CN113277518A - Silica raw material and preparation method thereof - Google Patents
Silica raw material and preparation method thereof Download PDFInfo
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- CN113277518A CN113277518A CN202110461759.XA CN202110461759A CN113277518A CN 113277518 A CN113277518 A CN 113277518A CN 202110461759 A CN202110461759 A CN 202110461759A CN 113277518 A CN113277518 A CN 113277518A
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- raw material
- silicon
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- silica raw
- powder
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/483—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides for non-aqueous cells
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/40—Electric properties
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a silica raw material and a preparation method thereof, relates to the field of silica raw materials, and is characterized in that: comprises 2-3 g of silicon powder, 4-5 g of oxygen, 1-2 g of carbon and 50 ml of aniline acidic aqueous solution. The invention has the beneficial effects that: the method is favorable for improving the conductivity of the silicon oxide, preventing the silicon oxide from expanding in the charging process, improving the charging efficiency and effectively inhibiting the volume expansion problem of the material in the charging and discharging process.
Description
Technical Field
The invention relates to the field of silica raw materials, in particular to a silica raw material and a preparation method thereof.
Background
The silicon oxide is the first choice material for the next generation of high energy density lithium ion battery due to its advantages of high energy density, wide material source, etc.
At present, the conductivity of silicon oxide is poor, the first efficiency is low, and the expansion is large in the charging and discharging processes, so that the conductivity and the first efficiency of the lithium ion battery are poor.
Disclosure of Invention
Based on the above, the invention aims to provide a silica raw material and a preparation method thereof, so as to solve the technical problems.
In order to achieve the purpose, the invention provides the following technical scheme: a silica raw material and a preparation method thereof comprise 2-3 g of silica powder, 4-5 g of oxygen, 1-2 g of carbon and 50 ml of aniline acidic aqueous solution.
By adopting the technical scheme, the conductivity of the silicon oxide is favorably improved, the expansion in the charging process is favorably prevented, the charging efficiency is favorably improved, and the problem of volume expansion of the material in the charging and discharging process can be effectively inhibited.
The invention is further configured that the manufacturing steps of the silicon oxygen raw material comprise:
a1, placing the silicon powder into a sealed heating dish;
a2, filling 4-5 g of oxygen into a sealed heating dish;
a3, adjusting the heating temperature to 500-600 ℃, and heating for 10-20 minutes to obtain silicon dioxide;
a4, reacting silicon dioxide with simple substance silicon at high temperature, and cooling rapidly to obtain SiO
A5, adding 1-2 g of carbon powder into the prepared silicon monoxide powder, and uniformly stirring the carbon powder and the silicon monoxide powder by using a stirring tool;
a6, carrying out constant current polymerization on the aniline acidic aqueous solution by an electrochemical polymerization method, so that the aniline in the aniline acidic aqueous solution generates oxidative polymerization reaction on the anode and reacts on the surface of the electrode to generate a polymer.
And A7, coating the stirred silicon powder and carbon powder by a polyaniline coating in-situ coating mode to obtain the silicon-oxygen raw material.
By adopting the technical scheme, the arranged carbon powder is beneficial to improving the conductive efficiency of silicon dioxide and the use value of silicon oxide raw materials.
The invention further provides that the method for constant current polymerization comprises the following steps: electrolyzing the aniline acidic aqueous solution by using constant current, wherein the constant voltage of the electrolysis is minus 0.3-0.5V, and the aniline is subjected to oxidation polymerization reaction for electrolysis, wherein carbon powder and silicon monoxide powder are dried before being coated in an in-situ coating mode, and are coated after being dried for 5 minutes.
Through adopting above-mentioned technical scheme, the polymer is favorable to preventing to take place the inflation in the charging process, is favorable to improving the efficiency of charging, can effectively restrain the volume expansion problem of material in the charge-discharge process.
6. The invention is further provided that the preparation method of the silicon monoxide powder comprises two methods:
the first method comprises the following steps: raw materials of silicon and silicon dioxide are converted into silicon monoxide steam at the high temperature of 1200-1400 ℃ and under the vacuum condition of 10-2-10-3Pa, and then condensed to prepare a silicon monoxide material;
and the second method comprises the following steps: the silicon dioxide reacts with the simple substance silicon at high temperature and then is rapidly cooled to prepare the silicon monoxide.
By adopting the technical scheme, multiple manufacturing methods are adopted, and the two methods are matched with each other, so that the oxygen waste can be effectively reduced.
The invention is further set that the constant current of the constant current polymerization method is 500-1000A, an initiator is added in the polymerization process, the concentration of the aniline acidic aqueous solution is 1-20% Wt, and the initiator in the preparation process of the polyaniline is ammonium persulfate.
By adopting the technical scheme, the reaction speed and the reaction efficiency of the constant current polymerization method can be effectively improved, and the time waste in the manufacturing process is favorably reduced.
In summary, the invention mainly has the following beneficial effects: the silicon oxide conductive material is beneficial to improving the conductivity of silicon oxide, preventing the expansion in the charging process, improving the charging efficiency and effectively inhibiting the volume expansion problem of the material in the charging and discharging process.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. The following examples are given by way of illustration only and are not to be construed as limiting the present invention.
The following describes an embodiment of the present invention based on its overall structure.
A silica raw material and a preparation method thereof comprise 2-3 g of silicon powder, 4-5 g of oxygen, 1-2 g of carbon and 50 ml of aniline acidic aqueous solution, wherein the preparation steps of the silica raw material comprise:
a1, placing the silicon powder into a sealed heating dish;
a2, filling 4-5 g of oxygen into a sealed heating dish;
a3, adjusting the heating temperature to 500-600 ℃, and heating for 10-20 minutes to obtain silicon dioxide;
a4, reacting silicon dioxide with simple substance silicon at high temperature, and cooling rapidly to obtain SiO
A5, adding 1-2 g of carbon powder into the prepared silicon monoxide powder, and uniformly stirring the carbon powder and the silicon monoxide powder by using a stirring tool;
a6, carrying out constant current polymerization on the aniline acidic aqueous solution by an electrochemical polymerization method, so that the aniline in the aniline acidic aqueous solution generates oxidative polymerization reaction on the anode and reacts on the surface of the electrode to generate a polymer.
And A7, coating the stirred silicon powder and carbon powder by a polyaniline coating in-situ coating mode to obtain the silicon-oxygen raw material.
Example 1
Example 2
Example 3
Although embodiments of the present invention have been shown and described, it is intended that the present invention should not be limited thereto, that the particular features, structures, materials or characteristics described may be combined in any suitable manner in any one or more embodiments or examples, and that modifications, substitutions, variations or the like, which are not inventive and may be made by those skilled in the art without departing from the principle and spirit of the present invention and within the scope of the appended claims, are intended to be protected by the following claims.
Claims (7)
1. A silica raw material and a preparation method thereof are characterized in that: comprises 2-3 g of silicon powder, 4-5 g of oxygen, 1-2 g of carbon and 50 ml of aniline acidic aqueous solution.
2. The silica raw material and the preparation method thereof according to claim 1, wherein the silica raw material comprises: the preparation method of the silicon oxygen raw material comprises the following steps:
a1, placing the silicon powder into a sealed heating dish;
a2, filling 4-5 g of oxygen into a sealed heating dish;
a3, adjusting the heating temperature to 500-600 ℃, and heating for 10-20 minutes to obtain silicon dioxide;
a4, reacting silicon dioxide with simple substance silicon at high temperature, and cooling rapidly to obtain SiO
A5, adding 1-2 g of carbon powder into the prepared silicon monoxide powder, and uniformly stirring the carbon powder and the silicon monoxide powder by using a stirring tool;
a6, carrying out constant current polymerization on the aniline acidic aqueous solution by an electrochemical polymerization method, so that the aniline in the aniline acidic aqueous solution generates oxidative polymerization reaction on the anode and reacts on the surface of the electrode to generate a polymer.
And A7, coating the stirred silicon powder and carbon powder by a polyaniline coating in-situ coating mode to obtain a silicon-oxygen raw material.
3. The silica raw material and the preparation method thereof according to claim 1, wherein the silica raw material comprises: the method of constant current polymerization comprises the following steps: electrolyzing the aniline acidic aqueous solution at constant current, wherein the constant voltage of the electrolysis is minus 0.3-0.5V, and the aniline is subjected to oxidation polymerization reaction for electrolysis.
4. The silica raw material and the preparation method thereof according to claim 1, wherein the silica raw material comprises: the carbon powder and the silicon monoxide powder are dried before being coated by an in-situ coating mode, and are coated after being dried for 5 minutes.
5. The silica raw material and the preparation method thereof according to claim 1, wherein the silica raw material comprises: the preparation method of the silicon monoxide powder comprises two methods:
the first method comprises the following steps: raw materials of silicon and silicon dioxide are converted into silicon monoxide steam at the high temperature of 1200-1400 ℃ and under the vacuum condition of 10-2-10-3Pa, and then condensed to prepare a silicon monoxide material;
and the second method comprises the following steps: the silicon dioxide reacts with the simple substance silicon at high temperature and then is rapidly cooled to prepare the silicon monoxide.
6. The silica raw material and the preparation method thereof according to claim 1, wherein the silica raw material comprises: the constant current of the constant current polymerization method is 500-1000A, and an initiator is added in the polymerization process.
7. The silica raw material and the preparation method thereof according to claim 1, wherein the silica raw material comprises: the concentration of the aniline acidic aqueous solution is 1-20% Wt, and the initiator in the polyaniline preparation process is ammonium persulfate.
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Citations (10)
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---|---|---|---|---|
JPH04139214A (en) * | 1990-09-29 | 1992-05-13 | Central Glass Co Ltd | Production of polyaniline |
CN102738440A (en) * | 2011-04-08 | 2012-10-17 | 信越化学工业株式会社 | Method for manufacturing negative electrode active material for use in non-aqueous electrolyte secondary battery, negative electrode material for use in non-aqueous electrolyte secondary battery and non-aqueous electrolyte secondary battery |
US20140302396A1 (en) * | 2011-11-10 | 2014-10-09 | General Research Institute For Nonferrous Metals | Nano silicon-carbon composite material and preparation method thereof |
JP2015106563A (en) * | 2013-11-29 | 2015-06-08 | 深▲セン▼市貝特瑞新能源材料股▲ふん▼有限公司 | SIOx BASED COMPOSITE NEGATIVE ELECTRODE MATERIAL, PREPARATION METHOD AND BATTERY |
CN108987686A (en) * | 2018-06-20 | 2018-12-11 | 深圳市比克动力电池有限公司 | Polyaniline-coated silicon based composite material and preparation method thereof |
CN109786707A (en) * | 2019-01-18 | 2019-05-21 | 常州大学 | A kind of composite cathode material of lithium ion battery and preparation method thereof |
CN109994723A (en) * | 2019-04-04 | 2019-07-09 | 常州大学 | A kind of SiOxThe preparation method of-G/PAA-PANi/Cu composite material |
CN111115639A (en) * | 2019-12-25 | 2020-05-08 | 湖北万润新能源科技发展有限公司 | Preparation of SiO by centering reactionxMethod and application of @ C material |
US20200148545A1 (en) * | 2017-07-21 | 2020-05-14 | Imerys Graphite & Carbon Switzerland Ltd. | Carbon-coated silicon oxide/graphite composite particles, methods of making, and applications of the same |
CN112467114A (en) * | 2020-11-30 | 2021-03-09 | 湖南中科星城石墨有限公司 | Silica composite material, preparation method thereof and lithium ion battery |
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2021
- 2021-04-27 CN CN202110461759.XA patent/CN113277518A/en active Pending
Patent Citations (10)
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JPH04139214A (en) * | 1990-09-29 | 1992-05-13 | Central Glass Co Ltd | Production of polyaniline |
CN102738440A (en) * | 2011-04-08 | 2012-10-17 | 信越化学工业株式会社 | Method for manufacturing negative electrode active material for use in non-aqueous electrolyte secondary battery, negative electrode material for use in non-aqueous electrolyte secondary battery and non-aqueous electrolyte secondary battery |
US20140302396A1 (en) * | 2011-11-10 | 2014-10-09 | General Research Institute For Nonferrous Metals | Nano silicon-carbon composite material and preparation method thereof |
JP2015106563A (en) * | 2013-11-29 | 2015-06-08 | 深▲セン▼市貝特瑞新能源材料股▲ふん▼有限公司 | SIOx BASED COMPOSITE NEGATIVE ELECTRODE MATERIAL, PREPARATION METHOD AND BATTERY |
US20200148545A1 (en) * | 2017-07-21 | 2020-05-14 | Imerys Graphite & Carbon Switzerland Ltd. | Carbon-coated silicon oxide/graphite composite particles, methods of making, and applications of the same |
CN108987686A (en) * | 2018-06-20 | 2018-12-11 | 深圳市比克动力电池有限公司 | Polyaniline-coated silicon based composite material and preparation method thereof |
CN109786707A (en) * | 2019-01-18 | 2019-05-21 | 常州大学 | A kind of composite cathode material of lithium ion battery and preparation method thereof |
CN109994723A (en) * | 2019-04-04 | 2019-07-09 | 常州大学 | A kind of SiOxThe preparation method of-G/PAA-PANi/Cu composite material |
CN111115639A (en) * | 2019-12-25 | 2020-05-08 | 湖北万润新能源科技发展有限公司 | Preparation of SiO by centering reactionxMethod and application of @ C material |
CN112467114A (en) * | 2020-11-30 | 2021-03-09 | 湖南中科星城石墨有限公司 | Silica composite material, preparation method thereof and lithium ion battery |
Non-Patent Citations (1)
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