Lithium sulfide series solid electrolyte material added with lithium silicon alloy and silver bromide and preparation method thereof
A solid electrolyte, lithium-silicon alloy technology, applied in solid electrolytes, non-aqueous electrolytes, circuits, etc., to achieve the effect of improving lithium ion conductivity and high lithium ion conductivity
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Embodiment 1
[0028] 1) Mixed high energy ball milling process:
[0029] In a glove box protected by an argon atmosphere with low moisture (≤1ppm) and low oxygen content (≤1ppm), the molar ratio of lithium sulfide, phosphorus sulfide, lithium-silicon alloy powder and sulfur powder is 2.5:0.75:0.05: The proportion of 0.05 ingredients, stirring and mixing, and the zirconia balls with a diameter of 3-10mm are sealed into the ball milling tank. The mass ratio of the zirconia balls in the tank to the mixture is 2:0.7; the sealed ball milling tank Dry mixing ball milling is adopted in a planetary high-energy ball mill, and the ball milling time is 5 hours to obtain a mixture of lithium sulfur phosphorus silicon;
[0030] 2) Second high energy ball milling process:
[0031] In a glove box protected by an argon atmosphere with low moisture (≤1ppm) and low oxygen content (≤1ppm) with safe lights (such as red light), bromide equivalent to 2.5% of the mass of the above lithium sulfur phosphorus silic...
Embodiment 2
[0039] Repeat Example 1, the difference is:
[0040] In step 1), lithium sulfide, phosphorus sulfide, lithium-silicon alloy and sulfur powder are mixed in a molar ratio of 3:1:0.1:0.05, and the mass ratio of zirconia balls to the mixture is 2:1. Ball milling time is 12 hours;
[0041] In step 2), the particle size of the silver bromide powder is 250 to 300 mesh, and the addition amount of the silver bromide powder is equivalent to 3% of the mass of the lithium sulfur phosphorus silicon mixture;
[0042] In step 3), the heat treatment is carried out at 150° C., and the heat treatment time is 2 hours.
[0043] After the solid electrolyte powder prepared in this example was pressed into a standard sample, the ion conductivity of the sample in this example was measured to be 5.6×10 at a room temperature of 25° C. -4 S / cm.
Embodiment 3
[0045] Repeat Example 1, the difference is:
[0046] In step 1), lithium sulfide, phosphorus sulfide, lithium-silicon alloy and sulfur powder are mixed in a molar ratio of 3:0.75:0.15:0.1, and the mass ratio of zirconia balls to the mixture is 2:0.5. Ball milling time is 8 hours;
[0047] In step 2), the particle size of the silver bromide powder is 250 mesh, and the addition of the silver bromide powder is equivalent to 5% of the mass of the lithium sulfur phosphorus silicon mixture;
[0048] In step 3), heat treatment at 160° C. for 1 hour under vacuum condition after sealing;
[0049] After the solid electrolyte powder prepared in this example was pressed into a standard sample, the ion conductivity of the sample in this example was measured at 25°C at room temperature by using the CHI660 electrochemical workstation by AC impedance method to be 6.2×10 -4 S / cm.
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