cMOF Evidence Base

Synthesis evidence

In Situ Growth of Conductive Metal-Organic Framework onto Cu2O for Highly Selective and Humidity-Independent Hydrogen Sulfide Detection in Food Quality Assessment

Zhang F., Jiao C., Shang Y. et al. · ACS Sensors · 2024 · 1310-1320

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: Other

p015 / S-14 · Supporting Information · Figure S11

Metal precursors35 mg Cu2O cubes
Linker precursors35 mg H3BTC ligands
Solvents20 mL benzyl alcohol; 2.5 mL ethanol linker solution; ethanol washing
Additivesnone specified
Atmospherenot specified
Temperature80 C oil bath
Time10 min sonication; 5 min room-temperature stirring; 5 min at 80 C
Substrate orientationCu2O cube template
Oxidant / reductantin situ etching of Cu2O with H3BTC
Work-upCentrifuged and washed with ethanol several times.
Activationnot specified
Scalability contextSmall-batch comparison route.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCu2O cubes35 mgp015 / S-14 · Supporting Information · Figure S11
LinkerH3BTC ligands35 mg · in 2.5 mL ethanolp015 / S-14 · Supporting Information · Figure S11
Solventbenzyl alcohol20 mLp015 / S-14 · Supporting Information · Figure S11
Solventethanol2.5 mL and washing solventp015 / S-14 · Supporting Information · Figure S11
Complete recipeSource: SI

Route 2: Other

p006 / S-5 · Supporting Information · Figure S3

Metal precursors10 mg Cu2O cubes; 7.5 mg Cu(Ac)2.H2O
Linker precursors8 mg HHTP ligands
Solvents6 mL DMF + 0.6 mL H2O dispersion; 10 mL DMF linker/Cu(Ac)2 solution; methanol and DMF washing
Additivesnone specified
Atmospherenot specified
Temperature120 C oil bath
Time10 min sonication; 5 min room-temperature stirring; 10 min at 120 C
Substrate orientationCu2O cubes
Oxidant / reductantCu(Ac)2.H2O supplies Cu2+
Work-upCentrifuged and washed with methanol and DMF several times.
Activationnot specified
Scalability contextMechanistic small-batch control route.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCu2O cubes10 mgp006 / S-5 · Supporting Information · Figure S3
Metal SourceCu(Ac)2.H2O7.5 mgp006 / S-5 · Supporting Information · Figure S3
LinkerHHTP ligands8 mgp006 / S-5 · Supporting Information · Figure S3
SolventDMF6 mL + 10 mLp006 / S-5 · Supporting Information · Figure S3
SolventH2O0.6 mLp006 / S-5 · Supporting Information · Figure S3
Complete recipeSource: Main

Route 3: Other

p003 / 1312 · Experimental Section

Metal precursors0.375 g CuSO4.5H2O
Linker precursorsnone
Solvents100 mL deionized water; ethanol for washing
Additives0.15 g sodium citrate tribasic dehydrate; 1 g NaOH; 50 mL 0.03 M L-ascorbic acid
Atmospherenot specified
Temperature80 C drying; reaction temperature not specified
Time10 min CuSO4 stirring; 15 min after citrate/NaOH; 40 min after ascorbic acid; 12 h drying
Substrate orientationnone
Oxidant / reductantL-ascorbic acid as reductant
Work-upWashed with DI water and ethanol several times.
ActivationDried at 80 C for 12 h in vacuum.
Scalability contextBatch solution synthesis at 0.375 g CuSO4.5H2O scale.
Show 6 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCuSO4.5H2O0.375 gp003 / 1312 · Experimental Section
BaseNaOH1 gp003 / 1312 · Experimental Section
Additivesodium citrate tribasic dehydrate0.15 gp003 / 1312 · Experimental Section
ReductantL-ascorbic acid solution50 mL · 0.03 Mp003 / 1312 · Experimental Section
Solventdeionized water100 mLp003 / 1312 · Experimental Section
Solventethanolwashing solventp003 / 1312 · Experimental Section
Complete recipeSource: Both

Route 4: Other

p003 / 1312 · Experimental Section

Metal precursors10 mg Cu2O cubes; 12 mg Cu(Ac)2.H2O per Cu2+ end-encapsulation/growth step
Linker precursors8 mg HHTP ligands per HHTP growth step
Solvents10 mL DMF + 0.6 mL H2O dispersion; 10 mL DMF HHTP solution; 10 mL DMF Cu(Ac)2 solution; methanol and DMF washing
AdditivesExogenous Cu2+ from Cu(Ac)2.H2O used to encapsulate ends and extend growth.
Atmospherenot specified; dissolved oxygen participates in initial in situ etching
Temperature120 C oil bath
Time10 min sonication; 5 min room-temperature stirring; 10 min at 120 C for HHTP step; 10 min at 120 C for Cu(Ac)2 step; repeated n cycles
Substrate orientationCu2O cube template
Oxidant / reductantDissolved oxygen oxidises etched Cu+ to Cu2+ in initial formation; Cu(Ac)2 supplies exogenous Cu2+.
Work-upCentrifuged and washed with methanol and DMF several times after each stated sequence.
ActivationNo separate final drying condition reported for Cu2O@CuHHTP powder before sensor fabrication.
Scalability contextLayer thickness controlled by growth-cycle number n; 12, 23, and 42 nm for n = 1, 3, and 5.
Show 6 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCu2O cubes10 mgp003 / 1312 · Experimental Section
Metal SourceCu(Ac)2.H2O12 mg · in 10 mL DMFp003 / 1312 · Experimental Section
LinkerHHTP ligands8 mg · in 10 mL DMFp003 / 1312 · Experimental Section
SolventDMF10 mL dispersion + 10 mL linker solution + 10 mL Cu solutionp003 / 1312 · Experimental Section
SolventH2O0.6 mLp003 / 1312 · Experimental Section
Solventmethanolwashing solventp003 / 1312 · Experimental Section
Complete recipeSource: Main

Route 5: Other

p003 / 1312 · Experimental Section

Metal precursors12 mg Cu(Ac)2.H2O, plus 12 mg Cu(Ac)2.H2O in post-treatment
Linker precursors13 mg HHTP ligands
Solvents5 mL DMF + 1 mL DI water metal solution; 5 mL DMF linker solution; 10 mL DMF post-treatment; DI water and DMF washing
Additivesnone specified
Atmospherenot specified
Temperature120 C oil bath; 80 C drying
Time5 min stirring; 2 h at 120 C; 10 min Cu(Ac)2 post-treatment at 120 C; 12 h drying
Substrate orientationnone
Oxidant / reductantnone specified
Work-upWashed with DI water and DMF for several times after synthesis and post-treatment.
ActivationDried at 80 C for 12 h in vacuum.
Scalability contextSmall-batch MOF powder synthesis at milligram scale.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCu(Ac)2.H2O12 mg + 12 mgp003 / 1312 · Experimental Section
LinkerHHTP ligands13 mgp003 / 1312 · Experimental Section
SolventDMF5 mL + 5 mL + 10 mLp003 / 1312 · Experimental Section
SolventDI water1 mL and washing solventp003 / 1312 · Experimental Section
Complete recipeSource: Main

Route 6: Drop Cast

p003 / 1312 · Sensor Fabrication and Measurement

Metal precursorsCu2O@CuHHTP-n powder, 5 mg
Linker precursorsalready incorporated in CuHHTP shell
Solvents50 uL ethanol
Additivesnone specified
Atmospherevacuum drying
Temperature80 C drying
Time8 h drying
Substrate orientationinterdigital electrode, 1 cm x 1.2 cm
Oxidant / reductantnone
Work-upUniform suspension dropped on electrode.
ActivationDried at 80 C for 8 h in vacuum.
Scalability contextSimple drop-casting route for chemiresistive electrode fabrication.
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
OtherCu2O@CuHHTP-n powder5 mgp003 / 1312 · Sensor Fabrication and Measurement
Solventethanol50 uLp003 / 1312 · Sensor Fabrication and Measurement