Phosphate lithium fast ion conductor material and preparation method thereof
A technology of conductor materials and ion conductors, applied in the field of component design and preparation of lithium fast ion conductor materials, can solve the problems of low material density, gap in ion conductivity, high room temperature conductivity, etc.
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[0086] Preparation of phosphate lithium fast ion conductor material
[0087] The invention also provides a method for preparing the material. In the prior art, the method for preparing lithium phosphate fast ion conductor materials requires that the glass formed after quenching be annealed immediately at a medium high temperature, such as 500°C. This process can easily cause the glass to crack due to stress, and finally Affect material properties.
[0088] In the present invention, the medium and high temperature annealing is not carried out immediately after the high temperature quenching to form the glass, but the complete cooling is carried out immediately, and then the glass powder is prepared, and finally the powder is pressed and annealed. This processing method can be very good To avoid the possibility of cracks in the current technology, and through subsequent cold isostatic pressing and annealing, dense and stable materials can be prepared well.
[0089] Specifically, the ...
Example Embodiment
[0120] Example 1:
[0121] Will Li 2 CO 3 : Al(OH) 3 : GeO 2 : SiO 2 : NH 4 H 2 PO 4 Follow Li 1.61 Al 0.5 Ge 1.5 Si 0.01 P 2.99 O 12.05 The stoichiometric ratio of ingredients, uniformly mixed and dried. The powder is heated to 700°C for 2h, and after cooling, it is crushed and dried under wet grinding conditions. Then heat the powder to 1400°C and keep it for 2h, then pour it into liquid nitrogen for quenching. After the product is cooled, it is crushed and dried under wet milling conditions, and the glass powder is pressed into a shape at 300 MPa. The block was first kept at 520°C for 6 hours, and then at 900°C for 6 hours, and then cooled in the furnace to obtain a glass ceramic lithium fast ion block material. After the glass ceramic block is machined, gold is used as the blocking electrode, and the AC impedance test is performed at room temperature, and the test frequency is 1MHz~0.1Hz. The ionic conductivity of the sample is obtained by calculation. The room temperature...
Example Embodiment
[0122] Example 2:
[0123] Will Li 2 CO 3 : Al(OH) 3 : GeO 2 : SiO 2 : NH 4 H 2 PO 4 Follow Li 1.62 Al 0.5 Ge 1.5 Si 0.02 P 2.98 O 12.05 The stoichiometric ratio of ingredients, uniformly mixed and dried. The powder is heated to 750°C for 2h, and after cooling, it is crushed and dried under wet milling conditions. Then heat the powder to 1450°C and keep it for 2h, then pour it into liquid nitrogen for quenching. After the product is cooled, it is crushed and dried under wet milling conditions, and the glass powder is pressed into a shape at 300 MPa. The block is first kept at 550°C for 4 hours, and then at 900°C for 6 hours. After cooling in the furnace, a glass ceramic lithium fast ion block material is obtained. After the glass ceramic block is machined, gold is used as the blocking electrode, and the AC impedance test is performed at room temperature, and the test frequency is 1MHz~0.1Hz. The ionic conductivity of the sample is calculated, and the room temperature ionic con...
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