CN110311118A - Disproportionated SiOx material for lithium ion battery and preparation method thereof - Google Patents
Disproportionated SiOx material for lithium ion battery and preparation method thereof Download PDFInfo
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- CN110311118A CN110311118A CN201910621011.4A CN201910621011A CN110311118A CN 110311118 A CN110311118 A CN 110311118A CN 201910621011 A CN201910621011 A CN 201910621011A CN 110311118 A CN110311118 A CN 110311118A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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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
- H01M4/362—Composites
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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
- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
- H01M4/386—Silicon or alloys based on silicon
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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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- 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
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- 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
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Abstract
The invention relates to the field of lithium ion battery materials, in particular to a disproportionated SiOx material for a lithium ion battery and a preparation method thereof. The preparation method mainly comprises the steps of raw material preparation, material mixing, charging, vacuumizing, heating reaction, disproportionation heat treatment, crushing and grading and the like. The lithium ion battery prepared from the SiOx material obtained by the preparation method provided by the invention has excellent electrochemical performance.
Description
Technical field
The present invention relates to field of lithium ion battery material, specifically a kind of lithium ion battery disproportionation SiOx material and
Preparation method.
Background technique
With the various mobile electronic devices such as smart phone, laptop be widely used and environmental protection is to new energy
The demand of source electric car is extremely urgent, and the energy density and power density of commercial li-ion battery all do not reach requirement at present.
Therefore, it is badly in need of the electrode material of exploitation high capacity.
The extensive concern of people is received by the Novel high-specific capacity flexible negative electrode material of representative of Si sill.Wherein, SiOx
Material has while playing height ratio capacity and compares the smaller volume change of pure Si, more practical latent in terms of cycle life
Power, therefore be also that speed is promoted and applied in current high capacity type negative electrode material.SiOx is needed as negative electrode material by disproportionation
A series of subsequent processings such as heat treatment, carbon coating, compound, can just make it have excellent chemical property, to meet lithium ion
The application of battery.Wherein disproportionation heat treatment is important one of key link, and current disproportionation heat treatment is prepared in SiOx
Carried out in subsequent handling afterwards, as CN201610209607 " a kind of SiOxC cathode material preparation method ",
" lithium ion secondary battery is used by CN201310352667 " preparation method of lithium ion battery negative material ", CN201380054869
" lithium ion battery is used by negative electrode material, lithium ion secondary battery cathode and lithium ion secondary battery ", CN201310073878.3
Silicon-carbon cathode material and preparation method thereof " etc..The preparation of SiOx and disproportionation heat treatment step are spaced apart from each other, so that energy consumption increases
Add, disproportionation extent control is bad, cannot give full play to the comprehensive performance of material.
Summary of the invention
The present invention is intended to provide a kind of lithium ion battery disproportionation SiOx material and preparation method thereof, so that using the present invention
The lithium ion battery that the preparation method of offer obtains the preparation of SiOx material has excellent chemical property.
In order to solve the above technical problems, the technical solution adopted by the present invention are as follows: a kind of lithium ion battery disproportionation SiOx
The preparation method of material, comprising the following steps:
1) silicon powder and silicon dioxide powder, are weighed respectively according to the mass ratio of 1-2:3, and the granularity of silicon powder and silicon dioxide powder is
Micron order;
2), the silicon powder weighed in step 1) and silicon dioxide powder are uniformly mixed, obtain mixture;
3), mixture obtained in step 2 is packed into heating furnace, heating furnace is evacuated to 0.075Pa or less;
4), after vacuum degree is met the requirements, the reaction zone of heating furnace is heated, is warming up to 1200 with the heating speed of 10 DEG C/min
DEG C~1400 DEG C, 3~5 hours are kept the temperature, SiOx, 0.5≤x≤1.6 therein are obtained;After reaction zone heat preservation, to heating
The condensing zone of furnace is heated, and is warming up to 900 DEG C~1000 DEG C with the heating rate of 10 DEG C/min, is kept the temperature 1~2 hour, is made
It is disproportionated SiOx;
5) SiOx obtained in step 4), is subjected to crushing and classification processing to get lithium ion battery disproportionation SiOx material is arrived.
Preferably, the purity of silicon powder is 99.9% or more in step 1), granularity D50≤8 μm;The purity of silicon dioxide powder is
99.5% or more, granularity D50≤8 μm.
Preferably, silicon powder and silicon dioxide powder are mixed by high-speed mixer in step 2.
Preferably, crushing and classification processing is carried out to disproportionation SiOx by airflow milling in step 6).
A kind of lithium ion battery disproportionation SiOx material, is prepared by any one of the above preparation method.
Detailed description of the invention
Fig. 1 is the diffracting spectrum for the SiOx material that disproportionated reaction does not occur for comparative example;
Fig. 2 is that the lithium ion battery of the embodiment of the present invention two is disproportionated the diffracting spectrum of SiOx material.
Beneficial effect
The present invention carries out disproportionated reaction during producing SiOx material, is effectively utilized the cooling preheating of SiOx, saves
Energy consumption, while the link being individually disproportionated is eliminated when preparing lithium cell negative pole material with it, improve production efficiency.
In the present invention, the mixture that disproportionated reaction generates nano-silicon and silica occurs for the SiOx of preparation, and nano-silicon is more
It is dispersed in SiOx matrix, is significantly improved by the first charge discharge efficiency of the lithium cell negative pole material of disproportionation SiOx preparation than what is be not disproportionated.
By control temperature and time in disproportionation SiOx preparation process, the crystallite dimension of nano-silicon also can be effectively controlled, avoid silicon wafer
Lithium battery cycle performance caused by particle size is excessive is deteriorated.
Specific embodiment
Lithium ion battery of the invention is carried out in detail with the preparation method of disproportionation SiOx material with three embodiments below
Explanation:
The preparation method of the lithium ion battery of embodiment one disproportionation SiOx material, comprising the following steps: 1), according to the matter of 1:2
Amount ratio weighs silicon powder and silicon dioxide powder respectively, and the granularity of silicon powder and silicon dioxide powder is micron order;The purity of silicon powder is
99.9% or more, granularity D50≤8 μm;The purity of silicon dioxide powder is 99.5% or more, granularity D50≤8 μm;
2) silicon powder weighed in step 1) and silicon dioxide powder are uniformly mixed by high-speed mixer, obtain mixture;
3), mixture obtained in step 2 is packed into heating furnace, heating furnace is evacuated to 0.075Pa or less;
4), after vacuum degree is met the requirements, the reaction zone of heating furnace is heated, is warming up to 1200 with the heating speed of 10 DEG C/min
DEG C, 5 hours are kept the temperature, SiOx, 0.5≤x≤1.6 therein are obtained;After reaction zone heat preservation, to the condensing zone of heating furnace into
Row heating is warming up to 900 DEG C with the heating rate of 10 DEG C/min, keeps the temperature 2 hours, and disproportionation SiOx is made;
5) SiOx obtained in step 4), is subjected to crushing and classification processing by airflow milling to get the lithium ion for arriving embodiment one
Battery disproportionation SiOx material.
The preparation method of the lithium ion battery of embodiment two disproportionation SiOx material, comprising the following steps: 1), according to 1:
2.5 mass ratio weighs silicon powder and silicon dioxide powder respectively, and the granularity of silicon powder and silicon dioxide powder is micron order;Silicon powder
Purity is 99.9% or more, granularity D50≤8 μm;The purity of silicon dioxide powder is 99.5% or more, granularity D50≤8 μm;
2) silicon powder weighed in step 1) and silicon dioxide powder are uniformly mixed by high-speed mixer, obtain mixture;
3), mixture obtained in step 2 is packed into heating furnace, heating furnace is evacuated to 0.075Pa or less;
4), after vacuum degree is met the requirements, the reaction zone of heating furnace is heated, is warming up to 1300 with the heating speed of 10 DEG C/min
DEG C, 4 hours are kept the temperature, SiOx, 0.5≤x≤1.6 therein are obtained;After reaction zone heat preservation, to the condensing zone of heating furnace into
Row heating is warming up to 950 DEG C with the heating rate of 10 DEG C/min, keeps the temperature 1.5 hours, and disproportionation SiOx is made;
5) SiOx obtained in step 4), is subjected to crushing and classification processing by airflow milling to get the lithium ion for arriving embodiment two
Battery disproportionation SiOx material.
The preparation method of the lithium ion battery of embodiment three disproportionation SiOx material, comprising the following steps: 1), according to 1:3
Mass ratio weigh silicon powder and silicon dioxide powder respectively, the granularity of silicon powder and silicon dioxide powder is micron order;Silicon powder it is pure
Degree is 99.9% or more, granularity D50≤8 μm;The purity of silicon dioxide powder is 99.5% or more, granularity D50≤8 μm;
2) silicon powder weighed in step 1) and silicon dioxide powder are uniformly mixed by high-speed mixer, obtain mixture;
3), mixture obtained in step 2 is packed into heating furnace, heating furnace is evacuated to 0.075Pa or less;
4), after vacuum degree is met the requirements, the reaction zone of heating furnace is heated, is warming up to 1400 with the heating speed of 10 DEG C/min
DEG C, 3 hours are kept the temperature, SiOx, 0.5≤x≤1.6 therein are obtained;After reaction zone heat preservation, to the condensing zone of heating furnace into
Row heating is warming up to 1000 DEG C with the heating rate of 10 DEG C/min, keeps the temperature 1 hour, and disproportionation SiOx is made;
5) SiOx obtained in step 4), is subjected to crushing and classification processing by airflow milling to get the lithium ion for arriving embodiment three
Battery disproportionation SiOx material.
The SiOx material of disproportionated reaction does not occur lithium ion battery disproportionation SiOx material obtained in embodiment two and
Material as a comparison case respectively carry out diffraction detection, wherein the diffracting spectrum of comparative example as shown in Figure 1, embodiment two diffracting spectrum
As shown in Fig. 2, by Fig. 1 and Fig. 2 it is found that there was only the amorphous peak of SiOx in comparative example.And except SiOx's in the embodiment of the present invention two
Outside amorphous peak, there is nano silicon crystal peak, silicon wafer particle size can be calculated by Scherrer formula.
Claims (5)
1. a kind of lithium ion battery preparation method of disproportionation SiOx material, it is characterised in that: the following steps are included:
1) silicon powder and silicon dioxide powder, are weighed respectively according to the mass ratio of 1-2:3, and the granularity of silicon powder and silicon dioxide powder is
Micron order;
2), the silicon powder weighed in step 1) and silicon dioxide powder are uniformly mixed, obtain mixture;
3), mixture obtained in step 2 is packed into heating furnace, heating furnace is evacuated to 0.075Pa or less;
4), after vacuum degree is met the requirements, the reaction zone of heating furnace is heated, is warming up to 1200 with the heating speed of 10 DEG C/min
DEG C~1400 DEG C, 3~5 hours are kept the temperature, SiOx, 0.5≤x≤1.6 therein are obtained;After reaction zone heat preservation, to heating
The condensing zone of furnace is heated, and is warming up to 900 DEG C~1000 DEG C with the heating rate of 10 DEG C/min, is kept the temperature 1~2 hour, is made
It is disproportionated SiOx;
5) SiOx obtained in step 4), is subjected to crushing and classification processing to get lithium ion battery disproportionation SiOx material is arrived.
2. a kind of preparation method of lithium ion battery disproportionation SiOx material according to claim 1, it is characterised in that: step
It is rapid 1) in silicon powder purity be 99.9% or more, granularity D50≤8 μm;The purity of silicon dioxide powder is 99.5% or more, granularity D50
≤8μm。
3. a kind of preparation method of lithium ion battery disproportionation SiOx material according to claim 1, it is characterised in that: step
It is rapid 2) in silicon powder and silicon dioxide powder mixed by high-speed mixer.
4. a kind of preparation method of lithium ion battery disproportionation SiOx material according to claim 1, it is characterised in that: step
It is rapid 6) in by airflow milling to disproportionation SiOx carry out crushing and classification processing.
5. a kind of lithium ion battery disproportionation SiOx material, it is characterised in that: by any one preparation method of claim 1-4
Preparation.
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN111370693A (en) * | 2020-03-24 | 2020-07-03 | 洛阳联创锂能科技有限公司 | Preparation method of high-first-efficiency silicon-oxygen lithium negative electrode material |
CN111377452A (en) * | 2020-03-24 | 2020-07-07 | 洛阳联创锂能科技有限公司 | Preparation method of silicon-oxygen cathode material |
CN112320804A (en) * | 2020-09-29 | 2021-02-05 | 上海皓越电炉技术有限公司 | Vacuum heat treatment equipment for continuously preparing SiO negative electrode material of lithium ion battery |
CN113937259A (en) * | 2021-09-07 | 2022-01-14 | 惠州市贝特瑞新材料科技有限公司 | Preparation method and device of silicon monoxide for lithium ion battery and lithium ion battery |
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Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
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CN111370693A (en) * | 2020-03-24 | 2020-07-03 | 洛阳联创锂能科技有限公司 | Preparation method of high-first-efficiency silicon-oxygen lithium negative electrode material |
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CN112320804A (en) * | 2020-09-29 | 2021-02-05 | 上海皓越电炉技术有限公司 | Vacuum heat treatment equipment for continuously preparing SiO negative electrode material of lithium ion battery |
CN113937259A (en) * | 2021-09-07 | 2022-01-14 | 惠州市贝特瑞新材料科技有限公司 | Preparation method and device of silicon monoxide for lithium ion battery and lithium ion battery |
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