Graphite material, method for producing same, negative electrode for lithium ion secondary battery, negative electrode material for lithium ion secondary battery, and lithium ion secondary battery
A manufacturing method and a graphite-based technology, which can be used in secondary batteries, non-aqueous electrolyte battery electrodes, fuel cells, etc., and can solve the problems of inability to meet rapid charge-discharge performance, cycle performance, and insufficiency.
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Embodiment 1
[0152] (precursor of graphitic materials)
[0153] Mesophase spheres heat-treated with coal tar pitch (manufactured by JFE Chemical Co., Ltd., average particle size: 25 μm) were calcined at 600° C. for 3 hours in a nitrogen atmosphere to prepare spherical graphite material precursors. The average aspect ratio is 1.2.
[0154] The precursor of the graphitic material prepared by this method was used as the precursor (1).
[0155] (graphite material)
[0156] 100 parts by mass of the above-mentioned precursor (1) was added to 100 parts by mass of an aqueous ferric chloride solution (acidic) having a concentration corresponding to 5 mass % in terms of iron, and then an aqueous sodium hydroxide solution was added to neutralize to pH=7. In the obtained neutral solution, the precursor (1) is dispersed in a suspension of iron hydroxide (FeO(OH)). This dispersion liquid was heated to 100° C. to remove water, and then vacuum-dried at 150° C. for 5 hours to completely remove water.
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Embodiment 2
[0198] Change the preparation method of the precursor of the graphitic material in embodiment 1. The small spheres of the mesophase were pulverized in advance to obtain lumpy particles with an average particle diameter of 15 μm. It was calcined at 600° C. for 3 hours under a nitrogen atmosphere to obtain a bulk precursor (2). Its average aspect ratio is 1.5.
[0199] Using the above-mentioned precursor (2), the graphitic material (2) was prepared by the same method and conditions as in Example 1. Graphite material (2) is a block with an average particle size of 14 μm, with 7 particles / 100 μm on the surface 2 The structure of hemispherical or spherical protrusions. The average height h of the protrusions was 2.8 μm, the average base length g was 2.3 μm, and the average h / g was 1.2. The average aspect ratio of the graphitic material (2) is 1.5, and the specific surface area is 4.5m 2 / g, interplanar spacing d 002 is 0.3356nm. Table 1 shows the properties of the precursor ...
Embodiment 3
[0207] Change the preparation method of the precursor of the graphitic material in embodiment 1. The coal tar pitch was calcined at 600 °C for 3 hours under nitrogen atmosphere to obtain the bulk mesophase. This was pulverized to prepare bulk and scale-like precursors (3) with an average particle diameter of 25 μm.
[0208] Next, 100 g of the precursor (3) was immersed in a mixture of 100 g of ethylene glycol and 0.5 g of hexamethylenetetramine together with 5 g of phenolic resin (residual rate after graphitization: 40%) as a carbon source material. middle. While stirring the obtained mixture, ethylene glycol was removed under reduced pressure (1.3 Pa) at 150° C. to obtain a resin-coated precursor. The resin-coated precursor was heat-treated in air at 270° C. for 5 hours to cure the resin to obtain a precursor (31) covered with the cured resin. Its average aspect ratio is 2.8.
[0209] In addition, when this precursor (31) was observed with a polarizing microscope, it was ...
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