Composite solid electrolyte and preparation method thereof, and solid lithium battery and preparation method thereof
A technology of solid electrolyte and solid lithium, which is applied in the manufacture of electrolyte batteries, composite electrolytes, non-aqueous electrolyte batteries, etc., can solve the problems of low decomposition voltage, small number of ion migration, poor ability to dissolve lithium salts, etc., to achieve small interface resistance, The effect of high ion transfer number and low price
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[0039] The present invention provides a method for preparing a composite solid electrolyte, including the following steps:
[0040] Dissolving at least one polymer of polycaprolactone and polycaprolactone derivatives and lithium salt in an organic solvent to obtain a first solution;
[0041] Adding garnet oxide to the first solution and mixing to obtain a second solution;
[0042] The second solution is cast and dried to obtain a composite solid electrolyte.
[0043] The above preparation method is explained in detail below.
[0044] The polycaprolactone derivatives involved are polystyrene-polycaprolactone, polyoxyethylene-polycaprolactone, polyvinylidene fluoride-polycaprolactone, polyacrylonitrile-polycaprolactone, perfluoropolyether -At least one of polycaprolactone, polymethacrylic acid-polycaprolactone, and polydimethylsiloxane-polycaprolactone.
[0045] The lithium salt is selected from lithium bistrifluoromethanesulfonimide, lithium bisfluorosulfonimide, lithium hexafluorophosph...
Example Embodiment
[0075] Example 1
[0076] A method for preparing a composite solid electrolyte includes the following steps:
[0077] S11. Dissolve 1 g of polycaprolactone (PCL) and 0.25 g of LiFSI in an acetonitrile solvent and mix them to obtain a first solution.
[0078] S12. 0.139g Li 6.4 La 3 Zr 1.4 Ta 0.6 O 12 Add to the first solution obtained in step S11 and mix well to obtain a second solution.
[0079] S13. Cast the second solution obtained in step S12 in a polytetrafluoroethylene container, and then place it in a vacuum drying oven, and dry at 80° C. for 12 hours to obtain a composite solid electrolyte.
[0080] The composite solid electrolyte obtained in Example 1 was tested for mechanical properties, AC impedance, ionic conductivity, electrochemical window, and ion migration number, where:
[0081] (1). Stress-strain curve: using conventional stress-strain measurement methods, the test results are as follows figure 1 Shown.
[0082] From figure 1 It can be seen that when the strain reaches 8...
Example Embodiment
[0091] Example 2
[0092] A method for preparing a composite solid electrolyte includes the following steps:
[0093] S21. Dissolve 1 g of polycaprolactone (PCL) and 0.5 g of LiFSI in a tetrahydrofuran solvent and mix them to obtain a first solution.
[0094] S22. 0.22g Li 5 La 3 Ta 2 O 12 Add to the first solution obtained in step S21 and mix well to obtain a second solution.
[0095] S23. Cast the second solution obtained in step S22 into a polytetrafluoroethylene board, and then place it in a vacuum drying oven, and dry at 60° C. for 15 hours to obtain a composite solid electrolyte.
[0096] According to the test method of Example 1, the composite solid electrolyte obtained in Example 2 was subjected to corresponding performance tests. After testing, at 60℃, the ionic conductivity of the composite solid electrolyte is 1.5×10 -4 S / cm, the decomposition voltage is 4.7V, and the ion migration number is 0.543.
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