Synthesis evidence

Facet Engineering in Ultrathin Two-Dimensional NiFe Metal-Organic Frameworks by Coordination Modulation for Enhanced Electrocatalytic Water Oxidation

Zhao H., Yu L., Zhang L. et al. · ACS Sustainable Chemistry and Engineering · 2021 · 10892-10901

11 structured synthesis routes

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

Partial recipeSource: Both

Route 1: Solvothermal

S19 · Supporting Information · Figure S17

Metal precursorsFeCl3
Linker precursors1,4-H2BDC
Solventssame as NiFe-MOF NSs
Additives2 mL 3 M NaOAc aqueous solution
Atmospherenot specified
Temperature120
Time12
Work-upsame as NiFe-MOF bulk
Activationkept in ethanol; no separate activation reported
Show 1 structured reagent record
RoleReagentAmount / concentrationSource
Metal SourceFeCl3not specified for Fe-only sampleS19 · Supporting Information · Figure S17
Partial recipeSource: Main

Route 2: Solvothermal

10893 · Experimental Section

Metal precursorsNiCl2.6H2O and 0.06 mmol FeCl3
Linker precursorssame as NiFe-MOF NSs
Solventssame as NiFe-MOF NSs
Additives2 mL 3 M NaOAc aqueous solution
Atmospherenot specified
Temperature120
Time12
Work-upsame as NiFe-MOF bulk
Activationkept in ethanol; no separate activation reported
Show 1 structured reagent record
RoleReagentAmount / concentrationSource
Metal SourceFeCl30.06 mmol10893 · Experimental Section
Partial recipeSource: Main

Route 3: Solvothermal

10893 · Experimental Section

Metal precursorsNiCl2.6H2O and 0.2 mmol FeCl3
Linker precursorssame as NiFe-MOF NSs
Solventssame as NiFe-MOF NSs
Additives2 mL 3 M NaOAc aqueous solution
Atmospherenot specified
Temperature120
Time12
Work-upsame as NiFe-MOF bulk
Activationkept in ethanol; no separate activation reported
Show 1 structured reagent record
RoleReagentAmount / concentrationSource
Metal SourceFeCl30.2 mmol10893 · Experimental Section
Complete recipeSource: Both

Route 4: Solvothermal

S17 · Supporting Information · Table S1

Metal precursorssame as NiFe-MOF NSs
Linker precursorssame as NiFe-MOF NSs
Solventssame as NiFe-MOF NSs
Additives2 mL 1 M NaOAc aqueous solution
Atmospherenot specified
Temperature120
Time12
Work-upsame as NiFe-MOF bulk
Activationkept in ethanol; no separate activation reported
Show 1 structured reagent record
RoleReagentAmount / concentrationSource
AdditiveNaOAc2 mL · 1 MS17 · Supporting Information · Table S1
Complete recipeSource: Both

Route 5: Solvothermal

S17 · Supporting Information · Table S1

Metal precursorssame as NiFe-MOF NSs
Linker precursorssame as NiFe-MOF NSs
Solventssame as NiFe-MOF NSs
Additives2 mL 2 M NaOAc aqueous solution
Atmospherenot specified
Temperature120
Time12
Work-upsame as NiFe-MOF bulk
Activationkept in ethanol; no separate activation reported
Show 1 structured reagent record
RoleReagentAmount / concentrationSource
AdditiveNaOAc2 mL · 2 MS17 · Supporting Information · Table S1
Complete recipeSource: Main

Route 6: Solvothermal

10893 · Experimental Section

Metal precursorssame as NiFe-MOF NSs
Linker precursorssame as NiFe-MOF NSs
Solventssame as NiFe-MOF NSs
Additives2 mL 4 M NaOAc aqueous solution
Atmospherenot specified
Temperature120
Time12
Work-upsame as NiFe-MOF bulk
Activationkept in ethanol; no separate activation reported
Show 1 structured reagent record
RoleReagentAmount / concentrationSource
AdditiveNaOAc2 mL · 4 M10893 · Experimental Section
Complete recipeSource: Main

Route 7: Solvothermal

10893 · Experimental Section

Metal precursors0.4 mmol NiCl2.6H2O; 0.12 mmol FeCl3
Linker precursors0.15 mmol 1,4-H2BDC
SolventsDMF/ethanol/deionised water, 1:1:1 v/v/v, 30 mL total
Additivesnone
Atmospherenot specified
Temperature120
Time12
Work-upprecipitates collected; washed with DMF and ethanol several times; kept in ethanol
Activationkept in ethanol; no separate activation reported
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Linker1,4-H2BDC0.15 mmol10893 · Experimental Section
SolventDMF, ethanol, and DI water30 mL total; 1:1:110893 · Experimental Section
Metal SourceNiCl2.6H2O0.4 mmol10893 · Experimental Section
Metal SourceFeCl30.12 mmol10893 · Experimental Section
Complete recipeSource: Both

Route 8: Solvothermal

S17 · Supporting Information · Table S1

Metal precursorssame as NiFe-MOF NSs
Linker precursorssame as NiFe-MOF NSs
Solventssame as NiFe-MOF NSs
Additives2 mL 3 M KOAc aqueous solution replacing NaOAc
Atmospherenot specified
Temperature120
Time12
Work-upsame as NiFe-MOF bulk
Activationkept in ethanol; no separate activation reported
Show 1 structured reagent record
RoleReagentAmount / concentrationSource
AdditiveKOAc2 mL · 3 MS17 · Supporting Information · Table S1
Complete recipeSource: Both

Route 9: Solvothermal

S17 · Supporting Information · Table S1

Metal precursorssame as NiFe-MOF NSs
Linker precursorssame as NiFe-MOF NSs
Solventssame as NiFe-MOF NSs
Additives2 mL 3 M NaCl aqueous solution replacing NaOAc
Atmospherenot specified
Temperature120
Time12
Work-upsame as NiFe-MOF bulk
Activationkept in ethanol; no separate activation reported
Show 1 structured reagent record
RoleReagentAmount / concentrationSource
AdditiveNaCl2 mL · 3 MS17 · Supporting Information · Table S1
Complete recipeSource: Both

Route 10: Solvothermal

10893 · Experimental Section

Metal precursors0.4 mmol NiCl2.6H2O; 0.12 mmol FeCl3
Linker precursors0.15 mmol 1,4-H2BDC
SolventsDMF/ethanol/deionised water, 1:1:1 v/v/v, 30 mL total plus 2 mL aqueous NaOAc
Additives2 mL 3 M NaOAc aqueous solution injected before reaction
Atmospherenot specified
Temperature120
Time12
Work-upsame as NiFe-MOF bulk: precipitates collected, washed with DMF and ethanol, kept in ethanol
Activationkept in ethanol; no separate activation reported
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Linker1,4-H2BDC0.15 mmol10893 · Experimental Section
Metal SourceNiCl2.6H2O0.4 mmol10893 · Experimental Section
Metal SourceFeCl30.12 mmol10893 · Experimental Section
AdditiveNaOAc aqueous solution2 mL · 3 M10893 · Experimental Section
Partial recipeSource: Both

Route 11: Solvothermal

10893 · Experimental Section

Metal precursorsNiCl2.6H2O; other samples replace or combine Ni/Co/Cu/Zn salts
Linker precursors1,4-H2BDC
Solventssame as NiFe-MOF NSs
Additives2 mL 3 M NaOAc aqueous solution
Atmospherenot specified
Temperature120
Time12
Work-upsame as NiFe-MOF bulk
Activationkept in ethanol; no separate activation reported
Show 1 structured reagent record
RoleReagentAmount / concentrationSource
Metal SourceNiCl2.6H2O / CoCl2.6H2O / CuCl2.2H2O / ZnCl2 as applicablenot specified for each non-NiFe sample10893 · Experimental Section