CN113113578A - Cathode material, preparation method thereof and lithium ion battery - Google Patents
Cathode material, preparation method thereof and lithium ion battery Download PDFInfo
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Abstract
The application relates to a positive electrode material, a preparation method thereof and a lithium ion battery, and belongs to the technical field of batteries. A preparation method of a positive electrode material comprises the following steps: mixing lithium salt, a positive electrode material precursor and an additive to obtain a mixture, wherein the additive is selected from H3PO4、LiH2PO4、Li2HPO4、Li3PO4、LiPO3、H3BO3、Li3BO3、Li2B8O13、Li2B4O7One or more of; and sintering the mixture to obtain the cathode material. The additive converts the magnetic substance in the anode material into gold without magnetism or with low magnetic moment through in-situ reaction with the magnetic substance at high temperatureThe composite material belongs to a compound, reduces the content of magnetic substances in the anode material, has good demagnetization effect, and improves the quality of the anode material and the safety performance of the lithium ion battery.
Description
Technical Field
The invention relates to the technical field of batteries, in particular to a positive electrode material, a preparation method thereof and a lithium ion battery.
Background
With the rapid development of new energy industries, lithium ion batteries are widely applied to mobile phones, digital cameras, notebook computers, unmanned planes, new energy automobiles, energy storage systems and the like by virtue of high energy density, rate capability and long service life. As is well known, the positive electrode material is one of the key core materials of the lithium ion battery, and the performance of the positive electrode material directly affects various performance indexes of the lithium ion battery. When magnetic substances such as iron (Fe), chromium (Cr), nickel (Ni), zinc (Zn), and the like exist in the positive electrode material, after the voltage of the battery in the formation stage reaches the oxidation-reduction potential of the magnetic foreign metal elements, the magnetic foreign metal elements are firstly oxidized and dissolved in the positive electrode, and then migrate to the negative electrode to be reduced into metal simple substances. The metal elementary substance at the negative electrode is accumulated to a certain degree to form metal dendrite to pierce the diaphragm, so that the self-discharge failure of the battery is caused, and the combustion and explosion of the lithium ion battery can be caused under severe conditions. Therefore, in the production process of the positive electrode material, it is important and critical to remove the magnetic substance in the material to the maximum possible extent.
At present, the traditional method for removing magnetic substances from the lithium ion battery anode material is mainly a physical method, and the permanent magnet or the electromagnet is used for carrying out adsorption and demagnetization for many times in the production and preparation process of the anode material. However, most of the materials originally have weak magnetism, and if the magnetic field intensity of the permanent magnet or the electromagnet is too high, the materials are easy to be magnetized, so that the content of magnetic impurities of the demagnetized positive electrode materials is increased; if the magnetic field intensity is too low, the magnetic impurities in the anode material can not be effectively adsorbed, and the purpose of demagnetizing can not be achieved. Therefore, the demagnetization effect of the physical method is poor, and the safety of the battery is affected.
Disclosure of Invention
Therefore, a method for preparing a positive electrode material with good demagnetization effect is needed.
In addition, a positive electrode material and a lithium ion battery are also provided.
A preparation method of a positive electrode material comprises the following steps:
mixing lithium salt, a positive electrode material precursor and an additive to obtain a mixture, wherein the additive is selected from H3PO4、LiH2PO4、Li2HPO4、Li3PO4、LiPO3、H3BO3、Li3BO3、Li2B8O13、Li2B4O7One or more of;
and sintering the mixture to obtain the cathode material.
The additive in the preparation method of the cathode material is selected from H3PO4、LiH2PO4、Li2HPO4、Li3PO4、LiPO3、H3BO3、Li3BO3、Li2B8O13、Li2B4O7The additive converts the magnetic substance in the anode material into a metal compound without magnetism or with low magnetic pole moment through in-situ reaction with the magnetic substance at high temperature, reduces the content of the magnetic substance in the anode material, has good demagnetization effect, and improves the quality of the anode material and the safety performance of the lithium ion battery.
In one embodiment, the molar ratio of the lithium salt, the positive electrode material precursor and the additive is a:1: b, wherein a is greater than or equal to 1.005 and less than or equal to 1.1, and b is greater than or equal to 0.0005 and less than or equal to 0.05.
In one embodiment, in the step of sintering the mixture, the sintering temperature is 710-1000 ℃.
In one embodiment, in the step of sintering the mixture, the temperature rise rate is 0.5 ℃/min to 10 ℃/min, and the heat preservation time is 8h to 24 h.
In one embodiment, after the step of sintering the mixture, a step of cooling is further included, wherein the rate of cooling is 3 ℃/min to 20 ℃/min.
In one embodiment, the step of sintering the mixture specifically comprises: and sintering the mixture under a sintering gas atmosphere, wherein the sintering gas is selected from one of oxygen, air and a mixed gas of oxygen and air.
In one embodiment, the positive electrode material precursor is NixCoyMn1-x-yO2Or NixCoyMn1-x-y(OH)2Wherein x is more than 0 and less than 1, y is more than 0 and less than 1, and 1-x-y is more than or equal to 0.
In one embodiment, the lithium salt is selected from LiOH, LiOH H2O、Li2CO3、LiHCO3、Li2O、Li2O2、Li2C2O4One or more of (a).
The cathode material prepared by the preparation method of the cathode material.
A lithium ion battery comprises the positive electrode material prepared by the preparation method of the positive electrode material or the positive electrode material.
Detailed Description
The present invention may be embodied in many different forms and is not limited to the embodiments described herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention.
A method of preparing a positive electrode material of an embodiment includes the steps of:
step S100: and mixing the lithium salt, the precursor of the positive electrode material and the additive to obtain a mixture.
In particular, the additive is selected from H3PO4、LiH2PO4、Li2HPO4、Li3PO4、LiPO3、H3BO3、Li3BO3、Li2B8O13、Li2B4O7One or more of (a). The demagnetizing additives are selected to react with magnetic substances in the material at high temperature in situ to convert the materials into metal compounds without magnetism or with low magnetic pole moment, so that the content of the magnetic substances in the anode material is reduced, the demagnetizing effect is good, and the quality of the anode material and the safety of the lithium ion battery are improvedCan be used. Meanwhile, the metal compound generated by the reaction is coated on the surface of the anode material to play a role in passivating the surface of the anode material, so that the contact between the anode material and the electrolyte can be effectively prevented in the working process of the lithium ion battery, the side reaction is reduced, and the service life of the lithium ion battery is prolonged.
Furthermore, the molar ratio of the lithium salt to the precursor of the positive electrode material to the additive is a:1: b, wherein a is more than or equal to 1.005 and less than or equal to 1.1, and b is more than or equal to 0.0005 and less than or equal to 0.05. The selection of the molar ratio range can ensure that the precursor of the positive electrode material is completely lithiated in the high-temperature lithiation reaction process, and improve the gram volume and crystallinity of the positive electrode material.
Specifically, the precursor of the positive electrode material is NixCoyMn1-x-yO2Or NixCoyMn1-x-y(OH)2Wherein x is more than 0 and less than 1, y is more than 0 and less than 1, and 1-x-y is more than or equal to 0. The precursor of the positive electrode material can fully react with lithium salt to generate the high-quality positive electrode material.
Specifically, the lithium salt is selected from LiOH, LiOH H2O、Li2CO3、LiHCO3、Li2O、Li2O2、Li2C2O4One or more of (a). The lithium salt can ensure the full reaction with the precursor of the positive electrode material, and improve the crystallinity of the positive electrode material.
Step S200: and sintering the mixture to obtain the cathode material.
Wherein, in the step of sintering the mixture, the sintering temperature is 710-1000 ℃. The sintering temperature can enable the lithium source to reach a molten state, the lithium source effectively reacts with the anode material to generate a layered anode material, and meanwhile, the demagnetization and magnetic substance reaction is promoted, and the demagnetization efficiency is improved.
Wherein, in the step of sintering the mixture, the heating rate is 0.5-10 ℃/min, and the heat preservation time is 8-24 h. The temperature rise program and the heat preservation time can ensure that the materials are heated uniformly and the anode material is developed completely, simultaneously, the demagnetizing additive and the magnetic substances in the materials can fully react, and reaction products can achieve a good coating effect on the anode material.
The sintering step of the mixture comprises the following specific steps: and sintering the mixture in a sintering gas atmosphere, wherein the sintering gas is selected from one of oxygen, air and a mixed gas of oxygen and air.
Further, the oxygen content in the sintering gas is 21% to 100%.
It should be noted that after the step of sintering the mixture, a step of cooling is further included, wherein the rate of cooling is 3 ℃/min to 20 ℃/min.
In the preparation method of the cathode material, the principle of removing the magnetic impurities is as follows:
the additive converts the magnetic substance in the material into a compound without magnetism or with low magnetic moment through in-situ reaction with the magnetic substance at high temperature, reduces the content of the magnetic substance in the anode material, and improves the quality of the anode material and the safety performance of the lithium ion battery; on the other hand, metal compounds formed by the reaction (e.g. FePO)4、FeBO3、Fe2(B8O13)3、Fe2(B4O7)3、CrPO4、CrBO3、Cr2(B8O13)3、Cr2(B4O7)3Etc.) is coated on the surface of the anode material, and plays a role in passivating the surface of the anode material.
Below with Fe2O3For example, the specific reaction formula is as follows:
Fe2O3+2Li3PO4→2FePO4+3Li2O
Fe2O3+2Li2HPO4→2FePO4+Li2O+2LiOH
Fe2O3+2LiH2PO4→2FePO4+H2O+2LiOH
Fe2O3+2H3PO4→2FePO4+3H2O
Fe2O3+6LiPO3→2Fe(PO3)3+3Li2O
Fe2O3+2Li3BO3→2FeBO3+3Li2O
Fe2O3+2H3BO3→2FeBO3+3H2O
Fe2O3+3Li2B8O13→Fe2(B8O13)3+3Li2O
Fe2O3+3Li2B4O7→Fe2(B4O7)3+3Li2O
the preparation method of the cathode material at least has the following advantages:
1) the additive in the preparation method of the cathode material is selected from H3PO4、LiH2PO4、Li2HPO4、Li3PO4、LiPO3、H3BO3、Li3BO3、Li2B8O13、Li2B4O7The additive converts the magnetic substance in the anode material into a metal compound without magnetism or with low magnetic pole moment through in-situ reaction with the magnetic substance at high temperature, reduces the content of the magnetic substance in the anode material, has good demagnetization effect, and improves the quality of the anode material and the safety performance of the lithium ion battery. With simultaneous reaction of the resulting metal compound (e.g. FePO)4、FeBO3、Fe2(B8O13)3、Fe2(B4O7)3、CrPO4、CrBO3、Cr2(B8O13)3、Cr2(B4O7)3Etc.) is coated on the surface of the anode material, plays a role in passivating the surface of the anode material, can effectively obstruct the contact of the anode material and electrolyte in the working process of the lithium ion battery, reduces side reactions and prolongs the service life of the lithium ion battery.
2) The preparation method of the cathode material is simple, energy-saving and efficient, and is suitable for industrial production.
The cathode material prepared by the preparation method of the cathode material. After the magnetic substances are removed from the positive electrode material, the stability and the dynamic performance of the positive electrode material can be improved, and the cycle and storage performance of the lithium ion battery can be improved.
A lithium ion battery comprises the positive electrode material prepared by the preparation method of the positive electrode material or the positive electrode material. The positive electrode material has a good demagnetization effect, and the safety of the lithium ion battery is effectively improved.
The following are specific examples:
example 1
The preparation steps of the cathode material of this example are as follows:
1) LiOH, ternary precursor (Ni)0.8Co0.1Mn0.1(OH)2)、Li3PO4Performing ball milling and full mixing according to the molar ratio of 1.04:1:0.002 to obtain a mixture;
2) the mixture was transferred to a muffle furnace under an oxygen atmosphere (O)2Content of 99.9 percent), heating to 785 ℃ at a heating rate of 2.5 ℃/min, then preserving heat for 12 hours, and finally cooling at a cooling rate of 5 ℃/min to obtain LiNi0.8Co0.11Mn0.1O2And (3) a positive electrode material.
Example 2
The preparation steps of the cathode material of this example are as follows:
1) LiOH, ternary precursor (Ni)0.8Co0.1Mn0.1(OH)2)、Li2HPO4Performing ball milling and full mixing according to the molar ratio of 1.04:1:0.002 to obtain a mixture;
2) the mixture was transferred to a muffle furnace under an oxygen atmosphere (O)2Content of 99.9 percent), heating to 785 ℃ at a heating rate of 2.5 ℃/min, then preserving heat for 12 hours, and finally cooling at a cooling rate of 5 ℃/min to obtain LiNi0.8Co0.11Mn0.1O2And (3) a positive electrode material.
Example 3
The preparation steps of the cathode material of this example are as follows:
1) LiOH, ternary precursor (Ni)0.8Co0.1Mn0.1(OH)2)、LiH2PO4Performing ball milling and full mixing according to the molar ratio of 1.04:1:0.002 to obtain a mixture;
2) transferring the mixture into a muffle furnace, heating to 785 ℃ at a heating rate of 2.5 ℃/min under the atmosphere of oxygen (the content of O2 is 99.9%), then preserving heat for 12h, and finally cooling at a cooling rate of 5 ℃/min to obtain LiNi0.8Co0.11Mn0.1O2And (3) a positive electrode material.
Example 4
The preparation steps of the cathode material of this example are as follows:
1) LiOH, ternary precursor (Ni)0.8Co0.1Mn0.1(OH)2)、LiPO3Performing ball milling and full mixing according to the molar ratio of 1.04:1:0.002 to obtain a mixture;
2) transferring the mixture into a muffle furnace, heating to 785 ℃ at a heating rate of 2.5 ℃/min under the atmosphere of oxygen (the content of O2 is 99.9%), then preserving heat for 12h, and finally cooling at a cooling rate of 5 ℃/min to obtain LiNi0.8Co0.11Mn0.1O2And (3) a positive electrode material.
Example 5
The preparation steps of the cathode material of this example are as follows:
1) ball-milling and fully mixing LiOH, a ternary precursor (Ni0.8Co0.1Mn0.1(OH)2) and Li3BO3 according to the molar ratio of 1.04:1: 0.002;
2) transferring the mixed materials in the first step into a muffle furnace, heating to 785 ℃ at a heating rate of 2.5 ℃/min under the atmosphere of O2(O2 content of 99.9%), then preserving heat for 12h, and finally cooling at a cooling rate of 5 ℃/min to obtain LiNi0.8Co0.11Mn0.1O2And (3) a positive electrode material.
Comparative example 1
The preparation steps of the positive electrode material of this comparative example were as follows:
1) LiOH, ternary precursor (Ni)0.8Co0.1Mn0.1(OH)2) Performing ball milling and fully mixing according to the molar ratio of 1.04:1 to obtain a mixture;
2) the mixture was transferred to a muffle furnace under an oxygen atmosphere (O)2Content of 99.9 percent), heating to 785 ℃ at a heating rate of 2.5 ℃/min, then preserving heat for 12 hours, and finally cooling at a cooling rate of 5 ℃/min to obtain LiNi0.8Co0.11Mn0.1O2And (3) a positive electrode material.
Comparative example 2
The preparation steps of the positive electrode material of this comparative example were as follows:
1) LiOH, ternary precursor (Ni)0.8Co0.1Mn0.1(OH)2) Performing ball milling and fully mixing according to the molar ratio of 1.04:1 to obtain a mixture;
2) the mixture was transferred to a muffle furnace under an oxygen atmosphere (O)2Content of 99.9 percent), heating to 785 ℃ at a heating rate of 2.5 ℃/min, then preserving heat for 12 hours, and finally cooling at a cooling rate of 5 ℃/min to obtain LiNi0.8Co0.11Mn0.1O2And (3) a positive electrode material.
3) Reacting LiNi0.8Co0.11Mn0.1O2Placing the positive electrode material into a container, placing two permanent magnets (the magnetic field intensity of the magnets is more than or equal to 6000GS) on the container wall, mechanically stirring the positive electrode material powder in the container to make the positive electrode material powder fully contact with the permanent magnets to obtain the LiNi subjected to physical demagnetization0.8Co0.11Mn0.1O2And (3) a positive electrode material.
And (3) testing:
the positive electrode materials obtained in example 1, example 2, example 3, example 4, example 5, comparative example 1 and comparative example 2 were subjected to the magnetic substance content and battery performance tests, and the results are shown in table 1.
The method for testing the magnetic substance of the material comprises the following steps: the content of the magnetic substances is tested by adopting an ICP method, and the specific method is that 190g of anode material is put into a 500ml plastic bottle, a magnetic rod is put into the plastic bottle, 300ml of ultrapure water is added, and the magnetic rod is enabled to fully adsorb the magnetic substances in the material under the action of a roller blending instrument. And after adsorption, carrying out ICP (inductively coupled plasma) test on the magnetic substance on the magnetic rod to obtain the content of the magnetic substance in the anode material.
The preparation method of the battery comprises the following steps: adding a certain amount of carbon black conductive agent (super P) and PVDF binder into the prepared positive electrode material, preparing positive electrode active slurry in a double-planet stirring tank, coating the positive electrode active slurry on an aluminum foil through an extrusion coating machine, and preparing the positive electrode sheet through the working procedures of rolling, slitting, cutting pieces and the like. The negative pole piece is prepared by adopting an artificial graphite system, adding a certain amount of carbon black conductive agent (super P) and a water-based binder, preparing negative active slurry in a double-planet stirring tank, coating the negative active slurry on copper foil through an extrusion coating machine, and performing the working procedures of rolling, slitting, cutting and the like. Assembling the prepared positive and negative pole pieces and the composite diaphragm together through a winding machine, and then carrying out the manufacturing procedures of hot pressing, welding of a pole lug, vacuum baking, liquid injection, formation and the like to obtain the battery.
The normal temperature circulation and 45 ℃ circulation test method comprises the following steps: and testing the cycle performance in a constant temperature room corresponding to the test temperature. The method comprises the steps of firstly carrying out 1C/1C charging and discharging on a battery according to the designed specific capacity, determining the actual 1C discharging capacity, and carrying out subsequent tests according to the actual 1C capacity, wherein the test voltage interval is 2.8-4.3V.
60 ℃ storage test method: after the battery was fully charged, the battery was stored in an incubator at 60 ℃ and the test battery capacity recovery rate was taken out every 15 days.
The method for testing the thermal runaway temperature of the fully charged core comprises the following steps: and (3) fully charging the battery cell, then placing the battery cell in a 130 ℃ hot box, and simultaneously detecting the thermal runaway temperature of the battery cell by adopting a thermal sensor.
TABLE 1
As can be seen from Table 1, compared with comparative examples 1-2, the content of the magnetic substances of the positive electrode materials prepared in examples 1-5 is obviously lower than that of the positive electrode material prepared by the conventional method and the positive electrode material subjected to physical demagnetization; the lithium ion battery adopting the cathode material prepared in the embodiments 1 to 5 is obviously superior to the lithium ion battery adopting the cathode material prepared by the conventional method and the lithium ion battery adopting the cathode material subjected to physical demagnetization in the aspects of normal temperature cycle, 45 ℃ cycle, 60 ℃ storage and full charge core thermal runaway temperature.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (10)
1. The preparation method of the cathode material is characterized by comprising the following steps of:
mixing lithium salt, a positive electrode material precursor and an additive to obtain a mixture, wherein the additive is selected from H3PO4、LiH2PO4、Li2HPO4、Li3PO4、LiPO3、H3BO3、Li3BO3、Li2B8O13、Li2B4O7One or more of;
and sintering the mixture to obtain the cathode material.
2. The method for preparing the positive electrode material according to claim 1, wherein the molar ratio of the lithium salt, the positive electrode material precursor and the additive is a:1: b, wherein a is 1.005 or less and is 1.1 or less, and b is 0.0005 or less and is 0.05 or less.
3. The method for producing a positive electrode material according to claim 1, wherein the sintering temperature in the step of sintering the mixture is 710 ℃ to 1000 ℃.
4. The method according to claim 3, wherein in the step of sintering the mixture, the temperature increase rate is 0.5 ℃/min to 10 ℃/min, and the holding time is 8h to 24 h.
5. The method according to claim 1, further comprising a step of cooling the mixture after the step of sintering the mixture, wherein the cooling rate is 3 ℃/min to 20 ℃/min.
6. The method for preparing a positive electrode material according to claim 1, wherein the step of sintering the mixture is specifically: and sintering the mixture under a sintering gas atmosphere, wherein the sintering gas is selected from one of oxygen, air and a mixed gas of oxygen and air.
7. The method for producing a positive electrode material according to claim 1, wherein the positive electrode material precursor is NixCoyMn1-x-yO2Or NixCoyMn1-x-y(OH)2Wherein x is more than 0 and less than 1, y is more than 0 and less than 1, and 1-x-y is more than or equal to 0.
8. The method for producing a positive electrode material according to claim 1, wherein the lithium salt is selected from the group consisting of LiOH and LiOH-H2O、Li2CO3、LiHCO3、Li2O、Li2O2、Li2C2O4One or more of (a).
9. A positive electrode material produced by the method for producing a positive electrode material according to any one of claims 1 to 8.
10. A lithium ion battery, characterized by comprising the positive electrode material obtained by the method for producing a positive electrode material according to any one of claims 1 to 8 or the positive electrode material according to claim 9.
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