CN114583121A - Anion-doped modified lithium ion battery positive electrode material and preparation method and application thereof - Google Patents
Anion-doped modified lithium ion battery positive electrode material and preparation method and application thereof Download PDFInfo
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- H01M4/505—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy
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Abstract
The invention discloses an anion-doped modified lithium ion battery anode material, wherein the chemical formula of the lithium ion battery anode material is Li [ ]1‑x‑2yNixCoyMn2‑2x‑y/3]O2‑zSezWherein x is more than 0.5 and less than or equal to 1; y is more than or equal to 0 and less than or equal to 0.2; x +2y is more than or equal to 0.776 and less than or equal to 1; z is more than 0 and less than or equal to 0.1; the invention also discloses a preparation method and application of the anion-doped modified lithium ion battery anode material; the selenium-doped modified lithium ion battery cathode material prepared by the invention shows excellent rate performance and cycle in lithium ion battery applicationThe performance of the lithium ion battery enables the lithium ion battery to have higher power density and better cycle life.
Description
Technical Field
The invention belongs to the technical field of energy storage and modification conversion, and particularly relates to an anion-doped modified lithium ion battery anode material.
The invention also relates to a preparation method and application of the anion-doped modified lithium ion battery anode material.
Background
The lithium ion battery has the advantages of high energy density, long cycle life and the like, and is widely applied to the fields of mobile power supplies, electric automobiles, aerospace and the like. In the lithium ion battery, the electrode material is the core of the lithium ion battery, and determines multiple key performances of the lithium ion battery, such as specific energy, cycle life and load resistance. At present, the next application stage of the lithium ion battery is mainly in the aspect of electric automobiles, and the most critical is the development of the power type lithium ion battery, wherein the cost of the lithium ion battery is mainly focused on the anode material of the lithium ion battery. Therefore, the development of a lithium ion battery cathode material with high specific energy and long cycle life is the current research focus at home and abroad, and how to further improve the energy density of the lithium ion battery cathode material is a primary problem in order to meet the application of the lithium ion battery cathode material in the aspect of electric automobiles.
The surface doping is to optimize the surface interface of the target material particles by adopting one or more physical and chemical means, thereby improving the comprehensive performance of the material. At present, most researchers use a plurality of elements to carry out cation doping modification on the anode material, and the result shows that the anode material doped with different elements has different effects, but most of the cation doping sacrifices the specific capacity of the anode material, so that the cycle performance of the anode material is improved. The anion-doped modified cathode material can improve the electrochemical performance of the cathode material theoretically under the condition of not losing the capacity of the cathode material.
The existing preparation method of the cathode material of the anion-doped lithium ion battery mainly comprises a sol-gel-high-temperature sintering method and the like, for example, in the patent publication CN103943841A, the problems of rough modification effect, various selected materials, complex process, difficult control and the like exist, although the discharge capacity of the cathode material is improved, water resources are seriously wasted, and the environment is not friendly. Therefore, the preparation method which has the advantages of effectiveness, simple operation, low cost and environmental friendliness is imperative to be found.
Disclosure of Invention
The invention aims to provide an anion-doped modified lithium ion battery cathode material, which solves the problem of poor high-rate performance of a lithium ion battery.
The second purpose of the invention is to provide a preparation method of the anion-doped modified lithium ion battery cathode material.
The third purpose of the invention is to provide the application of the anion-doped modified lithium ion battery cathode material in the preparation of the lithium ion battery.
The first technical scheme adopted by the invention is that the anion doping modified lithium ion battery anode material has a chemical formula of Li [ Li ]1-x-2yNixCoyMn2-2x-y/3]O2-zSezWherein x is more than 0.5 and less than or equal to 1; y is more than or equal to 0 and less than or equal to 0.2; x +2y is more than or equal to 0.776 and less than or equal to 1; z is more than 0 and less than or equal to 0.1.
The first technical solution of the present invention is also characterized in that:
the thickness of the modified layer of the negative ion doped modified lithium ion battery positive electrode material is 1-3 nm.
The second technical scheme adopted by the invention is that the preparation method of the anion-doped modified lithium ion battery anode material is implemented according to the following steps:
step 1, a selenium source and a lithium ion battery anode material are respectively placed at the upstream and the downstream of a tube furnace;
and 3, controlling the upstream and downstream temperatures, and performing a heating and heat preservation process to obtain the selenium-doped lithium ion battery anode material.
The second technical scheme of the invention is also characterized in that:
wherein the mass ratio of the selenium source to the lithium ion battery anode material in the step 1 is not less than 0.01 and not more than 0.5;
wherein the inert gas in the step 2 is nitrogen or argon;
controlling the downstream temperature in the step 3, heating to 300-400 ℃, preserving heat for 5 hours, simultaneously heating the upstream temperature to 400-700 ℃ at the speed of 1-5 ℃/min, and preserving heat for 3 hours;
the invention has the beneficial effects that:
according to the preparation method of the selenium-doped modified lithium ion battery cathode material, the selenium source with low decomposition temperature or boiling point, selenium and oxygen electronic structure similarity and easy reaction with the cathode material in inert atmosphere are fully utilized, oxygen on the surface of the cathode material can be replaced, an ultrathin, uniform and good-stability selenium-doped cathode material modified layer is formed on the surface of the cathode material, the side reaction of an electrode active material and an electrolyte is effectively relieved, the cycle life of the cathode material is prolonged, the electronic and lithium ion conductivity of the electrode active material is improved, and the electrochemical performance of the lithium ion battery is comprehensively improved.
Drawings
FIG. 1 shows LiNi before selenium doping in an embodiment of a method for preparing an anion-doped modified lithium ion battery cathode material according to the present invention0.8Co0.1Mn0.1O2Positive electrode material (a) and selenium-doped modified LiNi0.8Co0.1Mn0.1O2Scanning electron microscope images of the positive electrode material (b);
FIG. 2 shows LiNi before and after selenium doping in an embodiment of a method for preparing an anion-doped modified lithium ion battery cathode material according to the present invention0.8Co0.1Mn0.1O2A positive electrode material Se XPS spectrogram;
FIG. 3 shows LiNi in an embodiment of a method for preparing an anion-doped modified lithium ion battery cathode material according to the present invention0.8Co0.1Mn0.1O2A high-resolution scanning transmission electron microscope image of the anode material;
FIG. 4 shows LiNi before and after doping in the preparation method of the anion-doped modified lithium ion battery cathode material0.8Co0.1Mn0.1O2A cycle performance curve diagram of the anode material;
FIG. 5 shows L before and after doping in the preparation method of the anion-doped modified lithium ion battery anode materiali1.224Ni0.552Co0.163Mn0.064O2Cycle performance curve diagram of anode material.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings and specific embodiments.
The invention provides an anion-doped modified lithium ion battery anode material, which has a chemical formula of Li [ Li ]1-x- 2yNixCoyMn2-2x-y/3]O2-zSezWherein x is more than 0.5 and less than or equal to 1; y is more than or equal to 0 and less than or equal to 0.2; x +2y is more than or equal to 0.776 and less than or equal to 1; z is more than 0 and less than or equal to 0.1;
the invention also provides a preparation method of the anion-doped modified lithium ion battery anode material, which comprises the following steps:
step 1, taking a selenium source and a positive electrode material, respectively placing the selenium source and the positive electrode material at the upstream and the downstream of a tubular furnace, wherein the selenium source comprises the following components: the mass ratio of the positive electrode material is more than or equal to 0.01 and less than or equal to 0.5;
step 3, controlling the downstream temperature, raising the temperature to 400 ℃ at 300-5 ℃/min, preserving the heat for 5h, raising the upstream temperature to 700 ℃ at 400-5 ℃/min, and preserving the heat for 3 h; obtaining the selenium-doped modified lithium ion battery anode material, wherein the thickness of the doped modified layer is 1-3 nm;
preferably, the mass ratio of the selenium source to the positive electrode material in the step 1 is between 0.1 and 0.2.
Preferably, the temperature of the upstream part in the step 2 is increased to 500 ℃, and the holding time is 3 h; the downstream temperature is raised to 400 ℃ and the holding time is 5 h.
The selenium-doped modified lithium ion battery anode material is prepared by an advanced physical chemical vapor deposition method, and has the advantages of one-step operation, simple process and mild conditions. The method has the advantages of extremely small material consumption of the doping raw material, low cost, simple operation and environmental protection, and overcomes the defects of complicated process, low material utilization rate, rough modification effect, poor controllability and the like in the traditional doping modification method;
the selenium-doped modified lithium ion battery cathode material prepared by the invention shows excellent rate performance and cycle performance in the application of a lithium ion battery, so that the lithium ion battery has higher power density and better cycle life;
the invention further provides application of the anion-doped modified lithium ion battery cathode material in preparation of a lithium ion battery; the method comprises the following steps: fully mixing selenium-doped modified lithium ion positive electrode material, conductive carbon black (conductive agent), polyvinylidene fluoride (PVDF binder) and a small amount of N-methylpyrrolidone (NMP) by grinding to form uniform paste, coating the uniform paste on an aluminum foil substrate to be used as a test electrode, wherein the electrolyte is 1M LiPF6With dimethyl carbonate (DMC) and diethylene carbonate (DEC) solutions, specifically 1M LiPF 6/EC: DMC: DEC (V: V ═ 1:1:1) or 1M LiPF 6/EC: DMC (V: V ═ 3:7), and button cell was made with metallic lithium as counter electrode; the experimental results show that: selenium-doped modified positive electrode material LiNi0.8Co0.1Mn0.1O2After 100 times of charge and discharge tests, the capacity can still reach 186mA h/g.
Example 1
(1) Taking the following components in percentage by weight: selenium powder and LiNi of 10.8Co0.1Mn0.1O2The anode materials are respectively placed at the upstream and the downstream of the tube furnace;
(2) introducing inert gas such as nitrogen or argon to replace the atmosphere in the tubular furnace so as to keep the inert atmosphere in the tubular furnace;
(3) controlling the downstream temperature, heating to 300 ℃, preserving heat for 5 hours, simultaneously heating the upstream temperature to 400 ℃ at the speed of 3 ℃/min, and preserving heat for 3 hours; obtaining the selenium-doped lithium ion battery anode material;
(4) weighing 0.64g of the prepared selenium-doped lithium ion battery positive electrode material, adding 0.08g of conductive carbon black as a conductive agent and 0.08g of PVDF as a binder, dropwise adding a small amount of NMP, grinding and uniformly mixing to form uniform paste, coating the paste on an aluminum foil to serve as a test electrode, and performing electrochemical measurement on the paste by using a ratio of 1M LiPF 6/EC: DMC: DEC (V: V: V: 1:1) is used as electrolyte, the charge and discharge performance is tested, and the current density is 50 mAh/g;
the material characteristics and electrochemical properties of the selenium-doped lithium ion battery cathode material prepared by the embodiment are shown in the following chart:
FIG. 1 is a scanning electron microscope image, from which it can be seen that the unmodified lithium ion battery anode material has a spheroidal structure composed of primary particles with the size of 300-700nm, and the surface is smooth; the surface of the selenium-doped lithium ion battery anode material particles is provided with a uniformly distributed modified layer, and the surface is kept intact;
FIG. 2 is a Se 3p XPS full spectrum diagram, which shows that the surface of the lithium ion battery anode material contains selenium element mainly formed by Se after selenium doping2-The form exists;
FIG. 3 is a transmission electron microscope image of a selenium-doped lithium ion cathode material indicating that a uniform selenium-doped modification layer is formed on the surface of the cathode material after selenium doping;
fig. 4 is a cycle performance diagram of the lithium ion battery anode material before selenium doping and the lithium ion battery anode material after selenium doping, which shows that the specific capacity of the electrode made of the selenium-doped lithium ion battery anode material can be maintained at 186mA h/g after 100 cycles in a voltage window of 3-4.5V at room temperature and at a current density of 50mA h/g, and the capacity retention rate is as high as 90%, which is much higher than that of the undoped sample.
Example 2
(1) Taking the following components in percentage by weight: selenium powder and LiNi of 10.9Co0.05Mn0.0.5O2The anode materials are respectively placed at the upstream and the downstream of the tube furnace;
(2) before the experiment, introducing nitrogen or inert gases such as argon and the like, and replacing the atmosphere in the tube furnace to keep an inert atmosphere in the tube furnace;
(3) controlling the downstream temperature, heating to 400 ℃, preserving heat for 5h, simultaneously heating the upstream temperature to 700 ℃ at the speed of 4 ℃/min, and preserving heat for 3 h; obtaining the selenium-doped lithium ion battery anode material;
(4) weighing 0.64g of the prepared selenium-doped lithium ion battery positive electrode material, adding 0.08g of conductive carbon black as a conductive agent and 0.08g of PVDF as a binder, dropwise adding a small amount of NMP, grinding and uniformly mixing to form uniform paste, coating the paste on an aluminum foil to serve as a test electrode, and performing electrochemical measurement on the paste by using a ratio of 1M LiPF 6/EC: DMC: DEC (V: V: V: 1:1) is used as electrolyte, the charge and discharge performance is tested, and the current density is 50 mA/g;
the phosphorus-doped modified LiNi prepared in this example was used0.9Co0.5Mn0.5O2The positive electrode material is used for preparing an electrode and is assembled with a metal lithium sheet into a button cell, the cut-off voltage is 4.5V, when the button cell is subjected to constant current discharge at room temperature, the specific capacity can still be kept at 180mA h/g after the button cell is cycled for 100 times, and good cycle performance is shown.
Example 3
(1) Taking the following components in percentage by weight: selenium powder and Li of 11.224Ni0.552Co0.163Mn0.064O2The anode materials are respectively placed at the upstream and the downstream of the tube furnace;
(2) before the experiment, introducing nitrogen or inert gases such as argon and the like, and replacing the atmosphere in the tube furnace to keep an inert atmosphere in the tube furnace;
(3) controlling the downstream temperature, raising the temperature to 400 ℃ and preserving heat for 5h, raising the upstream temperature to 600 ℃ at the speed of 5 ℃/min, and preserving heat for 5 h; obtaining the selenium-doped lithium ion battery anode material;
(4) weighing 0.64g of the prepared selenium-doped lithium ion battery positive electrode material, adding 0.08g of conductive carbon black as a conductive agent and 0.08g of PVDF as a binder, dropwise adding a small amount of NMP, grinding and uniformly mixing to form uniform paste, coating the paste on an aluminum foil to serve as a test electrode, and performing electrochemical measurement on the paste by using a ratio of 1M LiPF 6/EC: DMC (V: V is 3:7) is used as electrolyte, the charge and discharge performance is tested, and the current density is 50 mA/g;
phosphorus-modified Li prepared in this example1.224Ni0.552Co0.163Mn0.064O2The anode material is used for preparing an electrode and is assembled with a metal lithium sheet into a button cell, the cut-off voltage is 4.8V, the specific capacity can still be maintained at 252mA h/g after the battery is cycled for 100 times in a figure 5 when the battery is discharged at a constant current at room temperature, and good cycle performance is shown.
Claims (7)
1. The anion-doped modified lithium ion battery cathode material is characterized in that the chemical formula of the lithium ion battery cathode material is Li[Li1-x-2yNixCoyMn2-2x-y/3]O2-zSezWherein x is more than 0.5 and less than or equal to 1; y is more than or equal to 0 and less than or equal to 0.2; x +2y is more than or equal to 0.776 and less than or equal to 1; z is more than 0 and less than or equal to 0.1.
2. The anion-doped modified lithium ion battery cathode material according to claim 1, wherein the thickness of the modified layer of the anion-doped modified lithium ion battery cathode material is 1-3 nm.
3. The preparation method of the anion-doped modified lithium ion battery anode material is characterized by comprising the following steps of:
step 1, a selenium source and a lithium ion battery anode material are respectively placed at the upstream and the downstream of a tube furnace;
step 2, introducing inert gas, replacing the atmosphere in the tube furnace, and keeping an inert atmosphere in the tube furnace;
and 3, controlling the upstream and downstream temperatures, and performing a heating and heat preservation process to obtain the selenium-doped lithium ion battery anode material.
4. The preparation method of the anion-doped modified lithium ion battery cathode material according to claim 3, wherein the mass ratio of the selenium source to the lithium ion battery cathode material in the step 1 is 0.01-0.5.
5. The method for preparing the anion-doped modified lithium ion battery cathode material according to claim 3, wherein the inert gas in the step 2 is nitrogen or argon.
6. The preparation method of the anion-doped modified lithium ion battery cathode material according to claim 3, wherein in the step 3, the downstream temperature is controlled, the temperature is raised to 300-400 ℃ and kept for 5 hours, and meanwhile, the upstream temperature is raised to 400-700 ℃ at a speed of 1-5 ℃/min and kept for 3 hours.
7. The anion-doped modified lithium ion battery cathode material is applied to the preparation of the lithium ion battery.
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