A kind of nano oxide/lithium borohydride high conductivity solid electrolyte material and preparation method thereof
A solid electrolyte and nano-oxide technology, applied in solid electrolytes, alumina/aluminum hydroxide, non-aqueous electrolytes, etc., can solve the problem of ionic conductivity decreasing by orders of magnitude, and achieve phase transition inhibition and high ionic conductivity. Effect
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Embodiment 1
[0044] Nano-oxide / lithium borohydride amides high conductivity of the solid electrolyte material, the solid electrolyte of the formula LiBH 4 · 0.5NH 3 -Al 2 O 3 Alla 2 O 3 Of nanoscale powders, and added in an amount of 60% (mass fraction).
[0045] The method of preparing the solid electrolyte material, comprising the steps of:
[0046] Step 1: under vacuum, taking 0.6g aluminum oxide dried at 350 deg.] C 24h, aluminum oxide obtained after drying, stored into the glove box.
[0047] Take 0.1926g lithium borohydride, 0.1058g of lithium hydroxide, 0.1015g lithium amide and 0.6g of aluminum oxide in the raw material 1g were manually mixed and ground in a glove box 5min, transferred to a 50mL stainless steel ball mill jar was added a stainless steel ball feed ratio 20: 1, taken after sealing; stainless steel ball mill jar placed in a planetary ball mill, a ball mill under argon protection, the rotational speed at 300 rpm, milling 30min, 5min each ball suspended 2min, ⅰ obtain a po...
Embodiment 2～7
[0056] The difference is that Example 1 only with different amounts of aluminum oxide, specifically shown in Table 1 below.
[0057] Table 1 Example of different aluminum oxide added in an amount of 2 to 7 (wt%)
[0058]
[0059] Examples 1 to 7 was added different concentrations of aluminum oxide powder Ⅱ, differential scanning calorimetry and the temperature profile - see ionic conductivity are respectively attached diagram Image 6 with 7 .
[0060] From Image 6 It can be observed when no added aluminum oxide, LiBH4 4 · 0.5NH 3 The exothermic peak and the endothermic peak of the material is very obvious, and with the content of the nano-oxide (aluminum oxide) is increased, the endothermic peak and exothermic peak intensity is gradually decreased, when the oxide content of 75%, has no significant exotherm suction phenomenon, a phase change was completely inhibited.
[0061] From Figure 7 Can be observed, when the added aluminum oxide content of 45%, the material obtained at 30 ...
Embodiment 8
[0063] The difference is that in Example 1, Step 1, 1g of raw materials comprising lithium borohydride 0.1744g, 0.1918 hydroxide, lithium hydroxide, 0.1838g lithium amide and 0.45g aluminum oxide, thus obtained powder is lithium borohydride Ⅰ · 1 ammonia / 45% alumina, the powder obtained after heat treatment ⅱLiBH 4 · NH 3 -45% Al 2 O3 .
[0064] The chemical reaction between the material in Example 8 was:
[0065] Libh 4 + LiOH + LINH 2 + Al 2 O 3 → Libh 4 · NH 3 + Li 2 O + Al 2 O 3
[0066] The temperature-ion conductivity relationship of powder II obtained in Example 8 is attached Figure 8 Indicated.
[0067] From Figure 8 It can be observed in Libh. 4 · NH 3 -45% Al 2 O 3 When the material is 40 ° C below the phase change temperature, its ionic conductivity has reached 1.87 × 10 -3 S · cm -1 .
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