Synthesis · Reversible Molecule Interactions Enable Ultrastretchable and Recyclable Ionogels for Wearable Piezoionic Sensors

5 structured synthesis routes

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

Partial recipeSource: Main

Route 1: Drop Cast

50028 · 2.2.3 · Figure 2a

Metal precursorsUiO-66-NH2@PAA additive supplies Zr-containing MOF component

Linker precursorsUiO-66-NH2@PAA, TPU and [EMIM][EtSO4]

SolventsDMAC (10 mL for TPU solution)

Additives[EMIM][EtSO4] ionic liquid, 20-40 wt%; UiO-66-NH2@PAA, 0-20 wt%

Atmosphereambient/not specified

Temperature80

Time3 h TPU dissolution; about 5 h stirring after additions; drying time not specified

Substrate orientation3 mL cast on glass plate

Work-upDissolve 1 g TPU in 10 mL DMAC; add ionic liquid and UiO-66-NH2@PAA; stir to uniform liquid; cast 3 mL on glass plate.

ActivationHeat at 80 C to remove solvent and obtain ionogels.

Scalability contextConclusion states preparation can be mass-produced, but no production scale or yield is demonstrated.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	TPU	1 g	50028 · 2.2.3 · Figure 2a
Solvent	DMAC	10 mL	50028 · 2.2.3 · Figure 2a
Electrolyte	[EMIM][EtSO4]	20-40 wt% · relative to TPU	50028 · 2.2.3 · Figure 2a
Additive	UiO-66-NH2@PAA	0-20 wt% · relative to TPU	50028 · 2.2.3 · Figure 2a

Partial recipeSource: Main

Route 2: Other

50028 · 2.2.5 · Figure 3a

Metal precursorsZr-containing UiO-66-NH2@PAA retained in recovered ionogel

Linker precursorsrecovered ionogel network

SolventsDMAC, appropriate amount just enough to dissolve recovered ionogels

Additivesnone reported

Atmosphereambient/not specified

Temperatureroom temperature dissolution; 80 drying

Time4 h stirring; 4 h drying

Substrate orientation3 mL recast on glass plate

Work-upClean ionogel surface; dissolve recovered ionogels in DMAC; stir at room temperature; cast 3 mL on glass plate.

ActivationHeat at 80 C for 4 h, cool to room temperature and cut.

Scalability contextSolvent remoulding at room temperature without specialised instruments; no cycle-count scale-up data given.

Show 2 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	recovered ionogels	not specified	50028 · 2.2.5 · Figure 3a
Solvent	DMAC	just enough to dissolve recovered ionogels	50028 · 2.2.5 · Figure 3a

Partial recipeSource: Main

Route 3: Other

50028 · 2.2.4 · Figure 4a

Metal precursorsZr-containing UiO-66-NH2@PAA present in ionogel membrane

Linker precursorsionogel membrane plus MWCNT electrode membrane

SolventsNMP for MWCNT dispersion

AdditivesMWCNT electrodes; copper wire contacts

Atmosphereambient/not specified; vacuum filtration used

Temperature80 for electrode drying; 140 hot press

Time0.5 h sonication; 8 h electrode drying; 0.25 h hot press

Substrate orientationMWCNT electrode membranes laminated on both sides of ionogel membrane

Work-upDisperse 10 mg MWCNT in 10 mL NMP; filter 2 mL onto membrane under vacuum; dry; cut ionogel and electrode membranes; attach two electrodes.

ActivationHot press at 140 C for 15 min; cut sensor to 0.5 cm width and solder copper wires.

Scalability contextManual membrane assembly; conclusion claims simple assembly and potential mass production without process metrics.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Additive	MWCNT	10 mg · in 10 mL NMP	50028 · 2.2.4 · Figure 4a
Solvent	NMP	10 mL	50028 · 2.2.4 · Figure 4a
Other	ionogel membrane	2 cm x 1 cm	50028 · 2.2.4 · Figure 4a
Other	electrode membrane	3 cm x 1 cm	50028 · 2.2.4 · Figure 4a

Partial recipeSource: Main

Route 4: Other

50028 · 2.2.2 · Figure 1a

Metal precursorsUiO-66-NH2 powder containing Zr nodes (10 mg)

Linker precursorsUiO-66-NH2 framework; PAA polymer

Solventsdeionised water (10 mL)

Additivespoly(acrylic acid), 300 mg thick liquid

Atmospherenot specified; sealed sample bottle

Temperature80

Time0.5 h sonication, 12 h standing, 0.5 h sonication; drying time not specified

Substrate orientationmould casting

Work-upSeal bottle; sonicate 30 min; stand 12 h; sonicate 30 min before use; pour into mould.

ActivationHeat at 80 C to remove water and obtain UiO-66-NH2@PAA.

Scalability contextSmall-batch 10 mg MOF coating step; no yield given.

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	UiO-66-NH2	10 mg	50028 · 2.2.2 · Figure 1a
Additive	poly(acrylic acid) (PAA)	300 mg · M.W. ~5000, 50 wt% aqueous solution stock	50028 · 2.2.2 · Figure 1a
Solvent	deionized water	10 mL	50028 · 2.2.2 · Figure 1a

Partial recipeSource: Main

Route 5: Solvothermal

50028 · 2.2.1

Metal precursorsZrCl4 (932 mg, 4 mmol)

Linker precursorsH2BDCNH2 (724 mg, 4 mmol)

SolventsDMF; formic acid (26.8 mL); methanol for soaking

Additivesformic acid modulator

Atmospherenot specified

Temperature120; drying 60

Time24; methanol soak 3 days

Substrate orientationnone

Work-upCool to room temperature; centrifuge at 8000 rpm for 10 min; wash several times; soak in methanol for 3 days; centrifuge again.

ActivationDry at 60 C to obtain light-yellow powder.

Scalability context100 mL Teflon-sealed autoclave; no yield or scale-up data reported.

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	ZrCl4	932 mg, 4 mmol	50028 · 2.2.1
Linker	H2BDCNH2	724 mg, 4 mmol	50028 · 2.2.1
Acid	formic acid	26.8 mL	50028 · 2.2.1
Solvent	DMF	not specified	50028 · 2.2.1
Solvent	methanol	not specified	50028 · 2.2.1