Synthesis evidence

Temperature effect on the synthesis of two Ni-MOFs with distinct performance in supercapacitor

Deng L., Qu H., Zhang Y. et al. · Journal of Solid State Chemistry · 2020 · 121026

4 structured synthesis routes

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

Complete recipeSource: Main

Route 1: Other

2 · 2.5 Electrochemical measurements

SolventsEthanol
AdditivesCarbon black and PTFE binder
AtmosphereNot specified
Temperature70
Time12
Substrate orientationNickel foam pieces, 1 cm x 2 cm
Work-upHomogeneous paste dried at 70 deg C for 12 h; 2.5 mg coated between two nickel foam pieces; pressed under 10 MPa for 5 s
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
OtherNi-MOF-2D active material80 wt%; 2.5 mg total electrode mixture coated2 · 2.5 Electrochemical measurements
Additivecarbon black10 wt%2 · 2.5 Electrochemical measurements
AdditivePTFE10 wt%2 · 2.5 Electrochemical measurements
SolventethanolNot specified2 · 2.5 Electrochemical measurements
Complete recipeSource: Main

Route 2: Hydrothermal

2 · 2.2 Synthesis of compound 1

Metal precursorsNi(NO3)2.6H2O (29.8 mg, 0.1 mmol)
Linker precursorsH2DTA (14.9 mg, 0.05 mmol)
SolventsH2O (5 mL)
AdditivesNaOH (20 uL, 1 M)
AtmosphereSealed Teflon-lined autoclave; gas atmosphere not specified
Temperature120
Time48
Work-upSlowly cooled to room temperature; product washed three times with deionised water
ActivationDried at 50 deg C in vacuum; no separate activation reported
Scalability contextYield 56% based on metal; batch autoclave synthesis.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceNi(NO3)2.6H2O29.8 mg, 0.1 mmol2 · 2.2 Synthesis of compound 1
LinkerH2DTA14.9 mg, 0.05 mmol2 · 2.2 Synthesis of compound 1
BaseNaOH20 uL · 1 M2 · 2.2 Synthesis of compound 1
SolventH2O5 mL2 · 2.2 Synthesis of compound 1
Complete recipeSource: Main

Route 3: Other

2 · 2.5 Electrochemical measurements

SolventsEthanol
AdditivesCarbon black and PTFE binder
AtmosphereNot specified
Temperature70
Time12
Substrate orientationNickel foam pieces, 1 cm x 2 cm
Work-upHomogeneous paste dried at 70 deg C for 12 h; 2.5 mg coated between two nickel foam pieces; pressed under 10 MPa for 5 s
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
OtherNi-MOF-3D active material80 wt%; 2.5 mg total electrode mixture coated2 · 2.5 Electrochemical measurements
Additivecarbon black10 wt%2 · 2.5 Electrochemical measurements
AdditivePTFE10 wt%2 · 2.5 Electrochemical measurements
SolventethanolNot specified2 · 2.5 Electrochemical measurements
Complete recipeSource: Main

Route 4: Hydrothermal

2 · 2.3 Synthesis of compound 2

Metal precursorsNi(NO3)2.6H2O (same as compound 1)
Linker precursorsH2DTA (same as compound 1)
SolventsH2O (same as compound 1)
AdditivesNaOH (same as compound 1)
AtmosphereSealed Teflon-lined autoclave; gas atmosphere not specified
Temperature180
Time48
Work-upReported as similar to compound 1; slow cooling, water wash and vacuum drying inferred from stated same synthesis process
ActivationNo separate activation reported
Scalability contextYield 46% based on metal; batch autoclave synthesis.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceNi(NO3)2.6H2Osame as compound 1: 29.8 mg, 0.1 mmol2 · 2.3 Synthesis of compound 2
LinkerH2DTAsame as compound 1: 14.9 mg, 0.05 mmol2 · 2.3 Synthesis of compound 2
BaseNaOHsame as compound 1: 20 uL · 1 M2 · 2.3 Synthesis of compound 2
SolventH2Osame as compound 1: 5 mL2 · 2.3 Synthesis of compound 2