Synthesis evidence

Mixed-metallic MOF based electrode materials for high performance hybrid supercapacitors

Jiao Y., Pei J., Chen D. et al. · Journal of Materials Chemistry A · 2017 · 1094-1102

9 structured synthesis routes

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

Partial recipeSource: Main

Route 1: Other

p002 / 1095 · 2.3 Electrochemical measurements

Solvents3 M KOH aqueous electrolyte
Atmosphereroom temperature; atmosphere not specified
Work-upTwo-electrode cell assembled using Co/Ni-MOF positive electrode and CNTs-COOH negative electrode; masses balanced using charge-balance equation.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
OtherCo/Ni-MOF electrodepositive electrode; mass balancedp002 / 1095 · 2.3 Electrochemical measurements
OtherCNTs-COOH electrodenegative electrode; mass balancedp002 / 1095 · 2.3 Electrochemical measurements
ElectrolyteKOH aqueous solution3 Mp002 / 1095 · 2.3 Electrochemical measurements
Complete recipeSource: Main

Route 2: Drop Cast

p002 / 1095 · 2.3 Electrochemical measurements

SolventsN-methyl-2-pyrrolidinone
Additivescarbon black; PVDF binder
Atmospherevacuum drying
Temperature120
Time12
Substrate orientationnickel foam current collector, 1 cm x 1 cm
Work-upSlurry coated onto nickel foam, vacuum dried at 120 C for 12 h, then pressed at 6 MPa.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
OtherCo/Ni-MOF80 wt% of electrode solidsp002 / 1095 · 2.3 Electrochemical measurements
Additivecarbon black10 wt% of electrode solidsp002 / 1095 · 2.3 Electrochemical measurements
AdditivePVDF10 wt% of electrode solidsp002 / 1095 · 2.3 Electrochemical measurements
SolventN-methyl 2-pyrrolidinonenot reportedp002 / 1095 · 2.3 Electrochemical measurements
Complete recipeSource: Main

Route 3: Hydrothermal

p002 / 1095 · 2.1 Synthesis

Metal precursorsCo(NO3)2.6H2O (0.35 g); NiCl2 (0.52 g)
Linker precursorsH2BDC (0.168 g)
SolventsDMF (25.6 mL); alcohol wash; methanol solvent exchange
Atmospherenot specified
Temperature120
Time16
Work-upCentrifuged at 10000 rpm for 3 min; washed several times with DMF and alcohol; solvent exchanged with methanol four times over two days.
ActivationVacuum activation at 100 C for 12 h.
Scalability contextBatch hydrothermal synthesis in 50 mL Teflon-lined autoclave.
Show 6 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCo(NO3)2.6H2O0.35 gp002 / 1095 · 2.1 Synthesis
Metal SourceNiCl20.52 gp002 / 1095 · 2.1 Synthesis
LinkerH2BDC0.168 gp002 / 1095 · 2.1 Synthesis
SolventDMF25.6 mLp002 / 1095 · 2.1 Synthesis
Solventmethanolsolvent exchange four times over two daysp002 / 1095 · 2.1 Synthesis
Solventalcoholwash solventp002 / 1095 · 2.1 Synthesis
Partial recipeSource: Main

Route 4: Other

p002 / 1095 · 2.3 Electrochemical measurements

Solvents3 M KOH aqueous electrolyte
Atmosphereroom temperature; atmosphere not specified
Work-upTwo-electrode cell assembled using Ni-MOF positive electrode and CNTs-COOH negative electrode; masses balanced using charge-balance equation.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
OtherNi-MOF electrodepositive electrode; mass balancedp002 / 1095 · 2.3 Electrochemical measurements
OtherCNTs-COOH electrodenegative electrode; mass balancedp002 / 1095 · 2.3 Electrochemical measurements
ElectrolyteKOH aqueous solution3 Mp002 / 1095 · 2.3 Electrochemical measurements
Vague recipeSource: Main

Route 5: Unknown

p001 / 1094 · Introduction

Metal precursorsnot reported in this paper
Linker precursorsnot reported in this paper
Solventsnot reported in this paper
Complete recipeSource: Main

Route 6: Drop Cast

p002 / 1095 · 2.3 Electrochemical measurements

SolventsN-methyl-2-pyrrolidinone
Additivescarbon black; PVDF binder
Atmospherevacuum drying
Temperature120
Time12
Substrate orientationnickel foam current collector, 1 cm x 1 cm
Work-upSlurry coated onto nickel foam, vacuum dried at 120 C for 12 h, then pressed at 6 MPa.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
OtherNi-MOF80 wt% of electrode solidsp002 / 1095 · 2.3 Electrochemical measurements
Additivecarbon black10 wt% of electrode solidsp002 / 1095 · 2.3 Electrochemical measurements
AdditivePVDF10 wt% of electrode solidsp002 / 1095 · 2.3 Electrochemical measurements
SolventN-methyl 2-pyrrolidinonenot reportedp002 / 1095 · 2.3 Electrochemical measurements
Complete recipeSource: Main

Route 7: Drop Cast

p002 / 1095 · 2.3 Electrochemical measurements

SolventsN-methyl-2-pyrrolidinone
Additivescarbon black; PVDF binder
Atmospherevacuum drying
Temperature120
Time12
Substrate orientationnickel foam current collector, 1 cm x 1 cm
Work-upSlurry coated onto nickel foam, vacuum dried at 120 C for 12 h, then pressed at 6 MPa.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
OtherZn/Ni-MOF80 wt% of electrode solidsp002 / 1095 · 2.3 Electrochemical measurements
Additivecarbon black10 wt% of electrode solidsp002 / 1095 · 2.3 Electrochemical measurements
AdditivePVDF10 wt% of electrode solidsp002 / 1095 · 2.3 Electrochemical measurements
SolventN-methyl 2-pyrrolidinonenot reportedp002 / 1095 · 2.3 Electrochemical measurements
Partial recipeSource: Main

Route 8: Hydrothermal

p002 / 1095 · 2.1 Synthesis

Metal precursorsNiCl2 (0.52 g); Zn(NO3)2.6H2O inferred by sample name, but text wording is internally reversed
Linker precursorsH2BDC (0.168 g)
SolventsDMF (25.6 mL); alcohol wash; methanol solvent exchange
Atmospherenot specified
Temperature120
Time16
Work-upSame centrifugation, DMF/alcohol washing, and methanol exchange as Co/Ni-MOF route.
ActivationVacuum activation at 100 C for 12 h.
Scalability contextBatch hydrothermal synthesis in 50 mL Teflon-lined autoclave.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceZn(NO3)2.6H2Onot reliably reported; likely analogous to Co salt amountp002 / 1095 · 2.1 Synthesis
Metal SourceNiCl20.52 g (from analogous procedure)p002 / 1095 · 2.1 Synthesis
LinkerH2BDC0.168 g (from analogous procedure)p002 / 1095 · 2.1 Synthesis
SolventDMF25.6 mL (from analogous procedure)p002 / 1095 · 2.1 Synthesis
Partial recipeSource: Main

Route 9: Other

p002 / 1095 · 2.3 Electrochemical measurements

Solvents3 M KOH aqueous electrolyte
Atmosphereroom temperature; atmosphere not specified
Work-upTwo-electrode cell assembled using Zn/Ni-MOF positive electrode and CNTs-COOH negative electrode; masses balanced using charge-balance equation.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
OtherZn/Ni-MOF electrodepositive electrode; mass balancedp002 / 1095 · 2.3 Electrochemical measurements
OtherCNTs-COOH electrodenegative electrode; mass balancedp002 / 1095 · 2.3 Electrochemical measurements
ElectrolyteKOH aqueous solution3 Mp002 / 1095 · 2.3 Electrochemical measurements