Preparation method of lithium borohydride-based solid electrolyte material
A solid electrolyte, lithium borohydride technology, applied in solid electrolytes, non-aqueous electrolytes, circuits, etc., can solve problems such as insufficient to meet the normal use requirements of batteries, incompatibility of electrode materials, and increase of lithium ion migration rate. Achieve excellent ionic conductivity and electrochemical stability, improve electrode compatibility, and achieve good repeatability
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[0027] The preparation method of the lithium borohydride-based solid electrolyte material of the present invention comprises the following steps:
[0028] Step 1. After mixing lithium borohydride and lithium halide according to a certain ratio, heat treatment is carried out under a non-oxidizing atmosphere, and after cooling, halogen-doped lithium borohydride is obtained;
[0029] Step 2: After mixing the halogen-doped lithium borohydride and the mesoporous material according to a certain ratio, heat, melt and impregnate in a high-pressure hydrogen atmosphere, and obtain a nano-confined halogen-doped lithium borohydride-based solid electrolyte material after cooling.
[0030] Preferably, the lithium halide includes lithium iodide, lithium bromide, lithium chloride, lithium fluoride and mixtures thereof.
[0031] Preferably, the lithium borohydride and lithium halide are mixed in a molar ratio of 1:1 to 5:1.
[0032] Preferably, the non-oxidizing atmosphere is an atmosphere of...
Embodiment 1
[0040] 0.6546 g of lithium borohydride (purity > 95%) and 1.793 g of lithium iodide (purity > 95%) were mixed in a glove box, and then mixed by ball milling under the protection of high-purity nitrogen (purity 99.99%) Then the powder after ball milling is put into airtight container, after being filled with the hydrogen of 10 MPa pressure, be heated to 260 ℃ with the rate of increase of temperature of 5 ℃ per minute, and insulation 4 hours, naturally cool to room temperature; The cooled material was taken out of the airtight container and manually ground with a mortar to obtain the electrolyte material sample.
[0041] like figure 1 As shown, the obtained lithium iodide-doped lithium borohydride material was tested by differential scanning calorimetry to determine its melting point, and the above material was mixed with SBA-15 molecular sieve at a mass fraction of 60%, and the mixed powder was put into Put it into a closed reactor, fill it with 15 MPa pressure high-pressure h...
Embodiment ２
[0046] 0.6546 g of lithium borohydride (purity > 95%) and 1.345 g of lithium iodide (purity > 95%) were mixed in a glove box, and then ball-milled under the protection of high-purity argon (99.99% pure) Mixing; then put the ball-milled powder in an airtight container, after filling with hydrogen of 15 MPa pressure, heat to 250 ° C with a heating rate of 2 ° C per minute, and keep the temperature for 4 hours, and naturally cool to room temperature; The cooled material was removed from the airtight container and ground by hand with a mortar. Then, the above materials were mixed with SBA-15 molecular sieve at mass fractions of 30%, 50%, 60%, 70% and 100%, respectively, and the mixed powder was put into a closed reactor and filled with a high pressure of 15 MPa. After hydrogen, it was heated to 350 °C at a heating rate of 2 °C per minute, and subjected to high temperature melting for 3 hours, then cooled to room temperature naturally, and the cooled sample was taken out of the rea...
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Abstract
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