Anode active material for secondary battery and method for producing the same, anode and lithium ion battery using the same
一种负极活性物质、非晶性的技术,应用在二次电池用负极活性物质及其制造、使用其的负极以及锂离子电池领域,能够解决生产性不充分、容量不充分、无法充分发挥硅系材料特性等问题,达到充放电容量优异、循环特性优异的效果
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[0122] Hereinafter, although an Example and a comparative example are shown and this invention is demonstrated more concretely, this invention is not limited to these Examples.
[0123] In this example, various analyzes and evaluations were performed on the silicon oxide-based composite materials, silica, and the like prepared in Examples 1 to 5, and Comparative Examples 1 and 2.
[0124] In addition, in the formula, Ph represents a phenyl group, and Me represents a methyl group.
[0125] In addition, the measuring devices and measuring methods of "X-ray diffraction measurement", "elemental analysis measurement", "laser Raman spectroscopy measurement" and "X-ray small-angle scattering measurement" and "battery characteristics" in each example and comparative example evaluation", as described below.
[0126] (measured by X-ray diffraction method)
[0127] X-ray diffraction is to use Bruker AXS (Bruker AXS) (stock) D8Discover manufactured as X-ray diffraction device, through t...
Synthetic example 1
[0144] Synthesis of Octaphenylsilsesquioxane (10)
[0145] 360 ml of toluene (Wako Pure Chemical Industry), 42.2 g of tetrabutylammonium hydroxide (Tokyo Chemical Industry) (37% tetrabutylammonium hydroxide (Tetrabutylammonium Hydroxide, TBAH) in MeOH), pure 16.2 g of water, stirred and cooled in an ice bath. 360 ml of diethyl ether (Wako Pure Chemical Industry) and 118.9 g of phenyltrimethoxysilane (Tokyo Chemical Industry) were put into a 500 ml dropping funnel, and were added dropwise over 5 minutes. After the dropwise addition, the ice bath was removed, and the mixture was stirred at room temperature for 70 hours. After 70 hours, filter through a pressure filter.
[0146] The obtained powder was transferred to a beaker, washed with toluene, and filtered again under pressure. After filtration, 14.3 g of octaphenylsilsesquioxane (10) was obtained by vacuum drying at 120 degreeC for 6 hours with a vacuum dryer.
Synthetic example 2
[0148] (PhSiO 3 / 2 ) n Synthesis
[0149] Into a 500 ml four-necked flask, 99.1 g of phenyltrimethoxysilane (Tokyo Chemical Industry) and 16 g of methanol (Wako Pure Chemical Industries) were charged. While stirring at room temperature, 36 g of 1N HCl was slowly added dropwise through the dropping funnel over 30 minutes. After completion of the dropwise addition, it was heated and stirred at 60° C. for 2 hours. After cooling for 2 hours, 200 g of toluene (Wako Pure Chemical Industry) was added dropwise.
[0150] Then, the reaction solution was transferred to a 500 ml separatory funnel. After washing with saturated saline, washed with saturated sodium bicarbonate water, then washed twice with saturated saline, and finally washed twice with pure water. After washing with water, dehydration was performed with magnesium sulfate (Wako Pure Chemical Industries, Ltd.). The liquid was moved to a separable flask, the solvent was distilled off, and heated under reduced pressure to ...
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