis.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Linker	NH2-BDC	0.2172 g	3 · S1.2 Materials and Synthetic Procedures
Metal Source	tetrabutyl titanate	0.105 mL	3 · S1.2 Materials and Synthetic Procedures
Solvent	DMF	9 mL	3 · S1.2 Materials and Synthetic Procedures
Solvent	dry methanol	1 mL	3 · S1.2 Materials and Synthetic Procedures