CN113241434B - Nano-aluminum cathode material of lithium ion battery and preparation method of nano-aluminum cathode material - Google Patents
Nano-aluminum cathode material of lithium ion battery and preparation method of nano-aluminum cathode material Download PDFInfo
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- H—ELECTRICITY
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- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
- H01M4/46—Alloys based on magnesium or aluminium
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/20—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds
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- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
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- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
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Abstract
The invention relates to the technical field of lithium ion battery materials, in particular to a nano aluminum cathode material of a lithium ion battery and a preparation method thereof. The preparation method comprises the following steps: mixing anhydrous aluminum chloride, second anhydrous chloride salt and alkali metal, and ball-milling under a non-oxidizing atmosphere condition to obtain a mixture A; and washing the mixture A for multiple times by adopting a solvent, and performing solid-liquid separation and drying to obtain the nano aluminum alloy powder. The method has the advantages of simplicity, rapidness, high yield, low cost, high purity of reaction products and easy amplification, and the prepared high-purity nano aluminum alloy has small particle size and a lamellar structure and can be used in various aspects of lithium ion battery cathode materials, energetic materials, wave-absorbing materials and the like.
Description
Technical Field
The invention relates to the technical field of lithium ion battery materials, in particular to a nano aluminum cathode material of a lithium ion battery and a preparation method thereof.
Background
In recent years, lithium ion batteries are widely applied to the fields of consumer batteries and power batteries, but the current commercial negative electrode material is mainly a graphite negative electrode (372 mAh g-1), the theoretical capacity is low, and the demand of high energy density of future electric vehicles cannot be met gradually.
The existing nonferrous metal aluminum in China has abundant reserves and high yield, is one of the most common industrial metals at present, not only has low density, but also has good ductility, electrical conductivity, thermal conductivity and radiation resistance, and is an important basic raw material for national economic development. But currently, metal aluminum still faces the situation of excess capacity, the development of multipurpose application of aluminum is helpful for enriching the client requirements of aluminum products, and aluminum is very favored in the field of lithium ion batteries because of low cost. The copper foil is replaced by the aluminum foil, so that the cost of the lithium ion battery can be obviously reduced, and meanwhile, the energy density and the space utilization rate of the lithium ion battery are improved. The aluminum negative electrode has high lithium storage capacity (993 mAh g-1), a broad and flat voltage plateau (-0.28V vs. Li/Li +) and a relatively small volume expansion ratio (95%). However, the aluminum electrode still easily undergoes mechanical instability such as volume crushing and the like in the circulation process, so that the electrochemical capacity of the aluminum electrode is attenuated, and the aluminum electrode is also subjected to the dynamic deterioration of lithium intercalation and deintercalation caused by the formation of an irreversible lithium-rich phase under the stress-strain action.
The preparation of nano-aluminum is an effective way for solving the problem, but the current preparation means of nano-materials is complex, the flow is complex, and industrial production such as plasma sputtering, wet chemical synthesis and the like is difficult to carry out.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to solve the defects of poor conductivity, serious change of lithium intercalation volume, high cost and long process of the existing preparation method of the aluminum cathode of the existing lithium ion battery; the preparation method is based on redox reaction, the preparation of the aluminum alloy nanoparticles is realized by ball milling at room temperature for a short time, the preparation method is simple, the cost is low, and the obtained material can be used as a lithium ion battery cathode material.
In order to achieve the purpose, the invention provides a preparation method of a nano aluminum cathode material of a lithium ion battery, which comprises the following steps:
mixing anhydrous aluminum chloride, second anhydrous chlorate and alkali metal, and ball-milling under a non-oxidizing atmosphere condition to obtain a mixture A;
and washing the mixture A for multiple times by adopting a solvent, and performing solid-liquid separation and drying to obtain the nano aluminum alloy powder.
Further, the second anhydrous chloride salt is any one of ferric chloride, antimony chloride, copper chloride or silicon chloride.
Further, the alkali metal is magnesium.
Further, the mass ratio of the anhydrous aluminum chloride, the second anhydrous chloride salt and the alkali metal is 1.
Further, the ball milling process parameters are as follows:
the ball milling time is 1-12h, the ball milling speed is 150-500 r/min, and the ball-material ratio is 20.
Further, the solvent includes: absolute ethanol, tetrahydrofuran or ultrapure water.
Further, the drying method is one or more of forced air drying, vacuum drying and freeze drying.
A nano aluminum negative electrode material of a lithium ion battery is characterized in that the nano aluminum negative electrode material is prepared by the preparation method of any claim 1 to 7.
Based on the same inventive concept, the invention also provides a nano-aluminum cathode material of the lithium ion battery, and the nano-aluminum cathode material is prepared by the preparation method.
Has the advantages that:
(1) The preparation method disclosed by the invention realizes the bottom-up preparation of the nano-aluminum based on the alkali metal replacement reaction with strong reducibility, avoids the defects of high energy consumption and difficulty in preparation from top to bottom, realizes the preparation of the aluminum alloy nanoparticles by ball milling at room temperature for a short time, is rapid and efficient in reaction, can complete the preparation of a large amount of alloy nanoparticles in a short time, and can completely react the reaction raw materials.
(2) The preparation method is simple and rapid, high in yield, low in cost, high in purity of reaction products and easy to amplify, and the prepared high-purity nano aluminum alloy particles are small in size, are in a lamellar structure and can be used in various aspects such as lithium ion battery cathode materials, energetic materials and wave-absorbing materials.
Drawings
FIG. 1 is an X-ray diffraction pattern of high purity nano-aluminum particles provided in example 1 of the present invention;
FIG. 2 is a scanning electron microscope image of high purity nano-aluminum particles provided in example 1 of the present invention;
FIG. 3 is a powder X-ray diffraction pattern of nano aluminum alloy particles provided in examples 2-6 of the present invention;
fig. 4 is an electrochemical cycle diagram of the nano aluminum alloy particles provided in example 3 of the present invention.
Detailed Description
In order to make the technical problems, technical solutions and advantages to be solved by the present invention clearer, the following detailed description is given with reference to specific embodiments, but the scope of protection of the present invention is not limited to the following specific embodiments.
Unless otherwise defined, all terms of art used hereinafter have the same meaning as commonly understood by one of ordinary skill in the art. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to limit the scope of the present invention.
Unless otherwise specifically indicated, various raw materials, reagents, instruments, equipment and the like used in the present invention are commercially available or can be prepared by existing methods.
Example 1
The molar ratio of the anhydrous aluminum chloride to the metal magnesium powder is 2:3, ball milling to prepare nano aluminum
(1) The method comprises the steps of taking 7.9g of anhydrous aluminum chloride salt and 2.06g of micron magnesium powder as raw materials, adding 40 zirconia ball milling beads with different particle sizes, wherein the mass is 199.2g in total, and carrying out ball milling for 2 hours at the rotating speed of 300 r/min.
(2) Adding tetrahydrofuran into the mixture, removing MgCl2, centrifugally separating nano aluminum at 1000rpm, washing with ultrapure water after MgCl2 is completely removed, and drying in a freeze dryer for 12h to obtain the nano aluminum.
The X-ray diffraction and scanning electron microscope images of the high-purity nano aluminum powder obtained by the two steps are shown in figures 1 and 2, and it can be seen from the figures that the nano aluminum has better crystallinity and the particle size is between 80 and 120 nm. The probe scanning microscope results showed a relatively thin thickness of about 25nm.
Example 2:
the molar ratio of the anhydrous aluminum chloride to the anhydrous copper chloride to the micron magnesium powder is 149:2:98, the molar ratio of Cu to Al is 2: and 98, preparing the nano aluminum-copper alloy by ball milling.
(1) The method comprises the steps of taking 7.7g of anhydrous aluminum chloride, 0.158g of anhydrous copper chloride and 2.13g of micron magnesium powder as raw materials, adding 40 zirconia ball grinding beads with different particle sizes, wherein the mass is 199.2g in total, and carrying out ball milling for 2 hours at a rotating speed of 300 revolutions per minute.
(2) Adding tetrahydrofuran into the mixture, removing MgCl2, centrifugally separating nano aluminum at 1000rpm, washing with ultrapure water after MgCl2 is completely removed, and drying in a freeze dryer for 12 hours to obtain nano aluminum-copper alloy particles with copper content of 2%.
The nano aluminum alloy obtained by the two steps has better crystallinity, and the grain diameter is about 100 nm.
Example 3
The molar ratio of Cu to Al in the anhydrous aluminum chloride and the anhydrous copper chloride is 5: and 95, preparing the nano aluminum-copper alloy by ball milling.
(1) The method comprises the steps of taking 7.48g of anhydrous aluminum chloride, 0.397g of anhydrous copper chloride and 2.11g of micron magnesium powder as raw materials, adding 40 zirconia ball grinding beads with different particle sizes, wherein the mass is 199.2g in total, and carrying out ball milling for 2 hours at the rotating speed of 300 revolutions per minute.
(2) Adding tetrahydrofuran into the mixture, removing MgCl2, centrifugally separating nano aluminum at 1000rpm, washing with ultrapure water after MgCl2 is completely removed, and drying in a freeze dryer for 12 hours to obtain nano aluminum-copper alloy particles with the copper content of 5%.
The nano aluminum alloy obtained by the two steps has better crystallinity, and the grain diameter is about 100 nm.
Example 4
The molar ratio of Cu to Al in anhydrous aluminum chloride and anhydrous copper chloride is 10: and 90, preparing the nano aluminum-copper alloy by ball milling.
(1) The raw materials of 7.11g of anhydrous aluminum chloride, 0.79g of anhydrous copper chloride and 2.08g of average micron magnesium powder are taken, 40 zirconia ball grinding beads with different particle sizes are added, the mass is 199.2g in total, and the raw materials are ball-milled for 2 hours at the rotating speed of 300 r/min.
(2) Adding tetrahydrofuran into the mixture, removing MgCl2, centrifugally separating nano aluminum at 1000rpm, washing with ultrapure water after MgCl2 is completely removed, and drying in a freeze dryer for 12 hours to obtain nano aluminum-copper alloy particles with the copper content of 10%.
The nano aluminum alloy obtained by the two steps has better crystallinity, and the grain diameter is about 100 nm.
Example 5
The molar ratio of Cu to Al in the anhydrous aluminum chloride and the anhydrous copper chloride is 20: and 80, ball-milling to prepare the nano aluminum-copper alloy.
(1) Taking 6.36g of anhydrous aluminum chloride, 1.6g of anhydrous copper chloride and 2.03g of micron magnesium powder as raw materials, adding 40 zirconia ball milling beads with different particle sizes, wherein the mass is 199.2g in total, and performing ball milling for 2 hours at a rotating speed of 300 revolutions per minute.
(2) Adding tetrahydrofuran into the mixture, removing MgCl2, centrifugally separating nano aluminum at 1000rpm, washing with ultrapure water after MgCl2 is completely removed, and drying in a freeze dryer for 12 hours to obtain nano aluminum-copper alloy particles with the copper content of 2%.
The nano aluminum alloy obtained by the two steps has good crystallinity, and the grain diameter is about 100 nm.
Example 6
The molar ratio of Cu to Al in the anhydrous aluminum chloride and the anhydrous copper chloride is 30: and 70, ball-milling to prepare the nano aluminum-copper alloy.
(1) Taking 5.6g of anhydrous aluminum chloride, 2.42g of anhydrous copper chloride and 1.97g of micron magnesium powder as raw materials, adding 40 zirconia ball grinding beads with different particle sizes, wherein the mass is 199.2g in total, and carrying out ball milling for 2 hours at the rotating speed of 300 revolutions per minute.
(2) Adding tetrahydrofuran into the mixture, removing MgCl2, centrifugally separating nano aluminum at 1000rpm, washing with ultrapure water after MgCl2 is completely removed, and drying in a freeze dryer for 12 hours to obtain nano aluminum-copper alloy particles with the copper content of 2%.
The nano aluminum alloy obtained by the two steps has better crystallinity, and the grain diameter is about 100 nm.
When the aluminum alloy nanomaterials obtained in examples 2 to 6 were subjected to X-ray diffraction, it is understood from the graph shown in fig. 3 that Cu in the alloy material has a large influence on the crystallinity of the nano aluminum.
Mixing the obtained aluminum alloy nano material according to a mass ratio of an active substance, a conductive agent and a binder (polyvinylidene fluoride), adding a certain amount of dried NMP (N-methyl pyrrolidone), stirring and grinding for 4 hours to obtain uniformly mixed slurry, coating the slurry on a copper foil, drying in a vacuum drying box at 60 ℃ for 12 hours, taking out the slurry, compacting the copper foil by a tablet press at 80MPa to densify the copper foil, cutting the copper foil into a pole piece with the size of 1.2cm & lt 2 & gt, and carrying out an electrical performance test, wherein the aluminum alloy nano material obtained in example 3 is taken as an example, a constant current circulation performance of nano Al-Cu-2% is shown in a graph 4, a current density is tested under 100mAg & lt-1 & gt, a cut-off voltage is 0.01-1.5V, and a curve in the graph shows that the capacity is firstly attenuated and then stably maintained, so that the aluminum alloy nano material has long-term circulation capacity and stability, and can be used for a negative electrode material of a lithium ion battery.
The above-mentioned embodiments are only preferred embodiments of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered as the technical scope of the present invention, and equivalents and modifications of the technical solutions and concepts of the present invention should be covered by the scope of the present invention.
Claims (5)
1. A preparation method of a lithium ion battery nano aluminum cathode material is characterized by comprising the following steps:
mixing anhydrous aluminum chloride, second anhydrous chlorate and magnesium, and ball-milling under a non-oxidizing atmosphere condition to obtain a mixture A; the second anhydrous chloride salt is any one of ferric chloride, antimony chloride, copper chloride or silicon chloride;
the technological parameters of the ball milling are as follows: the ball milling time is 1-12h, the ball milling speed is 150-500 r/min, and the ball material ratio is 20;
and washing the mixture A for multiple times by adopting a solvent, and performing solid-liquid separation and drying to obtain the nano aluminum alloy powder.
2. The preparation method of the nano aluminum anode material for the lithium ion battery according to claim 1, wherein the mass ratio of the anhydrous aluminum chloride to the second anhydrous chloride to the magnesium is 1.2-2.
3. The preparation method of the nano-aluminum anode material for the lithium ion battery according to claim 1, wherein the solvent comprises: absolute ethanol, tetrahydrofuran or ultrapure water.
4. The preparation method of the nano-aluminum anode material for the lithium ion battery according to claim 1, wherein the drying method is one or more of forced air drying, vacuum drying and freeze drying.
5. The nano aluminum negative electrode material of the lithium ion battery is characterized by being prepared by the preparation method of any one of claims 1 to 4.
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