cMOF Evidence Base

Synthesis evidence

In-situ Growth of Ultrathin ZIF-67 Nanosheets on Conductive Ti@TiO2/CdS Substrate for High-efficient Electrochemical Catalysis

Zhang T., Du J., Zhang H. et al. · Electrochimica Acta · 2016 · 623-629

8 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

SI text · Fabrication

Metal precursorsCdS nanoparticles and ZIF-67 precursors
Linker precursors2-methylimidazole
Substrate orientationTi nanowire substrate without annealed TiO2 shell
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
OtherTi nanowire substrateNot specifiedSI text · Fabrication
Metal SourceCdCl2Not specifiedSI text · Fabrication
Linker2-methylimidazoleNot specifiedSI text · Fabrication
Complete recipeSource: SI

Route 2: Electrochemical

SI text · Fabrication

Metal precursorsCo(NO3)2
Solventsaqueous solution
Atmospheredried in air
Substrate orientationTi@TiO2/CdS as working electrode
Oxidant / reductantelectrodeposition at -1.0 V vs SCE; electric quantity 0.1-0.2 C
Work-upwashed with distilled water several times and dried in air
Scalability contextElectrodeposition loading controlled coulometrically.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCo(NO3)20.05 MSI text · Fabrication
SolventwaterNot specifiedSI text · Fabrication
OtherTi@TiO2/CdS electrodeNot specifiedSI text · Fabrication
Complete recipeSource: SI

Route 3: Electrochemical

SI text · Fabrication

Metal precursorsCdCl2
Solventsaqueous solution, pH 2.0
AdditivesNa2S2O3 sulfur source
Temperature50
Substrate orientationTi@TiO2 nanowire substrate as working electrode
Oxidant / reductantelectrodeposition at -0.65 V vs SCE
Work-uprinsed several times with distilled water and dried naturally in the atmosphere
Scalability contextConventional three-electrode electrodeposition with Pt plate auxiliary electrode and SCE reference.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCdCl20.83 MSI text · Fabrication
OtherNa2S2O30.17 MSI text · Fabrication
SolventwaterpH 2.0SI text · Fabrication
OtherTi@TiO2 nanowire substrateNot specifiedSI text · Fabrication
Complete recipeSource: SI

Route 4: Drop Cast

SI text · Fabrication

Metal precursorspreformed ZIF-67 powder
Linker precursorspreformed ZIF-67 powder
Solventsethanol
Time0.083 ultrasonication
Substrate orientationTi@TiO2/CdS substrate
Work-updrop-cast 30 uL ink
Scalability contextInk-based control electrode fabrication.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
OtherZIF-67 powders5 mg · 5 mg/mL in ethanolSI text · Fabrication
Solventethanol1 mLSI text · Fabrication
OtherTi@TiO2/CdS substrateNot specifiedSI text · Fabrication
Complete recipeSource: SI

Route 5: Other

SI text · Fabrication

Metal precursorsCo(OH)2 layer on Ti@TiO2/CdS
Linker precursors2-methylimidazole
Solventswater; acetone workup
Atmosphereroom-temperature stirring; final oven drying
Temperatureroom temperature reaction; 80 drying
Time6 reaction (4 or 8 h variants); 0.5 acetone exchange; 24 drying
Substrate orientationTi@TiO2/CdS/Co(OH)2 substrate immersed in linker solution
Oxidant / reductantself-sacrificial conversion of Co(OH)2 precursor to ZIF-67
Work-upacetone solution for 30 min to replace residual 2-methylimidazole solution
Activationkept in an oven at 80 degC for 24 h
Scalability contextSolution conversion on preformed electrode; reaction time variants of 4, 6 and 8 h were evaluated in SI.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Linker2-methylimidazole5.5 g · 5.5 g/20 mL H2OSI text · Fabrication
SolventH2O20 mLSI text · Fabrication
SolventacetoneNot specifiedSI text · Fabrication
OtherTi@TiO2/CdS/Co(OH)2 substrateNot specifiedSI text · Fabrication
Complete recipeSource: SI

Route 6: Hydrothermal

SI text · Synthesis of the Ti@TiO2 nanowire substrates

Metal precursorsTi foil
Solvents2.5% HCl aqueous solution; deionized water cleaning
Atmosphereair annealing
Temperature190 hydrothermal; 450 annealing
Time12 hydrothermal; 10 annealing
Substrate orientationTi foil pieces 0.5 cm x 2 cm
Work-upcooled to room temperature; cleaned with deionized water; dried in air
Activationannealed in air at 450 degC for 10 h
Scalability contextBatch autoclave process in 50 mL Teflon-lined stainless steel autoclave.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceTitanium (Ti) foils (99.0%, 0.5 mm)0.5 cm x 2 cm piecesSI text · Synthesis of the Ti@TiO2 nanowire substrates
AcidHCl10 mL · 2.5%SI text · Synthesis of the Ti@TiO2 nanowire substrates
SolventacetoneNot specifiedSI text · Synthesis of the Ti@TiO2 nanowire substrates
SolventethanolNot specifiedSI text · Synthesis of the Ti@TiO2 nanowire substrates
Solventdeionized waterNot specifiedSI text · Synthesis of the Ti@TiO2 nanowire substrates
Complete recipeSource: SI

Route 7: Other

SI text · Fabrication

Metal precursorsCo(OH)2 nanosheets electrodeposited from Co(NO3)2
Linker precursors2-methylimidazole
Solventswater; acetone workup
Atmosphereroom-temperature stirring; final oven drying
Temperatureroom temperature reaction; 80 drying
Time6 reaction; 0.5 acetone exchange; 24 drying
Substrate orientationTi@TiO2 electrode
Oxidant / reductantCo(OH)2 self-sacrificial conversion
Work-upwashed, dried in air, acetone solution for 30 min
Activation80 degC for 24 h
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCo(NO3)20.05 MSI text · Fabrication
Linker2-methylimidazole5.5 g · 5.5 g/20 mL H2OSI text · Fabrication
SolventH2O20 mLSI text · Fabrication
SolventacetoneNot specifiedSI text · Fabrication
OtherTi@TiO2 electrodeNot specifiedSI text · Fabrication
Complete recipeSource: SI

Route 8: Other

SI text · Fabrication

Metal precursorsCo(NO3)2.6H2O
Linker precursors2-methylimidazole
Solventsdeionized water
Atmosphereroom-temperature vigorous stirring
Temperatureroom temperature
Time6
Work-upprecipitates centrifuged and dried
Activationdried
Scalability contextVial-scale powder synthesis.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Linker2-methylimidazole5.5 g · in 20 mL deionized waterSI text · Fabrication
Metal SourceCo(NO3)2.6H2O10 mL · 0.05 MSI text · Fabrication
Solventdeionized water20 mLSI text · Fabrication