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3 protocols using lithium sulfide

1

Synthesis of Li-S Battery Components

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Methyl-2-pyrrolidone (NMP, 99.5 wt%), polyvinylidene fluoride (PVDF, 99.5 wt%), elemental sulfur (99.5 wt%), lithium sulfide (Li2S, 99.98 wt%), 1,3-dioxolane (DOL, 99.8 wt%), 1,2-dimethoxyethane (DME, 99.5 wt%), tetraglyme (99 wt%), lithium bis (trifluoromethanesulfonyl) imide (LiTFSI, 99.95 wt%), lithium nitrate (LiNO3, 99.99 wt%), cobalt chloride hexahydrate (CoCl2·6H2O), potassium permanganate (KMnO4, 99.5 wt%), graphite powder, ammonium tetrathiomolybdate ((NH4)2MoS4, 99.95 wt%), reduced graphene oxide (rGO, chemically reduced) were purchased from Sigma-Aldrich. Graphene oxide (GO, >99 wt%) was purchased from Aladdin reagent. Hydrochloric acid (HCl, 37 wt%), sodium nitrate (NaNO3, 99 wt%), hydrogen peroxide (H2O2, 30 wt%) were purchased from Chuandong Reagent. Super P carbon (99.5 wt%) from Timcal were used as received. The carbon paper (HCP120, thickness 0.21 mm) was purchased from Shanghai HESEN Co., Ltd.
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2

Lithium Polysulfide Electrolyte Preparation

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The preparation of lithium polysulfide electrolyte blends followed
a procedure previously reported within the group.22 (link) In an argon-filled glovebox, lithium sulfide (99.98%, Sigma-Aldrich)
and sulfur (S8, 100 mesh, sublimed, Sigma-Aldrich, dried
at room temperature under vacuum over 72 h) were added into a vial
in ratios to give the desired Li2S6 composition,
followed by adding the electrolyte solution 1 M LiTFSI in DOL/DME
(1:1 by vol). The solution was stirred at 60 °C for 10 days to
ensure full dissolution. After 10 days of stirring, a clear ruby-red
polysulfide solution is obtained with an average chain length of Li2S6.
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3

Synthesis of Lithium Sulfur Batteries

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All chemicals were used as received. Cobalt nitrate hexahydrate (Co(NO3)2·6H2O, 99.99%), thiourea (H2NCSNH2, 99%), sodium dodecyl sulfate (CH3(CH2)11OSO3Na, 99%), sodium hydrosulfide hydrate (NaHS·xH2O, NaHS ≥ 60%), sodium hydroxide (NaOH, 98%), 1,3-dioxolane (DOL, 99.8 wt%), 1,2-dimethoxyethane (DME, 99.5 wt%), lithium bis(trifluoromethanesulfonyl) imide (LiTFSI, 99.95 wt%), lithium nitrate (LiNO3, 99.99%), lithium sulfide (Li2S, 99.98%) and sulfur (S, flakes, 99.99%) were purchased from Sigma-Aldrich. Ultrapure water (UPW) filtered by a Millipore Milli-Q Integral Water Purification System (Millipore Corp.) was used as the common solvent.
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