Li-la-ti-o composite solid electrolyte material containing silicon and synthesizing method thereof

Li-la-ti-o composite solid electrolyte material containing silicon and synthesizing method thereof

  • CN 101,971,408 A
  • Filed: 07/24/2009
  • Published: 02/09/2011
  • Est. Priority Date: 07/25/2008
  • Status: Active Application
First Claim
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1. Claim1st, a kind of siliceous Li-La-Ti oxygen composite solid electrolyte material, it is characterised in that chemical formula be Li3xLa2/3_xTi03The intercrystalline crystal boundary of lithium lanthanum titanium oxide in there are amorphous Si or Si compounds, wherein 0<

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    16.2nd, siliceous Li-La-Ti oxygen composite solid electrolyte material as claimed in claim 1, wherein Si the or Si compounds are 0.27% ~ 1.35% relative to the mass ratio of lithium lanthanum titanium oxide based on Si.3rd, siliceous Li-La-Ti oxygen composite solid electrolyte material as claimed in claim 1 or 2, wherein the Si compounds include Si02And/or the Si compounds containing Li ions.4th, the siliceous Li-La-Ti oxygen composite solid electrolyte material as described in claim 1,2 or 3, wherein Si the or Si compounds are present in the form of noncrystalline nanometer silicon-rich layer.5th, a kind of preparation method of siliceous Li-La-Ti oxygen composite solid electrolyte material, wherein, add Li in Si precursor solutions3xLa2/3_xTi03, after being thermally dried, make Li3xLa2/3_xTi03Powdered is sintered again, wherein 0<

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    16.6. the preparation method of Li-La-Ti oxygen composite solid electrolyte material as claimed in claim 5, wherein, the Si precursor solutions as 0.27% ~ 1.35% amount are equipped with using the mass ratio relative to lithium lanthanum titanium oxide based on Si.7. the preparation method of the Li-La-Ti oxygen composite solid electrolyte material as described in claim 5 or 6, wherein the sintering temperature being sintered is 1100 ~ 1400 °

    C.8. the preparation method of Li-La-Ti oxygen composite solid electrolyte material as claimed in claim 7, wherein described sintering temperature is 1200 ~ 1400 °

    C.9. the preparation method of the Li-La-Ti oxygen composite solid electrolyte material as described in any one in claim 5 ~ 8, wherein the sintering time being sintered is 1 ~ 10 hour.10. the preparation method of Li-La-Ti oxygen composite solid electrolyte material as claimed in claim 9, wherein described sintering time is 2 ~ 10 hours.11. the preparation method of Li-La-Ti oxygen composite solid electrolyte material as claimed in claim 10, wherein described sintering time is 2 ~ 8 hours.12nd, the siliceous Li-La-Ti oxygen composite solid electrolyte material as described in claim 5 or 6Preparation method, wherein the preparation method is carried out in accordance with the following steps:

    (1) preparation of LLTO raw materials powder:

    Li is prepared using solid phase method or sol-gal process3xLa2/3_xTi03, raw material powder is distributed in ethanol to obtain turbid solution a stand-by;

    (2) preparation of catalyst:

    Water, ethanol, ammoniacal liquor are prepared into mixed solution b according to a certain volume;

    (3) preparation of silicon precursor solution:

    Weigh silanes and be scattered in ethanol and obtain solution c;

    (4) preparation of mixed liquor:

    After turbid solution a and mixed solution b is mixed, solution c is added drop-wise in the mixed liquor, stirred;

    (5) heating response:

    Mixed liquor after stirring is heated 1 ~ 5 hour under 50 ~ 250 °

    C;

    (6) dry:

    Composite granule is dried to obtain under 10 ~ 100 °

    C;

    (7) sinter:

    After composite granule tabletting, sintered 1 ~ 10 hour under 1100 ~ 1400 °

    C of high temperature, obtain composite solid electrolyte material.13rd, preparation method according to claim 12, wherein in the preparation process of above-mentioned silicon precursor solution, the silanes weighed are at least one of tetraethyl orthosilicate and four Yue.14th, preparation method according to claim 12, wherein the preparation process reclaimed water of the catalyst, ethanol, ammonia volume ratio 1;

    2 ;

    2~1 ;

    4 ;

    Proportioning in the range of 10 prepares mixed solution b.

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