CN105977431A - Preparation method for boron nitride fiber diaphragm for lithium-system thermal battery - Google Patents
Preparation method for boron nitride fiber diaphragm for lithium-system thermal battery Download PDFInfo
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- CN105977431A CN105977431A CN201610459117.5A CN201610459117A CN105977431A CN 105977431 A CN105977431 A CN 105977431A CN 201610459117 A CN201610459117 A CN 201610459117A CN 105977431 A CN105977431 A CN 105977431A
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- boron nitride
- nitride fiber
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- barrier film
- thermal cell
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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
- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/403—Manufacturing processes of separators, membranes or diaphragms
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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
- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/409—Separators, membranes or diaphragms characterised by the material
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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
- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/409—Separators, membranes or diaphragms characterised by the material
- H01M50/431—Inorganic material
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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
- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/409—Separators, membranes or diaphragms characterised by the material
- H01M50/44—Fibrous material
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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Abstract
The invention belongs to the technical field of a battery diaphragm, and specifically relates to a preparation method for a boron nitride fiber diaphragm for a lithium-system thermal battery. Boron nitride fiber fabric is cleaned; a precursor solution is prepared; and then the boron nitride fiber fabric is subjected to immersing, drying and heat treatment. The invention creatively provides a solution immersion high-temperature conversion process to process the boron nitride fiber fabric in a compounding manner; due to the process, the electrolyte infiltration effect of the boron nitride fiber fabric is obviously improved; the electrolyte adsorption rate of the diaphragm can reach greater than 160%; in addition, the retention on the electrolyte is relatively high in the compression, vibration and battery operating process; and furthermore, the preparation process is simple, and the scale production can be achieved easily.
Description
Technical field
The invention belongs to battery diaphragm technical field, be specifically related to the preparation method of a kind of lithium system thermal cell boron nitride fiber barrier film.
Background technology
Lithium system thermal cell has that discharge current density is big, specific energy is high, specific power is high, activationary time is short, uses temperature range width
Deng prominent premium properties, there is the battery product of multiple series, in modern weapons, new-energy automobile, emergency system, underground
The fields such as high temperature mine locating power supply are successfully applied, and are the leading products of current high-temperature molten salt battery.
Lithium system thermal cell storage life requires that long-term goal was 25 years, and after battery is activated, operating temperature is more than 10 years
450℃-550℃.Barrier film is one of vitals of battery, and the positive electrode of lithium system thermal cell is lithium or lithium alloy, negative material
Mainly FeS2, electrolyte is LiCl/KCl binary system or LiCl-LiBr-KBr ternary system electrolyte.Barrier film is in this system
Directly by sulfide, electrolyte and the erosion of lithium (or lithium alloy) in battery, it is therefore desirable to diaphragm material has the most resistance to
The while of corrosive, it is necessary to there is long-life, resistant to elevated temperatures feature.The performance of barrier film has significant impact to battery performance.
The function of lithium system thermal cell barrier film is mixed the shaping piece of compacting by powder magnesium oxide and a certain proportion of electrolyte at present
Realizing, this shaping piece can suppress electrolyte flow and have preferable corrosion resistance, but mechanical strength is relatively low, in fortune
During defeated, it is easily broken off breakage, affects the life-span of battery, reliability and safety.Organic barrier film is at high temperature and has corrosion
In the environment of property oxidizable, aging speed accelerate, easily cause barrier film breakage to cause because of overheated in the battery of Effec-tive Function
Battery short circuit, affects the security performance of battery；The inorfil barrier film of high temperature resisting corrosion resisting is in high temperature corrosion environment, mechanical
Intensity and flexible, electrolyte high adsorption capacity, therefore replace magnesium oxide shaping piece and organic barrier film with inorfil barrier film,
Specific energy and the specific power of battery can be improved, improve the energy density of power-supply system, safety, reliability and working life simultaneously.
Summary of the invention
It is an object of the invention to provide the preparation method of a kind of lithium system thermal cell boron nitride fiber barrier film, technique is simple, it is easy to real
Existing large-scale production, the boron nitride fiber membrane properties of preparation is excellent.
The preparation method of lithium system of the present invention thermal cell boron nitride fiber barrier film, step is as follows:
(1) boron nitride fiber fabric cleans: is carried out boron nitride fiber fabric with ethanol, dries stand-by；
(2) precursor solution preparation: mixed with surface modifier by solvent, stirs 5-10min, then adds magnesium salt or yttrium salt,
Stirring 20-30min, it is thus achieved that precursor solution；
(3) impregnate, be dried: by molten for presoma that the boron nitride fiber fabric of step (1) gained is soaked into step (2) gained
In liquid, take out post-drying stand-by；
(4) heat treatment: the fabric after the drying of step (3) gained is carried out heat treatment in Muffle furnace；
(5) naturally it is down to room temperature when Muffle furnace, takes out sample, obtain lithium system thermal cell boron nitride fiber barrier film.
Boron nitride fiber fabric described in step (1) is boron nitride fiber felt or boron nitride fiber cloth.
Drying temperature described in step (1) is 80-100 DEG C.
Solvent described in step (2) is the one in ethanol, methanol or water.
Surface modifier described in step (2) is the one in isopropanol, Polyethylene Glycol or polyvinyl alcohol.
Magnesium salt described in step (2) or yttrium salt are 10-20:5-10:0.5-2 with solvent, the weight ratio of surface modifier.
Dip time described in step (3) is 10-20h.
Drying temperature described in step (3) is 80-100 DEG C.
Heat treatment temperature described in step (4) is 400-600 DEG C, and heat treatment time is 8-15h.
The present invention compared with prior art, has the advantages that
(1) present invention is creative first proposes with boron nitride fiber fabric as carrier, utilizes presoma conversion process within it
Portion's combined oxidation magnesium or yttria particles, be prepared for a kind of thermal cell boron nitride fiber barrier film with special composite structure.
(2) the solution impregnation pyrolytic conversion technique that proposes of the invention carries out Combined Processing to boron nitride fiber fabric, should
Technique can significantly improve the electrolyte effect of impregnation of boron nitride fiber fabric, make the electrolyte adsorption rate of barrier film 160% with
On, and in pressurized, vibrations and cell operation, higher to the holding capacity of electrolyte.In recombination process, excellent
Selecting the concentration formula of composite solution, infiltrate boron nitride fiber fabric by impregnation technology, preferably suitably Technology for Heating Processing, passes through
Heat treatment adds the composite particles that specific surface area is bigger in boron nitride fiber fabric, improves the electrolyte wetting property of barrier film, with
Shi Zuowei electrolyte flow inhibitor, makes electrolyte can keep at high operating temperatures not flowing out in fiber cloth, it is to avoid battery short circuit.
(3) this invention barrier film is with boron nitride fiber fabric as carrier, and structural strength is higher than current thermal cell magnesium oxide shaping piece,
Avoid in situations such as vibrations, the battery short circuits that causes due to shaping piece breakage in transportation, improve the safety of thermal cell
And service life.
(4) preparation technology of the present invention is simple, it is easy to accomplish large-scale production.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is described further.
Embodiment 1
Being carried out boron nitride fiber cloth with ethanol, 80 DEG C of drying are stand-by；By methanol and isopropanol according to the weight ratio of 5:0.5
Mixing, stirs 5min, then according to magnesium salt: solvent: the weight ratio of surface modifier is that the ratio of 10:5:0.5 weighs acetic acid
Magnesium granules, joins in the mixed liquor of methanol and isopropanol by magnesium acetate granule, continues stirring 30min, it is thus achieved that precursor solution；
Will clean after boron nitride fiber cloth be immersed in above precursor solution, dip time is 10h, takes out 80 DEG C drying after horse
Stove not carries out 400 DEG C of heat treatment 8h, obtains described lithium system thermal cell boron nitride fiber barrier film.
Prepared boron nitride fiber membrane thicknesses is 350 μm, and surface density is 230g/m2, hot strength is 690g/15mm.
Embodiment 2
Being carried out boron nitride fiber cloth with ethanol, 100 DEG C of drying are stand-by；By ethanol and Polyethylene Glycol according to the weight of 5:1
Than mixing, stir 8min, then according to magnesium salt: solvent: the weight ratio of surface modifier is that the ratio of 20:5:1 weighs vinegar
Acid magnesium granules, joins in the mixed liquor of ethanol and Polyethylene Glycol by magnesium acetate granule, continues stirring 30min, it is thus achieved that presoma
Solution；Boron nitride fiber cloth after cleaning is immersed in above precursor solution, and dip time is 20h, takes out 100 DEG C of drying
After in Muffle furnace, carry out 600 DEG C of heat treatment 15h, obtain described lithium system thermal cell boron nitride fiber barrier film.
Prepared boron nitride fiber membrane thicknesses is 380 μm, and surface density is 250g/m2, hot strength is 700g/15mm.
Embodiment 3
Being carried out boron nitride fiber felt with ethanol, 90 DEG C of drying are stand-by；Water is mixed according to the weight ratio of 8:1 with isopropanol,
Stirring 10min, then according to magnesium salt: solvent: the weight ratio of surface modifier is the ratio weighing magnesium nitrate granule of 15:8:1,
Magnesium acetate granule is joined in the mixed liquor of water and isopropanol, stir 30min, it is thus achieved that precursor solution；Nitrogen after cleaning
Changing boron fibre felt to be immersed in above precursor solution, dip time is 15h, carries out 500 after taking out 90 DEG C of drying in Muffle furnace
DEG C heat treatment 12h, obtains described lithium system thermal cell boron nitride fiber barrier film.
Prepared boron nitride fiber membrane thicknesses is 390 μm, and surface density is 275g/m2, hot strength is 230g/15mm.
Claims (9)
1. the lithium system thermal cell preparation method of boron nitride fiber barrier film, it is characterised in that step is as follows:
(1) boron nitride fiber fabric cleans: is carried out boron nitride fiber fabric with ethanol, dries stand-by；
(2) precursor solution preparation: mixed with surface modifier by solvent, stirs 5-10min, then adds magnesium salt or yttrium salt,
Stirring 20-30min, it is thus achieved that precursor solution；
(3) impregnate, be dried: by molten for presoma that the boron nitride fiber fabric of step (1) gained is soaked into step (2) gained
In liquid, take out post-drying stand-by；
(4) heat treatment: the fabric after the drying of step (3) gained is carried out heat treatment in Muffle furnace；
(5) naturally it is down to room temperature when Muffle furnace, takes out sample, obtain lithium system thermal cell boron nitride fiber barrier film.
The preparation method of lithium system the most according to claim 1 thermal cell boron nitride fiber barrier film, it is characterised in that step (1)
Described in boron nitride fiber fabric be boron nitride fiber felt or boron nitride fiber cloth.
The preparation method of lithium system the most according to claim 1 thermal cell boron nitride fiber barrier film, it is characterised in that step (1)
Described in drying temperature be 80-100 DEG C.
The preparation method of lithium system the most according to claim 1 thermal cell boron nitride fiber barrier film, it is characterised in that step (2)
Described in solvent be the one in ethanol, methanol or water.
The preparation method of lithium system the most according to claim 1 thermal cell boron nitride fiber barrier film, it is characterised in that step (2)
Described in surface modifier be the one in isopropanol, Polyethylene Glycol or polyvinyl alcohol.
The preparation method of lithium system the most according to claim 1 thermal cell boron nitride fiber barrier film, it is characterised in that step (2)
Described in magnesium salt or yttrium salt and solvent, the weight ratio of surface modifier be 10-20:5-10:0.5-2.
The preparation method of lithium system the most according to claim 1 thermal cell boron nitride fiber barrier film, it is characterised in that step (3)
Described in dip time be 10-20h.
The preparation method of lithium system the most according to claim 1 thermal cell boron nitride fiber barrier film, it is characterised in that step (3)
Described in drying temperature be 80-100 DEG C.
The preparation method of lithium system the most according to claim 1 thermal cell boron nitride fiber barrier film, it is characterised in that step (4)
Described in heat treatment temperature be 400-600 DEG C, heat treatment time is 8-15h.
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| CN201610459117.5A CN105977431A (en) | 2016-06-23 | 2016-06-23 | Preparation method for boron nitride fiber diaphragm for lithium-system thermal battery |
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| CN201610459117.5A CN105977431A (en) | 2016-06-23 | 2016-06-23 | Preparation method for boron nitride fiber diaphragm for lithium-system thermal battery |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106711382A (en) * | 2017-02-10 | 2017-05-24 | 武汉理工大学 | Non-oxide porous diaphragm material for high-temperature batteries and preparation method thereof |
| CN106972182A (en) * | 2017-04-28 | 2017-07-21 | 中国工程物理研究院电子工程研究所 | A kind of slim thermal cell spacer and preparation method thereof |
| CN107528072A (en) * | 2017-07-06 | 2017-12-29 | 上海空间电源研究所 | A kind of thermal cell development phase change heat storage type explosion-suppressing material and preparation method thereof |
| CN110690397A (en) * | 2019-09-17 | 2020-01-14 | 厦门大学 | Fused salt composite electrolyte diaphragm, preparation method and application |
| CN111564592A (en) * | 2020-05-21 | 2020-08-21 | 贵州梅岭电源有限公司 | High-specific-power single thermal battery and preparation method thereof |
| CN113644379A (en) * | 2021-01-18 | 2021-11-12 | 华南理工大学 | Porous ceramic fiber diaphragm material for thermal battery and preparation method thereof |
| CN113764821A (en) * | 2021-09-08 | 2021-12-07 | 山东工业陶瓷研究设计院有限公司 | Boron nitride fiber diaphragm, diaphragm preparation method and lithium thermal battery |
| US11223071B2 (en) * | 2016-12-01 | 2022-01-11 | The Regents Of The University Of California | High temperature Li-ion battery cells utilizing boron nitride aerogels and boron nitride nanotubes |
| CN113991248A (en) * | 2021-10-27 | 2022-01-28 | 中国工程物理研究院电子工程研究所 | Diaphragm for thermal battery loaded with molten salt electrolyte and preparation method and application thereof |
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| US20030228520A1 (en) * | 2002-06-06 | 2003-12-11 | Kaun Thomas D. | Process for manufacturing thermal battery with thin fiber separator |
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Patent Citations (4)
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| US3510359A (en) * | 1967-03-22 | 1970-05-05 | Standard Oil Co | Fused salt electrochemical battery with inorganic separator |
| US20030228520A1 (en) * | 2002-06-06 | 2003-12-11 | Kaun Thomas D. | Process for manufacturing thermal battery with thin fiber separator |
| US20090181292A1 (en) * | 2002-06-06 | 2009-07-16 | Kaun Thomas D | Flexible, porous ceramic composite film |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US11223071B2 (en) * | 2016-12-01 | 2022-01-11 | The Regents Of The University Of California | High temperature Li-ion battery cells utilizing boron nitride aerogels and boron nitride nanotubes |
| CN106711382A (en) * | 2017-02-10 | 2017-05-24 | 武汉理工大学 | Non-oxide porous diaphragm material for high-temperature batteries and preparation method thereof |
| CN106972182A (en) * | 2017-04-28 | 2017-07-21 | 中国工程物理研究院电子工程研究所 | A kind of slim thermal cell spacer and preparation method thereof |
| CN106972182B (en) * | 2017-04-28 | 2019-11-01 | 中国工程物理研究院电子工程研究所 | A kind of slim thermal cell spacer and preparation method thereof |
| CN107528072A (en) * | 2017-07-06 | 2017-12-29 | 上海空间电源研究所 | A kind of thermal cell development phase change heat storage type explosion-suppressing material and preparation method thereof |
| CN110690397A (en) * | 2019-09-17 | 2020-01-14 | 厦门大学 | Fused salt composite electrolyte diaphragm, preparation method and application |
| CN111564592A (en) * | 2020-05-21 | 2020-08-21 | 贵州梅岭电源有限公司 | High-specific-power single thermal battery and preparation method thereof |
| CN113644379A (en) * | 2021-01-18 | 2021-11-12 | 华南理工大学 | Porous ceramic fiber diaphragm material for thermal battery and preparation method thereof |
| CN113764821A (en) * | 2021-09-08 | 2021-12-07 | 山东工业陶瓷研究设计院有限公司 | Boron nitride fiber diaphragm, diaphragm preparation method and lithium thermal battery |
| CN113991248A (en) * | 2021-10-27 | 2022-01-28 | 中国工程物理研究院电子工程研究所 | Diaphragm for thermal battery loaded with molten salt electrolyte and preparation method and application thereof |
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Application publication date: 20160928 |