CN109244314B - Sodium ion battery ceramic diaphragm, sodium ion secondary battery and application - Google Patents
Sodium ion battery ceramic diaphragm, sodium ion secondary battery and application Download PDFInfo
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- CN109244314B CN109244314B CN201810933542.2A CN201810933542A CN109244314B CN 109244314 B CN109244314 B CN 109244314B CN 201810933542 A CN201810933542 A CN 201810933542A CN 109244314 B CN109244314 B CN 109244314B
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- sodium
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- sodium ion
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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
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
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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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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a sodium ion battery ceramic diaphragm, a sodium ion secondary battery and application, wherein the sodium ion battery ceramic diaphragm comprises: a separator substrate and a ceramic powder coating layer coated at least on one side surface of the separator substrate; the thickness of the diaphragm substrate is 1-100 um; the thickness of the ceramic powder coating is 0.5-10 um; the ceramic powder coating is formed by sodium ion solid electrolyte powder and specifically comprises Na-Beta-Al2O3And/or a sodium super ion conductor NASICON material. By using the ceramic powder coating with sodium ion conductivity, the wettability with a cyclic carbonate solvent is improved, so that the safety performance of the diaphragm is improved, and the cycle performance of the battery is also improved.
Description
Technical Field
The invention relates to the technical field of lithium battery materials, in particular to a sodium ion battery ceramic diaphragm, a sodium ion secondary battery and application.
Background
Lithium ion batteries have been applied in 3C field in large scale due to their high energy density and power density, and the problem of scarcity of exposed lithium resources has been gradually paid attention. Sodium and lithium have similar physicochemical properties, and sodium reserves are abundant and uniformly distributed, so sodium-ion batteries are considered as 'candidates' for next-generation energy storage batteries.
As in the lithium ion battery, the sodium ion battery is also largely divided into three parts of a positive electrode, an electrolyte, and a negative electrode, and a separator mainly functions therein to separate the positive electrode and the negative electrode from short circuits. The performance of the separator directly affects the characteristics of the battery, such as capacity, internal resistance, rate, and cycle.
In the electrolyte of a common sodium ion battery, cyclic carbonate is an indispensable choice because of high dielectric constant, but the separators commonly used in the market, such as a common polyolefin separator and an alumina-coated separator, have a disadvantage of poor wettability to cyclic carbonate.
In addition, the polyolefin separator commonly used at present can generate thermal shrinkage when the temperature is increased, so that the battery is directly short-circuited, and potential safety hazards are brought.
Therefore, a separator which can improve wettability with cyclic carbonate and has high safety has been desired.
Disclosure of Invention
The invention provides a sodium ion battery ceramic diaphragm, a secondary battery and application thereof. The sodium ion battery ceramic diaphragm provided by the invention can improve the safety of the diaphragm and simultaneously solves the problem that the existing diaphragm is not infiltrated by cyclic carbonate.
In a first aspect, an embodiment of the present invention provides a sodium-ion battery ceramic separator, including: a separator substrate and a ceramic powder coating layer coated at least on one side surface of the separator substrate; the thickness of the diaphragm substrate is 1-100 um; the thickness of the ceramic powder coating is 0.5-10 um; the ceramic powder coating is specifically composed of sodium ion solid electrolyte powder and comprises Na-Beta-Al2O3And/or a sodium super ion conductor NASICON material.
Preferably, the diaphragm substrate comprises one or more of a Polyethylene (PE) diaphragm, a polypropylene (PP) diaphragm or a PP/PE/PP diaphragm.
Preferably, the Na-Beta-Al2O3General formula M2O﹒yAl2O3Wherein M is Na or Na and one or more doping elements of K, Rb, Ag, Li, Mg, Y, Ti and Nb, Y is more than or equal to 5 and less than or equal to 11, and the space group is P63/mmc or R3M.
Preferably, the NASICON material has the general formula Na1+xZr2Si2-xPxO12X is more than or equal to 0 and less than or equal to 3, and the space group is R-3 c.
Further preferably, the Na1+xZr2Si2-xPxO12The Zr site In the alloy has cation substitution elements, including one or more of Al, As, Cd, Co, Cr, Fe, Ga, Ge, Hf, In, La, Lu, Mg, Mn, Mo, Nb, Ni, Sb, Sc, Si, Sn, Ta, Ti, V, Y and Zn; the Si/P site has a substitution element of As and/or Ge.
Preferably, the particle size of the sodium ion solid electrolyte powder is 1nm-5 um.
Further preferably, the particle size of the sodium ion solid electrolyte powder is 0.01 to 1 um.
In a second aspect, an embodiment of the present invention provides a sodium-ion secondary battery comprising the ceramic separator for a sodium-ion battery according to the first aspect.
In a third aspect, embodiments of the present invention provide a use of the sodium ion secondary battery according to the second aspect, wherein the sodium ion secondary battery is used for an electric tool, an electric vehicle, and an energy storage device of solar power generation, wind power generation, smart grid peak shaving, a distributed power station, a backup power source or a communication base station.
According to the sodium ion battery ceramic diaphragm disclosed by the embodiment of the invention, the safety performance of the diaphragm is improved and the cycle performance of the battery is also improved by coating the ceramic powder with sodium ion conductivity. The ceramic diaphragm of the sodium ion battery improves the wettability with a cyclic carbonate solvent. The energy storage device can be used for power supplies of electric tools and electric automobiles, and also can be used for large-scale energy storage equipment of solar power generation, wind power generation, smart grid peak shaving, distributed power stations, backup power supplies or communication base stations.
Drawings
The technical solutions of the embodiments of the present invention are further described in detail with reference to the accompanying drawings and embodiments.
FIG. 1 is a scanning electron microscope image of a sodium-ion battery ceramic diaphragm 1 provided in example 2 of the present invention;
fig. 2 is a graph showing the soaking result of the sodium ion battery ceramic diaphragm 1 and the cyclic carbonate solvent provided in embodiment 2 of the present invention;
FIG. 3 is a diagram showing the internal resistance of a sodium-ion battery ceramic diaphragm 1 assembled battery provided in example 2 of the present invention;
FIG. 4 is a scanning electron microscope image of the ceramic diaphragm 2 of the Na-ion battery provided in example 3 of the present invention;
fig. 5 is a graph showing the infiltration result of the sodium ion battery ceramic diaphragm 2 and the cyclic carbonate solvent provided in embodiment 3 of the present invention;
FIG. 6 is a graph of internal resistance of a sodium ion battery ceramic separator 2 assembled cell provided in example 3 of the present invention;
FIG. 7 is a graph showing the results of solvent immersion of an uncoated membrane and a cyclic carbonate according to comparative example 1 of the present invention;
FIG. 8 is a graph of internal resistance of an uncoated separator provided in comparative example 1 of the present invention;
FIG. 9 is a graph showing the results of impregnating a common alumina-coated membrane with a cyclic carbonate solvent according to comparative example 2 of the present invention;
fig. 10 is a graph of the internal resistance of the uncoated separator provided by comparative example 2 of the present invention.
Detailed Description
The present invention will be described in further detail with reference to examples, but the present invention is not limited thereto.
The embodiment of the invention provides a sodium ion battery ceramic diaphragm, which comprises: a diaphragm substrate and a ceramic powder coating layer coated at least on one side surface of the diaphragm substrate;
the thickness of the diaphragm substrate is 1-100 um; the thickness of the ceramic powder coating is 0.5-10 um; the ceramic powder coating is specifically composed of sodium ion solid electrolyte powder and comprises Na-Beta-Al2O3 and/or sodium super ion conductor (NASICON) materials.
Wherein, Na-Beta-Al2O3General formula M2O﹒yAl2O3Wherein M is Na or Na and one or more doping elements of K, Rb, Ag, Li, Mg, Y, Ti and Nb, Y is more than or equal to 5 and less than or equal to 11, and the space group is P63/mmc or R3M.
NASICON materials of the general formula Na1+xZr2Si2-xPxO12X is more than or equal to 0 and less than or equal to 3, and the space group is R-3 c; wherein, Na1+xZr2Si2- xPxO12The Zr site In the alloy can be partially replaced by other cation elements, and the alloy comprises one or more of Al, As, Cd, Co, Cr, Fe, Ga, Ge, Hf, In, La, Lu, Mg, Mn, Mo, Nb, Ni, Sb, Sc, Si, Sn, Ta, Ti, V, Y and Zn; the Si/P site may be partially substituted with As and/or Ge.
The particle size of the sodium ion solid electrolyte powder is 1nm-5um, preferably 0.01-1 um.
The diaphragm substrate includes: one or more of a Polyethylene (PE) diaphragm, a polypropylene (PP) diaphragm or a PP/PE/PP diaphragm.
The sodium ion battery ceramic diaphragm is applied to a sodium ion secondary battery, and the safety performance of the diaphragm is improved and the cycle performance of the battery is also improved by coating the ceramic powder with sodium ion conductivity. The ceramic diaphragm of the sodium ion battery improves the wettability with a cyclic carbonate solvent. The energy storage device can be used for power supplies of electric tools and electric automobiles, and also can be used for large-scale energy storage equipment of solar power generation, wind power generation, smart grid peak shaving, distributed power stations, backup power supplies or communication base stations.
The sodium ion battery ceramic separator of the present invention and its applications and performance are described in the following specific examples.
Example 1
This example is used to illustrate a method for preparing a sodium ion soft pack battery using the ceramic separator for a sodium ion battery provided by the present invention.
Preparation of the positive electrode: adding 100 parts by weight of solvent N-methylpyrrolidone (NMP) and 3 parts by weight of binder polyvinylidene fluoride (PVDF) powder into a stirrer, and stirring for 2 hours by revolving for 30 revolutions per minute and rotating for 3000 revolutions per minute; then adding 4 parts by weight of conductive agent acetylene black and 0.2 part by weight of regulator oxalic acid, and stirring for 1 hour; then 100 parts by weight of a positive electrode active material O was added3-Na0.9[Cu0.22Fe0.30Mn0.48]O2Stirring for 2 hours, defoaming,sieving with a 200-mesh sieve to prepare the required positive electrode slurry of the sodium-ion battery.
And uniformly coating the obtained positive electrode slurry of the sodium-ion battery on an aluminum foil with the thickness of 20 microns in a slurry drawing mode, drying, tabletting and cutting into a positive electrode piece.
Preparation of a negative electrode: 100 parts by weight of negative active material soft carbon, 3 parts by weight of Styrene Butadiene Rubber (SBR) as a binder, and 3 parts by weight of carboxymethyl cellulose (CMC) were added to 50 parts by weight of water, and then stirred in a vacuum stirrer to form stable and uniform negative slurry. And uniformly coating the negative electrode slurry on a copper foil, drying at 120 ℃, rolling and cutting into a negative electrode plate.
Preparing a battery: the above-mentioned positive electrode sheet, the selected separator (different in specific examples, see examples 2 and 3 and comparative examples 1 and 2 below, respectively), and the negative electrode sheet were laminated in this order to form an electrode group having a capacity of 1Ah, and were housed in a battery case. The electrolyte is 1 mol per liter of propylene carbonate solution of sodium hexafluorophosphate, the electrolyte is injected into a battery shell in an amount of 7g/Ah, so that electrode plates are completely soaked, an experimental soft package battery is assembled, and the soft package sodium ion battery is manufactured by sealing.
And (3) impedance testing: and standing the battery for 24 hours after liquid injection, and testing by using an impedance tester.
Example 2
This example is provided to illustrate the performance of the sodium ion soft package battery prepared by the preparation method provided in example 1 of the present invention.
A1 Ah sodium ion pouch cell was prepared as in example 1, using a NASICON coated polypropylene ceramic separator and Na as the electrolyte material3.4Zr1.8Mg0.2Si2PO12The particle size was 200nm and the coating thickness was 2 um.
Firstly, the sodium ion battery ceramic diaphragm is analyzed by a scanning electron microscope, and as is obvious from figure 1, the particles are uniformly distributed.
Next, the wettability with the cyclic carbonate was analyzed. A small amount of Propylene Carbonate (PC) was drawn and dropped on the membrane as shown in fig. 2, and it was evident that the wettability was very good and the membrane became transparent.
The uncoated separator in comparative example 1 was not substantially impregnated with PC, and was in the form of drops. Even the alumina-coated separator of comparative example 2 showed a dripping-like state after dropping PC, and the wettability was poor.
Finally, the internal resistance of the soft package battery before charging and discharging is analyzed, and as can be seen from fig. 3, compared with comparative example 1 and comparative example 2, the internal resistance of the battery in the embodiment is greatly optimized, which is due to the good wettability of the diaphragm to PC.
Example 3
This example is provided to illustrate the performance of the sodium ion soft package battery prepared by the preparation method provided in example 1 of the present invention.
A1 Ah sodium ion pouch cell was prepared as in example 1, using a separator of beta-Al2O3Coated polypropylene separator with Na as electrolyte material1.67Al10.67Li0.33O17The particle size was 300nm and the coating thickness was 2 um.
It was first analyzed by scanning electron microscopy and it is evident from fig. 4 that the particles are uniformly distributed.
Next, the wettability with the cyclic carbonate was analyzed. A small amount of Propylene Carbonate (PC) was drawn and dropped on the diaphragm, and it is apparent from fig. 5 that the wettability was very good and the diaphragm became transparent.
The uncoated separator of comparative example 1 was substantially non-wetting to PC and appeared as a drop. The alumina-coated separator in comparative example 2 showed a dripping-like state after dropping PC, and had poor wettability.
Finally, the internal resistance of the soft-package battery before charging and discharging is analyzed, as can be seen from fig. 6, the internal resistance is about 0.3 ohm, and compared with hundreds of ohms of comparative example 1 and comparative example 2, the internal resistance is greatly optimized, which is benefited by the good wetting performance of the diaphragm on PC.
Comparative example 1
A 1Ah sodium ion pouch cell was prepared as in example 1, using a common polypropylene separator without coating.
As shown in fig. 7, the polypropylene separator was not substantially impregnated with PC in view of wettability with PC, and the pouch battery prepared had an internal resistance of more than 150 ohms as shown in fig. 8, and thus the battery was not operated.
Comparative example 2
A 1Ah sodium ion pouch cell was prepared as in example 1 using a common alumina coated polypropylene separator with a particle size of 200nm and a coating thickness of 2 um.
From the viewpoint of wettability with PC, the ordinary alumina ceramic-coated separator was difficult to wet with PC, and showed a remarkable droplet shape, as shown in fig. 9. But is a significant improvement over uncoated separators. From the internal resistance of the pouch cell, as shown in fig. 10, the resistance value was reduced compared to the conventional uncoated separator, but the cell was still unable to operate with as much as 120 ohms.
The above-mentioned embodiments are intended to illustrate the objects, technical solutions and advantages of the present invention in further detail, and it should be understood that the above-mentioned embodiments are merely exemplary embodiments of the present invention, and are not intended to limit the scope of the present invention, and any modifications, equivalent substitutions, improvements and the like made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (8)
1. A sodium-ion battery ceramic membrane, comprising: the film comprises a diaphragm substrate and a ceramic powder coating at least coated on one side surface of the diaphragm substrate, and is used for improving the wettability of a sodium ion battery ceramic diaphragm and an annular carbonate solvent;
the thickness of the diaphragm substrate is 1-100 um; the thickness of the ceramic powder coating is 0.5-10 um; the ceramic powder coating is specifically composed of sodium ion solid electrolyte powder and comprises Na-Beta-Al2O3And/or a sodium super ion conductor NASICON material; wherein the particle size of the sodium ion solid electrolyte powder is 1nm-5 um.
2. The sodium-ion battery ceramic separator of claim 1, wherein the separator substrate comprises one or more of a Polyethylene (PE) separator, a polypropylene (PP) separator, or a PP/PE/PP separator.
3. The sodium-ion battery ceramic separator of claim 1, wherein the Na-Beta-Al is present in the electrolyte solution2O3General formula M2O﹒yAl2O3Wherein M is Na or Na and one or more doping elements of K, Rb, Ag, Li, Mg, Y, Ti and Nb, Y is more than or equal to 5 and less than or equal to 11, and the space group is P63/mmc or R3M.
4. The sodium-ion battery ceramic separator of claim 1, wherein the NASICON material has the general formula Na1+xZr2Si2-xPxO12X is more than or equal to 0 and less than or equal to 3, and the space group is R-3 c.
5. The sodium-ion battery ceramic separator of claim 4, wherein the Na1+xZr2Si2-xPxO12The Zr site In the alloy has cation substitution elements, including one or more of Al, As, Cd, Co, Cr, Fe, Ga, Ge, Hf, In, La, Lu, Mg, Mn, Mo, Nb, Ni, Sb, Sc, Si, Sn, Ta, Ti, V, Y and Zn; the Si/P site has a substitution element of As and/or Ge.
6. The sodium-ion battery ceramic separator according to claim 1, wherein the particle size of the sodium-ion solid electrolyte powder is 0.01-1 um.
7. A sodium-ion secondary battery comprising the sodium-ion battery ceramic separator of any of claims 1-6.
8. Use of the sodium ion secondary battery according to claim 7 for power tools, electric vehicles, and energy storage devices for solar power generation, wind power generation, smart grid peak shaving, distributed power plants, backup power sources, or communication base stations.
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| CN110970589A (en) * | 2019-11-28 | 2020-04-07 | 中国电力科学研究院有限公司 | Sodium ion battery diaphragm, preparation method and sodium ion battery |
| CN110970588A (en) * | 2019-12-18 | 2020-04-07 | 江苏厚生新能源科技有限公司 | Coating diaphragm for sodium ion battery, preparation method of coating diaphragm and sodium ion battery |
| CN113113730A (en) * | 2021-04-01 | 2021-07-13 | 溧阳中科海钠科技有限责任公司 | Sodium ion battery ceramic diaphragm and preparation method thereof, and sodium ion battery and preparation method thereof |
| CN113675533B (en) * | 2021-06-29 | 2023-12-01 | 东莞凯德新能源有限公司 | Composite coating sodium ion battery diaphragm and preparation method thereof |
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