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2 protocols using nmc622

1

SEM Analysis of Lithium-Ion Battery Electrodes

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The electrodes
used for SEM analysis were prepared with the LiNi0.6Co0.2Mn0.2O2 (NMC622, BASF), C65 carbon
black (Imerys), and PVDF binder (Solvay) in the weight ratio of 96:2:2.
A dual-beam Xe+ ion plasma focused ion beam (Thermo Scientific
Helios G4 PFIB CXe DualBeam) was used for electrode cross-sectioning
and imaging. A platinum protection layer was deposited on the top
of the electrode surface to reduce the curtaining effect. Secondary
electron images of both as-cast and calendered electrodes were taken
at 10 kV (1.6 nA) by an Everhart–Thornley detector.
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2

Synthesis of Lithium-Ion Battery Materials

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p-Toluenesulfonyl
chloride (97%), p-toluenesulfonyl amide (97%), lithium
hydroxide monohydrate, potassium permanganate, calcium chloride, N-methyl-2-pyrrolidone (NMP, anhydrous, 99.8%), pyridine
(anhydrous, 99.8%), lithium aluminum hydride (95%), tetrahydrofuran
(THF, anhydrous, 99.8%), lithium bis(trimethylsilyl) amide solution
(1 M in THF), tributyl phosphate (≥99%), and titanium(IV) isopropoxide
(97%) were purchased from Sigma-Aldrich. Aluminum nitrate (Al(NO3)3 × 9H2O), 3-(aminopropyl)triethoxysilane,
1-propanol, and propionic acid were acquired from Merck. 4,4-(Hexa-fluoroisopropylidene)dianiline
(98%) was obtained from TCI Europe, poly(vinylidene difluoride-co-hexafluoropropylene)
(PVdF-HFP, Kynar FLEX LBG) from Arkema, and lithium
nitrate (LiNO3 × xH2O)
from Alfa Aesar. Concentrated hydrochloric acid, methanol, dimethyl
sulfoxide (DMSO), and triphenyl phosphite were acquired from VWR.
Ethylene carbonate, propylene carbonate, and NMC622 were purchased
from BASF. Carbon black (Super C65) was obtained from Imerys Graphite
& Carbon and polyvinylidene difluoride (PVdF, Solef 5130) from
Solvay. Prior to use, calcium chloride was dried at 180 °C under
reduced pressure (10–3 mbar) for 48 h.
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