CN116161667B - Method for preparing silicon monoxide by adding fluxing agent - Google Patents
Method for preparing silicon monoxide by adding fluxing agent Download PDFInfo
- Publication number
- CN116161667B CN116161667B CN202211097023.XA CN202211097023A CN116161667B CN 116161667 B CN116161667 B CN 116161667B CN 202211097023 A CN202211097023 A CN 202211097023A CN 116161667 B CN116161667 B CN 116161667B
- Authority
- CN
- China
- Prior art keywords
- silicon monoxide
- precursor
- fluxing agent
- powder
- uniformly mixing
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Chemical compound [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 title claims abstract description 71
- 239000003795 chemical substances by application Substances 0.000 title claims abstract description 24
- 238000000034 method Methods 0.000 title claims abstract description 17
- 239000000463 material Substances 0.000 claims abstract description 66
- 239000002243 precursor Substances 0.000 claims abstract description 37
- 238000002156 mixing Methods 0.000 claims abstract description 17
- 238000010438 heat treatment Methods 0.000 claims abstract description 16
- 239000000843 powder Substances 0.000 claims abstract description 13
- 239000007795 chemical reaction product Substances 0.000 claims abstract description 7
- 238000000151 deposition Methods 0.000 claims abstract description 3
- 239000002245 particle Substances 0.000 claims description 16
- 238000006243 chemical reaction Methods 0.000 claims description 11
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 10
- 239000011863 silicon-based powder Substances 0.000 claims description 10
- 229910004261 CaF 2 Inorganic materials 0.000 claims description 4
- 229910001610 cryolite Inorganic materials 0.000 claims description 4
- 238000002360 preparation method Methods 0.000 abstract description 10
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 abstract description 3
- 239000010406 cathode material Substances 0.000 abstract description 3
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 229910001416 lithium ion Inorganic materials 0.000 abstract description 3
- 229910000851 Alloy steel Inorganic materials 0.000 abstract description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 19
- 229910021417 amorphous silicon Inorganic materials 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 5
- 238000009833 condensation Methods 0.000 description 5
- 230000005494 condensation Effects 0.000 description 5
- 239000000377 silicon dioxide Substances 0.000 description 5
- 229910052681 coesite Inorganic materials 0.000 description 4
- 229910052906 cristobalite Inorganic materials 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 229910052682 stishovite Inorganic materials 0.000 description 4
- 229910052905 tridymite Inorganic materials 0.000 description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 3
- 229910052802 copper Inorganic materials 0.000 description 3
- 239000010949 copper Substances 0.000 description 3
- 239000007773 negative electrode material Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- OIFBSDVPJOWBCH-UHFFFAOYSA-N Diethyl carbonate Chemical compound CCOC(=O)OCC OIFBSDVPJOWBCH-UHFFFAOYSA-N 0.000 description 2
- KMTRUDSVKNLOMY-UHFFFAOYSA-N Ethylene carbonate Chemical compound O=C1OCCO1 KMTRUDSVKNLOMY-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 238000007792 addition Methods 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- -1 polypropylene Polymers 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 239000006245 Carbon black Super-P Substances 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 238000005280 amorphization Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 238000005056 compaction Methods 0.000 description 1
- 239000006258 conductive agent Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000007770 graphite material Substances 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000012982 microporous membrane Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 238000004080 punching Methods 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 229910001868 water Inorganic materials 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Classifications
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Silicon Compounds (AREA)
Abstract
The invention relates to a method for preparing silicon monoxide by adding a fluxing agent, which belongs to the technical field of silicon monoxide preparation and comprises the following steps: firstly, carrying out a molar ratio of S i powder to S i O 2 powder of 1:1, uniformly mixing to obtain a precursor I material; secondly, adding a fluxing agent into the precursor I material, and uniformly mixing to obtain a precursor II material; and thirdly, placing the precursor II material in a vacuum heating furnace, and depositing, condensing and collecting the precursor II material to obtain a reaction product, namely silicon monoxide. The invention can finish the preparation of silicon monoxide at a lower temperature, greatly reduces the requirements on equipment, adopts the heating tank body which is made of common alloy steel, and has low energy consumption, low cost and wide material sources. Meanwhile, when the prepared silicon monoxide material is used as a cathode material for the field of the cathode material of the emerging lithium ion battery, the prepared silicon monoxide material has the advantages of high first charge capacity, high first charge and discharge efficiency, good cycle performance and small volume expansion.
Description
Technical Field
The invention belongs to the technical field of silicon monoxide preparation, and particularly relates to a method for preparing silicon monoxide by adding a fluxing agent.
Background
The silicon monoxide material can be used as a lithium ion battery cathode material, has high application value, has the initial discharge specific capacity of 2200-2500mAh/g, is more than 5 times of that of the traditional graphite material, has a unique microscopic crystal structure, has small volume expansion in the charge and discharge process, and can greatly improve the battery energy density.
The preparation of silicon monoxide involves mainly the following reactions:
SiO2+H2→SiO+H2O (1)
SiO2+C→SiO+CO (2)
SiO2+SiC→2SiO+C (3)
SiO2+Si→2SiO (4)
The method for preparing the silicon monoxide by the reaction (4) is more applicable in consideration of the factors such as the actual industrialized preparation difficulty, cost and the like, and is the most common method for preparing and obtaining the silicon monoxide in the industry. The method comprises the steps of mixing Si and SiO 2 powder according to a ratio of 1:1 (molar ratio) and heating the mixture for 4 hours at 1300-1500 ℃ under the vacuum condition of 10 -4 torr (1 torr=133.3 Pa) to react, and condensing and separating out the product at the other end with lower temperature to obtain silicon monoxide.
Chinese patent CN108199031a discloses a highly amorphous silicon monoxide material, a preparation method and use thereof, and the reaction period is shortened by adding a nucleation additive in the preparation process, which increases the amorphization degree of the silicon monoxide material, but requires higher reaction temperature and reaction equipment. Great difficulty is brought to the selection of industrial high-temperature-resistant materials and equipment in a high-vacuum environment.
Disclosure of Invention
The invention aims to provide a method for preparing silicon monoxide by adding fluxing agent, which solves the problems in the prior art.
The aim of the invention can be achieved by the following technical scheme:
A method for preparing silicon monoxide by adding fluxing agent, comprising the following steps:
in the first step, si powder and SiO 2 powder are mixed according to a mol ratio of 1:1, uniformly mixing to obtain a precursor I material;
Secondly, adding a fluxing agent into the precursor I material, and uniformly mixing to obtain a precursor II material;
And thirdly, placing the precursor II material in a vacuum heating furnace, and depositing, condensing and collecting the precursor II material to obtain a reaction product, namely silicon monoxide.
Further, the median particle diameter of the Si powder was 325 mesh, and the median particle diameter of the SiO 2 powder was 325 mesh.
Further, the fluxing agent is one of CaF 2 and cryolite.
Further, the addition amount of the fluxing agent is 3-10% of the mass of the precursor I material.
Further, the vacuum degree in the vacuum heating furnace is controlled to be less than 10Pa, the temperature of the heating area is 1050-1250 ℃, and the reaction is carried out for 12-24 hours.
Further, the condensation collection end temperature is < 750 ℃.
The invention has the beneficial effects that:
Aiming at the improvement of the prior art that the temperature is required to be higher and the industrialized preparation condition is larger, one of the purposes of the preparation method is to provide a method for preparing silicon monoxide material by adding fluxing agent. The fluxing agent is added into the raw materials, the temperature of the reaction substances is reduced when the raw materials are heated, the reaction substances are prepared to react at a lower temperature, the equipment requirement in the whole reaction process is reduced, the energy consumption is reduced, the cost is reduced, the added fluxing agent is not required to be removed, the fluxing agent cannot sublimate at the temperature (can be left in a heating area), and silicon dioxide can become gases to be collected in a cooling area, so that the treatment is simple.
The invention can finish the preparation of silicon monoxide at a lower temperature, greatly reduces the requirements on equipment, adopts the heating tank body which is made of common alloy steel, and has low energy consumption, low cost and wide material sources. Meanwhile, when the prepared silicon monoxide material is used as a negative electrode material for the field of the negative electrode materials of the emerging lithium ion batteries, the prepared silicon monoxide material has the advantages of high first charge capacity, high first charge and discharge efficiency (first discharge capacity/first charge capacity), good cycle performance (high capacity maintenance rate after cycle) and small volume expansion.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are needed for the description of the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
Figure 1 is an XRD pattern of the product prepared in example 1 of the present invention.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
In the first step, si powder with a median particle diameter (D50) of 325 meshes and SiO 2 powder with a median particle diameter (D50) of 325 meshes are mixed according to a mol ratio of 1:1, uniformly mixing the materials in proportion to obtain a precursor I material;
Secondly, adding 3% of CaF 2 into the precursor I material, and uniformly mixing to obtain a precursor II material;
And thirdly, adding the precursor II material into vacuum furnace equipment, controlling the vacuum degree in the vacuum furnace to be less than 10Pa, the temperature of a heating area to be 1100 ℃, reacting for 15 hours, and controlling the temperature of a condensation collecting end to be less than 500 ℃ to obtain a reaction product, namely the amorphous silicon monoxide material, wherein the yield is more than 85%. When the obtained product was tested, the XRD pattern of the product prepared in example 1 is shown in fig. 1, and it can be seen from fig. 1 that silicon monoxide is amorphous and has no distinct characteristic peaks.
Example 2
In the first step, si powder with a median particle diameter (D50) of 325 meshes and SiO 2 powder with a median particle diameter (D50) of 325 meshes are mixed according to a mol ratio of 1:1, uniformly mixing the materials in proportion to obtain a precursor I material;
Secondly, adding 3% of CaF 2 into the precursor I material, and uniformly mixing to obtain a precursor II material;
And thirdly, adding the precursor II material into vacuum furnace equipment, controlling the vacuum degree in the vacuum furnace to be less than 10Pa, the temperature of a heating area to be 1200 ℃, reacting for 15 hours, and controlling the temperature of a condensation collecting end to be less than 500 ℃ to obtain a reaction product, namely the amorphous silicon monoxide material, wherein the yield is more than 85%.
Example 3
In the first step, si powder with a median particle diameter (D50) of 325 meshes and SiO 2 powder with a median particle diameter (D50) of 325 meshes are mixed according to a mol ratio of 1:1, uniformly mixing the materials in proportion to obtain a precursor I material;
Secondly, adding 3% cryolite into the precursor I material, and uniformly mixing to obtain a precursor II material;
And thirdly, adding the precursor II material into vacuum furnace equipment, controlling the vacuum degree in the vacuum furnace to be less than 10Pa, the temperature of a heating area to be 1050 ℃, reacting for 24 hours, and controlling the temperature of a condensation collecting end to be less than 750 ℃ to obtain a reaction product, namely the amorphous silicon monoxide material, wherein the yield is more than 85%.
Example 4
In the first step, si powder with a median particle diameter (D50) of 325 meshes and SiO 2 powder with a median particle diameter (D50) of 325 meshes are mixed according to a mol ratio of 1:1, uniformly mixing the materials in proportion to obtain a precursor I material;
Secondly, adding 3% cryolite into the precursor I material, and uniformly mixing to obtain a precursor II material;
And thirdly, adding the precursor II material into vacuum furnace equipment, controlling the vacuum degree in the vacuum furnace to be less than 10Pa, the temperature of a heating area to be 1250 ℃, reacting for 12 hours, and controlling the temperature of a condensation collecting end to be less than 750 ℃ to obtain a reaction product, namely the amorphous silicon monoxide material, wherein the yield is more than 85%.
Comparative example 1
In the first step, si powder with a median particle diameter (D50) of 325 meshes and SiO 2 powder with a median particle diameter (D50) of 325 meshes are mixed according to a mol ratio of 1:1, uniformly mixing the materials in proportion to obtain a precursor I material;
And secondly, adding the precursor I material into vacuum furnace equipment, controlling the vacuum degree in the vacuum furnace to be less than 10Pa, controlling the temperature of a heating area to be 1100 ℃, and reacting for 15 hours, wherein the material is not changed.
Comparative example 2
In the first step, si powder with a median particle diameter (D50) of 325 meshes and SiO 2 powder with a median particle diameter (D50) of 325 meshes are mixed according to a mol ratio of 1:1, uniformly mixing the materials in proportion to obtain a precursor I material;
and thirdly, adding the precursor I material into vacuum furnace equipment, controlling the vacuum degree in the vacuum furnace to be less than 10Pa, and reacting for 15 hours at the temperature of 1200 ℃ without changing the material.
Comparative example 3
The second step was not performed as compared to example 3, and the material was unchanged.
Comparative example 4
The second step was not performed as compared to example 4, and the material was unchanged.
As can be seen from the comparison of examples 1-4 and comparative examples 1-4, the materials are not changed at 1050-1250 ℃ under the same conditions of other steps without adding any fluxing agent, and compared with the fluxing agent, the temperature of the raw materials for reaction can be reduced, the difficulty of preparing silicon monoxide materials in large quantities in industry is greatly improved, and the advantages of strong in equipment, process and cost are achieved.
Example 5
The silicon oxide prepared in example 1 was used as a negative electrode material, and was mixed with a binder CMC+SRB and a conductive agent (Super-P) according to 80:5:5:10, adding a proper amount of deionized water as a dispersing agent to prepare slurry, coating the slurry on a copper box with the diameter of 9 mu m by using a coating machine, drying the copper box at the temperature of 90 ℃ in vacuum (-0.1 MPa) for 6 hours, rolling the copper box, controlling the compaction density to be 1.20g/cm 3, preparing a wafer with the diameter of 13mm by using a punching machine, weighing and calculating the weight of active substances. Assembled into a CR2430 button cell in a glove box, a metal lithium sheet is taken as a counter electrode, a polypropylene microporous membrane is taken as a diaphragm, and lmol/LLiPF 6 (lithium hexafluorophosphate) is dissolved in a volume ratio of 1: EC (ethylene carbonate) and DEC (diethyl carbonate) of 1. The battery is kept stand for 12 hours at room temperature, then is subjected to constant current charge and discharge test on a blue electric test system, is discharged to 0.005V at 0.1C, and is charged to 1.5V at 0.1C to perform the test of the first reversible specific capacity and the first efficiency.
Obtaining the first charge specific capacity: 1524.5mAh/g; first effect: 65.4%.
In the description of the present specification, the descriptions of the terms "one embodiment," "example," "specific example," and the like, mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present invention. In this specification, schematic representations of the above terms do not necessarily refer to the same embodiments or examples. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The foregoing is merely illustrative and explanatory of the principles of the invention, as various modifications and additions may be made to the specific embodiments described, or similar thereto, by those skilled in the art, without departing from the principles of the invention or beyond the scope of the appended claims.
Claims (5)
1. A method for preparing silicon monoxide by adding fluxing agent, which is characterized by comprising the following steps:
in the first step, si powder and SiO 2 powder are mixed according to a mol ratio of 1:1, uniformly mixing to obtain a precursor I material;
Secondly, adding a fluxing agent into the precursor I material, and uniformly mixing to obtain a precursor II material; the fluxing agent is one of CaF 2 and cryolite;
And thirdly, placing the precursor II material in a vacuum heating furnace, and depositing, condensing and collecting the precursor II material to obtain a reaction product, namely silicon monoxide.
2. A method for preparing silicon monoxide by adding a fluxing agent according to claim 1, wherein the median particle size of the Si powder is 325 mesh and the median particle size of the Si O 2 powder is 325 mesh.
3. A method for preparing silicon monoxide by adding a fluxing agent according to claim 1, wherein the amount of fluxing agent added is 3-10% of the mass of the precursor i material.
4. The method for preparing silicon monoxide by adding fluxing agent according to claim 1, wherein the vacuum degree in the vacuum heating furnace is controlled to be less than 10Pa, the temperature of the heating area is 1050-1250 ℃, and the reaction is carried out for 12-24 hours.
5. A method for preparing silicon monoxide by adding a fluxing agent according to claim 1, wherein the condensing tip temperature is less than 750 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211097023.XA CN116161667B (en) | 2022-09-08 | 2022-09-08 | Method for preparing silicon monoxide by adding fluxing agent |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211097023.XA CN116161667B (en) | 2022-09-08 | 2022-09-08 | Method for preparing silicon monoxide by adding fluxing agent |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN116161667A CN116161667A (en) | 2023-05-26 |
| CN116161667B true CN116161667B (en) | 2024-05-31 |
Family
ID=86418868
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202211097023.XA Active CN116161667B (en) | 2022-09-08 | 2022-09-08 | Method for preparing silicon monoxide by adding fluxing agent |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN116161667B (en) |
Citations (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2823979A (en) * | 1954-05-28 | 1958-02-18 | Goodrich Co B F | Method of making pigment |
| RU2207979C1 (en) * | 2001-10-18 | 2003-07-10 | Восточно-Сибирский государственный технологический университет | Method and apparatus for producing silicon monoxide |
| JP2005225691A (en) * | 2004-02-10 | 2005-08-25 | Nippon Steel Corp | METHOD AND APPARATUS FOR MANUFACTURING HIGH PURITY SiO SOLID |
| CN101139095A (en) * | 2006-04-24 | 2008-03-12 | 信越化学工业株式会社 | Method for producing silicon oxide powder |
| KR20080076075A (en) * | 2007-02-14 | 2008-08-20 | 삼성에스디아이 주식회사 | Anode active material, method of preparing the same, anode and lithium battery containing the material |
| EP2130585A1 (en) * | 2008-06-06 | 2009-12-09 | Total Petrochemicals Research Feluy | Process for making crystalline metallosilicates |
| CN103987660A (en) * | 2012-11-30 | 2014-08-13 | Lg化学株式会社 | Silicon oxide, and method for preparing same |
| CN204162438U (en) * | 2014-10-18 | 2015-02-18 | 李绍光 | A kind of fluidized-bed reactor producing silicon monoxide |
| WO2015037462A1 (en) * | 2013-09-12 | 2015-03-19 | コニカミノルタ株式会社 | Production method for silicon oxide sintered body, and silicon oxide sintered body |
| CN107640774A (en) * | 2017-10-27 | 2018-01-30 | 北方民族大学 | A kind of method for preparing SiO powder |
| KR20200134476A (en) * | 2019-05-22 | 2020-12-02 | 충북대학교 산학협력단 | Preparation Method of Porous Si for anode material of lithium-ion battery |
| CN112054180A (en) * | 2020-08-24 | 2020-12-08 | 湖南宸宇富基新能源科技有限公司 | Low-oxygen-content porous silicon composite powder material and preparation and application thereof |
| CN114057201A (en) * | 2021-11-23 | 2022-02-18 | 安徽科达新材料有限公司 | Device and method for preparing powdered silicon monoxide |
| CN114180585A (en) * | 2021-11-30 | 2022-03-15 | 长沙矿冶研究院有限责任公司 | Method and device for preparing high-purity silicon monoxide in batches |
| CN114351447A (en) * | 2022-01-21 | 2022-04-15 | 辽宁科技大学 | Preparation method for in-situ growth of cubic silicon carbide fiber on carbon fiber |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108793169A (en) * | 2017-03-27 | 2018-11-13 | 储晞 | A kind of square law device and system recycling Buddha's warrior attendant wire cutting silicon material by-product silicon mud |
-
2022
- 2022-09-08 CN CN202211097023.XA patent/CN116161667B/en active Active
Patent Citations (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2823979A (en) * | 1954-05-28 | 1958-02-18 | Goodrich Co B F | Method of making pigment |
| RU2207979C1 (en) * | 2001-10-18 | 2003-07-10 | Восточно-Сибирский государственный технологический университет | Method and apparatus for producing silicon monoxide |
| JP2005225691A (en) * | 2004-02-10 | 2005-08-25 | Nippon Steel Corp | METHOD AND APPARATUS FOR MANUFACTURING HIGH PURITY SiO SOLID |
| CN101139095A (en) * | 2006-04-24 | 2008-03-12 | 信越化学工业株式会社 | Method for producing silicon oxide powder |
| KR20080076075A (en) * | 2007-02-14 | 2008-08-20 | 삼성에스디아이 주식회사 | Anode active material, method of preparing the same, anode and lithium battery containing the material |
| EP2130585A1 (en) * | 2008-06-06 | 2009-12-09 | Total Petrochemicals Research Feluy | Process for making crystalline metallosilicates |
| CN103987660A (en) * | 2012-11-30 | 2014-08-13 | Lg化学株式会社 | Silicon oxide, and method for preparing same |
| WO2015037462A1 (en) * | 2013-09-12 | 2015-03-19 | コニカミノルタ株式会社 | Production method for silicon oxide sintered body, and silicon oxide sintered body |
| CN204162438U (en) * | 2014-10-18 | 2015-02-18 | 李绍光 | A kind of fluidized-bed reactor producing silicon monoxide |
| CN107640774A (en) * | 2017-10-27 | 2018-01-30 | 北方民族大学 | A kind of method for preparing SiO powder |
| KR20200134476A (en) * | 2019-05-22 | 2020-12-02 | 충북대학교 산학협력단 | Preparation Method of Porous Si for anode material of lithium-ion battery |
| CN112054180A (en) * | 2020-08-24 | 2020-12-08 | 湖南宸宇富基新能源科技有限公司 | Low-oxygen-content porous silicon composite powder material and preparation and application thereof |
| CN114057201A (en) * | 2021-11-23 | 2022-02-18 | 安徽科达新材料有限公司 | Device and method for preparing powdered silicon monoxide |
| CN114180585A (en) * | 2021-11-30 | 2022-03-15 | 长沙矿冶研究院有限责任公司 | Method and device for preparing high-purity silicon monoxide in batches |
| CN114351447A (en) * | 2022-01-21 | 2022-04-15 | 辽宁科技大学 | Preparation method for in-situ growth of cubic silicon carbide fiber on carbon fiber |
Non-Patent Citations (1)
| Title |
|---|
| Na3AlF6－SiO2熔盐中Si的电化学行为;何林等人;武汉客家大学学报;20211231;423-428页 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN116161667A (en) | 2023-05-26 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| JP7288059B2 (en) | Silicon-oxygen composite negative electrode material, its preparation method and lithium ion battery | |
| CN113104824B (en) | Se doped Fe 2 Preparation method of P self-supporting sodium ion battery cathode material | |
| CN113526483B (en) | Ferro-phosphorus sodalite type cathode material and preparation method and application thereof | |
| CN111009647B (en) | Lithium borosilicate alloy cathode active material of lithium secondary battery, cathode, preparation and application thereof | |
| CN113479860B (en) | SbPO (styrene-ethylene-propylene-diene monomer) 4 Preparation method of nitrogen-doped carbon composite material | |
| CN107732164B (en) | Mesoporous crystalline Si-amorphous SiO for sodium ion battery2Preparation method and application of ordered mesoporous carbon composite material | |
| CN114665058A (en) | Preparation method of lithium ion battery anode material lithium iron manganese phosphate | |
| CN110589791A (en) | Preparation method of tin-doped titanium pyrophosphate | |
| CN115954443B (en) | Preparation method of carbon-coated silicon-copper alloy negative electrode material of lithium ion battery | |
| CN110336003A (en) | A kind of porous silicon-base composite material and preparation method and application | |
| CN111470487A (en) | Preparation method and application of biomass carbon material | |
| JP2023548993A (en) | Method for producing high-rate lithium iron phosphate cathode material | |
| CN114275762B (en) | Nitrogen-doped hard carbon sodium ion battery anode material and preparation method thereof | |
| CN114171729A (en) | Preparation method of graphene-based lithium iron phosphate positive electrode material | |
| CN116314622B (en) | Single crystal cobalt-free aluminum doped lithium nickelate positive electrode material with self-precipitation coating layer, and preparation method and application thereof | |
| CN116730310A (en) | Method for preparing lithium ion battery anode material lithium iron manganese phosphate | |
| CN116161667B (en) | Method for preparing silicon monoxide by adding fluxing agent | |
| CN108075127B (en) | Nickel-phosphorus-based sodium ion battery cathode composite material and preparation method and application thereof | |
| CN113735180B (en) | Method for preparing sodium ion battery anode material by using LDH-based precursor to obtain cobalt iron sulfide | |
| CN115241436A (en) | High-first-efficiency lithium-doped silicon oxide composite negative electrode material and preparation method thereof | |
| CN108493449B (en) | Controllable preparation method of sodium manganese fluorophosphate cathode material | |
| CN111470544A (en) | Solid-phase sintering method of carbon-coated ferroferric oxide | |
| CN113140724A (en) | Method for synthesizing sodium manganate serving as cathode material of sodium-ion battery with tunnel lamellar intergrowth phase | |
| CN110518195A (en) | A kind of preparation method and application of nano-silicon/graphene composite material | |
| CN113479858B (en) | Composite material for high-performance alkali metal ion battery cathode |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |