CN111377452A - Preparation method of silicon-oxygen cathode material - Google Patents
Preparation method of silicon-oxygen cathode material Download PDFInfo
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- CN111377452A CN111377452A CN202010210380.7A CN202010210380A CN111377452A CN 111377452 A CN111377452 A CN 111377452A CN 202010210380 A CN202010210380 A CN 202010210380A CN 111377452 A CN111377452 A CN 111377452A
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- OBNDGIHQAIXEAO-UHFFFAOYSA-N [O].[Si] Chemical compound [O].[Si] OBNDGIHQAIXEAO-UHFFFAOYSA-N 0.000 title claims abstract description 37
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 239000010406 cathode material Substances 0.000 title claims abstract description 18
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 94
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 45
- 239000007789 gas Substances 0.000 claims abstract description 32
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 26
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims abstract description 23
- 229910000077 silane Inorganic materials 0.000 claims abstract description 23
- 239000000463 material Substances 0.000 claims abstract description 17
- 239000002994 raw material Substances 0.000 claims abstract description 6
- 238000010438 heat treatment Methods 0.000 claims description 40
- 238000000034 method Methods 0.000 claims description 24
- 238000001816 cooling Methods 0.000 claims description 16
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 15
- 229910052799 carbon Inorganic materials 0.000 claims description 15
- 239000010405 anode material Substances 0.000 claims description 12
- 238000006243 chemical reaction Methods 0.000 claims description 11
- 239000000203 mixture Substances 0.000 claims description 9
- 229910052814 silicon oxide Inorganic materials 0.000 claims description 9
- 239000011248 coating agent Substances 0.000 claims description 7
- 238000000576 coating method Methods 0.000 claims description 7
- 239000012071 phase Substances 0.000 claims description 7
- 239000002243 precursor Substances 0.000 claims description 7
- 239000007791 liquid phase Substances 0.000 claims description 6
- 239000007773 negative electrode material Substances 0.000 claims description 6
- 239000010703 silicon Substances 0.000 claims description 6
- 238000000197 pyrolysis Methods 0.000 claims description 5
- 238000000498 ball milling Methods 0.000 claims description 4
- 150000001336 alkenes Chemical class 0.000 claims description 3
- 150000001345 alkine derivatives Chemical class 0.000 claims description 3
- 229910052681 coesite Inorganic materials 0.000 claims description 3
- 229910052906 cristobalite Inorganic materials 0.000 claims description 3
- 238000003825 pressing Methods 0.000 claims description 3
- 238000007670 refining Methods 0.000 claims description 3
- 238000012216 screening Methods 0.000 claims description 3
- 229910052710 silicon Inorganic materials 0.000 claims description 3
- 239000007790 solid phase Substances 0.000 claims description 3
- 229910052682 stishovite Inorganic materials 0.000 claims description 3
- 229910052905 tridymite Inorganic materials 0.000 claims description 3
- 150000001335 aliphatic alkanes Chemical class 0.000 claims description 2
- 239000010426 asphalt Substances 0.000 claims description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 9
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 9
- 229910052744 lithium Inorganic materials 0.000 description 9
- 229910001416 lithium ion Inorganic materials 0.000 description 9
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 5
- 239000000843 powder Substances 0.000 description 4
- 238000009831 deintercalation Methods 0.000 description 3
- 238000003860 storage Methods 0.000 description 3
- 238000012512 characterization method Methods 0.000 description 2
- 239000011247 coating layer Substances 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- 239000007772 electrode material Substances 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- 238000003780 insertion Methods 0.000 description 2
- 230000037431 insertion Effects 0.000 description 2
- 230000002687 intercalation Effects 0.000 description 2
- 238000009830 intercalation Methods 0.000 description 2
- 239000010410 layer Substances 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 229910001290 LiPF6 Inorganic materials 0.000 description 1
- ZVLDJSZFKQJMKD-UHFFFAOYSA-N [Li].[Si] Chemical compound [Li].[Si] ZVLDJSZFKQJMKD-UHFFFAOYSA-N 0.000 description 1
- RXBBZJPEEIUBJG-UHFFFAOYSA-N [O].[Si].[Li] Chemical group [O].[Si].[Li] RXBBZJPEEIUBJG-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000003139 buffering effect Effects 0.000 description 1
- 150000001722 carbon compounds Chemical class 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 239000011889 copper foil Substances 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000007323 disproportionation reaction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- PAZHGORSDKKUPI-UHFFFAOYSA-N lithium metasilicate Chemical compound [Li+].[Li+].[O-][Si]([O-])=O PAZHGORSDKKUPI-UHFFFAOYSA-N 0.000 description 1
- 229910052912 lithium silicate Inorganic materials 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 230000003446 memory effect Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
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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
-
- 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
-
- 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
-
- 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
-
- 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
-
- 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 relates to a preparation method of a silicon-oxygen cathode material, which relates to the technical field of batteries, and the invention obtains raw materials with different silicon-oxygen ratios by controlling the amounts of two gases of silicon dioxide and silane, can controllably prepare silicon-oxygen materials with different capacities and different electrochemical properties.
Description
Technical Field
The invention relates to the technical field of batteries, in particular to a preparation method of a negative electrode material, and specifically relates to a preparation method of a silica negative electrode material.
Background
As is known, with the increasingly prominent environmental and energy problems, the new energy field is widely regarded by various social circles, and as a clean energy conversion device, a lithium ion battery can realize the conversion between electric energy and chemical energy and has the advantages of high energy density, long service life, high safety factor, no memory effect and the like, so that the lithium ion battery has been widely applied to the aspects of electric vehicles, portable electronic devices and the like. Meanwhile, along with the increase of competition and the continuous improvement of the requirements of people on the product performance, higher requirements are provided for the energy density, the rate characteristic, the cycle stability, the safety performance and the like of the lithium ion battery, wherein the energy density is the crucial performance index of the lithium ion battery.
One of the most direct and effective means for increasing the energy density of a lithium ion battery is to apply an electrode active material with higher capacity, so that an electrode material with high capacity and applicability is urgently sought, wherein silicon (Si) is applied to a negative electrode of the lithium ion battery as a negative electrode active material, has a theoretical specific capacity of about 4200mAh/g, which is far higher than the theoretical gram capacity of graphite of a traditional negative electrode material, but the volume expansion of up to 300% in a silicon lithium deintercalation process causes poor electrode stability and short cycle life, and becomes a big difficulty in the application process.
The research shows that the silicon-oxygen material (SiOx) is applied to the lithium ion battery cathode and is characterized in that the silicon-oxygen material has higher lithium storage specific capacity, and lithium silicate formed in the lithium embedding process can play a role in buffering, so that the volume expansion effect of silicon in the charging and discharging process can be effectively improved, and the stability of the electrode is improved.
Therefore, how to provide a preparation method of a silicon-oxygen anode material is a long-term technical appeal for the skilled person.
Disclosure of Invention
In order to overcome the defects in the background technology, the invention provides a preparation method of a silica cathode material, which is applied to a cathode material in a battery system, has good cycle stability, and has the characteristics of high gram capacity and the like compared with the traditional lithium ion battery cathode material.
In order to achieve the above purpose, the invention adopts the following technical scheme:
a preparation method of a silicon-oxygen anode material specifically comprises the following steps:
firstly, pressing silicon dioxide to form a blocky silicon dioxide cake, and then uniformly placing the blocky silicon dioxide cake in a heating zone of a resistance heating device;
second oneHeating the massive silicon dioxide cake to 1000-1500 ℃, vacuumizing a cavity of the resistance heating device to ensure that the vacuum degree in the cavity is less than or equal to 50Pa, then uniformly introducing silane gas into the cavity to keep the temperature in the cavity constant, ensuring that the silane gas is fully contacted with the silicon dioxide in the whole reaction process, and SiH4With SiO2SiOx is generated by reaction, and the value of X is adjusted by controlling the reaction condition;
thirdly, condensing at a cooling end of the resistance heating device to obtain a silica product;
fourthly, crushing the obtained silica product to obtain a micron-scale or nano-scale precursor;
and fifthly, carrying out carbon coating on the precursor in a liquid phase, solid phase or gas phase mode to obtain the required silicon-oxygen cathode material.
In the preparation method of the silica cathode material, in the first step, the silica is nano-scale silica powder or the nano-scale silica powder is obtained by refining and screening silica raw materials.
The preparation method of the silica cathode material comprises the following steps that in the second step, the resistance heating device comprises a cooling tower, a collector, a pressure valve, a heating source, a vacuum valve and a silane gas storage device, wherein the heating source is arranged in the cavity, a silicon and silicon dioxide mixture is arranged in the heating source, the cooling tower is arranged above the cavity, the collector is arranged in the cooling tower, the vacuum valve is arranged on one side of the lower portion of the cavity, the pressure valve is arranged on the other side of the lower portion of the cavity, and the pressure valve 3 is connected with the silane gas storage device through a pipeline.
In the preparation method of the silicon-oxygen cathode material, silane in the second step is high-purity silane gas.
According to the preparation method of the silicon-oxygen cathode material, the heating rate during heating in the second step is 10 min/min.
In the fourth step, the silicon-oxygen product is crushed by any one or a combination of two or more of jaw crushing, gas crushing and ball milling.
In the preparation method of the silicon-oxygen cathode material, in the fourth step, the silicon-oxygen product is crushed to enable the silicon-oxygen product D50 to be within the range of 2-10 um.
In the preparation method of the silicon-oxygen cathode material, the liquid phase in the fifth step mainly takes pitch as a carbon source.
In the fifth step, the gas phase mainly comprises alkanes, alkenes and alkynes with low carbon content, and the gas phase is pyrolyzed at high temperature to obtain the carbon coating layer.
According to the preparation method of the silicon-oxygen cathode material, the temperature during pyrolysis is 500-1200 ℃.
By adopting the technical scheme, the invention has the following advantages:
the invention obtains the raw materials with different silicon-oxygen ratios by controlling the amount of the two gases of silicon dioxide and silane, can controllably prepare the silicon-oxygen materials with different capacities and different electrochemical properties, is applied to the cathode material in a battery system, has good circulation stability, has the characteristics of high gram capacity and the like compared with the traditional cathode material of a lithium ion battery, has simple preparation process and controllable material properties, performs electrochemical property characterization on the material, has excellent electrochemical properties and the like, and is suitable for large-scale popularization and application.
Drawings
FIG. 1 is a schematic view of a resistance heating apparatus according to the present invention;
FIG. 2 is a graph showing the first lithium insertion and extraction curves of the present invention;
FIG. 3 is a graph of cycle performance of the present invention;
in the figure: 1. a cooling tower; 2. a collector; 3. a pneumatic valve; 4. a heating source; 5. a vacuum valve; 6. a silane gas reservoir.
Detailed Description
The present invention will be explained in more detail by the following examples, which are not intended to limit the invention;
the preparation method of the silicon-oxygen anode material specifically comprises the following steps:
firstly, pressing silicon dioxide by a press to form a blocky silicon dioxide cake, and then uniformly placing the blocky silicon dioxide cake in a heating zone of a resistance heating device; the silicon dioxide is nano-scale silicon dioxide powder or nano-scale silicon dioxide powder is obtained by refining and screening silicon dioxide raw materials;
secondly, heating the massive silicon dioxide cake to 1000-1500 ℃ through a resistance heating device, wherein the heating rate during heating is 10min/min, vacuumizing the cavity of the resistance heating device to ensure that the vacuum degree in the cavity is less than or equal to 50Pa, then opening a pressure reducing valve, uniformly introducing silane gas into the cavity, wherein the silane is high-purity silane gas, so that the two gases are uniformly mixed in the cavity, the temperature in the cavity is kept constant, the silane gas and the silicon dioxide are ensured to be fully contacted in the whole reaction process, and SiH is added4With SiO2SiOx is generated by reaction, and the value of X is adjusted by controlling the reaction condition; as shown in fig. 1, the resistance heating device comprises a cooling tower 1, a collector 2, a pneumatic valve 3, a heating source 4, a vacuum valve 5 and a silane gas reservoir 6, wherein the heating source 4 is arranged in a cavity, a silicon and silicon dioxide mixture is arranged in the heating source 4, the cooling tower 1 is arranged above the cavity, the collector 2 is arranged in the cooling tower 1, the vacuum valve 5 is arranged on one side of the lower part of the cavity, the pneumatic valve 3 is arranged on the other side of the lower part of the cavity, and the pneumatic valve 3 is connected with the silane gas reservoir 6 through a pipeline;
thirdly, condensing the mixture of silane and silicon dioxide gas, namely a silicon-oxygen product, at the cooling end of the resistance heating device, optimally controlling the temperature of a cooling tower of the resistance heating device in the cooling process, and condensing the mixture on the inner lining of the equipment;
fourthly, crushing the obtained silica product in any one or a combination of two or more of jaw crushing, air crushing and ball milling to obtain a micron-sized or nano-sized precursor; crushing the silica product to ensure that the silica product D50 is within the range of 2-10 um;
and fifthly, coating a layer of conductive material, generally carbon or a carbon compound, on the surface of the material, wherein the precursor is a silicon-oxygen lithium compound with poor electronic conductivity, and performing carbon coating on the precursor by adopting a liquid phase, solid phase or gas phase mode to obtain the required silicon-oxygen cathode material, wherein the liquid phase mainly uses asphalt as a carbon source, the gas phase mainly uses low-carbon alkane, alkene and alkyne as main materials, and the pyrolysis is performed at a high temperature to obtain a carbon coating layer, and the temperature during the pyrolysis is 500-1200 ℃.
The specific embodiment of the invention is as follows:
firstly, heating equipment in a resistance heating mode, wherein the heating rate is 10min/min, heating silicon and silicon dioxide to 1350 ℃, and the vacuum degree is less than or equal to 50 Pa;
further, when the temperature and the pressure of the equipment reach set values, a pressurizing valve is opened, so that silane gas enters the equipment and is uniformly mixed with silicon dioxide gas;
further, collecting a massive mixture on the substrate at the cooling end, wherein the color of the mixture is brown;
further, crushing the blocks in a ball milling mode, and grading to obtain powder with D50 of 2-10 um;
further, carrying out CVD coating on the obtained powder to obtain a material with a surface coated with a compact carbon layer, wherein the carbon content is 1-10%;
further, preparing an electrode for the obtained material, and evaluating the electrochemical performance and the cycle performance of the material;
the negative electrode material prepared by the invention is subjected to electrode preparation, a scraper is used for uniformly coating the mixture of AM, SP, CMC and SBR in a certain proportion on a copper foil current collector, then an electrode piece is obtained by vacuum baking, the electrode piece is prepared by cutting and rolling processes, a button cell is prepared by the electrode piece and metal lithium for electrochemical performance characterization, electrolyte adopts 1.0Mol/L LiPF6, the solvent composition is EC, EMC =3:7, and 5% of FEC is added into the electrolyte to serve as a film forming additive.
Then, the battery was discharged to 0.005V at 0.1C and then to 0.005V at 0.05C to obtain a first lithium intercalation capacity, and charged to 1.5V at 0.1C to obtain a first lithium deintercalation capacity.
First efficiency = first delithiation capacity/first lithium insertion capacity × 100%
And meanwhile, carrying out cycle performance test on the battery and analyzing the electrochemical performance.
FIG. 2 is the first charging and discharging curve of the material, and the first lithium intercalation is 2180mAh/g and the first lithium deintercalation is 1635mAh/g according to the test data; the efficiency of the material is 75%;
FIG. 3 shows the cycle performance test results of the material, from which it can be seen that the material has capacity retention rate of 99.6% and excellent electrochemical performance after 20 weeks of cycle;
the silicon-oxygen compound ratio obtained by the method and the conventional disproportionation reaction can obtain raw materials with different silicon-oxygen ratios by controlling the amount of the two gases, and can controllably prepare silicon-oxygen materials with different capacities and different electrochemical properties.
The present invention is not described in detail in the prior art.
The embodiments selected for the purpose of disclosing the invention, are presently considered to be suitable, it being understood, however, that the invention is intended to cover all variations and modifications of the embodiments which fall within the spirit and scope of the invention.
Claims (10)
1. A preparation method of a silicon-oxygen negative electrode material is characterized by comprising the following steps: the preparation method specifically comprises the following steps:
firstly, pressing silicon dioxide to form a blocky silicon dioxide cake, and then uniformly placing the blocky silicon dioxide cake in a heating zone of a resistance heating device;
secondly, heating the massive silicon dioxide cake to 1000-1500 ℃, vacuumizing the cavity of the resistance heating device to ensure that the vacuum degree in the cavity is less than or equal to 50Pa, then uniformly introducing silane gas into the cavity to keep the temperature in the cavity constant, ensuring that the silane gas is fully contacted with the silicon dioxide and SiH in the whole reaction process4With SiO2SiOx is generated by reaction, and the value of X is adjusted by controlling the reaction condition;
thirdly, condensing at a cooling end of the resistance heating device to obtain a silica product;
fourthly, crushing the obtained silica product to obtain a micron-scale or nano-scale precursor;
and fifthly, carrying out carbon coating on the precursor in a liquid phase, solid phase or gas phase mode to obtain the required silicon-oxygen cathode material.
2. The method for preparing a silicon-oxygen anode material according to claim 1, wherein the method comprises the following steps: in the first step, the silicon dioxide is nano-scale silicon dioxide powder or the nano-scale silicon dioxide powder is obtained by refining and screening silicon dioxide raw materials.
3. The method for preparing a silicon-oxygen anode material according to claim 1, wherein the method comprises the following steps: resistance heating device includes cooling tower (1), collector (2), atmospheric pressure valve (3), heating source (4), vacuum valve (5) and silane gas reservoir (6) in the second step, heating source (4) set up in the cavity, are equipped with silicon and silica mixture in heating source (4), are equipped with cooling tower (1) on the cavity be equipped with collector (2) in cooling tower (1), be equipped with vacuum valve (5) in one side of cavity lower part, be equipped with atmospheric pressure valve (3) at the opposite side of cavity lower part, silane gas reservoir (6) are connected through the pipeline in atmospheric pressure valve (3).
4. The method for preparing a silicon-oxygen anode material according to claim 1, wherein the method comprises the following steps: and the silane in the second step is high-purity silane gas.
5. The method for preparing a silicon-oxygen anode material according to claim 1, wherein the method comprises the following steps: the heating rate during heating in the second step is 10 min/min.
6. The method for preparing a silicon-oxygen anode material according to claim 1, wherein the method comprises the following steps: and in the fourth step, the silicon oxide product is crushed by any one or a combination of two or more of jaw crushing, gas crushing and ball milling.
7. The method for preparing a silicon-oxygen anode material according to claim 1, wherein the method comprises the following steps: and in the fourth step, after the silicon oxide product is crushed, the silicon oxide product D50 is within the range of 2-10 um.
8. The method for preparing a silicon-oxygen anode material according to claim 1, wherein the method comprises the following steps: and in the fifth step, the liquid phase mainly takes asphalt as a carbon source.
9. The method for preparing a silicon-oxygen anode material according to claim 1, wherein the method comprises the following steps: and in the fifth step, the gas phase mainly takes alkane, alkene and alkyne with low carbon content as main materials, and the pyrolysis is carried out at high temperature to obtain the carbon coating.
10. The method for preparing a silicon-oxygen anode material according to claim 9, wherein the method comprises the following steps: the temperature during pyrolysis is 500-1200 ℃.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113184858A (en) * | 2021-04-27 | 2021-07-30 | 郑州市博卓科技有限公司 | Silicon-oxygen negative electrode material composition and preparation method thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102255082A (en) * | 2010-05-21 | 2011-11-23 | 信越化学工业株式会社 | Silicon oxide material, making method, negative electrode, lithium ion secondary battery, and electrochemical capacitor |
| CN103647056A (en) * | 2013-11-29 | 2014-03-19 | 深圳市贝特瑞新能源材料股份有限公司 | SiOx based composite negative electrode material, preparation method and battery |
| CN104638237A (en) * | 2015-01-20 | 2015-05-20 | 深圳市贝特瑞新能源材料股份有限公司 | Lithium ion battery SiO composite material as well as preparation method and application thereof |
| CA2835583A1 (en) * | 2013-11-28 | 2015-05-28 | Hydro-Quebec | Preparation method for an siox nano-structure and its use as anode for a lithium-ion battery |
| CN110311118A (en) * | 2019-07-10 | 2019-10-08 | 洛阳联创锂能科技有限公司 | Disproportionated SiOx material for lithium ion battery and preparation method thereof |
-
2020
- 2020-03-24 CN CN202010210380.7A patent/CN111377452A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102255082A (en) * | 2010-05-21 | 2011-11-23 | 信越化学工业株式会社 | Silicon oxide material, making method, negative electrode, lithium ion secondary battery, and electrochemical capacitor |
| CA2835583A1 (en) * | 2013-11-28 | 2015-05-28 | Hydro-Quebec | Preparation method for an siox nano-structure and its use as anode for a lithium-ion battery |
| CN103647056A (en) * | 2013-11-29 | 2014-03-19 | 深圳市贝特瑞新能源材料股份有限公司 | SiOx based composite negative electrode material, preparation method and battery |
| CN104638237A (en) * | 2015-01-20 | 2015-05-20 | 深圳市贝特瑞新能源材料股份有限公司 | Lithium ion battery SiO composite material as well as preparation method and application thereof |
| CN110311118A (en) * | 2019-07-10 | 2019-10-08 | 洛阳联创锂能科技有限公司 | Disproportionated SiOx material for lithium ion battery and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 潘红娜等: "《晶体硅太阳能电池制备技术》", 31 October 2017, 北京邮电大学出版社 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113184858A (en) * | 2021-04-27 | 2021-07-30 | 郑州市博卓科技有限公司 | Silicon-oxygen negative electrode material composition and preparation method thereof |
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