Producing method for non-aqueous electrolyte secondary battery and negative electrode materials for non-aqueous electrolyte secondary battery, negative electrode active materials for non-aqueous electrolyte secondary battery and producing method thereof
A negative electrode active material, non-aqueous electrolyte technology, applied in non-aqueous electrolyte batteries, secondary batteries, active material electrodes, etc., can solve the problem of reduced cycle characteristics, and achieve the effect of good cycle characteristics and initial charge-discharge characteristics
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Embodiment 1-1
[0196] First, silicon-based active material particles are produced. First, a raw material (also referred to as a gasification starting material) obtained by mixing metal silicon and silicon dioxide is placed in a reaction furnace, and deposited under a vacuum of 10 Pa. After cooling sufficiently, the deposit is taken out and pulverized with a ball mill. After adjusting the particle size, a carbon film is obtained by performing pyrolysis chemical vapor deposition (pyrolysis CVD). The powder after the formation of the carbon film is mixed with lithium hydride and heat-treated at 600°C to 800°C. kg Lithium hexafluorophosphate: LiPF 6 ), using an electrochemical method to carry out electrochemical lithium doping modification. Next, the modified silicon compound was washed with water containing 10% ethanol. Next, the rinsed silicon compound is dried under reduced pressure.
[0197] Silicon compounds (silicon-based active material particles) after washing and drying, containing ...
Embodiment 1-2～1-5
[0213] (Examples 1-2 to 1-5, Comparative Example 1-1, Comparative Example 1-2)
[0214] A test battery and a secondary battery were produced in the same manner as in Example 1-1, except that the amount of oxygen in the bulk of the silicon compound was adjusted. At this time, the oxygen amount was adjusted by changing the ratio and temperature of the vaporized starting materials. In Examples 1-1 to 1-5 and Comparative Examples 1-1 and 1-2, SiO x Table 1 shows the values of x for the silicon compounds represented.
[0215] In the same manner as in Example 1-1, the initial charge and discharge characteristics of the test batteries of Examples 1-2 to 1-5 and Comparative Examples 1-1 and 1-2 and the cycle of the laminated film-type lithium ion secondary battery were examined. After the characteristics (capacity retention rate), the results shown in Table 1 were obtained.
[0216] In addition, the capacity retention ratios of secondary batteries shown in Table 1 to Table 9 belo...
Embodiment 2-1～ Embodiment 2-2、 comparative example 2-1～ comparative example 2-3
[0226] Basically the same as in Example 1-3, the manufacture of the test battery and the secondary battery was carried out, but the SiO x In the silicon compound shown, the conditions of the lithium doping treatment (in-bulk modification), that is, the lithium doping treatment method are changed, and the type of lithium compound contained in the silicon compound is changed. After checking the initial charge and discharge characteristics of the test batteries of Examples 2-1 to 2-2 and Comparative Examples 2-1 to 2-3 and the cycle characteristics (capacity retention rate) of the laminated film-type secondary battery, the table 2 shows the results.
[0227] [Table 2]
[0228] SiO x (x=0.9), D 50 =5μm, XRD full width at half maximum 2θ=1.218°, Si(111) crystallite 7.21nm,
[0229] Carbon coating amount: 5% by mass, 44% of discharge capacity at 0.40V,
[0230] The charging capacity at 0.17V is 16.8%. Modification method: heating doping + electrochemical doping,
[0231] Adhes...
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