Molybdenum-doped lithium germanium phosphorus sulfur solid electrolyte material and preparation method thereof
A solid electrolyte and solid electrolyte technology, applied in the manufacture of electrolyte batteries, non-aqueous electrolyte batteries, circuits, etc., can solve problems such as difficulty in ensuring long-term stability and cycle performance, restrictions on the application of lithium-sulfur solid electrolytes, and poor chemical stability. Good ionic conductivity, improved interface stability, and reduced activation barrier
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[0034] A second aspect of the present invention provides a method for preparing a molybdenum-doped lithium-germanium-phosphorus-sulfur solid-state electrolyte material, comprising the following steps: 2 S, GeS 2 , MoO 3 , P 2 S 5The stoichiometric ratios were ground and mixed, and ball milled with a ball mill, followed by tableting, heating, calcining, and cooling. The surface roughness of the solid electrolyte is controlled by controlling the ball milling time and rotation speed, and then cooperates with the positive and negative electrode materials to reduce the contact resistance and at the same time improve the strength and toughness of the solid electrolyte. Preferably, the ball milling conditions include: the rotation speed can be 250rpm, 300rpm, 350rpm, 400rpm, 450rpm, 500rpm, 600rpm or any value between the aforementioned values, more preferably 500rpm. The ball milling time can be specifically 3 hours, 5 hours, 8 hours, 10 hours, 15 hours, 20 hours, 25 hours, 30 h...
Embodiment 1
[0037] A method for preparing a 5% molybdenum-doped lithium-germanium-phosphorus-sulfur solid-state electrolyte is implemented, comprising the following steps:
[0038] Step 1. Put Li 2 S, GeS 2 , MoO 3 , P 2 S 5 The mixture was ground and mixed in an argon atmosphere at a molar ratio of 4.95:0.95:0.05:1 to obtain a mixed powder.
[0039] Step 2, sealing the mixed powder in a ball-milling jar under an argon atmosphere; using a ball mill to ball-mill the mixed powder; the rotational speed of the ball mill is 300-500 rpm, and the ball-milling time is 5-30 hours;
[0040] Step 3. Compress the ball-milled mixed powder into a tablet and put it into a closed container, vacuumize and seal it;
[0041] Step 4, heating and calcining the sample encapsulated in the airtight container to 500-650° C., and performing a solid-phase reaction for 5-48 hours;
[0042] Step 5. After the reaction is finished, it is naturally cooled to room temperature to obtain a composition consisting of L...
Embodiment 2
[0044] A method for preparing a 5% molybdenum-doped lithium-germanium-phosphorus-sulfur solid-state electrolyte is implemented, comprising the following steps:
[0045] Step 1. Put Li 2 S, GeS 2 , MoO 3 , P 2 S 5 According to the molar ratio of 4.95:0.95:0.05:1, grind and mix under argon atmosphere to obtain mixed powder;
[0046] Step 2, sealing the mixed powder in a ball milling jar under an argon atmosphere; using a ball mill to mill the mixed powder; the rotational speed of the ball mill is 500 rpm, and the ball milling time is 5 hours; the water content of the argon atmosphere is less than 1 ppm, and the oxygen content is less than 1 ppm ;
[0047] Step 3. Compress the ball-milled mixed powder into a tablet and put it into an airtight container, vacuumize and package; wherein the thickness of the tablet is 1-15mm;
[0048] Step 4. Heating and calcining the sample encapsulated in the airtight container to 500°C, and performing solid-phase reaction for 48 hours;
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