CN113206212A - Preparation of thermal battery Fe1-xCoxF3Method for producing anode material - Google Patents
Preparation of thermal battery Fe1-xCoxF3Method for producing anode material Download PDFInfo
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- CN113206212A CN113206212A CN202110408925.XA CN202110408925A CN113206212A CN 113206212 A CN113206212 A CN 113206212A CN 202110408925 A CN202110408925 A CN 202110408925A CN 113206212 A CN113206212 A CN 113206212A
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- anode material
- thermal battery
- ball milling
- preparation
- mixing
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- 239000010405 anode material Substances 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 48
- 238000000498 ball milling Methods 0.000 claims abstract description 26
- 239000000463 material Substances 0.000 claims abstract description 17
- 238000000034 method Methods 0.000 claims abstract description 16
- 238000002156 mixing Methods 0.000 claims abstract description 16
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 14
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000000843 powder Substances 0.000 claims abstract description 11
- 229910052742 iron Inorganic materials 0.000 claims abstract description 10
- 229910052786 argon Inorganic materials 0.000 claims abstract description 7
- 238000000227 grinding Methods 0.000 claims abstract description 7
- 238000010438 heat treatment Methods 0.000 claims abstract description 7
- -1 polytetrafluoroethylene Polymers 0.000 claims abstract description 7
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims abstract description 7
- 239000004810 polytetrafluoroethylene Substances 0.000 claims abstract description 7
- 229910001220 stainless steel Inorganic materials 0.000 claims abstract description 7
- 239000010935 stainless steel Substances 0.000 claims abstract description 7
- DDFHBQSCUXNBSA-UHFFFAOYSA-N 5-(5-carboxythiophen-2-yl)thiophene-2-carboxylic acid Chemical compound S1C(C(=O)O)=CC=C1C1=CC=C(C(O)=O)S1 DDFHBQSCUXNBSA-UHFFFAOYSA-N 0.000 claims abstract description 6
- LDDQLRUQCUTJBB-UHFFFAOYSA-N ammonium fluoride Chemical compound [NH4+].[F-] LDDQLRUQCUTJBB-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229910017665 NH4HF2 Inorganic materials 0.000 claims abstract description 4
- 239000000203 mixture Substances 0.000 claims abstract description 4
- 238000004519 manufacturing process Methods 0.000 claims description 6
- 238000007873 sieving Methods 0.000 description 4
- 238000005303 weighing Methods 0.000 description 4
- 229910052960 marcasite Inorganic materials 0.000 description 3
- 229910052683 pyrite Inorganic materials 0.000 description 3
- 238000001035 drying Methods 0.000 description 2
- 239000000178 monomer Substances 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 230000004913 activation Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
Classifications
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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
- H01M4/06—Electrodes for primary cells
- H01M4/08—Processes of manufacture
-
- 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
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/582—Halogenides
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M6/00—Primary cells; Manufacture thereof
- H01M6/30—Deferred-action cells
- H01M6/36—Deferred-action cells containing electrolyte and made operational by physical means, e.g. thermal 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
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/028—Positive electrodes
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Inorganic Chemistry (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
Preparation of thermal battery Fe1‑xCoxF3A method for preparing an anode material relates to a method for preparing a thermal battery, and comprises the following preparation processes: mixing Fe2O3Micropowder and CoO and/or Co (OH)2Mixing the micro powder according to a ratio, placing the mixture into a polytetrafluoroethylene ball milling tank, adding an ammonium fluoride solution, then adding an iron ball for ball milling, taking the material out of the ball milling tank, placing the material into a stainless steel container, heating to the temperature of 700 ℃ and 750 ℃ under the protection of argon, and preserving the temperature for 2-3.5 hours to prepare Fe1‑xCoxF3. Anode material Fe1‑xCoxF3Middle, 0.01<x<0.1. The ammonium fluoride comprises NH4F and NH4HF2；Fe2O3Micro powderAnd CoO and/or Co (OH)2The granularity of the micro powder is sieved by a 325-mesh sieve. Adding iron grinding balls and ball milling for 2-10 hours. Fe prepared by the invention1‑xCoxF3The anode material has simple process and low cost, and can obviously improve the power of the thermal battery.
Description
Technical Field
The invention relates to a method for preparing a thermal battery material, in particular to a method for preparing thermal battery Fe1-xCoxF3A method of anode material.
Background
The thermal battery has the advantages of high output energy, long storage life, no maintenance in the storage period, quick activation, compact structure and the like, becomes a preferred power supply of intelligent ammunition, and is widely applied to power supply systems of military equipment such as missiles, artillery, nuclear weapons and the like.
Along with the development of national defense technology and sophisticated weapons, smart ammunition capable of realizing accurate striking is more and more highly valued. The actual combat results show that: compared with common ammunition, the operational efficiency of intelligent ammunition can be improved by 1000 times and the efficiency-cost ratio can be improved by 30-40 times, so that new challenges are faced to a thermal battery known as 'intelligent ammunition heart', some remote intelligent ammunition systems require the thermal battery to have a working life of dozens of minutes or even hours, and the research on the thermal battery with long service life is more and more urgent.
FeS2Is the anode material which is most widely applied in the thermal battery at present, FeS2The composite material has low cost and good comprehensive performance, is the most mature anode material of a thermal battery, but FeS2The voltage of the monomer is less than 2V, the thermal decomposition temperature is 550 ℃, and the thermal resistance is high, so that the monomer is not suitable for a thermal battery with high power and long working time.
Disclosure of Invention
The invention aims to provide a method for preparing Fe of a thermal battery1-xCoxF3Method for producing anode material, the invention is Fe2O3Micropowder and CoO and/or Co (OH)2Mixing the micro powder, adding NH4F solution, ball milling, drying and deaminizing to prepare Fe1-xCoxF3An anode material. Prepared Fe1-xCoxF3The anode material has simple process and low cost, and can obviously improve the power of the thermal battery.
The purpose of the invention is realized by the following technical scheme:
preparation of thermal battery Fe1-xCoxF3A method of preparing an anode material, the method comprising the steps of:
mixing Fe2O3Micropowder andCoO and/or Co (OH)2Mixing the micro powder according to a ratio, placing the mixture into a polytetrafluoroethylene ball milling tank, adding an ammonium fluoride solution, then adding an iron ball for ball milling, taking the material out of the ball milling tank, placing the material into a stainless steel container, heating to the temperature of 700 ℃ and 750 ℃ under the protection of argon, and preserving the temperature for 2-3.5 hours to prepare Fe1-xCoxF3。
The preparation of the thermal battery Fe1-xCoxF3Method for producing anode material, said anode material Fe1-xCoxF3Middle, 0.01<x<0.1。
The preparation of the thermal battery Fe1-xCoxF3A method of making an anode material, said ammonium fluoride comprising NH4F and NH4HF2。
The preparation of the thermal battery Fe1-xCoxF3Method of anode material, said Fe2O3Micropowder and CoO and/or Co (OH)2The granularity of the micro powder is sieved by a 325-mesh sieve.
The preparation of the thermal battery Fe1-xCoxF3The method of the anode material comprises the step of adding an iron grinding ball for ball milling for 2-10 hours.
The invention has the advantages and effects that:
in the invention, Fe2O3Micropowder and CoO and/or Co (OH)2Mixing the micro powder, adding NH4F solution, ball milling, drying and deaminizing to prepare Fe1-xCoxF3An anode material. Prepared Fe1-xCoxF3The anode material has simple process and low cost, and can obviously improve the power of the thermal battery.
Detailed Description
The present invention will be described in detail with reference to examples.
Example 1
Mixing Fe2O3Sieving the micro powder and the CoO micro powder with a 325-mesh sieve, weighing a certain mass of micro powder according to the molar ratio of 9:1, mixing, placing in a polytetrafluoroethylene ball milling tank, adding NH4Adding the solution F into an iron grinding ball to perform ball milling for 10 hoursTaking the materials out of the ball milling tank, putting the materials into a stainless steel container, heating the materials to a certain temperature of 700 ℃ under the protection of argon, and preserving the heat for 3.5 hours to prepare Fe0.9Co0.1F3An anode material.
Example 2
Mixing Fe2O3Micropowder and Co (OH)2Sieving the micropowder with a 325 mesh sieve, weighing a certain mass of micropowder according to the proportion of the mol number of 99:1, mixing, placing the mixture in a polytetrafluoroethylene ball milling tank, adding NH4HF2Adding an iron grinding ball into the solution, ball-milling the solution for 2 hours, taking the material out of a ball-milling tank, putting the material into a stainless steel container, heating the material to a certain temperature of 700 DEG and 750 ℃ under the protection of argon, and preserving the heat for 2 hours to prepare Fe0.99Co0.01F3An anode material.
Example 3
Mixing Fe2O3Micropowder and Co (OH)2Sieving the micropowder with a 325-mesh sieve, weighing a certain mass of micropowder according to the molar ratio of 95:5, mixing, placing in a polytetrafluoroethylene ball milling tank, adding NH4Adding an iron grinding ball into the solution F, carrying out ball milling for 6 hours, taking the material out of a ball milling tank, putting the material into a stainless steel container, heating to a certain temperature of 700 ℃ under the protection of argon, and carrying out heat preservation for 3 hours to prepare Fe0.95Co0.05F3An anode material.
Example 4
Mixing Fe2O3Micropowder and Co (OH)2Sieving the micropowder with a 325 mesh sieve, weighing a certain mass of micropowder according to the molar ratio of 98:2, mixing, placing in a polytetrafluoroethylene ball milling tank, adding NH4Adding an iron grinding ball into the solution F, carrying out ball milling for 6 hours, taking the material out of a ball milling tank, putting the material into a stainless steel container, heating to a certain temperature of 700 ℃ under the protection of argon, and carrying out heat preservation for 3 hours to prepare Fe0.98Co0.02F3An anode material.
Claims (5)
1. Preparation of thermal battery Fe1-xCoxF3A method of preparing an anode material, comprising the steps of:
mixing Fe2O3Micropowder and CoO and/or Co (OH)2Mixing the micro powder according to a ratio, placing the mixture into a polytetrafluoroethylene ball milling tank, adding an ammonium fluoride solution, then adding an iron ball for ball milling, taking the material out of the ball milling tank, placing the material into a stainless steel container, heating to the temperature of 700 ℃ and 750 ℃ under the protection of argon, and preserving the temperature for 2-3.5 hours to prepare Fe1-xCoxF3。
2. Preparation of a thermal battery Fe according to claim 11-xCoxF3Method for producing an anode material, characterized in that the anode material is Fe1-xCoxF3Middle, 0.01<x<0.1。
3. Preparation of a thermal battery Fe according to claim 11-xCoxF3Method for producing an anode material, characterized in that said ammonium fluoride comprises NH4F and NH4HF2。
4. Preparation of a thermal battery Fe according to claim 11-xCoxF3Method for producing an anode material, characterized in that said method comprises
Fe2O3Micropowder and CoO and/or Co (OH)2The granularity of the micro powder is sieved by a 325-mesh sieve.
5. Preparation of a thermal battery Fe according to claim 11-xCoxF3The method for preparing the anode material is characterized in that iron grinding balls are added for ball milling for 2-10 hours.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110408925.XA CN113206212A (en) | 2021-04-16 | 2021-04-16 | Preparation of thermal battery Fe1-xCoxF3Method for producing anode material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110408925.XA CN113206212A (en) | 2021-04-16 | 2021-04-16 | Preparation of thermal battery Fe1-xCoxF3Method for producing anode material |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN113206212A true CN113206212A (en) | 2021-08-03 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110408925.XA Pending CN113206212A (en) | 2021-04-16 | 2021-04-16 | Preparation of thermal battery Fe1-xCoxF3Method for producing anode material |
Country Status (1)
| Country | Link |
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| CN (1) | CN113206212A (en) |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102623707A (en) * | 2012-04-02 | 2012-08-01 | 湘潭大学 | Cobalt-doped carbon-coated ferric fluoride anode material and preparation method thereof |
| CN111313019A (en) * | 2020-01-19 | 2020-06-19 | 贵州梅岭电源有限公司 | Ultrahigh-power-output high-voltage positive electrode material for thermal battery |
-
2021
- 2021-04-16 CN CN202110408925.XA patent/CN113206212A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102623707A (en) * | 2012-04-02 | 2012-08-01 | 湘潭大学 | Cobalt-doped carbon-coated ferric fluoride anode material and preparation method thereof |
| CN111313019A (en) * | 2020-01-19 | 2020-06-19 | 贵州梅岭电源有限公司 | Ultrahigh-power-output high-voltage positive electrode material for thermal battery |
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