cMOF Evidence Base

Synthesis evidence

Electrochemical Transformation of Metal Organic Framework into Ultrathin Metal Hydroxide-(oxy)hydroxide Nanosheets for Alkaline Water Oxidation

Singh B., Prakash O., Maiti P. et al. · ACS Applied Nano Materials · 2020 · 6693-6701

10 structured synthesis routes

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

Complete recipeSource: Both

Route 1: Electrochemical

S-3 · Table S1 · Table S1

Metal precursorsCoFe-PBA@CC
Linker precursorsPBA cyanide ligands removed during transformation
Solvents1.0 M aqueous KOH electrolyte
Atmospheresingle-compartment three-electrode electrochemical cell
Time12
Substrate orientationultrathin nanosheets@CC working electrode
Oxidant / reductantanodic oxidation at 1.45 V vs RHE
Activationchronoamperometric treatment
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
OtherCoFe-PBA@CCNot specifiedS-3 · Table S1 · Table S1
Electrolyteaqueous KOH1.0 MS-3 · Table S1 · Table S1
Complete recipeSource: Both

Route 2: Electrochemical

6694 · 2.3 · Table S1

Metal precursorsCoFe-PBA@CC
Linker precursorsPBA cyanide ligands removed during transformation
Solvents1.0 M aqueous KOH electrolyte
Atmospheresingle-compartment three-electrode electrochemical cell
Time12
Substrate orientationultrathin nanosheets@CC working electrode
Oxidant / reductantanodic oxidation at 1.55 V vs RHE
Activationchronoamperometric treatment
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
OtherCoFe-PBA@CCNot specified6694 · 2.3 · Table S1
Electrolyteaqueous KOH1.0 M6694 · 2.3 · Table S1
Complete recipeSource: Both

Route 3: Electrochemical

S-3 · Table S1 · Table S1

Metal precursorsCoFe-PBA@CC
Linker precursorsPBA cyanide ligands removed during transformation
Solvents1.0 M aqueous KOH electrolyte
Atmospheresingle-compartment three-electrode electrochemical cell
Time12
Substrate orientationultrathin nanosheets@CC working electrode
Oxidant / reductantanodic oxidation at 1.65 V vs RHE
Activationchronoamperometric treatment
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
OtherCoFe-PBA@CCNot specifiedS-3 · Table S1 · Table S1
Electrolyteaqueous KOH1.0 MS-3 · Table S1 · Table S1
Complete recipeSource: Both

Route 4: Electrochemical

S-3 · Table S1 · Table S1

Metal precursorsCoFe-PBA@CC
Linker precursorsPBA cyanide ligands removed during transformation
Solvents1.0 M aqueous KOH electrolyte
Atmospheresingle-compartment three-electrode electrochemical cell
Time24
Substrate orientationultrathin nanosheets@CC working electrode
Oxidant / reductantanodic oxidation at 1.55 V vs RHE
Activationchronoamperometric treatment
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
OtherCoFe-PBA@CCNot specifiedS-3 · Table S1 · Table S1
Electrolyteaqueous KOH1.0 MS-3 · Table S1 · Table S1
Complete recipeSource: Main

Route 5: Hydrothermal

6694 · 2.4

Metal precursorsCoCl2.6H2O (1 mmol); FeCl2 (1 mmol)
Solventswater (12 mL)
AdditivesNH4F (4 mmol); NH2CONH2 (10 mmol)
Atmosphereair oven drying
Temperature120 °C; 50 °C drying
Time5 h hydrothermal; 12 h drying
Substrate orientationcarbon cloth support
Work-upwashed with water followed by ethanol
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCoCl2.6H2O1 mmol6694 · 2.4
Metal SourceFeCl21 mmol6694 · 2.4
AdditiveNH4F4 mmol6694 · 2.4
AdditiveNH2CONH210 mmol6694 · 2.4
Solventwater12 mL6694 · 2.4
Complete recipeSource: Main

Route 6: Other

6694 · 2.2

Metal precursorsCoHC@CC template; K3[Fe(CN)6] (0.2 mmol)
Linker precursorshexacyanoferrate/cyanide from K3[Fe(CN)6]
Solventswater (5 mL)
Atmospheresealed glass vial, air oven
Temperatureroom temperature; 60 °C; 50 °C drying
Time1 h room temperature; 6 h at 60 °C; overnight drying
Substrate orientationCoHC@CC pieces placed in K3[Fe(CN)6] solution
Work-upwashed with water four times; dried at 50 °C overnight
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
OtherCoHC@CCpieces6694 · 2.2
LinkerK3[Fe(CN)6]0.2 mmol6694 · 2.2
Solventwater5 mL6694 · 2.2
Complete recipeSource: Main

Route 7: Hydrothermal

6694 · 2.1

Metal precursorsCoCl2.6H2O (2 mmol)
Solventswater (12 mL); double-distilled water and acetone washing
AdditivesNH4F (4 mmol); NH2CONH2 (10 mmol); concentrated nitric acid pretreatment
Atmosphereair oven drying
Temperature100 °C acid treatment; 120 °C hydrothermal; 50 °C drying
Time4 h acid treatment; 5 h hydrothermal; overnight/12 h drying
Substrate orientationcarbon cloth pieces immersed vertically with only 1 cm2 inside solution
Work-upwashed with water followed by ethanol
Activationcarbon cloth treated with concentrated nitric acid at 100 °C for 4 h
Scalability contextSelf-supported on 1 cm2 carbon cloth active area.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCoCl2.6H2O2 mmol6694 · 2.1
AdditiveNH4F4 mmol6694 · 2.1
AdditiveNH2CONH210 mmol6694 · 2.1
Solventwater12 mL6694 · 2.1
Acidconcentrated nitric acidNot specified6694 · 2.1
Complete recipeSource: SI

Route 8: Electrochemical

S-3 · 3.3

Metal precursorsNiFe-PBA@CC
Linker precursorsPBA cyanide ligands removed during transformation
Solvents1.0 M aqueous KOH electrolyte
Atmospheresingle-compartment three-electrode electrochemical cell
Time12
Substrate orientationultrathin nanosheets@CC working electrode
Oxidant / reductantanodic oxidation at 1.55 V vs RHE
Activationchronoamperometric treatment
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
OtherNiFe-PBA@CCNot specifiedS-3 · 3.3
Electrolyteaqueous KOH1.0 MS-3 · 3.3
Complete recipeSource: SI

Route 9: Other

S-2-S-3 · 3.2

Metal precursorsNiHC@CC template; K3[Fe(CN)6] (0.2 mmol)
Linker precursorshexacyanoferrate/cyanide from K3[Fe(CN)6]
Solventswater (5 mL)
Atmospheresealed glass vial, air oven
Temperatureroom temperature; 60 °C; 50 °C drying
Time1 h room temperature; 6 h at 60 °C; overnight drying
Substrate orientationNiHC@CC pieces placed in K3[Fe(CN)6] solution
Work-upwashed with water four times; dried at 50 °C overnight
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
OtherNiHC@CCpiecesS-2-S-3 · 3.2
LinkerK3[Fe(CN)6]0.2 mmolS-2-S-3 · 3.2
Solventwater5 mLS-2-S-3 · 3.2
Complete recipeSource: SI

Route 10: Hydrothermal

S-2 · 3.1

Metal precursorsNiCl2.6H2O (2 mmol)
Solventswater (12 mL)
AdditivesNH4F (4 mmol); NH2CONH2 (10 mmol)
Atmosphereair oven drying
Temperature120 °C; 50 °C drying
Time5 h hydrothermal; 12 h drying
Substrate orientationcarbon cloth immersed vertically with only 1 cm2 inside solution
Work-upwashed with water followed by ethanol
Scalability contextSelf-supported on 1 cm2 carbon cloth active area.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceNiCl2.6H2O2 mmolS-2 · 3.1
AdditiveNH4F4 mmolS-2 · 3.1
AdditiveNH2CONH210 mmolS-2 · 3.1
Solventwater12 mLS-2 · 3.1