Synthesis evidence

Wet-Adhesive On-Skin Sensors Based on Metal–Organic Frameworks for Wireless Monitoring of Metabolites in Sweat

Yang X., Yi J., Wang T. et al. · Advanced Materials · 2022 · 2201768

7 structured synthesis routes

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

Partial recipeSource: SI

Route 1: Other

S2 · Sensor Fabrication and Preparation · Figure S1-S2

Linker precursorsCommercial bacterial nanocellulose gel (10 g)
SolventsDI water (150 mL)
AdditivesPolyvinylidene fluoride filter membrane used for filtration support
AtmosphereAmbient air during drying; not otherwise specified
Temperature60 drying
Time5 min ultrasonication; drying time not specified
Substrate orientationVacuum filtration through PVDF filter membrane
Work-upBNC membrane dried on filter paper and peeled off from the filter membrane.
ActivationNone reported
Scalability contextFacile vacuum filtration; final membrane thickness shown as about 15 um.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Othercommercial BNC gel10 gS2 · Sensor Fabrication and Preparation · Figure S1-S2
SolventDI water150 mLS2 · Sensor Fabrication and Preparation · Figure S1-S2
Otherpolyvinylidene fluoride filter membraneNot specifiedS2 · Sensor Fabrication and Preparation · Figure S1-S2
Complete recipeSource: SI

Route 2: Solvothermal

S3 · Synthesis of cMOFs

Metal precursorsCopper acetate (6.4 mg)
Linker precursorsHHTP (5.2 mg)
SolventsMethanol (4.5 mL); DI water and acetone for washing; acetone for solvent exchange
AtmosphereSealed glass bottle; gas atmosphere not specified
Temperature65 reaction; 80 solvent removal
Time24 reaction; acetone exchange for one week; overnight heating
Substrate orientationNone; powder synthesis
Work-upWashed several times with DI water and acetone; activated by acetone solvent exchange refreshed three times for one week.
ActivationHeated overnight at 80 C to remove solvent.
Scalability context10 mL sealed glass bottle; no yield reported.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Metal Sourcecopper acetate6.4 mgS3 · Synthesis of cMOFs
LinkerHHTP5.2 mgS3 · Synthesis of cMOFs
Solventmethanol4.5 mLS3 · Synthesis of cMOFs
SolventDI waterwash several timesS3 · Synthesis of cMOFs
Solventacetonewash and solvent exchangeS3 · Synthesis of cMOFs
Complete recipeSource: SI

Route 3: Drop Cast

S2 · Sensor Fabrication and Preparation · Figure S4-S5

Metal precursorsPrepared Ni3HHTP2 MOF powder (2 mg)
Linker precursorsHHTP already incorporated in Ni3HHTP2
SolventsPBS solution; Nafion solution supplied in lower aliphatic alcohols and water
AdditivesNafion solution, 10 vol% relative to PBS; 5% Nafion stock
AtmosphereNatural drying atmosphere not specified
TemperatureRoom temperature drying implied
TimeAt least 6 h ultrasonication; dried overnight
Substrate orientationDrop-cast onto Au working electrode on BNC membrane
Work-upMOF/PBS/Nafion dispersion ultrasonicated to homogeneity; total 10 uL added as four 2.5 uL additions.
ActivationNaturally dried overnight on the working electrode.
Scalability contextSmall-area electrode; main text reports working electrode area d = 3 mm, S = 0.070 cm2.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Otherprepared MOFs2 mgS2 · Sensor Fabrication and Preparation · Figure S4-S5
Electrolytephosphate-buffered saline (PBS) solution10% volume ratio between Nafion and PBSS2 · Sensor Fabrication and Preparation · Figure S4-S5
AdditiveNafion solution5% stock; 10% in PBS mixtureS2 · Sensor Fabrication and Preparation · Figure S4-S5
Solventlower aliphatic alcohols and waterin Nafion stockS2 · Sensor Fabrication and Preparation · Figure S4-S5
Complete recipeSource: SI

Route 4: Other

S3 · Synthesis of cMOFs

Metal precursorsNi(OAc)2*4H2O (456 mg)
Linker precursorsHHTP (200 mg)
SolventsDI water (28 mL); acetone for washing/solvent exchange
AtmosphereNot specified
Temperature85 reaction; 80 vacuum activation
Time24 reaction; acetone exchange for one week; overnight vacuum heating
Substrate orientationNone; powder synthesis
Work-upWashed several times with DI water and acetone; solvent exchange with acetone refreshed three times for one week.
ActivationHeated under vacuum at 80 C overnight to remove solvent.
Scalability context100 mL round-bottom flask, stirred at 600 rpm; no yield reported.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceNi(OAc)2*4H2O456 mgS3 · Synthesis of cMOFs
LinkerHHTP200 mgS3 · Synthesis of cMOFs
SolventDI water28 mLS3 · Synthesis of cMOFs
Solventacetonerefreshed three times for one weekS3 · Synthesis of cMOFs
Partial recipeSource: SI

Route 5: Other

S3 · Synthesis of cMOFs

Metal precursorsNi(OAc)2 (3.383 mg)
Linker precursorsHITP (40.526 mg)
SolventsDI water (10 mL + 5 mL); acetone for washing
AdditivesAmmonium hydroxide (30%, 300 uL)
AtmosphereNot specified
Temperature85
Time24
Substrate orientationNone; powder synthesis
Oxidant / reductantAmmonium hydroxide base additive
Work-upProduct washed several times with DI water and acetone.
ActivationNot reported for Ni3HITP2 beyond washing.
Scalability contextHot oil bath at 600 rpm; no yield reported.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceNi(OAc)23.383 mgS3 · Synthesis of cMOFs
LinkerHITP40.526 mgS3 · Synthesis of cMOFs
Baseammonium hydroxide300 uL · 30%S3 · Synthesis of cMOFs
SolventDI water10 mL + 5 mLS3 · Synthesis of cMOFs
Solventacetonewash several timesS3 · Synthesis of cMOFs
Partial recipeSource: SI

Route 6: Other

S6-S7 · The process of connecting enameled wire · Figure S21

Metal precursorsEnameled Cu wires, 0.04 mm diameter
AdditivesAnisotropic conductive film adhesive (3M Film 9703), 50 um adhesive thickness; cellulose fixing film
AtmosphereNot specified
Substrate orientationCu wires connected to tattoo sensor with z-axis conductive ACF
Work-upACF and enameled wire fixed with an appropriately sized cellulose film.
ActivationNone reported
Scalability contextUsed for wireless on-body sweat measurement connection.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Metal Sourceenameled Cu wires0.04 mm diameterS6-S7 · The process of connecting enameled wire · Figure S21
Additiveanisotropic conductive film adhesive3M Film 9703; 50 um adhesive thicknessS6-S7 · The process of connecting enameled wire · Figure S21
Othercellulose filmappropriately sizedS6-S7 · The process of connecting enameled wire · Figure S21
Partial recipeSource: Both

Route 7: Other

2 · Results and Discussions · Figure 1b

Metal precursorsCr and Au evaporated layers; commercial Ag/AgCl conductive ink
AdditivesEcoflex insulation described in main text for encapsulation
AtmosphereThermal evaporation atmosphere not specified
TimeAg/AgCl ink dried overnight
Substrate orientationCr/Au evaporated on BNC membrane through a metal shadow mask
Work-upAg/AgCl conductive ink dropped onto the specified Au electrode area and dried overnight.
ActivationNone reported
Scalability contextPatterned Cr (5 nm)/Au (75 nm) electrode enables two WEs, one CE, and one RE on a BNC membrane.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCr5 nm layer2 · Results and Discussions · Figure 1b
Metal SourceAu75 nm layer2 · Results and Discussions · Figure 1b
OtherAg/AgCl conductive ink60/402 · Results and Discussions · Figure 1b
OtherEcoflexencapsulation layer2 · Results and Discussions · Figure 1b