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Preparation method of porous SiOx core-shell microspheres

A technology of core-shell and microspheres, which is applied in the direction of electrical components, electrochemical generators, battery electrodes, etc., can solve the problems of complex operation, high cost, and unsuitability for industrialization, and achieve volume effect relief, high carbon content, and wide application wide effect

Inactive Publication Date: 2017-05-10
ZHONGTIAN ENERGY STORAGE TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the method is complicated to operate and the cost is high, so it is not suitable for industrialization

Method used

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  • Preparation method of porous SiOx core-shell microspheres
  • Preparation method of porous SiOx core-shell microspheres
  • Preparation method of porous SiOx core-shell microspheres

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preparation example Construction

[0027] A preparation method of porous SiO core-shell microspheres, comprising the following steps:

[0028] (1) Prepare 100 parts of HF solution with a mass fraction of 1wt%-10wt% by mass, and start stirring;

[0029] (2) Slowly add 15 parts of the disproportionated SiO sample into the HF solution, stir for 0.5-2h, filter and wash, and vacuum dry to obtain porous SiOx, the SiO in the disproportionated SiO sample 2 The content is 10%-25%;

[0030] (3) Ultrasonic disperse the obtained porous SiOx and epoxy resin for 10-30 min, then dilute with 5-15 parts of chloroform, and then add 8-10 parts of curing agent to prepare a mixture. The curing agent is diethylaminopropylamine, 3 , 9-bis(3-aminopropyl)-2,4,8,10-tetraoxa spiroundecane adduct, diaminodiphenylmethane, 650 low molecular weight polyamide, triethylenetetramine A sort of;

[0031] (4) Slowly add the above mixture into the aqueous solution in which the surfactant is dissolved, stir and react at 40-60°C for 3-6h, then fil...

Embodiment 1

[0033] A preparation method of porous SiO core-shell microspheres, comprising the following steps:

[0034] (1) Preparation of porous SiOx

[0035] Configure 100 g of HF solution with a mass fraction of 5 wt%, and start stirring; slowly add 15 g of disproportionated SiO samples into the HF solution, stir for 1 h, filter and wash, and vacuum dry to obtain porous SiOx;

[0036] (2) Preparation of porous SiOx core-shell microspheres coated with epoxy resin

[0037] The obtained porous SiOx was ultrasonically dispersed with epoxy resin for 20 min, diluted with 10 g of chloroform, and 10 g of curing agent diethylaminopropylamine was added; the mixture was slowly added to an aqueous solution in which surfactant was dissolved, stirred and reacted at 60°C for 6 h, filtered and washed and vacuum drying to obtain porous SiOx core-shell microspheres coated with epoxy resin.

[0038] See attached figure 1 and 2 , which are the scanning electron micrograph and particle size distributio...

Embodiment 2

[0041] A preparation method of porous SiO core-shell microspheres, comprising the following steps:

[0042] (1) Preparation of porous SiOx

[0043] Configure 100 g of HF solution with a mass fraction of 6 wt%, and start stirring; slowly add 15 g of disproportionated SiO samples into the HF solution, stir for 1.5 h, filter and wash, and vacuum dry to obtain porous SiOx;

[0044] (2) Preparation of porous SiOx core-shell microspheres coated with epoxy resin

[0045] The obtained porous SiOx was ultrasonically dispersed with epoxy resin for 30 min, diluted with 11 g of chloroform, and 9 g of curing agent diethylaminopropylamine was added; the mixture was slowly added to an aqueous solution in which surfactant was dissolved, stirred and reacted at 55°C for 5 h, filtered and washed and vacuum drying to obtain porous SiOx core-shell microspheres coated with epoxy resin.

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Abstract

The invention discloses a preparation method of porous SiOx core-shell microspheres. The preparation method of the porous SiOx core-shell microspheres comprises the following steps: firstly corroding SiO through an HF solution to obtain porous SiOx; ultrasonically dispersing the obtained porous SiOx and epoxy resin, then diluting by using chloroform, adding a curing agent, then slowly adding the materials into a polyvinylpyrrolidone solution together, stirring and reacting; and filtering, washing and drying the product to finally obtain epoxy resin coated porous SiOx core-shell microspheres which can be used for preparing precursors of negative materials of lithium ion batteries; the preparation method of the core-shell microspheres has the advantages of wide raw material sources, simple process and wide application.

Description

technical field [0001] The invention belongs to the field of lithium ion battery materials, and in particular relates to a preparation method of porous SiOx core-shell microspheres. Background technique [0002] With the decrease of fossil energy and the increasing environmental pollution, more and more attention has been paid to green energy, and lithium-ion batteries are one of them. Anode materials are an important part of lithium-ion batteries. Silicon, which has been studied the most at present, not only has a theoretical specific capacity 10 times higher than that of graphite (4200 mAh / g, Li 22 Si 5 ) and large volumetric energy density (9786mAh / cm 3 ), and the relatively moderate delithiation platform makes it have good safety performance. In addition, the wide source and low cost are also a major advantage of silicon. However, silicon has a huge volume effect (volume change of about 300%) when intercalating lithium, and the internal stress generated is easy to pul...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/36H01M4/48H01M4/62H01M10/0525
CPCH01M4/366H01M4/483H01M4/628H01M10/0525Y02E60/10
Inventor 董鑫怡贺劲鑫郑媛媛靳承铀薛驰缪永华
Owner ZHONGTIAN ENERGY STORAGE TECH
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