CN113651368A - Method for preparing sodium ion battery anode materials with different crystal forms through lithium doping regulation and control - Google Patents
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Abstract
The invention discloses a method for preparing sodium ion battery anode materials with different crystal forms by lithium doping regulation and control, wherein the chemical formula of the anode material is Na0.7NixFeyMn1‑x‑y‑zLizO2Wherein x + y is more than 0 and less than or equal to 0.4, z is more than 0 and less than or equal to 0.4, and the doping amount of Li is regulated and controlled by regulating and controlling the value of z, so that the obtained material is a P2 phase material, a P2/O3 mixed phase material or an O3 phase material. According to the invention, lithium is doped in the transition metal layer, so that a Na-O-Li structure can be formed to activate the redox reaction of oxygen, thereby providing extra capacity; the invention relates to aThe structure of the positive electrode material of the sodium-ion battery can be regulated and controlled by changing the lithium doping proportion, so that materials of a P2 phase, an O3 phase and a P2/O3 mixed phase are obtained; the coprecipitation method adopted by the invention is simple and feasible, the material with regular appearance and uniform size can be obtained, and the obtained material has better electrochemical performance within the voltage range of 1.5-4.5V.
Description
Technical Field
The invention belongs to the field of positive electrode materials of sodium-ion batteries, and particularly relates to a method for preparing Na with different crystal forms by lithium-doped regulation and control0.7NixFeyMn1-x-yO2A method of preparing a cathode material.
Background
Along with the development of renewable energy and the urgent need of the information era, the demand of people on energy storage devices is higher and higher. The lithium ion battery has the advantages of high energy density, high working voltage, long cycle life and the like, and is widely applied to various energy storage devices. However, the problems of lithium price rise and insufficient storage capacity and the like promote people to search for a novel energy storage system with rich resources and low price. The sodium ion battery is proposed in 1980 at first, and due to the characteristics of rich raw material sources, relatively low price, environmental friendliness and the like, the sodium ion battery receives more and more attention in recent years and is a battery system which is most expected to be applied to large-scale electrochemical energy storage. Currently, the research is more on the layered transition metal oxide materials, the layered transition metal oxides can be mainly classified into P2 and O3 types according to the sodium ion coordination structure and the interlayer stacking sequence, the english letters P and O represent that the sodium ion coordination structure is a rhombohedral column and an octahedron, and the numbers 2 and 3 represent that the interlayer stacking sequence is ABBAAB … and abcabcabc …. The P2 type material is a low-sodium phase (Na < 1), and Na in the low-sodium phase is contained during the charge and discharge of the battery+Ions directly migrate among the three diamond columns, and the volume of the three diamond columns is relatively large, so that sodium ions have a lower migration energy barrier; the O3 type material is typically a sodium rich phase (Na ═ 1), although more can be storedSodium, but Na+The migration needs to be via tetrahedrons, which have a smaller volume and therefore a slower diffusion rate of sodium ions. Therefore, the P2 type material has a relatively low capacity, but has the advantage of a high discharge rate, and is suitable for special occasions requiring a high charge-discharge rate, such as field communication equipment. The O3 type material has relatively low charge and discharge multiplying power, but has the characteristic of high charge and discharge capacity because more sodium ions can be accommodated in a material system, and is suitable for environments with high capacity requirement and low multiplying power requirement, such as power grid energy storage and the like.
Patent CN110277555A discloses O3 type NaNi0.4Mn0.4Fe0.2O2The specific discharge capacity of the positive electrode material of the sodium-ion battery is 168.1mAh/g in the current density of 0.1C and the voltage range of 2-4V. Patent CN111244415A discloses P2/O3 type Na0.85Li0.15(Mn0.67Ni0.13Fe0.2)0.85O2The positive electrode material of the sodium-ion battery has the specific discharge capacity of 132mAh/g within the current density of 100mA/g and the voltage range of 1.6-4.5V. At present, the synthesis of P2 and O3 type materials is realized by changing the sodium content of an alkali metal layer, and other simple and controllable synthesis methods are lacked.
Disclosure of Invention
Aiming at the problems, the invention provides a method for preparing sodium ion battery anode materials with different crystal forms by lithium doping regulation and control, and the technical problems to be solved are as follows: in P2 type material Na0.7NixFeyMn1-x-yO2On the basis of the method, alkali metal lithium is doped to form a Na-O-Li structure, oxidation-reduction reaction of oxygen is activated under high voltage to provide extra capacity, and meanwhile, the structure of the positive electrode material of the sodium-ion battery is regulated and controlled by changing the lithium doping ratio, so that materials of a P2 phase, an O3 phase and a P2/O3 mixed phase are obtained.
In order to solve the technical problems, the invention adopts the following technical scheme:
a method for preparing sodium ion battery anode materials with different crystal forms by lithium doping regulation and control is characterized in that: the chemical formula of the positive electrode material of the sodium-ion battery is Na0.7NixFeyMn1-x-y-zLizO2Wherein x + y is more than 0 and less than or equal to 0.4, z is more than 0 and less than or equal to 0.4, and the doping amount of Li is regulated and controlled by regulating and controlling the value of z, so that the obtained material is a P2 phase material, a P2/O3 mixed phase material or an O3 phase material. The method specifically comprises the following steps:
(1) uniformly mixing a lithium source, a nickel source, an iron source and a manganese source in a mixed solution of deionized water and an organic solvent according to a molar ratio to obtain a metal salt solution with the total concentration of 0.1-0.5M;
(2) dissolving a precipitant in a mixed solution of deionized water and an organic solvent to obtain a precipitant solution with the concentration of 0.1-0.5M;
(3) quickly pouring the precipitant solution into a metal salt solution, continuously stirring and reacting for 4-8h, and drying the obtained suspension in a drying oven at the temperature of 60-80 ℃ for 10-15h to obtain a precursor;
(4) fully mixing the precursor with a sodium source, calcining for 4-6h at the temperature of 400-450 ℃ in the air atmosphere, and calcining for 12-15h at the temperature of 750-850 ℃ to obtain a target product Na0.7NixFeyMn1-x-y-zLizO2。
Further, the ratio of the molar amount of the precipitant used to the total molar amount of the lithium source, the nickel source, the iron source, and the manganese source was 1.5: 1.
Further: in the step (1), the lithium source is at least one of lithium acetate, lithium chloride and lithium nitrate; the nickel source is at least one of nickel acetate, nickel sulfate and nickel nitrate; the iron source is at least one of iron acetate, ferrous sulfate and ferric nitrate; the manganese source is at least one of manganese acetate, manganese sulfate and manganese nitrate;
further: in the step (2), the precipitant is at least one of oxalic acid, sodium hydroxide and ammonium hydrogen oxalate.
Further, in the step (1) and the step (2), the organic solvent is at least one of methanol, ethanol and isopropanol.
Compared with the prior art, the invention has the beneficial effects that:
1. the invention can form Na-O-Li structure by introducing alkali metal lithium into the transition metal layerThe O2 p electrons are positioned near the Fermi level so as to generate redox reaction to improve extra capacity, and meanwhile, the lithium doping improves the disorder degree of the transition metal and inhibits the structural distortion caused by transition metal layer migration in the charging and discharging process. Further, P2 type layered metal oxide Na0.7NixFeyMn1-x-yO2The valence of Mn in the transition metal layer is between +3 valence and +4 valence, and according to the charge conservation rule, the valence of Mn can be improved by doping +1 valence lithium in the transition metal layer so as to change the coordination mode of Mn and oxygen, thereby further obtaining P2/O3 mixed phase and O3 phase materials.
2. The coprecipitation preparation method adopted by the invention has simple process and easy implementation, can respectively obtain the sodium-ion battery anode material with regular appearance and uniform size of the P2 phase, the O3 phase and the P2/O3 mixed phase, and has better electrochemical performance within the voltage range of 1.5-4.5V.
Drawings
FIG. 1 is an X-ray diffraction pattern of the products obtained in examples 1, 2 and 3;
FIG. 2 is a graph showing the cycle performance (100mA/g current density) of the products obtained in examples 1, 2 and 3 at 1.5 to 4.5V.
Detailed Description
The following examples are given for the detailed implementation and specific operation of the present invention, but the scope of the present invention is not limited to the following examples.
Example 1: p2 type Na ion battery0.7Ni0.1Fe0.1Mn0.6Li0.2O2Preparation of
(1) 0.102g of lithium acetate, 0.735g of manganese acetate, 0.124g of nickel acetate and 0.202g of ferric nitrate were dissolved in a mixed solution of 10mL of water and 50mL of ethanol to obtain a metal salt solution. 0.946g of oxalic acid was dissolved in a mixture of 10mL of water and 50mL of ethanol to obtain a precipitant solution. And quickly pouring the precipitant solution into the metal salt solution, continuously stirring and reacting for 6h, and drying the obtained suspension in an oven at the temperature of 80 ℃ for 15h to obtain the precursor.
(2) Mixing the precursor with0.185g of sodium carbonate is fully ground and mixed, calcined for 4 hours at 450 ℃ in air atmosphere and then calcined for 12 hours at 800 ℃ to obtain P2 type Na0.7Ni0.1Fe0.1Mn0.6Li0.2O2And (3) a positive electrode material.
Mixing the anode material obtained in the embodiment with acetylene black and PVDF according to the mass ratio of 7:2:1, adding a proper amount of NMP, stirring for 6 hours to prepare slurry, then coating the slurry on an aluminum foil with the thickness of 75 mu M, drying, cutting into electrode sheets, taking metal sodium as a cathode, taking WHATMAN G/F glass fiber as a diaphragm and 1M NaClO4The solution was used as an electrolyte and a CR2032 type cell was prepared in a glove box filled with argon gas.
Example 2: P2/O3 type sodium ion battery Na0.7Ni0.1Fe0.1Mn0.5Li0.3O2Preparation of
(1) 0.153g of lithium acetate, 0.613g of manganese acetate, 0.124g of nickel acetate and 0.202g of ferric nitrate were dissolved in a mixed solution of 10mL of water and 50mL of ethanol to obtain a metal salt solution. 0.946g of oxalic acid was dissolved in a mixture of 10mL of water and 50mL of ethanol to obtain a precipitant solution. And quickly pouring the precipitant solution into the metal salt solution, continuously stirring and reacting for 6h, and drying the obtained suspension in an oven at the temperature of 80 ℃ for 15h to obtain the precursor.
(2) Fully grinding and mixing the precursor with 0.185g of sodium carbonate, calcining for 4h at 450 ℃ in air atmosphere, and then calcining for 12h at 800 ℃ to obtain P2/O3 type Na0.7Ni0.1Fe0.1Mn0.5Li0.3O2And (3) a positive electrode material.
Mixing the anode material obtained in the embodiment with acetylene black and PVDF according to the mass ratio of 7:2:1, adding a proper amount of NMP, stirring for 6 hours to prepare slurry, then coating the slurry on an aluminum foil with the thickness of 75 mu M, drying, cutting into electrode sheets, taking metal sodium as a cathode, taking WHATMAN G/F glass fiber as a diaphragm and 1M NaClO4The solution was used as an electrolyte and a CR2032 type cell was prepared in a glove box filled with argon gas.
Example 3: o3 type Na ion battery0.7Ni0.1Fe0.1Mn0.4Li0.4O2Preparation of
(1) 0.204g of lithium acetate, 0.490g of manganese acetate, 0.124g of nickel acetate and 0.202g of ferric nitrate were dissolved in a mixed solution of 10mL of water and 50mL of ethanol to obtain a metal salt solution. 0.946g of oxalic acid was dissolved in a mixture of 10mL of water and 50mL of ethanol to obtain a precipitant solution. And quickly pouring the precipitant solution into the metal salt solution, continuously stirring and reacting for 6h, and drying the obtained suspension in an oven at the temperature of 80 ℃ for 15h to obtain the precursor.
(2) Fully grinding and mixing the precursor with 0.185g of sodium carbonate, calcining for 4h at 450 ℃ in air atmosphere, and then calcining for 12h at 800 ℃ to obtain O3 type Na0.7Ni0.1Fe0.1Mn0.4Li0.4O2And (3) a positive electrode material.
Mixing the anode material obtained in the embodiment with acetylene black and PVDF according to the mass ratio of 7:2:1, adding a proper amount of NMP, stirring for 6 hours to prepare slurry, then coating the slurry on an aluminum foil with the thickness of 75 mu M, drying, cutting into electrode sheets, taking metal sodium as a cathode, taking WHATMAN G/F glass fiber as a diaphragm and 1M NaClO4The solution was used as an electrolyte and a CR2032 type cell was prepared in a glove box filled with argon gas.
FIG. 1 shows the X-ray diffraction patterns of the cathode materials obtained in examples 1-3, and it can be seen that the products obtained in examples 1-3 are P2 phase, P2/O3 mixed phase and O3 phase, respectively.
FIG. 2 is a graph of the cycling performance (100mA/g current density) of the positive electrode materials obtained in examples 1-3 at 1.5-4.5V, from which it can be seen that: the discharge capacity of the anode material obtained in the embodiment 1 can reach 131.9mAh/g, the discharge capacity after 50 circles is 100.4mAh/g, and the capacity retention rate is 76.1%; the discharge capacity of the anode material obtained in the embodiment 2 can reach 97.2mAh/g, the discharge capacity after 50 circles is 97.1mAh/g, and the capacity retention rate is 99.9%; the discharge capacity of the positive electrode material obtained in example 3 can reach 126.3mAh/g, the discharge capacity after 50 circles is 115.0mAh/g, and the capacity retention rate is 91.1%.
The present invention is not limited to the above exemplary embodiments, and any modification, equivalent replacement, and improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (6)
1. A method for preparing sodium ion battery anode materials with different crystal forms through lithium doping regulation and control is characterized in that: the chemical formula of the positive electrode material of the sodium-ion battery is Na0.7NixFeyMn1-x-y-zLizO2Wherein x + y is more than 0 and less than or equal to 0.4, z is more than 0 and less than or equal to 0.4, and the doping amount of Li is regulated and controlled by regulating and controlling the value of z, so that the obtained material is a P2 phase material, a P2/O3 mixed phase material or an O3 phase material.
2. The method of claim 1, comprising the steps of:
(1) uniformly mixing a lithium source, a nickel source, an iron source and a manganese source in a mixed solution of deionized water and an organic solvent according to a molar ratio to obtain a metal salt solution with the total concentration of 0.1-0.5M;
(2) dissolving a precipitant in a mixed solution of deionized water and an organic solvent to obtain a precipitant solution with the concentration of 0.1-0.5M;
(3) quickly pouring the precipitant solution into a metal salt solution, continuously stirring and reacting for 4-8h, and drying the obtained suspension in a drying oven at the temperature of 60-80 ℃ for 10-15h to obtain a precursor;
(4) fully mixing the precursor with a sodium source, calcining for 4-6h at the temperature of 400-450 ℃ in the air atmosphere, and calcining for 12-15h at the temperature of 750-850 ℃ to obtain a target product Na0.7NixFeyMn1-x-y-zLizO2。
3. The method of claim 1, wherein: the ratio of the molar amount of precipitant used to the total molar amount of lithium, nickel, iron and manganese sources was 1.5: 1.
4. The method of claim 2, wherein: in the step (1), the lithium source is at least one of lithium acetate, lithium chloride and lithium nitrate; the nickel source is at least one of nickel acetate, nickel sulfate and nickel nitrate; the iron source is at least one of iron acetate, ferrous sulfate and ferric nitrate; the manganese source is at least one of manganese acetate, manganese sulfate and manganese nitrate.
5. The method of claim 2, wherein: in the step (2), the precipitant is at least one of oxalic acid, sodium hydroxide and ammonium hydrogen oxalate.
6. The method of claim 2, wherein: in the step (1) and the step (2), the organic solvent is at least one of methanol, ethanol and isopropanol.
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Cited By (10)
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| CN114132971A (en) * | 2021-11-26 | 2022-03-04 | 西安交通大学 | Sodium ion battery positive electrode material with composite symbiotic structure, preparation method and sodium ion battery |
| CN114551848A (en) * | 2021-12-16 | 2022-05-27 | 南京大学深圳研究院 | Li-doped sodium-ion battery cathode material and preparation method thereof |
| CN114715953A (en) * | 2022-03-14 | 2022-07-08 | 中国科学技术大学 | Method for preparing Cu and Zn doped layered oxide sodium ion battery anode material with assistance of precursor and application of method |
| CN114725346A (en) * | 2022-03-31 | 2022-07-08 | 钠远新材科技(无锡)有限公司 | Sodium ion battery positive electrode material, preparation method thereof and sodium ion battery |
| CN114937774A (en) * | 2022-05-16 | 2022-08-23 | 中国科学技术大学 | P2 and P3 mixed phase layered oxide sodium ion battery positive electrode material and preparation method and application thereof |
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| SEUNG-MIN OH ET AL.: "High Capacity O3-Type Na[Li0.05(Ni0.25Fe0.25Mn0.5)0.95]O2 Cathode for Sodium Ion Batteries", 《CHEMISTRY OF MATERIALS》 * |
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| CN115893526B (en) * | 2022-12-21 | 2024-05-28 | 广东佳纳能源科技有限公司 | Nickel-iron-manganese layered hydroxide precursor for sodium ion battery, preparation method and application |
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Application publication date: 20211116 |