Synthesis evidence

A Monocrystalline Coordination Polymer with Multiple Redox Centers as a High-Performance Cathode for Lithium-Ion Batteries

Luo Y., Liu J., Zhang L. · Angewandte Chemie - International Edition · 2022 · e202209458

4 structured synthesis routes

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

Complete recipeSource: Both

Route 1: Other

3 · Synthesis of copper(II) chloranilate of CuCA

Metal precursorscopper nitrate trihydrate (Cu(NO3)2.3H2O)
Linker precursorspotassium chloranilate (K2CA)
Solventsdeionized water
Atmospherenot specified, ambient implied
Temperatureambient reaction; drying at 60 C then 150 C
Time10 h reaction; 10 h drying at 60 C; 10 h drying at 150 C
Oxidant / reductantcoordination coprecipitation; no external oxidant/reductant
Work-upCollect dark green CuCA precipitate by centrifugation; wash three times with deionized water to remove excess Cu(NO3)2.
ActivationDried at 60 C for 10 h and then 150 C for 10 h in a vacuum oven.
Scalability contextRoom-temperature, water-based coprecipitation; no yield reported.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Linkerpotassium chloranilate (K2CA)0.0016 mol (0.4563 g)3 · Synthesis of copper(II) chloranilate of CuCA
Metal SourceCu(NO3)2.3H2O0.002 mol (0.4832 g)3 · Synthesis of copper(II) chloranilate of CuCA
Solventdeionized water30 mL for K2CA; 10 mL for Cu(NO3)2.3H2O3 · Synthesis of copper(II) chloranilate of CuCA
Complete recipeSource: SI

Route 2: Drop Cast

3 · Electrochemical Measurements

SolventsH2O
AdditivesKetjenblack ECP-600JD, CMC binder
Atmospherevacuum drying; electrodes stored in Ar glove box
Temperature120 C drying
Time10 h drying
Substrate orientationAl foil current collector; electrode discs 10 mm diameter
Work-upBlend 60 wt% active material, 30 wt% KB and 10 wt% CMC with water; cast on Al foil; dry; cut to discs.
ActivationStored in Ar glove box with H2O and O2 below 0.1 ppm.
Scalability contextStandard slurry-cast composite electrode fabrication.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Otheractive material (CuCA, K2CA, or CA)60 wt%3 · Electrochemical Measurements
AdditiveKetjenblack ECP-600JD (KB)30 wt%3 · Electrochemical Measurements
Additivecarboxymethyl cellulose sodium (CMC)10 wt%3 · Electrochemical Measurements
SolventH2ONot specified3 · Electrochemical Measurements
Complete recipeSource: SI

Route 3: Drop Cast

3 · Synthesis of PPC-PEO-LiTFSI-Al2O3 Composite Solid-State Electrolyte Film

Metal precursorsAl2O3 additive
Solvents10 mL acetonitrile
AdditivesPPC, PEO, LiTFSI, Al2O3, cellulose nonwoven membrane
Atmospheresealed bottle during 50 C stirring; air-dry oven then vacuum oven; stored in glove box
Temperature50 C mixing; 60 C air drying; 60 C vacuum drying
Time10 h mixing; 1 h air drying; 12 h vacuum drying
Substrate orientation6 cm x 8 cm cellulose nonwoven membrane in PTFE salver
Work-upPoured onto cellulose nonwoven membrane; dried; cut into 16 mm discs.
ActivationStored in glove box before use.
Scalability contextSolution-casting recipe reports masses and membrane size.
Show 6 structured reagent records
RoleReagentAmount / concentrationSource
Otherpolypropylene carbonate (PPC)0.25 g3 · Synthesis of PPC-PEO-LiTFSI-Al2O3 Composite Solid-State Electrolyte Film
Otherpolyethylene oxide (PEO)0.25 g3 · Synthesis of PPC-PEO-LiTFSI-Al2O3 Composite Solid-State Electrolyte Film
ElectrolyteLiTFSI0.15 g3 · Synthesis of PPC-PEO-LiTFSI-Al2O3 Composite Solid-State Electrolyte Film
AdditiveAl2O30.065 g3 · Synthesis of PPC-PEO-LiTFSI-Al2O3 Composite Solid-State Electrolyte Film
Solventacetonitrile10 mL3 · Synthesis of PPC-PEO-LiTFSI-Al2O3 Composite Solid-State Electrolyte Film
Othercellulose nonwoven membrane6 cm x 8 cm3 · Synthesis of PPC-PEO-LiTFSI-Al2O3 Composite Solid-State Electrolyte Film
Complete recipeSource: SI

Route 4: Other

3 · Synthesis of copper(II) chloranilate of CuCA

Metal precursorspotassium hydroxide (KOH)
Linker precursorschloranilic acid (CA)
Solvents10 mL deionized water + 20 mL ethanol for CA; 5 mL deionized water for KOH; 100 mL ethanol for precipitation
AdditivesKOH base
Atmosphereambient condition
Temperatureambient; drying at 60 C then 150 C
Time10 h reaction; 10 h drying at 60 C; 10 h drying at 150 C
Oxidant / reductantacid-base neutralisation
Work-upAdd 100 mL ethanol; collect precipitate by centrifugation; wash three times with ethanol to remove excess KOH.
ActivationDried at 60 C for 10 h and then 150 C for 10 h in a vacuum oven.
Scalability contextRoom-temperature precipitation from common solvents; no yield reported.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Linkerchloranilic acid (CA)0.004 mol (0.8359 g)3 · Synthesis of copper(II) chloranilate of CuCA
Basepotassium hydroxide (KOH)0.0096 mol (0.5386 g)3 · Synthesis of copper(II) chloranilate of CuCA
Solventdeionized water10 mL for CA; 5 mL for KOH3 · Synthesis of copper(II) chloranilate of CuCA
Solventethanol20 mL for CA; 100 mL precipitation; wash solvent3 · Synthesis of copper(II) chloranilate of CuCA