CN116093540B - Battery diaphragm, preparation method thereof and secondary battery - Google Patents
Battery diaphragm, preparation method thereof and secondary battery Download PDFInfo
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- CN116093540B CN116093540B CN202310111232.3A CN202310111232A CN116093540B CN 116093540 B CN116093540 B CN 116093540B CN 202310111232 A CN202310111232 A CN 202310111232A CN 116093540 B CN116093540 B CN 116093540B
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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
- H01M50/449—Separators, membranes or diaphragms characterised by the material having a layered structure
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
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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
- H01M50/403—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
- H01M50/446—Composite material consisting of a mixture of organic and inorganic materials
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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
- H01M50/489—Separators, membranes, diaphragms or spacing elements inside the cells, characterised by their physical properties, e.g. swelling degree, hydrophilicity or shut down properties
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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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- Chemical Kinetics & Catalysis (AREA)
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- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
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- Inorganic Chemistry (AREA)
- Materials Engineering (AREA)
- Secondary Cells (AREA)
- Cell Separators (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention belongs to the technical field of secondary batteries, and particularly relates to a battery diaphragm, a preparation method thereof and a secondary battery. The battery diaphragm comprises a diaphragm substrate and a modified coating coated on one side of the diaphragm substrate, wherein the modified coating comprises metal oxide and/or metal nitride and ionic liquid carbide, and the mass ratio of the (metal oxide and/or metal nitride) to the ionic liquid carbide is 0.9-1:1. The modified diaphragm of the metal oxide and/or the metal nitride and the ionic liquid carbide with a specific proportion can effectively inhibit the shuttle effect and absorb polysulfide, so that the lithium sulfur battery adopting the modified battery diaphragm has good cycle performance, and the discharge performance of the lithium sulfur battery is effectively improved.
Description
Technical Field
The invention belongs to the technical field of secondary batteries, and particularly relates to a battery diaphragm, a preparation method thereof and a secondary battery.
Background
With the increasing energy demand and excessive environmental problems, as well as the rapid development of electronic equipment, portable electronic information products and new energy automobiles, there is an increasing interest in developing sustainable and clean energy, such as wind energy, solar energy, tidal energy, and the like. But cannot meet the needs of large-scale applications due to the uncontrollability of these energy sources. Conventional lithium ion batteries such as lithium cobaltate (LiCoO 2), lithium manganate (LiMnO 4), lithium nickelate (LiNiO 2) batteries have failed to meet the overall demand due to energy shortfall and portability.
The lithium-sulfur secondary battery is a secondary battery which uses elemental sulfur or a sulfur-containing material as a positive electrode active material, wherein sulfur is widely distributed in nature, has the advantages of environmental friendliness, high theoretical specific energy and the like, and is considered to have a relatively development prospect. Unlike the ion deintercalation principle of lithium ion batteries, the charge-discharge process of lithium-sulfur batteries is an electrochemical mechanism, with sulfur as the positive electrode reactant and lithium as the negative electrode. The anode reaction is that lithium loses electrons to become lithium ions during discharging, the anode reaction is that sulfur reacts with lithium ions and electrons to generate polysulfide, the potential difference between the anode and the anode is that of a lithium sulfur battery, and the anode of the lithium sulfur battery react reversely under the action of an external voltage to obtain the charging process. During charge and discharge, polysulfide can dissolve and pass through the diaphragm, on the one hand can cause active material loss, and on the other hand polysulfide passes through the diaphragm and reaches the negative pole, can corrode lithium metal, aggravate lithium dendrite growth. This is the "shuttle effect" and is one of the key issues currently limiting the practical use of lithium sulfur batteries.
The separator is an important component of the battery and is a key to improving the performance of the battery in various aspects. At present, one of the more common methods is to load a material having adsorption and catalysis effects on polysulfide in a battery separator or interlayer to avoid the "shuttle effect", but the improvement effect is not ideal.
Disclosure of Invention
Therefore, the invention aims to overcome the defect of the prior art that the effect of avoiding the shuttle effect of a lithium-sulfur battery is not ideal, thereby providing a battery diaphragm, a preparation method thereof and a secondary battery.
Therefore, the invention provides the following technical scheme:
The invention provides a battery diaphragm, which comprises a diaphragm substrate and a modified coating coated on one side of the diaphragm substrate, wherein the modified coating comprises metal oxide and/or metal nitride and ionic liquid carbide,
Wherein the mass ratio of the (metal oxide and/or metal nitride) to the ionic liquid carbide is 0.9-1:1.
Optionally, the metal oxide is at least one selected from aluminum oxide, cobalt oxide, iron oxide and nickel oxide;
the metal nitride is at least one selected from cobalt nitride, titanium nitride and magnesium nitride.
Optionally, the ionic liquid carbide is obtained by calcining ionic liquid;
Optionally, the calcination temperature is 600-800 ℃ and the calcination time is 3-6h;
Optionally, the ionic liquid is at least one of 1-butyl-3-methylimidazole ionic liquid and 1-tetradecyl-3-methylimidazole ionic liquid. Typically, but not by way of limitation, the ionic liquid may be 1-tetradecyl-3-methylimidazole bromide, 1-tetradecyl-3-methylimidazole chloride, 1-butyl-3 methylimidazole chloride, and the like.
Optionally, the modified coating further comprises a conductive agent and a binder;
optionally (metal oxide and/or metal nitride + ionic liquid carbide) conductive agent to binder mass ratio = 7:1.9-2.1:0.9-1.1;
Optionally, the modified coating has a thickness of 150-200 μm.
Optionally, the conductive agent is at least one of conductive carbon black, ketjen black and acetylene black;
and/or the binder is polyvinylidene fluoride, and at least one of the binder LA 133;
And/or the membrane matrix is a polyethylene membrane, a polypropylene membrane or a polyethylene/polypropylene composite membrane.
The invention also provides a preparation method of the battery diaphragm, which comprises the following steps:
S1, mixing all raw materials (namely metal oxide and/or metal nitride, ionic liquid carbide, conductive agent and binder) of a modified coating with an organic solvent to obtain modified slurry;
s2, coating the modified slurry on one side surface of a diaphragm substrate, and drying to obtain the battery diaphragm.
Optionally, the modified slurry has a solids content of 52-65wt%;
and/or the organic solvent is at least one of N-methyl pyrrolidone and dimethyl sulfoxide.
Optionally, in step S2, the drying temperature is 55-60 ℃ and the drying time is 10-12 hours.
The invention also provides a secondary battery, which comprises the battery diaphragm or the battery diaphragm prepared by the preparation method.
Alternatively, the secondary battery is a lithium-sulfur battery.
The metal oxide and/or metal nitride used in the present invention may be obtained from commercial sources or may be self-made, and the preparation methods are conventional in the art. The pore size is generally micropores or mesopores, the larger the specific surface area is, the better the specific surface area is, and the material obtained or prepared by the conventional channel can basically meet the use requirement.
For example, taking cobalt nitride as an example, the preparation method comprises the following specific steps:
(1) Dissolving cobalt acetate and polyvinylpyrrolidone in ethylene glycol, and stirring for 2-3 hours;
(2) Transferring the mixture into an autoclave and keeping the temperature at 180-200 ℃ for 10-12 hours, then cooling the reactant to room temperature, collecting precipitate through centrifugation, washing the precipitate with ethanol and distilled water for several times, then drying the precipitate at 45-50 ℃ for 20-24 hours, and finally collecting the product for later use;
(3) Calcining the product in a muffle furnace, and heating to 550+/-5 ℃ for 4 hours at a heating rate of 3+/-1 ℃ per minute to obtain mesoporous cobalt oxide;
(4) Finally, introducing gas N 2 into a tube furnace, heating to 280-300 ℃ at a heating rate of 5+/-1 ℃ per minute, and then heating to 350-400 ℃ at a heating rate of 1+/-0.5 ℃ per minute for 3-4 hours to prepare the mesoporous cobalt nitride.
The precursor is prepared by the hydrothermal method, and the operation method is simpler.
The composition, structure and method of manufacturing the secondary battery provided in the present invention are all well known in the art.
Taking a lithium sulfur battery as an example, the lithium sulfur battery typically comprises a positive electrode, a negative electrode, a diaphragm and an electrolyte;
The positive electrode comprises a positive electrode active material (elemental sulfur), a conductive agent (Super P) and a binder (PVDF), wherein the positive electrode active material is elemental sulfur, the positive electrode also comprises the conductive agent and the binder, the positive electrode active material (elemental sulfur), the conductive agent (Super P) and the binder (PVDF) are weighed according to a certain mass ratio (7:2:1), NMP with a certain ratio is added into the mixture to be ground into slurry, then a scraper is coated on the surface of an aluminum foil, and finally the aluminum foil is put into a vacuum oven to be dried at 60 ℃ for 12 hours, and then the positive electrode is obtained.
The metal lithium sheet is used as a negative electrode.
The electrolyte composition was lithium bis (trifluoromethylsulfonate) imide (LITFSI)/Ethylene Carbonate (EC) +dimethyl carbonate (DMC) solution.
The preparation method comprises assembling and molding the button type simulated battery in a glove box filled with argon.
The technical scheme of the invention has the following advantages:
The battery diaphragm provided by the invention comprises a diaphragm substrate and a modified coating coated on one side of the diaphragm substrate, wherein the modified coating comprises metal oxide and/or metal nitride and ionic liquid carbide, and the mass ratio of the (metal oxide and/or metal nitride) to the ionic liquid carbide is 0.9-1:1. The modified diaphragm of the metal oxide and/or the metal nitride and the ionic liquid carbide with a specific proportion can effectively inhibit the shuttle effect and absorb polysulfide, so that the lithium sulfur battery adopting the modified battery diaphragm has good cycle performance, and the discharge performance of the lithium sulfur battery is effectively improved.
According to the battery diaphragm provided by the invention, the cycle performance and the discharge performance of the lithium-sulfur battery can be further improved through the limitation of the metal nitride, the metal oxide and the ionic liquid.
Detailed Description
The following examples are provided for a better understanding of the present invention and are not limited to the preferred embodiments described herein, but are not intended to limit the scope of the invention, any product which is the same or similar to the present invention, whether in light of the present teachings or in combination with other prior art features, falls within the scope of the present invention.
The specific experimental procedures or conditions are not noted in the examples and may be followed by the operations or conditions of conventional experimental procedures described in the literature in this field. The reagents or apparatus used were conventional reagent products commercially available without the manufacturer's knowledge.
Example 1
A battery diaphragm comprises a diaphragm substrate and a modified coating coated on one side of the diaphragm substrate, wherein the mass ratio of cobalt nitride to ionic liquid carbide in the raw materials of the modified coating is 1:1.
The preparation method and specific step parameters of the battery diaphragm are as follows:
Preparation of cobalt nitride (1) dissolving 10g of cobalt acetate and 1g of polyvinylpyrrolidone in 55mL of ethylene glycol, stirring for 3 hours, (2) transferring the mixture into an autoclave and keeping the mixture at 200 ℃ for 12 hours, then cooling the reactant to room temperature, collecting the precipitate by centrifugation, washing the precipitate with ethanol and distilled water for several times, drying the precipitate at 50 ℃ for 24 hours, and finally collecting the product for later use (mesoporous cobalt oxide), (3) calcining the product in a muffle furnace, heating the product to 550 ℃ for 4 hours at a heating rate of 3 ℃ per minute, and cooling the product to room temperature, (4) finally introducing gas N 2 in a tube furnace, heating the product to 300 ℃ at a heating rate of 5 ℃ per minute, and then heating the product to 400 ℃ for 4 hours at a heating rate of 1 ℃ per minute, thus obtaining mesoporous cobalt nitride.
And (3) preparing the ionic liquid carbide, namely calcining the chloridized 1-butyl-3-methylimidazole in a muffle furnace at 700 ℃ for 4 hours to obtain the ionic liquid carbide.
Coating, namely preparing slurry (solid content is 52%) of the prepared cobalt nitride, ionic liquid carbide, super P (Super high model of manufacturer) and PVDF (candela model HSV900 of manufacturer) into slurry (solid content is 52%) by dissolving in NMP at a ratio of 3.5:3.5:2:1, coating the slurry on a common diaphragm (Celgard model 2400 of manufacturer) by using a scraper, wherein the coating thickness is 200 mu m, putting the diaphragm into a vacuum oven, drying at 60 ℃ for 12 hours, taking out the diaphragm to obtain a battery diaphragm, and cutting the battery diaphragm into 16mm wafers for standby.
Example 2
A battery separator differs from example 1 only in that the mass ratio of cobalt nitride, ionic liquid carbide to Super P and PVDF in the slurry is 3.2:3.8:2:1.
Example 3
A battery separator differs from example 1 only in that the mass ratio of cobalt nitride, ionic liquid carbide to Super P and PVDF in the slurry is 3.4:3.6:2:1.
Example 4
A battery separator was different from example 1 only in that alumina (vendor aladine, model Al 2O3) was used instead of cobalt nitride.
Example 5
A battery separator was different from example 1 only in that step (4) was not included in the preparation step of cobalt nitride, i.e., cobalt oxide was used instead of cobalt nitride.
Example 6
A battery separator was different from example 1 only in that 1-tetradecyl-3-methylimidazolium bromide was used instead of 1-butyl-3-methylimidazole chloride.
Example 7
A battery separator was different from example 1 only in that in the preparation step of the ionic liquid carbide, the calcination temperature was 600 ℃ and the calcination time was 6 hours.
Example 8
A battery separator was different from example 1 only in that in the preparation step of the ionic liquid carbide, the calcination temperature was 800 ℃ and the calcination time was 3 hours.
Comparative example 1
A battery separator differs from example 1 only in that an equivalent amount of cobalt nitride was used instead of the ionic liquid carbide.
Comparative example 2
A battery separator differs from example 1 only in that an equivalent amount of ionic liquid carbide was used instead of cobalt nitride.
Test case
The battery diaphragm provided by the embodiment of the invention and the comparative example is assembled into a button lithium sulfur battery, and the cycle performance and the discharge performance of the button lithium sulfur battery are tested by the specific test method that:
the preparation of the button cell comprises the steps of weighing the anode by adopting elemental sulfur, super P and PVDF according to a certain mass ratio (7:2:1), adding NMP with a certain proportion, grinding into slurry with the solid content of 52%, coating the slurry on an aluminum foil with the coating thickness of 200 mu m, and finally drying in a vacuum oven at 60 ℃ for 12 hours, and taking out the slurry to obtain the anode sheet. The battery separator provided in each of examples and comparative examples was a lithium sulfur specialty electrolyte, which was purchased from su-chow chemical technology limited, and was assembled into a button-type analog battery (model CR 2032) in a glove box filled with argon gas, using a metallic lithium sheet as a negative electrode.
The assembled simulated battery is kept stand for 12 hours at room temperature and then tested in a charging and discharging voltage range of 1.7-2.8V, wherein the specific testing steps are that the charging and discharging test is carried out at a multiplying power of 0.1C, the charging cut-off voltage is 2.8V, and the discharging cut-off voltage is 1.7V.
The specific test results are shown in the following table:
TABLE 1
Note that comparative example 3 is a conventional separator in example 1 that does not include a modified coating.
The test results in the table show that the diaphragm is modified by the metal oxide and/or the metal nitride and the ionic liquid carbide at the same time, so that the shuttle effect can be effectively inhibited, polysulfide can be absorbed, the lithium sulfur battery adopting the modified battery diaphragm provided by the embodiment has good cycle performance, and the discharge performance of the lithium sulfur battery is effectively improved. As is clear from the comparison of the data of examples 4,5 and 1, and examples 6 and 1, the metal nitride and 1-butyl-3-methylimidazole ionic liquid carbide were compounded to give the best effect of modifying the separator.
It is apparent that the above examples are given by way of illustration only and are not limiting of the embodiments. Other variations or modifications of the above teachings will be apparent to those of ordinary skill in the art. It is not necessary here nor is it exhaustive of all embodiments. And obvious variations or modifications thereof are contemplated as falling within the scope of the present invention.
Claims (9)
1. A lithium sulfur battery diaphragm is characterized by comprising a diaphragm substrate and a modified coating coated on one side of the diaphragm substrate, wherein the modified coating comprises metal oxide and/or metal nitride and ionic liquid carbide,
Wherein the mass ratio of the (metal oxide and/or metal nitride) to the ionic liquid carbide is 0.9-1:1, and the ionic liquid carbide is obtained by calcining the ionic liquid.
2. The lithium sulfur battery separator according to claim 1, wherein the metal oxide is at least one selected from the group consisting of aluminum oxide, cobalt oxide, iron oxide, and nickel oxide;
the metal nitride is at least one selected from cobalt nitride, titanium nitride and magnesium nitride.
3. The lithium sulfur battery separator according to claim 1, wherein the calcination temperature is 600 to 800 ℃ and the calcination time is 3 to 6 hours;
And/or the ionic liquid is at least one of 1-butyl-3-methylimidazole ionic liquid and 1-tetradecyl-3-methylimidazole ionic liquid.
4. The lithium sulfur battery separator of any of claims 1-3 wherein the modified coating further comprises a conductive agent and a binder therein;
And/or the modified coating has a thickness of 150-200 μm.
5. The lithium sulfur battery separator according to claim 4, wherein in the modified coating layer, (metal oxide and/or metal nitride+ionic liquid carbide) the mass ratio of the conductive agent to the binder=7:1.9-2.1:0.9-1.1;
and/or the conductive agent is at least one of conductive carbon black, ketjen black and acetylene black;
and/or the binder is polyvinylidene fluoride, and at least one of the binder LA 133;
And/or the membrane matrix is a polyethylene membrane, a polypropylene membrane or a polyethylene/polypropylene composite membrane.
6. A method for preparing the lithium sulfur battery separator according to any one of claims 1 to 5, comprising the steps of:
s1, mixing all raw materials of a modified coating with an organic solvent to obtain modified slurry;
s2, coating the modified slurry on one side surface of a diaphragm substrate, and drying to obtain the battery diaphragm.
7. The method for producing a lithium sulfur battery separator according to claim 6, wherein the modified slurry has a solid content of 52 to 65wt%;
and/or the organic solvent is at least one of N-methyl pyrrolidone and dimethyl sulfoxide.
8. The method for preparing a lithium sulfur battery separator according to claim 6 or 7, wherein in step S2, the drying temperature is 55 to 60 ℃ and the drying time is 10 to 12 hours.
9. A secondary battery comprising the battery separator according to any one of claims 1 to 5 or the lithium-sulfur battery separator prepared by the preparation method according to any one of claims 6 to 8.
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| CN109004189A (en) * | 2018-07-10 | 2018-12-14 | 河北师范大学 | A method of nickel compound of the calcining containing ionic liquid prepares lithium cell cathode material |
| CN110350132A (en) * | 2019-07-10 | 2019-10-18 | 南京海泰纳米材料有限公司 | A kind of phosphate-modified diaphragm of lithium-sulfur cell and its preparation, coating method |
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| WO2015165762A1 (en) * | 2014-04-30 | 2015-11-05 | Basf Se | Process for producing a monolithic body of a porous carbon material, monolithic bodies of special porous carbon materials and their use |
| KR101832709B1 (en) * | 2015-12-24 | 2018-02-27 | 한국세라믹기술원 | Manufacturing method of cathode active material for lithium-sulfur battery and manufacturing method of lithium-sulfur battery cathode |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109004189A (en) * | 2018-07-10 | 2018-12-14 | 河北师范大学 | A method of nickel compound of the calcining containing ionic liquid prepares lithium cell cathode material |
| CN110350132A (en) * | 2019-07-10 | 2019-10-18 | 南京海泰纳米材料有限公司 | A kind of phosphate-modified diaphragm of lithium-sulfur cell and its preparation, coating method |
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