CN115939344A - Silane coupling agent coated modified sodium-electricity positive electrode material, preparation method and application - Google Patents
Silane coupling agent coated modified sodium-electricity positive electrode material, preparation method and application Download PDFInfo
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Abstract
The invention belongs to the technical field of preparation of sodium-ion battery materials, and discloses a silane coupling agent coated modified sodium-electricity positive electrode material, a preparation method and application thereof, wherein the silane coupling agent coated modified sodium-electricity positive electrode material comprises a sodium-ion positive electrode material and a modified coating; the sodium ion anode material is a layered oxide material and has a structural general formula as follows: naxM1aM2bO2; the modified coating is hydrophobic alkyl, aryl or perfluoro-siloxane coupling agent; according to the mass ratio, the modified coating is 0.1-5% of the sodium ion anode material. The method for coating the sodium ion anode material by using the hydrophobic silane coupling agent has the advantages of obvious effect, simple treatment process, low energy consumption, cheap and easily-obtained coating polymer and suitability for large-scale industrial production. The hydrophobic polymer provided by the invention can effectively inhibit the reaction between water in the air and the sodium-electrode positive electrode material, improves the air stability of the material, and reduces the humidity requirement of the environment required by material coating.
Description
Technical Field
The invention belongs to the technical field of preparation of sodium-ion battery materials, and particularly relates to a silane coupling agent coated modified sodium-electricity positive electrode material, a preparation method and application.
Background
At present, with the development of economy, the energy demand is getting larger, but the utilization of fossil energy is limited due to the pressure of environmental protection, so that the large-scale utilization of renewable clean energy is not slow. However, the solar energy and wind energy are difficult to be directly connected to the grid for generating power due to the intermittent nature of the clean energy sources, and the demand of energy storage equipment, particularly electrochemical pure energy, is increasing day by day. Similarly, however, the problems of scarcity and uneven distribution of lithium resources become more and more severe after the large-scale industrialization of the lithium ion battery, which causes the cost of the lithium ion battery to rise, and seriously hinders the popularization of clean energy.
The abundance of sodium resources is high, the distribution is uniform, the working principle of the sodium ion battery is similar to that of the lithium ion battery, the anode can adopt a cheaper aluminum foil, the production and processing technology can be compatible with the existing equipment of the lithium ion battery, and the production cost of the sodium ions is further reduced. Sodium ion batteries are therefore considered the most promising complement of lithium ion batteries.
The stability of the cathode material plays a crucial role in the stable operation of the battery system. Among them, for example, sodium ion positive electrode material O 3 The layered transition metal oxide has strong hygroscopicity, and Na in the material structure when exposed to humid air + Ions are easy to react with H of water molecules in the air + Ion exchange generates sodium carbonate and hydrate on the surface of the material, which causes a large amount of residual alkali on the surface of the material. On the one hand destabilizing the layered structureQualitative property, causing the performance of the material to be reduced; on the other hand, the residual alkali on the surface is easy to cause the gelation of the binder during the slurry preparation and coating, and brings difficulty to the coating. Therefore, it is necessary to improve the air stability of the layered material and to suppress the generation of impurities such as sodium carbonate on the surface thereof.
Through the above analysis, the problems and defects of the prior art are as follows: the prior positive electrode material of the sodium-ion battery has poor stability and strong hygroscopicity, and sodium carbonate and hydrate thereof are generated on the surface when the material is exposed in humid air, so that a large amount of residual alkali is generated on the surface of the material, the stability of a layered structure is damaged, and the performance of the material is reduced; the residual alkali on the surface is easy to cause the gelation of the binder when the slurry is prepared and coated, and brings difficulty to coating.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a silane coupling agent coated modified sodium anode material, a preparation method and application thereof.
The invention is realized in such a way that the silane coupling agent coated modified sodium electric anode material comprises a sodium ion anode material and a modified coating; wherein, the sodium ion anode material is a layered oxide material, and the modified coating is a hydrophobic alkyl, aryl or perfluoro-siloxane coupling agent; according to the mass ratio, the modified coating is 0.1-5% of the sodium ion anode material.
Further, the general structural formula of the sodium ion positive electrode material is as follows: na (Na) x M1 a M2 b O 2 ；0.6≤x<1.1，a>0,b is more than or equal to 0, a + b =1 and makes the material satisfy electric neutrality; wherein M1 is a transition metal element selected from any one or more of Ti, mn, fe, co, ni, cu or Zn; m2 is a non-transition metal element and is selected from any one or more of Li, mg, al, B, nb, sn, zr or Ca.
Further, the modified coating is selected from one or more of gamma-methacryloxypropyltrimethoxysilane, allyltrimethoxysilane, gamma- (2,3-glycidoxy) propyltrimethoxysilane, heptadecafluorodecyltrimethoxysilane, tridecafluorooctyltriethoxysilane, trifluoropropylmethylcyclotrisiloxane, methyltrimethoxysilane, propyltrimethoxysilane, n-octyltriethoxysilane, or decyltrimethoxysilane.
The invention also aims to provide a preparation method of the silane coupling agent coated modified sodium cathode material, which is used for implementing the silane coupling agent coated modified sodium cathode material, and the preparation method of the silane coupling agent coated modified sodium cathode material comprises the following steps:
preparing a mixed solution of ethanol and water, adding acetic acid to adjust the pH value of the solution, and adding a certain amount of silane coupling agent under the stirring condition to prepare a modified solution;
secondly, putting the anode material into a solid stirrer, directly spraying a modifying liquid and grinding;
and step three, drying the sodium electrode material at a specific temperature to obtain the modified sodium electrode material.
Further, in the first step, the volume ratio of ethanol to water is 8:1 to 30:1, the pH value of the modifying solution is 3.5-5.5.
Further, in the first step, the silane coupling agent accounts for 0.1-5% of the modifying liquid by mass.
Further, the grinding speed in the second step is 200-500 r/min, and the grinding time is 4-12 h.
Further, the drying temperature in the third step is 80-120 ℃, and the drying time is 2-12 h.
The invention also aims to provide the silane coupling agent modified layered oxide prepared by the preparation method of the silane coupling agent coated modified sodium battery positive electrode material.
The invention also aims to provide application of the silane coupling agent modified layered oxide in preparation of a sodium ion secondary battery.
By combining the technical scheme and the technical problem to be solved, the technical scheme to be protected by the invention has the advantages and positive effects that:
first, aiming at the technical problems and difficulties in solving the problems in the prior art, the technical problems to be solved by the technical scheme of the present invention are closely combined with results, data and the like in the research and development process, and some creative technical effects are brought after the problems are solved. The specific description is as follows:
the invention provides a silane coupling agent coated modified sodium ion positive electrode material, a preparation method and application thereof. The sodium electric anode material is coated and modified by alkyl, aryl or perfluoro siloxane. The hydrophobic silane coupling agent provided by the invention can effectively improve the air stability of the anode material, especially the stability under high humidity.
The invention relates to a preparation method of a sodium ion battery material, in particular to improvement of air stability of a positive electrode material. The method for coating the sodium ion anode material by using the hydrophobic silane coupling agent has the advantages of obvious effect, simple treatment process, low energy consumption, cheap and easily-obtained coating polymer and suitability for large-scale industrial production. The hydrophobic polymer provided by the invention can effectively inhibit the reaction between water in the air and the sodium-electrolyte anode material, improves the air stability of the material, and reduces the humidity requirement of the environment required by material coating.
According to the invention, the modification liquid containing the specific hydrophobic silane coupling agent is mixed with the original anode material in a stirrer, wherein the silane coupling agent is subjected to in-situ hydrolysis condensation under an acidic condition to complete coating modification on the anode material, and the hydrophobic film on the surface of the anode material can effectively inhibit water molecules in the air from contacting and reacting with the water molecules, so that the purpose of providing air stability of the anode material is achieved. The treatment process is mature and simple, and the silane coupling agent is cheap and easy to obtain, so that the method is suitable for large-scale industrial production.
Secondly, considering the technical scheme as a whole or from the perspective of products, the technical effect and advantages of the technical scheme to be protected by the invention are specifically described as follows:
the method for coating the modified sodium ion positive electrode material by the silane coupling agent can effectively improve the air stability of the material, and shows higher first-turn coulombic efficiency when being assembled in a sodium ion battery.
Third, as an inventive supplementary proof of the claims of the present invention, there are also presented several important aspects:
the expected income and commercial value after the technical scheme of the invention is converted are as follows:
according to the invention, the hydrophobic protective layer is constructed on the surface of the sodium-ion battery material through the hydrophobic surface coupling agent, so that the reaction with water molecules in the air is effectively inhibited, the air stability of the sodium-ion battery material is improved, the humidity requirement of the use environment of the sodium-ion battery can be reduced, and the production cost of the sodium-ion battery can be reduced.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings required to be used in the embodiments of the present invention will be briefly described below, and it is obvious that the drawings described below are only some embodiments of the present invention, and it is obvious for those skilled in the art that other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a flow chart of a method for preparing a silane coupling agent coated modified sodium battery positive electrode material according to an embodiment of the present invention;
FIG. 2 is a graph of contact angles of unmodified positive electrode materials provided in comparative example 1 of the present invention;
FIG. 3 is an infrared spectrum of a modified gamma-methacryloxypropyltrimethoxysilane cathode material provided in example 1 of the present invention;
FIG. 4 is a schematic diagram of the contact angle of the modified γ -methacryloxypropyltrimethoxysilane cathode material provided in example 1 of the present invention;
fig. 5 is a first-cycle charge-discharge diagram of the positive electrode material modified by trifluoropropylmethylcyclotrisiloxane according to example 5 of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Aiming at the problems in the prior art, the invention provides a silane coupling agent coated modified sodium battery positive electrode material, a preparation method and application thereof, and the invention is described in detail with reference to the accompanying drawings.
This section is an explanatory embodiment expanding on the claims so as to fully understand how the present invention is embodied by those skilled in the art.
The silane coupling agent coated modified sodium electric anode material provided by the embodiment of the invention comprises a sodium ion anode material and a modified coating.
The modified coating provided by the embodiment of the invention is a hydrophobic alkyl, aryl or perfluorosiloxane coupling agent, and specifically comprises the following components: gamma-methacryloxypropyltrimethoxysilane, allyltrimethoxysilane, gamma- (2,3-glycidoxy) propyltrimethoxysilane, heptadecafluorodecyltrimethoxysilane, tridecafluorooctyltriethoxysilane, trifluoropropylmethylcyclotrisiloxane, methyltrimethoxysilane, propyltrimethoxysilane, n-octyltriethoxysilane, or decyltrimethoxysilane.
According to the mass ratio, the coating provided by the embodiment of the invention is 0.1-5% of the sodium ion positive electrode material.
The sodium ion anode material provided by the embodiment of the invention is a layered oxide material, and the structural general formula is as follows: naxM1aM2bO2; x is more than or equal to 0.6 and less than 1.1, a is greater than or equal to 0, b is greater than or equal to 0, a + b is not less than 1, and the material satisfies the electroneutrality;
wherein M1 is a transition metal element, including any one or more of Ti, mn, fe, co, ni, cu or Zn; m2 is non-transition metal element, including any one or more of Li, mg, al, B, nb, sn, zr or Ca.
As shown in fig. 1, the preparation method of the silane coupling agent coated modified sodium battery positive electrode material provided by the embodiment of the present invention includes the following steps:
s101, preparing a mixed solution of ethanol and water, adding acetic acid to adjust the pH value of the solution, and adding a certain amount of silane coupling agent under stirring to prepare a modified solution;
s102, putting the anode material into a solid stirrer, directly spraying the modified solution on the material particles, and grinding for 4-12 h at the rotating speed of 200-500 r/min;
and S103, drying the treated sodium electric anode material at a specific temperature to obtain the modified sodium electric anode material coated with the modified silane coupling agent.
The volume ratio of ethanol to water provided by the embodiment of the invention is 8:1 to 30:1.
the pH value of the modifying liquid provided by the embodiment of the invention is 3.5-5.5.
The mass fraction of the silane coupling agent in the modification liquid provided by the embodiment of the invention is 0.1-5%.
The grinding rotating speed provided by the embodiment of the invention is 200-500 r/min, and the grinding time is 4-12 h.
The drying temperature provided by the embodiment of the invention is 80-120 ℃, and the drying time is 2-12 h.
Example 1
A mixed solution of 9.5g of ethanol and 0.5g of water was prepared, and then acetic acid was added to adjust the pH to 3.5, and a silane coupling agent, gamma-methacryloxypropyltrimethoxysilane, was added with stirring to give a concentration of 2%. 20g of sodium ion cathode material NaNi 0.33 Fe 0.33 Mn 0.33 O 2 And (3) putting the modified solution into a solid stirrer, directly spraying the modified solution containing the silane coupling agent on the particles, stirring at the speed of 300r/min for 6 hours, and drying the product in a constant-temperature air-blast drying oven at 120 ℃ for 4 hours to obtain the modified cathode material.
The infrared spectrogram of the treated sodium ion cathode material provided by the embodiment 1 of the invention is shown in fig. 3, and the gamma-methacryloxypropyltrimethoxysilane is positioned at 2987cm -1 Nearby methyl, methylene absorption peak, 1686cm -1 C = O absorption peak indicating that γ -methacryloxypropyltrimethoxysilane coated on the particle surface.
The contact angle effect graph of the treated sodium ion cathode material provided by the embodiment 1 of the invention is shown in fig. 4, and the comparison with fig. 2 shows that the modified cathode material has a larger contact angle, which shows that the sodium ion cathode material modified by gamma-methacryloxypropyltrimethoxysilane shows a hydrophobic effect, and the air stability of the material is obviously improved.
Example 2
9.5g of ethanol and 0.5g of water were mixed to prepare a mixed solution, acetic acid was added to adjust the pH to 3.5, and a silane coupling agent γ - (2,3-glycidoxy) propyltrimethoxysilane was added with stirring to make the concentration 2%. 20g of sodium ion cathode material NaNi 0.33 Fe 0.33 Mn 0.33 O 2 And (3) putting the modified solution into a solid stirrer, directly spraying the modified solution containing the silane coupling agent on the particles, stirring at the speed of 300r/min for 6 hours, and drying the product in a constant-temperature air-blast drying oven at 120 ℃ for 4 hours to obtain the modified cathode material.
Example 3
10g of ethanol and 0.5g of water are prepared into a mixed solution, acetic acid is added to adjust the pH value to 4.0, and a silane coupling agent, namely methyltrimethoxysilane, is added under stirring to enable the concentration to reach 1%. 20g of sodium ion cathode material NaNi 0.33 Fe 0.33 Mn 0.33 O 2 And (3) putting the modified solution into a solid stirrer, directly spraying the modified solution containing the silane coupling agent on the particles, stirring at the speed of 300r/min for 6 hours, and drying the product in a constant-temperature air-blast drying oven at 120 ℃ for 4 hours to obtain the modified cathode material.
Example 4
10g of ethanol and 0.5g of water are prepared into a mixed solution, acetic acid is added to adjust the pH value to 4.0, and a silane coupling agent, namely n-octyltriethoxysilane, is added under stirring to make the concentration reach 1%. 20g of sodium ion cathode material NaNi 0.33 Fe 0.33 Mn 0.33 O 2 And (3) putting the modified solution into a solid stirrer, directly spraying the modified solution containing the silane coupling agent on the particles, stirring at the speed of 300r/min for 6 hours, and drying the product in a constant-temperature air-blast drying oven at 120 ℃ for 4 hours to obtain the modified cathode material.
Example 5
A mixed solution of 10g of ethanol and 0.5g of water was prepared, and then acetic acid was added to adjust the pH to 5.0, and a silane coupling agent, trifluoropropylmethylcyclotrisiloxane, was added with stirring to make the concentration 1%. 20g of sodium ion cathode material NaCu 0.22 Fe 0.3 Fe 0.48 O 2 And (3) putting the modified solution into a solid stirrer, directly spraying the modified solution containing the silane coupling agent on the particles, stirring at the stirring speed of 400r/min for 3 hours, and drying the product in a constant-temperature air drying oven at 100 ℃ for 4 hours to obtain the modified cathode material. The first-turn charge-discharge diagram of the positive electrode material modified by trifluoropropylmethyl cyclotrisiloxane provided by the embodiment of the invention is shown in fig. 5.
Example 6
10g of ethanol and 0.5g of water were mixed to prepare a mixed solution, acetic acid was added to adjust the pH to 5.0, and heptadecafluorodecyltrimethoxysilane, a silane coupling agent, was added with stirring to make the concentration 1%. 20g of sodium ion cathode material NaCu 0.22 Fe 0.3 Fe 0.48 O 2 And (3) putting the modified solution into a solid stirrer, directly spraying the modified solution containing the silane coupling agent on the particles, stirring at the stirring speed of 400r/min for 3 hours, and drying the product in a constant-temperature air drying oven at 100 ℃ for 4 hours to obtain the modified cathode material.
In order to prove the creativity and the technical value of the technical scheme of the invention, the part is the application example of the technical scheme of the claims on specific products or related technologies.
The application embodiment of the invention provides a silane coupling agent modified layered oxide prepared by a preparation method of a silane coupling agent coated modified sodium battery positive electrode material.
The application embodiment of the invention provides application of a silane coupling agent modified layered oxide in preparation of a sodium ion secondary battery.
The embodiment of the invention achieves some positive effects in the process of research and development or use, and has great advantages compared with the prior art, and the following contents are described by combining data, diagrams and the like in the test process.
Comparative example 1
NaNi which is not a sodium ion positive electrode material 0.33 Fe 0.33 Mn 0.33 O 2 (NFM) any treatments were performed, cell assembly was performed and electrochemical performance was tested.
Comparative example 2
NaCu as non-sodium ion positive electrode material 0.22 Fe 0.3 Mn 0.48 O 2 (CFM) any treatments were performed, cell assembly was performed and electrochemical performance was tested.
The sodium ion battery positive electrode materials of the above examples were assembled into a sodium ion battery, and a positive electrode slurry was prepared by mixing the sodium ion battery positive electrode material, a binder polyvinylidene fluoride (PVDF), and a conductive agent carbon black (Super P) at a weight ratio of 94. Coating the positive electrode slurry on a battery-grade aluminum foil by adopting a scraper technology, drying for 12 hours in a vacuum oven at 120 ℃, then punching into a positive electrode plate with the diameter of 12mm by using a punching machine, and drying for 24 hours under the vacuum condition at 100 ℃. And (3) assembling the button cell in an Ar atmosphere in a glove box by using a CR2032 type button cell case, wherein the positive plate is the positive electrode material, the negative electrode is a sodium plate, and the glass fiber is used as a diaphragm to obtain the button cell. The first cycle efficiency and discharge capacity rate of the battery were 20mA/g, and the cycle at normal temperature was performed at a rate of 200mA/g (25 ℃).
Specific test items and test results are shown in table 1.
TABLE 1 specific test items and test results
According to the above example 1-example 6 and comparative example 1-comparative example 2 and the test results obtained by testing the above, it can be seen that by adopting the method for modifying the sodium ion cathode material provided by the embodiment of the invention, the air stability of the material can be effectively improved, and the modified sodium ion cathode material is assembled in a sodium ion battery to show higher first-loop coulombic efficiency.
The above description is only for the purpose of illustrating the present invention and the appended claims are not to be construed as limiting the scope of the invention, which is intended to cover all modifications, equivalents and improvements that are within the spirit and scope of the invention as defined by the appended claims.
Claims (10)
1. A silane coupling agent coated modified sodium electric anode material is characterized in that the silane coupling agent coated modified sodium electric anode material comprises a sodium ion anode material and a modified coating; wherein, the sodium ion anode material is a layered oxide material, and the modified coating is a hydrophobic alkyl, aryl or perfluoro-siloxane coupling agent; according to the mass ratio, the modified coating is 0.1-5% of the sodium ion anode material.
2. The silane coupling agent coated modified sodium electrode material as claimed in claim 1, wherein the general structural formula of the sodium ion anode material is as follows: naxM1aM2bO2; x is more than or equal to 0.6 and less than 1.1, a is greater than or equal to 0, b is greater than or equal to 0, a + b is not less than 1, and the material satisfies the electroneutrality; wherein M1 is a transition metal element selected from any one or more of Ti, mn, fe, co, ni, cu or Zn; m2 is a non-transition metal element and is selected from one or more of Li, mg, al, B, nb, sn, zr or Ca.
3. The silane coupling agent-coated modified sodium electrical positive electrode material according to claim 1, wherein the modified coating is selected from the group consisting of γ -methacryloxypropyltrimethoxysilane, allyltrimethoxysilane, γ - (2,3-glycidoxy) propyltrimethoxysilane, heptadecafluorodecyltrimethoxysilane, tridecafluorooctyltriethoxysilane, trifluoropropylmethylcyclotrisiloxane, methyltrimethoxysilane, propyltrimethoxysilane, n-octyltriethoxysilane, and decyltrimethoxysilane.
4. A method for producing a silane coupling agent-coated modified sodium positive electrode material by using the silane coupling agent-coated modified sodium positive electrode material according to any one of claims 1 to 3, wherein the method for producing the silane coupling agent-coated modified sodium positive electrode material comprises the following steps:
preparing a mixed solution of ethanol and water, adding acetic acid to adjust the pH value of the solution, and adding a certain amount of silane coupling agent under the stirring condition to prepare a modified solution;
secondly, putting the anode material into a solid stirrer, directly spraying a modifying liquid and grinding;
and step three, drying the sodium electrode anode material at a specific temperature to obtain the modified sodium electrode anode material.
5. The method for preparing the silane coupling agent coated modified sodium electrode material as claimed in claim 4, wherein in the first step, the volume ratio of ethanol to water is 8:1 to 30:1, the pH value of the modified liquid is 3.5-5.5.
6. The method for preparing the silane coupling agent coated modified sodium-electric positive electrode material as claimed in claim 4, wherein in the first step, the silane coupling agent accounts for 0.1-5% of the modification solution by mass.
7. The method for preparing the silane coupling agent coated modified sodium electrode material as claimed in claim 4, wherein the grinding speed in the second step is 200-500 r/min, and the grinding time is 4-12 h.
8. The method for preparing the silane coupling agent coated modified sodium-electricity positive electrode material of claim 4, wherein the drying temperature in the third step is 80-120 ℃, and the drying time is 2-12 h.
9. A silane coupling agent-modified layered oxide prepared by carrying out the method for preparing a silane coupling agent-coated modified sodium battery positive electrode material according to any one of claims 4 to 8.
10. Use of the silane coupling agent-modified layered oxide according to claim 9 for the preparation of a sodium ion secondary battery.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116936809A (en) * | 2023-09-13 | 2023-10-24 | 深圳华钠新材有限责任公司 | Super-hydrophobic layered oxide material and preparation method thereof |
| CN117117160A (en) * | 2023-10-24 | 2023-11-24 | 宁德时代新能源科技股份有限公司 | Positive electrode active material, preparation method thereof, positive electrode plate, battery and electricity utilization device |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116936809A (en) * | 2023-09-13 | 2023-10-24 | 深圳华钠新材有限责任公司 | Super-hydrophobic layered oxide material and preparation method thereof |
| CN117117160A (en) * | 2023-10-24 | 2023-11-24 | 宁德时代新能源科技股份有限公司 | Positive electrode active material, preparation method thereof, positive electrode plate, battery and electricity utilization device |
| CN117117160B (en) * | 2023-10-24 | 2024-04-05 | 宁德时代新能源科技股份有限公司 | Positive electrode active material, preparation method thereof, positive electrode plate, battery and electricity utilization device |
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