Lithium borohydride-garnet type oxide composite solid electrolyte material, and preparation method and application thereof
A solid electrolyte, garnet-type technology, used in composite electrolytes, solid electrolytes, non-aqueous electrolytes, etc., can solve chemical stability, electrochemical stability has not been studied, poor contact between solid electrolyte and electrode interface, interface resistance Advanced problems, to achieve the effect of improving electrochemical stability and chemical stability, good application prospects, and excellent performance
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Embodiment 1
[0031] A LiBH 4 - Preparation of LLZTO composite solid electrolyte material:
[0032] Step 1: In the isolation of air (H 2 O2 4 with Li 7 La 3 Zr 1 al 2 o 12 Mix according to the mass ratio of 1:1, under the protection of high-purity (99.9999%) inert gas (argon), use a planetary wheel ball mill for high-energy ball milling treatment, set the ball-to-material ratio to 40:1, and the speed to 450 rpm. The time is 5 h, and the mixed powder is obtained.
[0033] Step 2: Put the mixed powder obtained in Step 1 into the sample cell of a Sievert-type gas-solid reaction airtight device, perform heating, melting and impregnation treatment under a 5MPa high-pressure hydrogen atmosphere, and heat it to 350 °C at a heating rate of 5 °C / min for high-temperature melting Immersion treatment for 12 h to melt LiBH 4 Full contact with LLZTO interface.
[0034] Step 3: Cool to 120°C temperature zone, and keep warm for 4 hours to fully refine the grains. Cool to room temperature at a ra...
Embodiment 2
[0036] A LiBH 4 - Preparation of LLZTO composite solid electrolyte material:
[0037] Step 1: In the isolation of air (H 2 O2 4 with Li 7 La 3 Zr 1 Ta 2 o 12Mix according to the mass ratio of 1:5, under the protection of high-purity (99.9999%) inert gas (argon), use a planetary wheel ball mill for high-energy ball milling, set the ball-to-material ratio to 30:1, and the speed to 400 rpm. The time is 3 h, and the mixed powder is obtained.
[0038] Step 2: Put the mixed powder obtained in Step 1 into the sample cell of a Sievert-type gas-solid reaction airtight device, perform heating, melting and impregnation treatment under a 1MPa high-pressure hydrogen atmosphere, and heat it to 300 °C at a heating rate of 5 °C / min for high-temperature melting Immersion treatment for 10 h to melt LiBH 4 Full contact with LLZTO interface.
[0039] Step 3: Cool to a temperature zone of 110°C, and keep warm for 4 hours to fully refine the crystal grains. Cool to room temperature at a r...
Embodiment 3
[0041] A LiBH 4 - Preparation of LLZTO composite solid electrolyte material:
[0042] Step 1: In the isolation of air (H 2 O2 4 with Li 7 La 3 Zr 1 Nb 2 o 12 Mix according to the mass ratio of 5:1, under the protection of high-purity (99.9999%) inert gas (argon), use a planetary wheel ball mill for high-energy ball milling treatment, set the ball-to-material ratio to 50:1, and rotate at 500 rpm. The time is 8 h, and the mixed powder is obtained.
[0043] Step 2: Put the mixed powder obtained in Step 1 into the sample cell of a Sievert-type gas-solid reaction closed device, perform heating, melting and impregnation treatment under a 10MPa high-pressure hydrogen atmosphere, and heat it to 400 °C at a heating rate of 5 °C / min for high-temperature melting Immersion treatment for 15 h to melt LiBH 4 Full contact with LLZTO interface.
[0044] Step 3: Cool to a temperature zone of 150°C, and keep warm for 4 hours to fully refine the crystal grains. Cool to room temperature...
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