cMOF Evidence Base

Synthesis evidence

Morphology Control of Mixed Metallic Organic Framework for High-Performance Hybrid Supercapacitors

Mohanty A., Kang K.-N., Saravanakumar B. et al. · Small · 2024 · 2308771

12 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

main p.9 · Experimental Section

Metal precursorsNiCoO2@Ni electrode supplies Ni/Co core; no additional metal salt reported for MOF growth.
Linker precursors0.210 mmol benzoic acid
SolventsDMF, DI water and ethanol; volumes not reported
AtmosphereNot specified during solvothermal growth; dried in oven.
Temperature110 C solvothermal; 85 C drying
Time1.667 h solvothermal; 12 h drying
Substrate orientationNiCoO2@Ni electrode in Teflon-lined stainless-steel autoclave
Work-upNatural cooling; washed several times using ethanol.
ActivationKept in oven at 85 C for 12 h.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Linkerbenzoic acid0.210 mmolmain p.9 · Experimental Section
SolventDMFNot specifiedmain p.9 · Experimental Section
SolventDI waterNot specifiedmain p.9 · Experimental Section
SolventethanolNot specifiedmain p.9 · Experimental Section
Partial recipeSource: Both

Route 2: Solvothermal

main p.9 · Experimental Section · Figures S2-S4

Metal precursorsNiCoO2@Ni electrode supplies Ni/Co core; no additional metal salt reported for MOF growth.
Linker precursors0.210 mmol benzoic acid
SolventsDMF, DI water and ethanol; volumes not reported
AtmosphereNot specified during solvothermal growth; dried in oven.
Temperature110 C solvothermal; 85 C drying
Time1.0 h solvothermal; 12 h drying
Substrate orientationNiCoO2@Ni electrode in Teflon-lined stainless-steel autoclave
Work-upNatural cooling; washed several times using ethanol.
ActivationKept in oven at 85 C for 12 h.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Linkerbenzoic acid0.210 mmolmain p.9 · Experimental Section · Figures S2-S4
SolventDMFNot specifiedmain p.9 · Experimental Section · Figures S2-S4
SolventDI waterNot specifiedmain p.9 · Experimental Section · Figures S2-S4
SolventethanolNot specifiedmain p.9 · Experimental Section · Figures S2-S4
Partial recipeSource: Both

Route 3: Solvothermal

main p.9 · Experimental Section

Metal precursorsNiCoO2@Ni electrode supplies Ni/Co core; no additional metal salt reported for MOF growth.
Linker precursors0.210 mmol benzoic acid
SolventsDMF, DI water and ethanol; volumes not reported
AtmosphereNot specified during solvothermal growth; dried in oven.
Temperature110 C solvothermal; 85 C drying
Time1.333 h solvothermal; 12 h drying
Substrate orientationNiCoO2@Ni electrode in Teflon-lined stainless-steel autoclave
Work-upNatural cooling; washed several times using ethanol.
ActivationKept in oven at 85 C for 12 h.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Linkerbenzoic acid0.210 mmolmain p.9 · Experimental Section
SolventDMFNot specifiedmain p.9 · Experimental Section
SolventDI waterNot specifiedmain p.9 · Experimental Section
SolventethanolNot specifiedmain p.9 · Experimental Section
Partial recipeSource: Both

Route 4: Solvothermal

main p.9 · Experimental Section

Metal precursorsNiCoO2@Ni electrode supplies Ni/Co core; no additional metal salt reported for MOF growth.
Linker precursors0.210 mmol terephthalic acid / H2BDC
SolventsDMF, DI water and ethanol; volumes not reported
AtmosphereNot specified during solvothermal growth; dried in oven.
Temperature110 C solvothermal; 85 C drying
Time1.667 h solvothermal; 12 h drying
Substrate orientationNiCoO2@Ni electrode in Teflon-lined stainless-steel autoclave
Work-upNatural cooling; washed several times using ethanol.
ActivationKept in oven at 85 C for 12 h.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Linkerterephthalic acid / H2BDC0.210 mmolmain p.9 · Experimental Section
SolventDMFNot specifiedmain p.9 · Experimental Section
SolventDI waterNot specifiedmain p.9 · Experimental Section
SolventethanolNot specifiedmain p.9 · Experimental Section
Partial recipeSource: Both

Route 5: Solvothermal

main p.9 · Experimental Section

Metal precursorsNiCoO2@Ni electrode supplies Ni/Co core; no additional metal salt reported for MOF growth.
Linker precursors0.210 mmol terephthalic acid / H2BDC
SolventsDMF, DI water and ethanol; volumes not reported
AtmosphereNot specified during solvothermal growth; dried in oven.
Temperature110 C solvothermal; 85 C drying
Time1.0 h solvothermal; 12 h drying
Substrate orientationNiCoO2@Ni electrode in Teflon-lined stainless-steel autoclave
Work-upNatural cooling; washed several times using ethanol.
ActivationKept in oven at 85 C for 12 h.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Linkerterephthalic acid / H2BDC0.210 mmolmain p.9 · Experimental Section
SolventDMFNot specifiedmain p.9 · Experimental Section
SolventDI waterNot specifiedmain p.9 · Experimental Section
SolventethanolNot specifiedmain p.9 · Experimental Section
Partial recipeSource: Both

Route 6: Solvothermal

main p.9 · Experimental Section

Metal precursorsNiCoO2@Ni electrode supplies Ni/Co core; no additional metal salt reported for MOF growth.
Linker precursors0.210 mmol terephthalic acid / H2BDC
SolventsDMF, DI water and ethanol; volumes not reported
AtmosphereNot specified during solvothermal growth; dried in oven.
Temperature110 C solvothermal; 85 C drying
Time1.333 h solvothermal; 12 h drying
Substrate orientationNiCoO2@Ni electrode in Teflon-lined stainless-steel autoclave
Work-upNatural cooling; washed several times using ethanol.
ActivationKept in oven at 85 C for 12 h.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Linkerterephthalic acid / H2BDC0.210 mmolmain p.9 · Experimental Section
SolventDMFNot specifiedmain p.9 · Experimental Section
SolventDI waterNot specifiedmain p.9 · Experimental Section
SolventethanolNot specifiedmain p.9 · Experimental Section
Partial recipeSource: Both

Route 7: Solvothermal

main p.9 · Experimental Section

Metal precursorsNiCoO2@Ni electrode supplies Ni/Co core; no additional metal salt reported for MOF growth.
Linker precursors0.210 mmol trimesic acid / H3BTC
SolventsDMF, DI water and ethanol; volumes not reported
AtmosphereNot specified during solvothermal growth; dried in oven.
Temperature110 C solvothermal; 85 C drying
Time1.667 h solvothermal; 12 h drying
Substrate orientationNiCoO2@Ni electrode in Teflon-lined stainless-steel autoclave
Work-upNatural cooling; washed several times using ethanol.
ActivationKept in oven at 85 C for 12 h.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Linkertrimesic acid / H3BTC0.210 mmolmain p.9 · Experimental Section
SolventDMFNot specifiedmain p.9 · Experimental Section
SolventDI waterNot specifiedmain p.9 · Experimental Section
SolventethanolNot specifiedmain p.9 · Experimental Section
Partial recipeSource: Both

Route 8: Solvothermal

main p.9 · Experimental Section

Metal precursorsNiCoO2@Ni electrode supplies Ni/Co core; no additional metal salt reported for MOF growth.
Linker precursors0.210 mmol trimesic acid / H3BTC
SolventsDMF, DI water and ethanol; volumes not reported
AtmosphereNot specified during solvothermal growth; dried in oven.
Temperature110 C solvothermal; 85 C drying
Time1.0 h solvothermal; 12 h drying
Substrate orientationNiCoO2@Ni electrode in Teflon-lined stainless-steel autoclave
Work-upNatural cooling; washed several times using ethanol.
ActivationKept in oven at 85 C for 12 h.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Linkertrimesic acid / H3BTC0.210 mmolmain p.9 · Experimental Section
SolventDMFNot specifiedmain p.9 · Experimental Section
SolventDI waterNot specifiedmain p.9 · Experimental Section
SolventethanolNot specifiedmain p.9 · Experimental Section
Partial recipeSource: Both

Route 9: Solvothermal

main p.9 · Experimental Section

Metal precursorsNiCoO2@Ni electrode supplies Ni/Co core; no additional metal salt reported for MOF growth.
Linker precursors0.210 mmol trimesic acid / H3BTC
SolventsDMF, DI water and ethanol; volumes not reported
AtmosphereNot specified during solvothermal growth; dried in oven.
Temperature110 C solvothermal; 85 C drying
Time1.333 h solvothermal; 12 h drying
Substrate orientationNiCoO2@Ni electrode in Teflon-lined stainless-steel autoclave
Work-upNatural cooling; washed several times using ethanol.
ActivationKept in oven at 85 C for 12 h.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Linkertrimesic acid / H3BTC0.210 mmolmain p.9 · Experimental Section
SolventDMFNot specifiedmain p.9 · Experimental Section
SolventDI waterNot specifiedmain p.9 · Experimental Section
SolventethanolNot specifiedmain p.9 · Experimental Section
Partial recipeSource: Main

Route 10: Other

main p.9 · Experimental Section

Metal precursorsNiCo-MOF@NiCoO2@Ni positive electrode; 3D NiCu-C@Fe4N/Cu negative electrode
Linker precursorsH2BDC in positive electrode
Solvents2 M KOH electrolyte
AdditivesCellulose separator
Temperatureroom temperature assumed
Substrate orientationTwo electrodes sandwiched with cellulose separator in split test cell; total active area 2 cm2
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
ElectrolyteKOH2 Mmain p.9 · Experimental Section
Othercellulose separatorNot specifiedmain p.9 · Experimental Section
Partial recipeSource: Main

Route 11: Electrochemical

main p.9 · Experimental Section

Metal precursors0.05 M CuSO4(H2O)5; 0.5 M NiSO4(H2O)6; FeCl3 for Fe4N formation
Linker precursorsnone
SolventsElectrolyte containing HCl/H2SO4; TEG for carbonisation step
Additives2.5 M HCl; 1.5 M H2SO4; 85 uL 0.35 M NaOH; 0.25 mg melamine
AtmosphereAnnealing atmosphere not specified
Temperature180 C TEG/NaOH treatment; 550 C anneal
Time60 s electrodeposition; 12 h TEG/NaOH; 1 h anneal
Substrate orientationCu foil negative electrode, Pt wire positive electrode, 1 cm separation
Oxidant / reductantChronopotentiometric deposition at 2 A cm-2
Work-up3D NiCu/Cu washed several times with DI water.
ActivationAnnealed with 1 mg FeCl3 and 0.25 mg melamine at 550 C for 1 h, ramp 10 C min-1.
Show 8 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCuSO4(H2O)50.05 Mmain p.9 · Experimental Section
Metal SourceNiSO4(H2O)60.5 Mmain p.9 · Experimental Section
AcidHCl2.5 Mmain p.9 · Experimental Section
AcidH2SO41.5 Mmain p.9 · Experimental Section
Solventtriethylene glycol (TEG)20 mLmain p.9 · Experimental Section
BaseNaOH85 uL · 0.35 Mmain p.9 · Experimental Section
Metal SourceFeCl31 mgmain p.9 · Experimental Section
Othermelamine0.25 mgmain p.9 · Experimental Section
Complete recipeSource: Main

Route 12: Hydrothermal

main p.9 · Experimental Section

Metal precursors2 mmol Ni(NO3)2.6H2O; 2 mmol Co(NO3)2.6H2O
Linker precursorsnone
Solvents36 mL DI water
Additives8 mmol NH4F; 10 mmol NH2CONH2
AtmosphereAnnealing under argon
Temperature120 C hydrothermal; 350 C anneal
Time10 h hydrothermal; 1 h anneal
Substrate orientationNi foil current collector; orientation not specified
Oxidant / reductantUrea hydrolysis supplies OH-; NH4F surfactant.
Work-upNatural cooling; washed many times with DI water.
ActivationAnnealed at 350 C under Ar for 1 h, ramp 5 C min-1.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceNi(NO3)2.6H2O2 mmolmain p.9 · Experimental Section
Metal SourceCo(NO3)2.6H2O2 mmolmain p.9 · Experimental Section
AdditiveNH4F8 mmolmain p.9 · Experimental Section
BaseNH2CONH2 / urea10 mmolmain p.9 · Experimental Section
SolventDI water36 mLmain p.9 · Experimental Section