cMOF Evidence Base

Synthesis evidence

One-Step Solvothermal Synthesis of Raspberry-like NiCo-MOF for High-Performance Flexible Supercapacitors for a Wide Operation Temperature Range

Zhang W., Shahnavaz Z., Yan X. et al. · Inorganic Chemistry · 2022 · 15287-15301

7 structured synthesis routes

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

Partial recipeSource: Main

Route 1: Solvothermal

15289 / p003 · 2.2 Preparation of the NiCo-MOF Electrode

Metal precursorsCo(NO3)2.6H2O, 0.437 g in analogous single-metal preparation
Linker precursorsH3BTC, inferred from common route
SolventsDMF, 60 mL; washing with DMF and anhydrous ethanol
Atmosphereair/not specified
Temperature120
Time15
Work-upCool naturally; centrifuge at 10000 rpm/min for 3 min; wash three times with DMF and anhydrous ethanol.
ActivationDry at 60 deg C for 24 h.
Scalability contextAuthors state metal nitrates were extracted from scrap metals in a factory, but no extraction process is detailed.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCo(NO3)2.6H2O0.437 g15289 / p003 · 2.2 Preparation of the NiCo-MOF Electrode
LinkerH3BTCnot separately specified for Co-MOF; common route uses 0.315 g15289 / p003 · 2.2 Preparation of the NiCo-MOF Electrode
SolventDMF60 mL inferred from common route15289 / p003 · 2.2 Preparation of the NiCo-MOF Electrode
Solventanhydrous ethanolwash15289 / p003 · 2.2 Preparation of the NiCo-MOF Electrode
Partial recipeSource: Main

Route 2: Other

15290 / p004 · 2.5 Construction and Electrochemical Testing of the FASC

Metal precursorsNiCo-MOF-3 positive electrode and ultrathin MnO2 negative electrode
SolventsNMP for electrode slurry; DI water for gel electrolyte
AdditivesAcetylene black, PVDF, PVA, KOH, K3[Fe(CN)6], glycerin
Atmosphereair/not specified
Temperature70 for electrode drying; 85 for gel electrolyte preparation
Timeovernight for positive-electrode drying
Substrate orientationNi foam, 1 cm x 1 cm
Oxidant / reductantK3[Fe(CN)6] redox additive
Work-upSpread NiCo-MOF-3 slurry on Ni foam and dry at 70 deg C overnight; prepare PVA/KOH gel in water bath; assemble positive electrode, negative electrode, and gel electrolyte.
Show 10 structured reagent records
RoleReagentAmount / concentrationSource
OtherNiCo-MOF-380 wt% of positive-electrode mixture15290 / p004 · 2.5 Construction and Electrochemical Testing of the FASC
Additiveacetylene black10 wt% of positive-electrode mixture15290 / p004 · 2.5 Construction and Electrochemical Testing of the FASC
AdditivePVDF10 wt% of positive-electrode mixture15290 / p004 · 2.5 Construction and Electrochemical Testing of the FASC
SolventNMPpure NMP solvent15290 / p004 · 2.5 Construction and Electrochemical Testing of the FASC
OtherMnO2negative-electrode active material; mass loading calculated as 1.11 mg/cm215290 / p004 · 2.5 Construction and Electrochemical Testing of the FASC
ElectrolytePVA3.0 g15290 / p004 · 2.5 Construction and Electrochemical Testing of the FASC
ElectrolyteKOH1.68 g15290 / p004 · 2.5 Construction and Electrochemical Testing of the FASC
SolventDI water30 mL15290 / p004 · 2.5 Construction and Electrochemical Testing of the FASC
AdditiveK3[Fe(CN)6]0.5 g15290 / p004 · 2.5 Construction and Electrochemical Testing of the FASC
Additiveglycerin3.0 mL15290 / p004 · 2.5 Construction and Electrochemical Testing of the FASC
Partial recipeSource: Main

Route 3: Solvothermal

15289 / p003 · 2.2 Preparation of the NiCo-MOF Electrode

Metal precursorsNi(NO3)2.6H2O, 0.872 g in analogous single-metal preparation
Linker precursorsH3BTC, inferred from common route
SolventsDMF, 60 mL; washing with DMF and anhydrous ethanol
Atmosphereair/not specified
Temperature120
Time15
Work-upCool naturally; centrifuge at 10000 rpm/min for 3 min; wash three times with DMF and anhydrous ethanol.
ActivationDry at 60 deg C for 24 h.
Scalability contextAuthors state metal nitrates were extracted from scrap metals in a factory, but no extraction process is detailed.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceNi(NO3)2.6H2O0.872 g15289 / p003 · 2.2 Preparation of the NiCo-MOF Electrode
LinkerH3BTCnot separately specified for Ni-MOF; common route uses 0.315 g15289 / p003 · 2.2 Preparation of the NiCo-MOF Electrode
SolventDMF60 mL inferred from common route15289 / p003 · 2.2 Preparation of the NiCo-MOF Electrode
Solventanhydrous ethanolwash15289 / p003 · 2.2 Preparation of the NiCo-MOF Electrode
Partial recipeSource: Main

Route 4: Solvothermal

15289 / p003 · 2.2 Preparation of the NiCo-MOF Electrode · Figure 2c

Metal precursorsNi(NO3)2.6H2O and Co(NO3)2.6H2O; Ni:Co = 1:1
Linker precursorsH3BTC
SolventsDMF, 60 mL; washing with DMF and anhydrous ethanol
Atmosphereair/not specified
Temperature120
Time15
Work-upCool naturally; centrifuge at 10000 rpm/min for 3 min; wash three times with DMF and anhydrous ethanol.
ActivationDry at 60 deg C for 24 h.
Scalability contextAuthors state metal nitrates were extracted from scrap metals in a factory, but no extraction process is detailed.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceNi(NO3)2.6H2O1.5 mmol from Figure 2c15289 / p003 · 2.2 Preparation of the NiCo-MOF Electrode · Figure 2c
Metal SourceCo(NO3)2.6H2O1.5 mmol from Figure 2c15289 / p003 · 2.2 Preparation of the NiCo-MOF Electrode · Figure 2c
LinkerH3BTC0.315 g inferred common route15289 / p003 · 2.2 Preparation of the NiCo-MOF Electrode · Figure 2c
SolventDMF60 mL15289 / p003 · 2.2 Preparation of the NiCo-MOF Electrode · Figure 2c
Partial recipeSource: Main

Route 5: Solvothermal

15289 / p003 · 2.2 Preparation of the NiCo-MOF Electrode · Figure 2c

Metal precursorsNi(NO3)2.6H2O and Co(NO3)2.6H2O; Ni:Co = 1:2
Linker precursorsH3BTC
SolventsDMF, 60 mL; washing with DMF and anhydrous ethanol
Atmosphereair/not specified
Temperature120
Time15
Work-upCool naturally; centrifuge at 10000 rpm/min for 3 min; wash three times with DMF and anhydrous ethanol.
ActivationDry at 60 deg C for 24 h.
Scalability contextAuthors state metal nitrates were extracted from scrap metals in a factory, but no extraction process is detailed.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceNi(NO3)2.6H2O1.5 mmol from Figure 2c15289 / p003 · 2.2 Preparation of the NiCo-MOF Electrode · Figure 2c
Metal SourceCo(NO3)2.6H2O3.0 mmol from Figure 2c15289 / p003 · 2.2 Preparation of the NiCo-MOF Electrode · Figure 2c
LinkerH3BTC0.315 g inferred common route15289 / p003 · 2.2 Preparation of the NiCo-MOF Electrode · Figure 2c
SolventDMF60 mL15289 / p003 · 2.2 Preparation of the NiCo-MOF Electrode · Figure 2c
Complete recipeSource: Main

Route 6: Solvothermal

15288 / p002 · 2.2 Preparation of the NiCo-MOF Electrode · Figure 1

Metal precursors0.872 g Ni(NO3)2.6H2O (3 mmol); 0.437 g Co(NO3)2.6H2O (1.5 mmol)
Linker precursors0.315 g H3BTC (1.5 mmol)
Solvents60 mL DMF; washing with DMF and anhydrous ethanol
Atmosphereair/not specified
Temperature120
Time15
Work-upDissolve under stirring at 900 rpm/min at room temperature; transfer to 100 mL reactor; heat at 5 deg C/min to 120 deg C for 15 h; cool naturally; centrifuge at 10000 rpm/min for 3 min; wash three times with DMF and ethanol.
ActivationDry at 60 deg C for 24 h.
Scalability contextAuthors state metal nitrates were extracted from scrap metals in a factory, but no extraction process is detailed.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceNi(NO3)2.6H2O0.872 g (3 mmol)15288 / p002 · 2.2 Preparation of the NiCo-MOF Electrode · Figure 1
Metal SourceCo(NO3)2.6H2O0.437 g (1.5 mmol)15288 / p002 · 2.2 Preparation of the NiCo-MOF Electrode · Figure 1
LinkerH3BTC0.315 g (1.5 mmol)15288 / p002 · 2.2 Preparation of the NiCo-MOF Electrode · Figure 1
SolventDMF60 mL15288 / p002 · 2.2 Preparation of the NiCo-MOF Electrode · Figure 1
Solventanhydrous ethanolwash15288 / p002 · 2.2 Preparation of the NiCo-MOF Electrode · Figure 1
Partial recipeSource: Main

Route 7: Solvothermal

15289 / p003 · 2.2 Preparation of the NiCo-MOF Electrode · Figure 2c

Metal precursorsNi(NO3)2.6H2O and Co(NO3)2.6H2O; Ni:Co = 4:1
Linker precursorsH3BTC
SolventsDMF, 60 mL; washing with DMF and anhydrous ethanol
Atmosphereair/not specified
Temperature120
Time15
Work-upCool naturally; centrifuge at 10000 rpm/min for 3 min; wash three times with DMF and anhydrous ethanol.
ActivationDry at 60 deg C for 24 h.
Scalability contextAuthors state metal nitrates were extracted from scrap metals in a factory, but no extraction process is detailed.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceNi(NO3)2.6H2O6.0 mmol from Figure 2c15289 / p003 · 2.2 Preparation of the NiCo-MOF Electrode · Figure 2c
Metal SourceCo(NO3)2.6H2O1.5 mmol from Figure 2c15289 / p003 · 2.2 Preparation of the NiCo-MOF Electrode · Figure 2c
LinkerH3BTC0.315 g inferred common route15289 / p003 · 2.2 Preparation of the NiCo-MOF Electrode · Figure 2c
SolventDMF60 mL15289 / p003 · 2.2 Preparation of the NiCo-MOF Electrode · Figure 2c