Reaktion #678078

ord-5fe7e0eac7a841c08b4a6b9759d5875a

Reaktionsgleichung

S=P12SP3(=S)SP(=S)(S1)SP(=S)(S2)S3
P2S5
S=P12SP3(=S)SP(=S)(S1)SP(=S)(S2)S3
phosphorus pentasulfide
[Li][S][Li]
Li2S
[Li][O][Li]
Li2O
[Li+].[Li+].[S-2]
lithium sulfide
S=P12SP3(=S)SP(=S)(S1)SP(=S)(S2)S3.[Li][O][Li].[Li][S][Li]
Li2S Li2O P2S5

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.ADDITIONwas introduced
  2. 2
    Sonstigethe pot was completely sealed
  3. 3
    SonstigeWith the pot mounted on a planetary type ball mill machine (P7™ produced by Fritsch Japan Co., Ltd.)
  4. 4
    Sonstigeprocess and 15 minutes
  5. 5
    SonstigeThereafter, the obtained specimen was dried on a hot plate
  6. 6
    Sonstigeset at 100° C.
  7. 7
    Sonstigefor removing the heptane so as

Vorschrift

As the starting materials, lithium sulfide (Li2S) and phosphorus pentasulfide (P2S5) were used. Powders thereof were measured to have a molar ratio of Li2S:P2S5=75:25 so as to be mixed in an agate mortar. Then, 2 g of the mixture was introduced into a 45 ml of zirconia pot, 4 g of dehydrated heptane (moisture content 30 ppm or less) was introduced, and furthermore, a zirconia ball (φ5.5 mm, 53 g) was introduced, and then the pot was completely sealed. With the pot mounted on a planetary type ball mill machine (P7™ produced by Fritsch Japan Co., Ltd.), a mechanical milling operation was carried out for 20 times with a 500 rpm base plate rotational frequency by a one hour process and 15 minutes pause cycle. Furthermore, after adding 6 mol % of Li2O, the mechanical milling was carried out in the same conditions as mentioned above. Thereafter, the obtained specimen was dried on a hot plate set at 100° C. for removing the heptane so as to obtain a sulfide solid electrolyte material (sulfide glass, Li2S—Li2O—P2S5).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US09236158B2uspto-grants-2016_01