CN119008919B - Modified sodium ion battery positive electrode material and preparation method thereof, sodium ion battery - Google Patents
Modified sodium ion battery positive electrode material and preparation method thereof, sodium ion battery Download PDFInfo
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Abstract
本发明提供改性钠离子电池正极材料，包括钠离子电池正极材料基体和位于基体至少部分表面的包覆层，包覆层为氮化钛包覆氮氯化钛。提供的改性正极材料采用氮氯化钛@氮化钛包覆层对钠离子电池正极材料进行包覆改性，能明显改善钠离子电池正极材料的结构稳定性和电性能，降低容量衰减，提高电池的循环寿命。本发明还提供该改性钠离子电池正极材料的制备方法及钠离子电池。
The present invention provides a modified sodium ion battery positive electrode material, comprising a sodium ion battery positive electrode material substrate and a coating layer located on at least part of the surface of the substrate, wherein the coating layer is titanium nitride coated with titanium nitride chloride. The modified positive electrode material provided uses titanium nitride chloride @ titanium nitride coating layer to coat and modify the sodium ion battery positive electrode material, which can significantly improve the structural stability and electrical properties of the sodium ion battery positive electrode material, reduce capacity attenuation, and increase the cycle life of the battery. The present invention also provides a preparation method of the modified sodium ion battery positive electrode material and a sodium ion battery.
Description
Technical Field
The invention belongs to the technical field of sodium ion battery anode materials, and particularly relates to coating modification of a sodium ion battery anode material.
Background
In recent years, sodium ion batteries are considered as an ideal energy storage material of a new generation due to abundant resources and wide distribution. The prior sodium ion battery layered oxide anode material has the advantages of large specific capacity, simple synthesis, low cost and the like, and is an ideal sodium ion battery anode material. However, the layered oxide cathode material of the sodium ion battery is easy to generate phase change in the sodium storage process, and the material structure is easy to collapse along with the deintercalation of sodium ions in the charge and discharge process due to the large ionic radius of the sodium ions, so that the capacity of the material is quickly attenuated, the cycle life is reduced, and the practical application of the material is seriously hindered.
In order to solve the above-mentioned drawbacks, strategies such as doping and cladding are currently adopted to improve the problems.
Disclosure of Invention
Aiming at the technical problems, the application provides a modified sodium ion battery anode material, a preparation method thereof and a sodium ion battery.
In order to achieve the above purpose, the present application proposes the following technical scheme:
in a first aspect, a modified sodium ion battery positive electrode material is provided, which comprises a sodium ion battery positive electrode material substrate and a coating layer positioned on at least part of the surface of the substrate, wherein the coating layer is titanium chloride@titanium nitride.
Preferably, the sodium ion battery positive electrode material matrix has a chemical formula NaTMO 2, wherein TM is one or more of Ni, fe, mn, co, cu, al, cr.
Preferably, the mass of the coating layer is 1-10% of the mass of the sodium ion battery anode material matrix.
In a second aspect, a method for preparing a modified sodium ion battery positive electrode material is provided, comprising:
S1, grinding and mixing a sodium ion battery anode material and titanium tetrachloride under a protective atmosphere to obtain a mixture;
And S2, introducing ammonia gas into a reaction furnace filled with the mixture under a protective atmosphere, and sequentially performing first heat treatment and second heat treatment to obtain the modified sodium ion battery anode material.
In some preferred embodiments, the sodium ion battery positive electrode material has a chemical formula NaTMO 2, wherein TM is one or more of Ni, fe, mn, co, cu, al, cr.
In some preferred embodiments, in step S2, the temperature of the first heat treatment is 300-350 ℃, and the time of the first heat treatment is 4-8 hours.
In some preferred embodiments, in step S2, the temperature of the second heat treatment is 650-750 ℃, and the time of the second heat treatment is 2-5 hours.
In a part of preferred embodiments, in step S1, the mass ratio of the positive electrode material of the sodium ion battery to titanium tetrachloride is 50 (1-10).
In some preferred embodiments, in step S2, the flow rate of the ammonia gas is 10 to 100ml/min.
In some preferred embodiments, in step S1 and step S2, the protective atmosphere is a nitrogen atmosphere or an inert gas atmosphere.
In a part of preferred embodiments, in step S2, ammonia is introduced into the reaction furnace filled with the mixture under a protective atmosphere, and the first heat treatment and the second heat treatment are sequentially performed, wherein the first heat treatment and the second heat treatment comprise introducing a protective gas or a mixture of the protective gas and the ammonia into the reaction furnace filled with the mixture to discharge air, and then continuously introducing a mixture of the protective gas and the ammonia into the reaction furnace, and sequentially performing the first heat treatment and the second heat treatment.
In a third aspect, a sodium ion battery is provided, including the modified sodium ion battery positive electrode material described above or a modified sodium ion battery positive electrode material prepared by the preparation method described above.
Compared with the prior art, one or more of the technical schemes can achieve at least one of the following beneficial effects:
the provided modified positive electrode material adopts titanium nitride coated layer to carry out coating modification on the positive electrode material of the sodium ion battery, can obviously improve the structural stability and the electrical property of the positive electrode material of the sodium ion battery, reduces the capacity attenuation and prolongs the cycle life of the battery.
The in-situ coating modification can ensure that the coating material is compacter combined on the surface of the material, thereby further improving the problems of poor structural stability, rapid capacity attenuation and the like of the positive electrode material of the sodium ion battery.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are required in the embodiments or the description of the prior art will be briefly described, and it is obvious that the drawings in the following description are some embodiments of the present invention, and other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
Fig. 1 is an SEM image of the modified cathode material prepared in example 1.
Fig. 2 is a cycle performance chart of the button cell assembled in examples 1 to 3 and comparative examples 1 to 3.
Detailed Description
The applicant has found that the structural stability and electrical property of the positive electrode material of the sodium ion battery can be obviously improved by coating the titanium nitride@titanium nitride material on the surface of the substrate of the positive electrode material of the sodium ion battery, the capacity attenuation is reduced, and the cycle life of the battery is prolonged.
The invention provides a modified sodium ion battery anode material which comprises a sodium ion battery anode material substrate and a coating layer positioned on at least part of the surface of the substrate, wherein the coating layer is titanium nitride coated titanium nitride chloride. Titanium nitride is coated on the surface of the positive electrode material to form a titanium nitride@titanium nitride material, the titanium nitride is used as a layered material, na + can be removed and embedded, obvious change of a crystal structure is not caused, the titanium nitride has high conductivity and excellent structural stability, the positive electrode material can be isolated from reacting with electrolyte, the material circulation stability and the electrical performance are improved, the material structure can be effectively stabilized through composite coating, side reactions of the material and the electrolyte and other substances are prevented, and further the battery circulation life and capacity are improved.
In some preferred embodiments, the sodium ion battery positive electrode material matrix has a chemical formula NaTMO 2, wherein TM is one or more of Ni, fe, mn, co, cu, al, cr.
In some preferred embodiments, the mass of the coating layer is 1 to 10%, for example 1%, 2%, 3%, 4%, 5%, 6%, 7%, 8%, 9%, 10% of the mass of the matrix of the positive electrode material of the sodium ion battery.
In some preferred embodiments, the coating layer is obtained by first depositing titanium nitride on the surface of the positive electrode material substrate in situ, and then performing heat treatment. The binding force between the positive electrode material matrix and the surface coating layer can be improved through in-situ coating, so that the structural stability and the cycle stability are further improved.
The invention provides a preparation method of a modified sodium ion battery anode material, which comprises the following steps:
S1, grinding and mixing a sodium ion battery anode material and titanium tetrachloride under a protective atmosphere to obtain a mixture;
And S2, introducing ammonia gas into a reaction furnace filled with the mixture under a protective atmosphere, and sequentially performing first heat treatment and second heat treatment to obtain the modified sodium ion battery anode material.
In some preferred embodiments, the sodium ion battery positive electrode material has a chemical formula NaTMO 2, wherein TM is one or more of Ni, fe, mn, co, cu, al, cr.
In some preferred embodiments, in step S2, the temperature of the first heat treatment is 300 to 350 ℃, for example 300 ℃, 310 ℃, 320 ℃, 330 ℃, 340 ℃, 350 ℃, etc., and the time of the first heat treatment is 4 to 8 hours, for example 4 hours, 5 hours, 6 hours, 7 hours, 8 hours, etc.
In some preferred embodiments, in step S2, the temperature of the second heat treatment is 650-750 ℃, such as 650 ℃, 660 ℃, 670 ℃, 680 ℃, 690 ℃, 700 ℃, 710 ℃, 720 ℃, 730 ℃, 740 ℃, 750 ℃ and so on, and the time of the second heat treatment is 2-5 h, such as 2h, 3h, 4h, 5h and so on. The applicant has further found that the use of two heat treatments and the optimization of the heat treatment temperature is beneficial to improving the composition and microstructure of the coating layer, and further improving the chemical stability and high temperature stability of the cathode material.
In some preferred embodiments, in step S1, the mass ratio of the positive electrode material of the sodium ion battery to titanium tetrachloride is 50 (1-10), for example, 50:1, 50:2, 50:3, 50:4, 50:5, 50:6, 50:7, 50:8, 50:9, 50:10, etc.
In some preferred embodiments, in step S2, the flow rate of the ammonia gas is 10 to 100mL/min, for example, 10mL/min, 20mL/min, 30mL/min, 40mL/min, 50mL/min, 60mL/min, 70mL/min, 80mL/min, 90mL/min, 100mL/min, etc.
In some embodiments, in step S1 and step S2, the protective atmosphere may be a protective atmosphere conventional in the art, for example, may be a nitrogen atmosphere or an inert gas atmosphere (such as argon, helium, etc.).
In a part of preferred embodiments, in step S2, ammonia is introduced into the reaction furnace filled with the mixture under a protective atmosphere, and the first heat treatment and the second heat treatment are sequentially performed, wherein the first heat treatment and the second heat treatment comprise introducing a protective gas or a mixture of the protective gas and the ammonia into the reaction furnace filled with the mixture to discharge air, and then continuously introducing a mixture of the protective gas and the ammonia into the reaction furnace, and sequentially performing the first heat treatment and the second heat treatment.
Some embodiments of the present invention provide a sodium ion battery, including the modified sodium ion battery positive electrode material described above or the modified sodium ion battery positive electrode material prepared by the preparation method described above.
The invention will be described more fully hereinafter with reference to the accompanying drawings and preferred embodiments in order to facilitate an understanding of the invention, but the scope of the invention is not limited to the following specific embodiments.
Example 1:
The preparation method of the modified sodium ion battery positive electrode material is NaNi 1/3Fe1/3Mn1/3O2, and comprises the following steps:
(1) 5g of a sodium ion battery cathode material NaNi 1/3Fe1/3Mn1/3O2 g was mixed with 0.5g of titanium tetrachloride liquid and ground under an argon atmosphere to obtain a mixture.
(2) And placing the mixture into a burning boat, placing the burning boat into a tube furnace, introducing argon for a period of time to remove air in the tube furnace, heating to 340 ℃ for heat preservation for 7h, continuously heating to 680 ℃ for heat preservation for 4h, cooling to room temperature, introducing argon and ammonia mixed gas (volume ratio of 3:1) in the whole heat treatment process, and obtaining the titanium nitride@titanium nitride synergistic coating modified sodium ion battery anode material. An SEM image of the resulting modified sodium ion battery cathode material is shown in fig. 1.
Example 2:
The preparation method of the modified sodium ion battery anode material is NaNi 1/3Fe1/3Mn1/3O2, and comprises the following steps:
(1) 10g of a sodium ion battery cathode material NaNi 1/3Fe1/3Mn1/3O2 was mixed with 0.2g of titanium tetrachloride liquid under an argon atmosphere and ground to obtain a mixture.
(2) And (3) placing the mixture in a burning boat, placing the burning boat in a tube furnace, introducing argon for a period of time to remove air in the tube furnace, heating to 350 ℃ for heat preservation for 8 hours, continuously heating to 650 ℃ for heat preservation for 2 hours, cooling to room temperature, introducing argon and ammonia mixed gas (volume ratio of 3:1) in the whole heat treatment process, and obtaining the titanium nitride@titanium nitride synergistic coating modified sodium ion anode material.
Example 3
The preparation method of the modified sodium ion battery positive electrode material is NaNi 1/3Fe1/3Mn1/3O2, and comprises the following steps:
(1) 2g of a sodium ion battery cathode material NaNi 1/3Fe1/3Mn1/3O2 was mixed with 0.4g of titanium tetrachloride liquid under an argon atmosphere and ground to obtain a mixture.
(2) And (3) placing the mixture in a burning boat, placing the burning boat in a tube furnace, introducing argon for a period of time to remove air in the tube furnace, heating to 300 ℃ for heat preservation for 4 hours, continuously heating to 650 ℃ for heat preservation for 2 hours, cooling to room temperature, introducing argon and ammonia mixed gas (volume ratio of 3:1) in the whole heat treatment process, and obtaining the titanium nitride@titanium nitride synergistic coating modified sodium ion anode material.
Comparative example 1
The comparative example differs from example 1 only in that the sodium ion battery cathode material NaNi 1/3Fe1/3Mn1/3O2 was not subjected to coating modification.
Comparative example 2
The comparative example differs from example 1 only in that in step (2), the temperature is raised to 340℃and kept for 7 hours, and the temperature is continued to be raised to 400℃and kept for 4 hours.
Comparative example 3
The comparative example differs from example 1 only in that in step (2), the temperature is raised to 340℃and kept for 7 hours.
Assembling a sodium ion half cell:
The positive electrode materials obtained in the examples 1-3 and the comparative examples 1-3 are respectively weighed and ground according to the mass ratio of the positive electrode materials to the conductive graphite to the PVDF of 8:1:1, then a proper amount of N-methyl pyrrolidone (NMP) is dripped, grinding and stirring are continued to form uniform slurry, the slurry is uniformly coated on an aluminum foil by a die, the coating thickness is 200 mu m, and the aluminum foil is placed in a drying oven for drying at 90 ℃ for 10 hours, and then a wafer with the diameter of 12mm is cut. The wafer is used as an anode, the sodium sheet is used as a cathode, the electrolyte comprises lithium salt NaPF 6 and a solvent, the concentration of the lithium salt is 1mol/L, the solvent is EC:DEC:DMC, and the battery is assembled in a snap-fastener type battery assembling sequence in a glove box according to the volume ratio of 1:1:1.
Cell performance test:
and (3) performing performance test on the assembled battery, placing the assembled battery which stands for one night in a LAND2001CT battery test box for charge and discharge test, and performing test under the conditions of 25 ℃ and 2-4V of circulating voltage, wherein the number of circulating turns is 50. The relationship between the number of cycles and the specific discharge capacity is shown in FIG. 2.
As can be seen from fig. 2, compared with the battery assembled from the positive electrode material of comparative example 1, which is not subjected to coating modification, the coated modified positive electrode materials prepared in examples 1 to 3 and comparative example 2 have significantly improved cycle stability and electrical properties, and through analysis, the coated layer material itself has a layered structure, which can well realize Na ion deintercalation, and has better electrical conductivity and structural stability. And comparative example 3 has a higher specific discharge capacity than the battery assembled from the positive electrode material prepared in comparative example 1, which is also likely to be due to the fact that the coating material itself has a layered structure, can well achieve Na ion deintercalation, and has better conductivity.
As can be further seen from fig. 2, compared with example 1, the cycle performance of the battery assembled from the coated modified cathode material prepared in comparative example 2 is significantly reduced, which is probably because the second heat treatment process in the coating process in step (2) in example 1 is performed at a higher temperature, and the two phases in the generated coating material titanium chloride@titanium nitride have a better proportion, so that the thermal stability of the coating material is better and the comprehensive performance of the conductivity is better, and the cycle performance of the modified cathode material can be significantly improved on the premise that the specific capacity of the first discharge is not significantly reduced.
As is also apparent from fig. 2, the first discharge specific capacity of the battery assembled from the coated modified cathode material prepared in comparative example 3 was slightly improved, but the cycle performance was significantly reduced, as compared with example 1, which was analyzed, probably because only titanium nitride coating was possible to be achieved by performing the heat treatment only at 340 ℃, or a stable titanium nitride coated layer was not obtained, resulting in poor cycle performance.
As can also be seen from fig. 2, compared with example 1, the battery assembled from the coated modified cathode material prepared in example 3 has higher initial discharge specific capacity but lower cycle performance, which is analyzed to be likely due to the larger coating amount, thus the discharge specific capacity is improved more significantly, but the coating layer is difficult to be tightly coated on the surface of the cathode material due to the larger thickness of the coating layer, the coating layer may be easily dropped off during the cycle, and the two-stage heat treatment time is relatively short, the titanium nitride layer is thinner, resulting in relatively poor cycle stability.
As can also be seen from fig. 2, the battery assembled from the coated modified cathode material prepared in example 2 was inferior in both the first discharge specific capacity and the cycle performance compared to example 1, which was analyzed, probably because the coating amount was small, and thus the first discharge specific capacity was low, and the second heat treatment period resulted in a thin titanium nitride layer, resulting in relatively poor cycle stability.
The foregoing is merely a preferred embodiment of the present invention and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present invention, which are intended to be comprehended within the scope of the present invention.
Claims (9)
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