Synthesis evidence

Vertical Conductive Metal–Organic Framework Single-Crystalline Nanowire Arrays for Efficient Electrocatalytic Hydrogen Evolution

Dong J., Chi K., Zhao Y. et al. · Small · 2024 · 2404808

3 structured synthesis routes

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

Partial recipeSource: Both

Route 1: Liquid Liquid Interface

Supplementary Methods 1.3 Preparation of Ag-MOF

Metal precursorsAgNO3 aqueous solution: 25.5 mg AgNO3 in 1 mL aqueous solution, injected into water using a syringe pump.
Linker precursorsbenzenehexathiol (BHT) in toluene: 0.1 mM BHT/toluene solution, 50 mL.
Solvents30 mL deionised water aqueous layer; 50 mL toluene BHT layer.
Additivesnone reported for Ag-MOF growth; substrate/device processing used piranha solution, O2 plasma, Cr/Au and SU8 photoresist.
Atmospherenot specified
Temperature50
Time1
Substrate orientationAg-MOF formed at a toluene-water liquid-liquid interface and was transferred to hydrophilic pretreated Si/SiO2 by Langmuir-Schaefer technique; device samples used Cr/Au-patterned 2 x 2 cm silicon wafers.
Oxidant / reductantnone intentionally specified for MOF growth; piranha substrate treatment used H2SO4/H2O2 before transfer/device fabrication.
Work-upAfter growth, the silicon wafer was carefully extracted with tweezers. Device fabrication used hydrophilic Si/SiO2 cleaned with DI water, ethanol and acetone; piranha solution H2SO4/H2O2 2:1 for 6 h at room temperature; ultrasonic DI water/ethanol 5 min; nitrogen purge; O2 plasma 100 W for 2 min; Cr/Au 5/30 nm thermal evaporation, SU8 coating, UV-lithography 100 x 200 um window, and 120 C vacuum oven for 5 h.
ActivationNo separate MOF activation reported; microdevices were baked in vacuum oven at 120 C for 5 h after SU8 lithography.
Scalability contextMorphology controlled by reaction time at the confined liquid-liquid interface; no yield or scale-up data reported beyond 100 mL vial, 30 mL water and 50 mL toluene solution.
Show 8 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceSilver nitrate (AgNO3, 98%, Aldrich)25.5 mg in 1 mL aqueous solutionSupplementary Methods 1.3 Preparation of Ag-MOF
Linkerbenzenehexathiol (BHT)50 mL toluene solution · 0.1 mMSupplementary Methods 1.3 Preparation of Ag-MOF
Solventdeionized water30 mL in 100 mL vialSupplementary Methods 1.3 Preparation of Ag-MOF
Solventtoluene (99.8%, Aldrich)50 mLSupplementary Methods 1.3 Preparation of Ag-MOF
AcidH2SO4 in piranha solution for substrate pretreatment2:1 H2SO4/H2O2 mixture; 6 h room temperature · 95-98% H2SO4Supplementary Methods 1.3 Preparation of Ag-MOF
OxidantH2O2 in piranha solution for substrate pretreatment2:1 H2SO4/H2O2 mixture; 6 h room temperature · 30% H2O2Supplementary Methods 1.3 Preparation of Ag-MOF
OtherSi/SiO2 wafer substrate2 x 2 cmSupplementary Methods 1.3 Preparation of Ag-MOF
OtherSU8 photoresist for microdevice patterningspin-coated; 100 x 200 um window etchedSupplementary Methods 1.3 Preparation of Ag-MOF
Partial recipeSource: Both

Route 2: Liquid Liquid Interface

Supplementary Methods 1.3 Preparation of Ag-MOF

Metal precursorsAgNO3 aqueous solution: 25.5 mg AgNO3 in 1 mL aqueous solution, injected into water using a syringe pump.
Linker precursorsbenzenehexathiol (BHT) in toluene: 0.1 mM BHT/toluene solution, 50 mL.
Solvents30 mL deionised water aqueous layer; 50 mL toluene BHT layer.
Additivesnone reported for Ag-MOF growth; substrate/device processing used piranha solution, O2 plasma, Cr/Au and SU8 photoresist.
Atmospherenot specified
Temperature50
Time3
Substrate orientationAg-MOF formed at a toluene-water liquid-liquid interface and was transferred to hydrophilic pretreated Si/SiO2 by Langmuir-Schaefer technique; device samples used Cr/Au-patterned 2 x 2 cm silicon wafers.
Oxidant / reductantnone intentionally specified for MOF growth; piranha substrate treatment used H2SO4/H2O2 before transfer/device fabrication.
Work-upAfter growth, the silicon wafer was carefully extracted with tweezers. Device fabrication used hydrophilic Si/SiO2 cleaned with DI water, ethanol and acetone; piranha solution H2SO4/H2O2 2:1 for 6 h at room temperature; ultrasonic DI water/ethanol 5 min; nitrogen purge; O2 plasma 100 W for 2 min; Cr/Au 5/30 nm thermal evaporation, SU8 coating, UV-lithography 100 x 200 um window, and 120 C vacuum oven for 5 h.
ActivationNo separate MOF activation reported; microdevices were baked in vacuum oven at 120 C for 5 h after SU8 lithography.
Scalability contextMorphology controlled by reaction time at the confined liquid-liquid interface; no yield or scale-up data reported beyond 100 mL vial, 30 mL water and 50 mL toluene solution.
Show 8 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceSilver nitrate (AgNO3, 98%, Aldrich)25.5 mg in 1 mL aqueous solutionSupplementary Methods 1.3 Preparation of Ag-MOF
Linkerbenzenehexathiol (BHT)50 mL toluene solution · 0.1 mMSupplementary Methods 1.3 Preparation of Ag-MOF
Solventdeionized water30 mL in 100 mL vialSupplementary Methods 1.3 Preparation of Ag-MOF
Solventtoluene (99.8%, Aldrich)50 mLSupplementary Methods 1.3 Preparation of Ag-MOF
AcidH2SO4 in piranha solution for substrate pretreatment2:1 H2SO4/H2O2 mixture; 6 h room temperature · 95-98% H2SO4Supplementary Methods 1.3 Preparation of Ag-MOF
OxidantH2O2 in piranha solution for substrate pretreatment2:1 H2SO4/H2O2 mixture; 6 h room temperature · 30% H2O2Supplementary Methods 1.3 Preparation of Ag-MOF
OtherSi/SiO2 wafer substrate2 x 2 cmSupplementary Methods 1.3 Preparation of Ag-MOF
OtherSU8 photoresist for microdevice patterningspin-coated; 100 x 200 um window etchedSupplementary Methods 1.3 Preparation of Ag-MOF
Partial recipeSource: Both

Route 3: Liquid Liquid Interface

Supplementary Methods 1.3 Preparation of Ag-MOF

Metal precursorsAgNO3 aqueous solution: 25.5 mg AgNO3 in 1 mL aqueous solution, injected into water using a syringe pump.
Linker precursorsbenzenehexathiol (BHT) in toluene: 0.1 mM BHT/toluene solution, 50 mL.
Solvents30 mL deionised water aqueous layer; 50 mL toluene BHT layer.
Additivesnone reported for Ag-MOF growth; substrate/device processing used piranha solution, O2 plasma, Cr/Au and SU8 photoresist.
Atmospherenot specified
Temperature50
Time12
Substrate orientationAg-MOF formed at a toluene-water liquid-liquid interface and was transferred to hydrophilic pretreated Si/SiO2 by Langmuir-Schaefer technique; device samples used Cr/Au-patterned 2 x 2 cm silicon wafers.
Oxidant / reductantnone intentionally specified for MOF growth; piranha substrate treatment used H2SO4/H2O2 before transfer/device fabrication.
Work-upAfter growth, the silicon wafer was carefully extracted with tweezers. Device fabrication used hydrophilic Si/SiO2 cleaned with DI water, ethanol and acetone; piranha solution H2SO4/H2O2 2:1 for 6 h at room temperature; ultrasonic DI water/ethanol 5 min; nitrogen purge; O2 plasma 100 W for 2 min; Cr/Au 5/30 nm thermal evaporation, SU8 coating, UV-lithography 100 x 200 um window, and 120 C vacuum oven for 5 h.
ActivationNo separate MOF activation reported; microdevices were baked in vacuum oven at 120 C for 5 h after SU8 lithography.
Scalability contextMorphology controlled by reaction time at the confined liquid-liquid interface; no yield or scale-up data reported beyond 100 mL vial, 30 mL water and 50 mL toluene solution.
Show 8 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceSilver nitrate (AgNO3, 98%, Aldrich)25.5 mg in 1 mL aqueous solutionSupplementary Methods 1.3 Preparation of Ag-MOF
Linkerbenzenehexathiol (BHT)50 mL toluene solution · 0.1 mMSupplementary Methods 1.3 Preparation of Ag-MOF
Solventdeionized water30 mL in 100 mL vialSupplementary Methods 1.3 Preparation of Ag-MOF
Solventtoluene (99.8%, Aldrich)50 mLSupplementary Methods 1.3 Preparation of Ag-MOF
AcidH2SO4 in piranha solution for substrate pretreatment2:1 H2SO4/H2O2 mixture; 6 h room temperature · 95-98% H2SO4Supplementary Methods 1.3 Preparation of Ag-MOF
OxidantH2O2 in piranha solution for substrate pretreatment2:1 H2SO4/H2O2 mixture; 6 h room temperature · 30% H2O2Supplementary Methods 1.3 Preparation of Ag-MOF
OtherSi/SiO2 wafer substrate2 x 2 cmSupplementary Methods 1.3 Preparation of Ag-MOF
OtherSU8 photoresist for microdevice patterningspin-coated; 100 x 200 um window etchedSupplementary Methods 1.3 Preparation of Ag-MOF