Synthesis evidence

Split-cell symmetric supercapacitor performance of bimetallic MOFs yolk-shell hierarchical microstructure

Zeng J., Charyulu Devarayapalli K., Prabhakar Vattikuti S.V. et al. · Materials Letters · 2022 · 131305

3 structured synthesis routes

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

Complete recipeSource: SI

Route 1: Drop Cast

1.3 Electrochemical measurements

SolventsEthanol, 10 uL in electrode slurry; deionized water, ethanol and acetone for ultrasonic cleaning
AdditivesNafion binder, 2.5 uL
Atmospherenot reported
Temperature90
Time12 drying; 1 ultrasonic cleaning
Substrate orientationCarbon fabric discs, 12 mm diameter and 0.3 mm thickness
Work-upTwo pieces of carbon fabric were ultrasonically cleaned sequentially in DI water, ethanol and acetone for 1 h; active material/Nafion/ethanol slurry was covered on cleaned carbon cloth by drop casting
ActivationDried in an oven at 90 deg C for 12 h
Scalability contextSmall electrode discs; no scale-up data reported.
Show 6 structured reagent records
RoleReagentAmount / concentrationSource
Otheras-synthesized Ni-Zn MOF active material2.5 mg1.3 Electrochemical measurements
AdditiveNafion2.5 uL1.3 Electrochemical measurements
Solventethanol10 uL in slurry; also used for cleaning1.3 Electrochemical measurements
Solventdeionized waterused for ultrasonic cleaning1.3 Electrochemical measurements
Solventacetoneused for ultrasonic cleaning1.3 Electrochemical measurements
Othercarbon fabric/carbon clothtwo discs, 12 mm diameter, 0.3 mm thickness1.3 Electrochemical measurements
Complete recipeSource: Both

Route 2: Solvothermal

1-2 · 2.1 Synthesis of Ni-Zn MOF

Metal precursorsNickel(II) nitrate hexahydrate and zinc nitrate hexahydrate, 34.8 mg each
Linker precursorsBenzene-1,3,5-tricarboxylic acid (BTC, trimesic acid), 513 mg
SolventsDeionized water, DMF and ethanol in equal proportions, 70 mL each, total 210 mL
Atmospherenot reported
Temperature170; post-treatment 100
Time6; post-treatment 10
Work-upSolution A poured dropwise into solution B while stirring; mixture transferred to a Teflon autoclave; precipitate centrifuged at 9000 rpm and washed several times with deionized water and ethanol
ActivationMaintained/dried at 100 deg C for 10 h; atmosphere not reported
Scalability contextNo yield or scale-up data reported.
Show 6 structured reagent records
RoleReagentAmount / concentrationSource
LinkerBenzene-1,3,5-tricarboxylic acid (BTC); SI: Trimesic acid (C9H6O6), ALDRICH513 mg dissolved in 130 mL of prepared solution1-2 · 2.1 Synthesis of Ni-Zn MOF
Metal Sourcenickel (II) nitrate hexahydrate; SI: Ni(NO3)2.6H2O, DAEJUNG34.8 mg1-2 · 2.1 Synthesis of Ni-Zn MOF
Metal Sourcezinc nitrate hexahydrate; SI: Zn(NO3)2.6H2O, DAEJUNG34.8 mg1-2 · 2.1 Synthesis of Ni-Zn MOF
Solventdeionized water; SI: DI water, Samchun, Korea70 mL in 210 mL prepared solution; also used for washing1-2 · 2.1 Synthesis of Ni-Zn MOF
Solventdimethylformamide (DMF), ALFA AESAR70 mL in 210 mL prepared solution1-2 · 2.1 Synthesis of Ni-Zn MOF
Solventethanol, DAEJUNG70 mL in 210 mL prepared solution; also used for washing1-2 · 2.1 Synthesis of Ni-Zn MOF
Complete recipeSource: SI

Route 3: Other

1.3 Electrochemical measurements; 1.4 Preparation of PVA/KOH gel electrolyte

SolventsDeionized water for PVA/KOH electrolyte preparation
AdditivesPVA/KOH gel electrolyte; filter paper separator
Atmospherenot reported
Temperature90 for PVA dissolution; cooled to room temperature
Time1 h PVA dissolution; device test assembly time not reported
Substrate orientationTwo identical 12 mm Ni-Zn MOF/carbon-fabric electrodes in a split-cell symmetric configuration
Work-upPVA dissolved in 24 mL DI water at 90 deg C with vigorous stirring; KOH liquefied in 6 mL DI water and dropped into PVA solution until gel formed; two identical electrodes separated with filter paper
ActivationPVA/KOH gel cooled to room temperature before use
Scalability contextNo scale-up data reported for gel electrolyte or split-cell device.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
ElectrolytePVA/KOH gel electrolyte6.0 M PVA/KOH stated for GCD electrolyte1.3 Electrochemical measurements; 1.4 Preparation of PVA/KOH gel electrolyte
Additivepolyvinylalcohol (PVA)3 g dissolved in 24 mL deionized water1.3 Electrochemical measurements; 1.4 Preparation of PVA/KOH gel electrolyte
Electrolytepotassium hydroxide (KOH)3 g liquefied in 6 mL deionized water1.3 Electrochemical measurements; 1.4 Preparation of PVA/KOH gel electrolyte
Solventdeionized water24 mL for PVA plus 6 mL for KOH1.3 Electrochemical measurements; 1.4 Preparation of PVA/KOH gel electrolyte
Otherfilter paper separatorone separator between two 12 mm electrodes1.3 Electrochemical measurements; 1.4 Preparation of PVA/KOH gel electrolyte