CN108682840B - Nanometer (Mg)0.2Co0.2Ni0.2Cu0.2Zn0.2) Preparation method and application of O - Google Patents
Nanometer (Mg)0.2Co0.2Ni0.2Cu0.2Zn0.2) Preparation method and application of O Download PDFInfo
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Abstract
The invention discloses a nano (Mg)0.2Co0.2Ni0.2Cu0.2Zn0.2) Preparation method and application of O. Mixing magnesium oxide, cobalt oxide, nickel oxide, copper oxide and zinc oxide powder according to the stoichiometric ratio of equimolar metal atoms, and performing ball milling, cold pressing to form blocks and ball milling again to obtain nano (Mg)0.2Co0.2Ni0.2Cu0.2Zn0.2) And O. Using the nano (Mg)0.2Co0.2Ni0.2Cu0.2Zn0.2) O powder comprises the following components in percentage by mass: (Mg)0.2Co0.2Ni0.2Cu0.2Zn0.2) 70% of O nano powder, 20% of acetylene black and 10% of binder. The invention adopts a high-temperature solid phase method to synthesize (Mg) in one step0.2Co0.2Ni0.2Cu0.2Zn0.2) O block material, and high-energy ball milling to obtain nanometer (Mg) with sheet structure0.2Co0.2Ni0.2Cu0.2Zn0.2) O powder, simple operation process, low cost and no pollution. The present invention utilizes the nano (Mg)0.2Co0.2Ni0.2Cu0.2Zn0.2) The lithium ion battery cathode material prepared by O can keep higher specific capacity under the charging and discharging current density of 100mA/g, and has excellent cycling stability.
Description
Technical Field
The invention belongs to the field of nano material preparation and new energy devices, and particularly relates to nano (Mg)0.2Co0.2Ni0.2Cu0.2Zn0.2) Preparation method and application of O.
Background
The lithium ion battery has excellent characteristics, so that the lithium ion battery becomes a battery system with better comprehensive performance at present and becomes one of important new energy sources at present and in the future. With the further expansion of the application field from civil information industry (portable electronic devices such as mobile phones and notebook computers) to energy traffic (electric vehicles and the like), and the further expansion of the application field to the use as an indispensable important energy source for military equipment in the field of national defense and military, higher requirements are provided for the charge-discharge specific capacity and the rapid charge-discharge capacity of the lithium ion battery. The cathode material is one of the key factors for determining the comprehensive performance of the lithium ion battery. Research on negative electrode materials of lithium ion batteries has mainly focused on carbon materials, silicon materials and transition metal oxide materials. At present, the main problems of the commercial carbon negative electrode materials are: the actual specific capacity is low (about 300 mAh/g-330 mAh/g, the theoretical specific capacity is 372mAh/g), the first irreversible loss is large, the multiplying power charge-discharge performance is poor, the lithium intercalation potential is low, the deposition of metal lithium dendrite can be caused on the graphite surface in the charge-discharge process, and certain potential safety hazard exists. The main problem of the silicon negative electrode material is that the electrode material expands more than 400% in volume during charging and discharging, so the electrode material is easy to be crushed, and the charging and discharging specific capacity of the electrode material is rapidly reduced. Therefore, actively exploring a novel lithium ion battery cathode material system with high charge-discharge specific capacity, small capacity attenuation rate and good safety performance has become a hot spot of domestic and overseas concurrent research. Among available negative electrode materials, the transition metal oxide material occupies a large part and is a negative electrode material system with a relatively promising application prospect.
Early studies on transition metal oxides as lithium-storing negative electrode materials, such as Fe2O3、TiO2、 WO2And MoO2And the like. However, their studies have fallen into a valley due to a certain irreversible capacity loss after the first charge-discharge cycle. In 2000, j.m. tarascon et al reported nanoscale transition metal oxides MO (M ═ Co, Fe, Ni, or Cu) as negative electrode materials for lithium ion batteries in Nature. The electrochemical performance of the oxide with the nanoscale is obviously different from that of the conventional material, the reversible specific capacity is between 600mAh/g and 800mAh/g, and the oxide has higher capacity retention rate. The nano metal oxide shows certain advantages in the aspects of improving the lithium storage capacity of the negative electrode material and improving the cycle life of the lithium ion battery.
The material is a novel ceramic material which appears in recent years and has the characteristic that a plurality of metal elements are uniformly dispersed at the atomic level. And the material has a delayed diffusion effect, so that the microstructure of the material is stable. The current research focus on the following aspects: (1) fluorite type (Hf)0.25Zr0.25Ce0.25Y0.25)O2-δSuch as the literature [ Joshua g., Mojtaba s., Kenneth v.and Jian l.j.eur.ceram.soc.2018, 38,3578.](ii) a (2) A series of perovskite type (Sr)0.5Ba0.5)(Zr0.2Sn0.2Ti0.2Hf0.2Nb0.2)O3Such as the literature [ Sicong j., Tao h., Joshua g.and Jian l.script material, 2018,142,116.](ii) a (3) Phase stability and lattice distortion in materials, such as the literature [ g.anand, Alex p.wynn, Christopher m.handley and collagen l.freeman, Acta Materialia, 2018,146,119.](ii) a (4) Quinary synthesis and film preparation methods, such as literature [ Rost, C.M., Sachet, E., Borman, T., Mobilligh, A., Dickey, E.C., Hou, D., Jones, J.L., Curtarolo, S.&Maria,J.-P.Nature Comm.2015,6,8485]；(5)
Anomalous permittivity phenomena of materials, such as the documents [ berrandan, d., Franger, s., Dragoe, d., Meena, A.K. & Dragoe, n.phys. status Solidi RRL 2016,10,328 ]; (6)
doping with Li+、Na+、K+、Ga3+Has an ultrafast ionic conductivity, as described in Berardan, D., Franger, S., Meena, A.&Dragoe,N.J.Mater.Chem.A 2016,4,9536.]；(7)Cu2+The effect of the ion content ratio on lattice distortion, as described in the literature [ Berardan, d.; meena, a.k.; franger, s.; herrero, c.; dragoe, n.j.alloy.comp.2017,704,693.](ii) a (8) crystal structures studied using synchrotron radiation X-ray fine absorption spectroscopy, as described in literature [ Rost, c.m.; rak, z.; brenner, d.w.; maria, j.p.j.am.ceram.soc.2017,100,2732.](ii) a (9) a synthetic method of ternary to seven-element high-entropy rare earth oxide, such as documents [ Djenadic, R.; sarkar, a.; clemens, o.; loho, c.; botros, m.; chakravadhanua, v.s.k.; kubel, c.; bhattacharya, s.s.; gandhif, a.s.; hahn, h.mater.res.lett.,2017,5, 102.]。
In order to meet the requirement of commercialization of the oxide negative electrode material of the lithium ion battery, reduce the cost of raw materials, simplify the preparation process of the oxide negative electrode material, and solve the defects of low charge-discharge specific capacity, poor cycle stability and the like of the traditional metal oxide negative electrode material, the oxide negative electrode material is a technical problem to be solved at present.
Disclosure of Invention
In order to solve the above problems in the prior art, the present invention provides a nano (Mg)0.2Co0.2Ni0.2Cu0.2Zn0.2) Preparation method and application of O.
In a first aspect, the present invention provides a nano (Mg)0.2Co0.2Ni0.2Cu0.2Zn0.2) The preparation method of O comprises the following steps:
step (1): firstly weighing magnesium oxide, cobalt oxide, nickel oxide, copper oxide and zinc oxide powder with the purity higher than 99.99 percent according to the stoichiometric ratio of equimolar metal atoms, and filling ZrO2In a ball milling tank; then ZrO is filled according to the ball-to-material ratio of 10:1-20:12Grinding balls;
step (2): sealing the ball milling tank, vacuumizing and then filling inert gas;
and (3): installing the ball milling tank on a high-energy ball mill, covering an outer cover, and continuously ball milling for 3-6 hours at the rotating speed of 1000-2000r/min to obtain composite powder with the particle size of 10-100 nm;
and (4): filling the obtained composite powder into a die, and performing cold press molding by using a tablet press to prepare a pressed blank of 1cm multiplied by 0.5 cm;
and (5): placing the pressed compact in a muffle furnace for high-temperature calcination, and then slowly cooling to room temperature to obtain (Mg)0.2Co0.2Ni0.2Cu0.2Zn0.2) O block bodies;
and (6): mixing the (Mg)0.2Co0.2Ni0.2Cu0.2Zn0.2) Continuously high-energy ball-milling the O block in an ethanol-isopropanol mixed solvent for 60-70 hours to obtain nano (Mg) with the grain diameter of 10-100nm0.2Co0.2Ni0.2Cu0.2Zn0.2) And (4) O powder.
With reference to the first aspect, in a first possible embodiment of the first aspect, the cobalt oxide in step (1) is Co3O4Or CoO; the nickel oxide is Ni2O3Or NiO.
With reference to the first aspect, in a second possible embodiment of the first aspect, the method of placing the compact in a muffle furnace for high-temperature calcination in step (5) is: the green compact is heated to 1200-1500 ℃ in a muffle furnace at the heating rate of 1-10 ℃/min, is calcined at the constant temperature for 20-30 hours, and is then slowly cooled to the room temperature along with the furnace.
With reference to the first aspect, in a third possible embodiment of the first aspect, the nano (Mg) obtained in step (6)0.2Co0.2Ni0.2Cu0.2Zn0.2) The O powder is of nano-sheet structure and has a BET specific surface area of 26.38-32.43m2g-1The pore diameter is between 2 and 13 nm.
In a second aspect, the present invention provides a method of using the above-mentioned nano (Mg)0.2Co0.2Ni0.2Cu0.2Zn0.2) The lithium ion battery cathode material prepared by O comprises the following components in percentage by mass: (Mg)0.2Co0.2Ni0.2Cu0.2Zn0.2) 70% of O nano powder, 20% of acetylene black and 10% of binder.
Compared with the prior art, one or more technical schemes provided by the invention have the following technical effects or advantages:
the invention adopts a high-temperature solid phase method to synthesize (Mg) in one step0.2Co0.2Ni0.2Cu0.2Zn0.2) O block material, and high-energy ball milling to obtain nanometer (Mg) with sheet structure0.2Co0.2Ni0.2Cu0.2Zn0.2) O powder, simple operation process, low cost and no pollution.
The present invention utilizes the nano (Mg)0.2Co0.2Ni0.2Cu0.2Zn0.2) Charging the lithium ion battery cathode material prepared by O at 100mA/gThe high specific capacity can be kept under the discharge current density, and the high specific capacity has excellent cycling stability. The multiplying power charge-discharge test shows that the material still has good stability under the charge-discharge current density which is increased in sequence, and when the current density is increased to 1000mA/g, the specific capacity is stabilized at 690 mAh/g; when the current density is increased to 2000mA/g, the specific capacity is stabilized at 600 mAh/g; and when the current density is reduced to 100mA/g, the specific capacity can be basically and completely recovered, and the specific capacity is stabilized to be about 1090 mAh/g.
Drawings
FIG. 1 shows the nano- (Mg) obtained in example 1 of the present invention0.2Co0.2Ni0.2Cu0.2Zn0.2) An XRD pattern of O;
FIG. 2 shows the results of example 1 of the present invention in terms of nano- (Mg)0.2Co0.2Ni0.2Cu0.2Zn0.2) O field emission scanning electron microscopy images;
FIG. 3 shows the results of example 1 of the present invention in terms of nano- (Mg)0.2Co0.2Ni0.2Cu0.2Zn0.2) A field emission transmission electron microscopy image of O;
FIG. 4 (a) shows the nano (Mg) obtained in example 1 of the present invention0.2Co0.2Ni0.2Cu0.2Zn0.2) N of O2Adsorption/desorption isotherm curves;
FIG. 4 (b) shows the nano (Mg) obtained in example 1 of the present invention0.2Co0.2Ni0.2Cu0.2Zn0.2) Barrett-Joyner-Halenda pore size distribution curve for O;
FIG. 5 shows the cycle characteristics of the lithium ion battery negative electrode material obtained in example 5 of the present invention measured at different charging and discharging current densities;
FIG. 6 shows the cycle characteristics of the negative electrode material of the lithium ion battery obtained in example 5 of the present invention at a current density of 100 mA/g.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all, embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
It will be understood by those skilled in the art that, unless otherwise defined, all terms (including 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. It will be further understood that terms, such as those defined in commonly used dictionaries, should be interpreted as having a meaning that is consistent with their meaning in the context of the prior art and will not be interpreted in an idealized or overly formal sense unless expressly so defined herein.
Example 1
Nano (Mg)0.2Co0.2Ni0.2Cu0.2Zn0.2) The preparation method of O comprises the following steps:
(1) MgO (0.1mol, 4.030g) with purity higher than 99.99 percent and Co are weighed3O4(0.0333mol， 8.027g)、Ni2O3(0.05mol, 8.269g), CuO (0.1mol, 7.954g) and ZnO (0.1mol, 8.139g), ZrO was charged2In a ball milling tank; then ZrO is filled according to the ball-to-material ratio of 10:1-20:12Grinding balls;
(2) sealing the ball milling tank, vacuumizing and filling inert gas;
(3) installing the ball milling tank on a high-energy ball mill, covering an outer cover, and continuously ball milling for 3-6 hours at the rotating speed of 1000-2000r/min to obtain composite powder with the particle size of 10-100 nm;
(4) filling the obtained composite powder into a die, and performing cold press molding by using a tablet press to prepare a pressed blank of 1cm multiplied by 0.5 cm;
(5) placing the pressed compact in a muffle furnace for high-temperature calcination at 1200 ℃ for 20 hours, and then cooling to room temperature along with the furnace to obtain (Mg)0.2Co0.2Ni0.2Cu0.2Zn0.2) O block bodies;
(6) mixing the (Mg)0.2Co0.2Ni0.2Cu0.2Zn0.2) Continuously high-energy ball milling the O block in an ethanol-isopropanol mixed solvent for 60 hours to obtain nano (Mg) with the grain diameter of 10-100nm0.2Co0.2Ni0.2Cu0.2Zn0.2) And (4) O powder.
FIGS. 1 to 4 show the results obtained in example 1 (Mg)0.2Co0.2Ni0.2Cu0.2Zn0.2) And performing characterization on the O nano powder to obtain a picture. Wherein:
FIG. 1 shows (Mg)0.2Co0.2Ni0.2Cu0.2Zn0.2) The XRD pattern of the O nanopowder, in which the abscissa is the 2 diffraction angle and the ordinate is the diffraction intensity, is very mild to the line PDF- #45-0946 of magnesium oxide having a face centered cubic crystal structure in JCPDS database, indicating that the (Mg) produced in the examples of the present invention is very mild0.2Co0.2Ni0.2Cu0.2Zn0.2) The O nanopowder being single phase (Mg)0.2Co0.2Ni0.2Cu0.2Zn0.2) And (3) O solid solution.
FIGS. 2 and 3 are views of (Mg) shown in example 10.2Co0.2Ni0.2Cu0.2Zn0.2) Field emission scanning electron microscopy and field emission transmission electron microscopy of O nanopowders indicating the (Mg)0.2Co0.2Ni0.2Cu0.2Zn0.2) The O nano powder is of a nano flaky structure.
FIG. 4 (a) is (Mg) described in example 10.2Co0.2Ni0.2Cu0.2Zn0.2) N of O nanopowder2The Adsorption/Desorption isotherm curve is shown in FIG. 4 (b), which is a Barrett-Joyner-Halenda Pore size distribution curve, wherein Relative pressure is Relative pressure, quality Adsorbed is Adsorption capacity, Pore Diameter is Pore Diameter, Pore Volume is Pore Volume, Adsorption is Adsorption, and Desorption is Desorption. FIG. 4 (a) and FIG. 4 (b) show that (Mg)0.2Co0.2Ni0.2Cu0.2Zn0.2) BET ratio of O nanopowderSurface area 26.38m2g-1The aperture is 2-10 nm.
Example 2
Nano (Mg)0.2Co0.2Ni0.2Cu0.2Zn0.2) The preparation method of O comprises the following steps:
(1) MgO (0.1mol, 4.030g), CoO (0.1mol, 7.493g), NiO (0.1mol, 7.469g), CuO (0.1mol, 7.954g) and ZnO (0.1mol, 8.139g) with the purity higher than 99.99 percent are weighed and charged with ZrO2In a ball milling tank; then ZrO is filled according to the ball-to-material ratio of 10:1-20:12Grinding balls;
(2) sealing the ball milling tank, vacuumizing and filling inert gas;
(3) installing the ball milling tank on a high-energy ball mill, covering an outer cover, and continuously ball milling for 3-6 hours at the rotating speed of 1000-2000r/min to obtain composite powder with the particle size of 10-100 nm;
(4) filling the obtained composite powder into a die, and performing cold press molding by using a tablet press to prepare a pressed blank of 1cm multiplied by 0.5 cm;
(5) placing the pressed compact into a muffle furnace for high-temperature calcination at 1300 ℃, keeping the temperature for 20 hours, and then cooling to room temperature along with the furnace to obtain (Mg)0.2Co0.2Ni0.2Cu0.2Zn0.2) O block bodies;
(6) mixing the (Mg)0.2Co0.2Ni0.2Cu0.2Zn0.2) Continuously high-energy ball milling the O block in an ethanol-isopropanol mixed solvent for 60 hours to obtain (Mg) with the particle size of 10-100nm0.2Co0.2Ni0.2Cu0.2Zn0.2) And (4) O nano powder.
Example 3
Nano (Mg)0.2Co0.2Ni0.2Cu0.2Zn0.2) The preparation method of O comprises the following steps:
(1) MgO (0.1mol, 4.030g) with purity higher than 99.99 percent and Co are weighed3O4(0.0333mol, 8.027g), NiO (0.1mol, 7.469g), CuO (0.1mol, 7.954g) and ZnO (0.1mol, 8.139g), and ZrO was charged2In a ball milling tank; then according to the ball material ratio of 10:1-201 charging ZrO2Grinding balls;
(2) sealing the ball milling tank, vacuumizing and filling inert gas;
(3) installing the ball milling tank on a high-energy ball mill, covering an outer cover, and continuously ball milling for 3-6 hours at the rotating speed of 1000-2000r/min to obtain composite powder with the particle size of 10-100 nm;
(4) filling the obtained composite powder into a die, and performing cold press molding by using a tablet press to prepare a pressed blank of 1cm multiplied by 0.5 cm;
(5) placing the pressed compact in a muffle furnace for high-temperature calcination at 1200 ℃ for 25 hours, and then cooling to room temperature along with the furnace to obtain (Mg)0.2Co0.2Ni0.2Cu0.2Zn0.2) O block bodies;
(6) mixing the (Mg)0.2Co0.2Ni0.2Cu0.2Zn0.2) Continuously high-energy ball milling the O block in an ethanol-isopropanol mixed solvent for 60 hours to obtain (Mg) with the particle size of 10-100nm0.2Co0.2Ni0.2Cu0.2Zn0.2) And (4) O nano powder.
Example 4
Nano (Mg)0.2Co0.2Ni0.2Cu0.2Zn0.2) The preparation method of O comprises the following steps:
(1) weighing MgO (0.1mol, 4.030g), CoO (0.1mol, 7.493g) and Ni with the purity higher than 99.99 percent2O3(0.05mol, 8.269g), CuO (0.1mol, 7.954g) and ZnO (0.1mol, 8.139g), ZrO was charged2In a ball milling tank; then ZrO is filled according to the ball-to-material ratio of 10:1-20:12Grinding balls;
(2) sealing the ball milling tank, vacuumizing and filling inert gas;
(3) installing the ball milling tank on a high-energy ball mill, covering an outer cover, and continuously ball milling for 3-6 hours at the rotating speed of 1000-2000r/min to obtain composite powder with the particle size of 10-100 nm;
(4) filling the obtained composite powder into a die, and performing cold press molding by using a tablet press to prepare a pressed blank of 1cm multiplied by 0.5 cm;
(5) placing the pressed compact into a muffle furnace for high-temperature calcination at 1300 ℃, keeping the temperature for 20 hours, and then cooling to room temperature along with the furnace to obtain (Mg)0.2Co0.2Ni0.2Cu0.2Zn0.2) O block bodies;
(6) mixing the (Mg)0.2Co0.2Ni0.2Cu0.2Zn0.2) Continuously high-energy ball-milling the O block in an ethanol-isopropanol mixed solvent for 65 hours to obtain (Mg) with the particle size of 10-100nm0.2Co0.2Ni0.2Cu0.2Zn0.2) And (4) O nano powder.
The products obtained in examples 2 to 4 were characterized and gave very similar test results to those of example 1. The XRD patterns of the products obtained in examples 2, 3 and 4 have diffraction peaks with the same peak positions and peak shapes as those in FIG. 1, which shows that the products prepared in examples 2 to 4 have a face-centered cubic crystal structure (Mg)0.2Co0.2Ni0.2Cu0.2Zn0.2) O solid solution; n is a radical of2The adsorption/desorption test result shows that the BET specific surface area is 26.38-32.43m2g-1The pore diameter is between 2 and 13 nm.
Example 5
Using the (Mg)0.2Co0.2Ni0.2Cu0.2Zn0.2) The lithium ion battery cathode material prepared from O nano powder comprises the following components in percentage by mass: (Mg)0.2Co0.2Ni0.2Cu0.2Zn0.2) 70% of O nano powder, 20% of acetylene black and 10% of binder.
FIG. 5 is a graph illustrating the Cycle characteristics of the negative electrode material of the lithium ion battery in example 5 measured at charging and discharging current densities of 100mA/g, 200mA/g, 500mA/g, 1000mA/g, 2000mA/g, 3000mA/g, 1000mA/g, 200mA/g and 100mA/g, where Cycle Number is the Number of cycles, Specific Capacity is the Specific Capacity, Discharge Capacity is the Discharge Capacity, and Charge Capacity is the Charge Capacity.
FIG. 6 is the Cycle characteristics of the negative electrode material of the lithium ion battery in example 5 at a current density of 100mA/g, wherein Cycle Number is the Cycle Number, Specific Capacity is the Specific Capacity, Discharge Capacity is the Discharge Capacity, and Charge Capacity is the Charge Capacity.
It can be seen from fig. 5 and fig. 6 that the lithium ion battery has good stability under the sequentially increased charge and discharge current densities, and when the current density is increased to 1000mA/g, the specific capacity is stabilized at 690 mAh/g; when the current density is increased to 2000mA/g, the specific capacity is stabilized at 600 mAh/g; and when the current density is reduced to 100mA/g, the specific capacity can be basically and completely recovered, and the specific capacity is stabilized to be about 1090 mAh/g.
The invention is not limited to the above alternative embodiments, and any other various forms of products can be obtained by anyone in the light of the present invention, but any changes in shape or structure thereof, which fall within the scope of the present invention as defined in the claims, fall within the scope of the present invention.
Claims (5)
1. Nano (Mg) for lithium ion battery cathode material0.2Co0.2Ni0.2Cu0.2Zn0.2) The preparation method of the O powder is characterized by comprising the following steps:
step (1): firstly weighing magnesium oxide, cobalt oxide, nickel oxide, copper oxide and zinc oxide powder with the purity higher than 99.99 percent according to the stoichiometric ratio of equimolar metal atoms, and filling ZrO2In a ball milling tank; then ZrO is filled according to the ball-to-material ratio of 10:1-20:12Grinding balls;
step (2): sealing the ball milling tank, vacuumizing and then filling inert gas;
and (3): installing the ball milling tank on a high-energy ball mill, covering an outer cover, and continuously ball milling for 3-6 hours at the rotating speed of 1000-2000r/min to obtain composite powder with the particle size of 10-100 nm;
and (4): filling the obtained composite powder into a die, and performing cold press molding by using a tablet press to prepare a pressed blank of 1cm multiplied by 0.5 cm;
and (5): placing the pressed compact in a muffle furnace for high-temperature calcination, and then slowly cooling to room temperature to obtain (Mg)0.2Co0.2Ni0.2Cu0.2Zn0.2) O block bodies;
and (6): mixing the (Mg)0.2Co0.2Ni0.2Cu0.2Zn0.2) Continuously high-energy ball-milling the O block in an ethanol-isopropanol mixed solvent for 60-70 hours to obtain nano (Mg) with the grain diameter of 10-100nm0.2Co0.2Ni0.2Cu0.2Zn0.2) O powder, said nano (Mg)0.2Co0.2Ni0.2Cu0.2Zn0.2) The O powder is of a nano flaky structure.
2. The production method according to claim 1, wherein the cobalt oxide in step (1) is Co3O4Or CoO; the nickel oxide is Ni2O3Or NiO.
3. The production method according to claim 1, wherein the green compact is subjected to high-temperature calcination in a muffle furnace in the step (5) by: the green compact is heated to 1200-1500 ℃ in a muffle furnace at the heating rate of 1-10 ℃/min, is calcined at the constant temperature for 20-30 hours, and is then slowly cooled to the room temperature along with the furnace.
4. The method according to claim 1, wherein the nano (Mg) obtained in the step (6)0.2Co0.2Ni0.2Cu0.2Zn0.2) The BET specific surface area of the O powder is 26.38-32.43m2 g-1The pore diameter is between 2 and 13 nm.
5. The lithium ion battery negative electrode material is characterized by comprising the following components in percentage by mass: nano (Mg) prepared by the preparation method of claim 10.2Co0.2Ni0.2Cu0.2Zn0.2) 70% of O powder, 20% of acetylene black and 10% of binder.
Priority Applications (1)
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| CN110364717B (en) * | 2019-07-24 | 2020-08-11 | 东北大学秦皇岛分校 | Spinel type high-entropy oxide electrode material and preparation method thereof |
| WO2021040932A1 (en) * | 2019-08-29 | 2021-03-04 | Novonix Battery Testing Services Inc. | Improved microgranulation methods and product particles therefrom |
| CN110600724B (en) * | 2019-09-19 | 2022-08-02 | 安徽工业大学 | Five-element transition-non-transition high-entropy oxide negative electrode material for lithium ion battery |
| CN110556536B (en) * | 2019-09-19 | 2022-06-14 | 安徽工业大学 | Six-element high-entropy oxide material for lithium ion battery and preparation method thereof |
| CN110950654A (en) * | 2019-12-16 | 2020-04-03 | 东南大学 | High-entropy magnesium aluminate spinel type complex oxide and preparation method thereof |
| CN112467119B (en) * | 2020-12-02 | 2022-11-29 | 东北大学秦皇岛分校 | Preparation method and application of layered high-entropy oxide sodium-ion battery positive electrode material |
| CN112614986B (en) * | 2020-12-18 | 2021-12-07 | 安徽工业大学 | Rock salt type high-entropy anode material containing sulfur-oxygen dianions and preparation method |
| CN113437260B (en) * | 2021-06-29 | 2022-12-13 | 中钢天源股份有限公司 | Single crystal battery anode material and preparation method thereof |
| CN113636607A (en) * | 2021-08-03 | 2021-11-12 | 中国矿业大学 | Preparation method of high-entropy oxide of lithium ion battery negative electrode material |
| CN113353996B (en) * | 2021-08-09 | 2021-11-05 | 浙江大学杭州国际科创中心 | High-entropy conversion type sodium ion battery electrode material |
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