CN108269990B - Sodium ion battery negative electrode material, preparation method thereof and battery - Google Patents
Sodium ion battery negative electrode material, preparation method thereof and battery Download PDFInfo
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- CN108269990B CN108269990B CN201810183129.9A CN201810183129A CN108269990B CN 108269990 B CN108269990 B CN 108269990B CN 201810183129 A CN201810183129 A CN 201810183129A CN 108269990 B CN108269990 B CN 108269990B
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- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
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- H—ELECTRICITY
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
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- H—ELECTRICITY
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- H01M4/02—Electrodes composed of, or comprising, active material
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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
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/027—Negative electrodes
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- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention belongs to the technical field of batteries, and particularly relates to a sodium ion battery cathode material, a preparation method thereof and a battery. The invention provides a preparation method of a sodium-ion battery cathode material, which comprises the following preparation steps: A. mixing 1, 4-bis (p-carboxyphenyl) -1, 3-butadiene with an ethanol solution of an alkaline compound of sodium to obtain a mixed solution; B. and mixing the graphite load material with the mixed solution, and then freezing and drying to obtain the sodium-ion battery negative electrode material. The invention provides a sodium ion battery cathode material, a preparation method thereof and a battery, which can effectively overcome the technical defects of poor cycle performance, low rate performance and low capacity of an organic compound with electrochemical activity because the organic compound is easy to dissolve in an organic electrolyte solution.
Description
Technical Field
The invention belongs to the technical field of batteries, and particularly relates to a sodium ion battery cathode material, a preparation method thereof and a battery.
Background
Currently, lithium ion batteries are widely favored due to their high specific capacity, low self-discharge, high functional density, good cycling performance, and high cost performance. However, the problems of reduced lithium resource storage amount, uneven distribution and the like are increasingly highlighted.
The metal sodium and the metal lithium are metals in the same main group, so the metal sodium and the metal lithium have similar physical properties and chemical properties, and the sodium element has rich sources, easily obtained raw materials and wide distribution. MetalThe sodium is an electrochemically reversible material and has the characteristics of negative electrode potential (the potential is +0.3V relative to the lithium potential), high energy density and the like, and the theoretical specific capacity of a sodium simple substance reaches 1100 mAh/g. Relevant researches show that the performance of the sodium ion battery is quite close to that of the lithium ion battery, and the sodium ion battery is very likely to replace the lithium ion battery. Therefore, the research on the sodium ion battery material is significant. Sodium 4, 4-Biphenyldicarboxylic acid (Na) has been reported2C14H8O4) Sodium terephthalate (Na)2C8H4O4) The specific discharge capacity of the lead-acid battery is respectively 200mAh/g and 288 mAh/g. Since the radius of sodium ion is much larger than that of lithium ion (r (Na)+)=0.102nm.vs.r(Li+) 0.076nm), sodium ions are difficult to freely insert and remove between graphite layers, so that graphite cannot be used as a negative electrode material of a sodium ion battery.
The most typical organic conjugated carbonyl compound is a conjugated system, which essentially determines the diversity of the structure of the material and has high electrochemical reaction rate. In addition, the organic conjugated carbonyl compound has wide sources and low price, and the electrochemical reaction mechanism is the process of multi-electron redox reaction. These properties theoretically determine that the cycle performance and rate capability of the material are better. Therefore, in order to develop an economical sodium ion battery negative electrode material with high capacity and good rate capability, an organic carbonyl compound is a direction worth researching. For example, CN10103794825A discloses a high-performance rechargeable fully-symmetric organic sodium-ion battery and a preparation method thereof. The sodium ion battery prepared by the method has good cycle performance and high working voltage.
In summary, the problems of the current organic sodium ion battery are: 1) most of the electrochemically active organic compounds are easily dissolved in the organic electrolyte solution, resulting in poor cycle performance. 2) The organic compound is poor in conductivity, resulting in poor rate performance. 3) The carbonyl active site utilization is not high, resulting in low capacity. Therefore, the development of an organic sodium-ion battery material which is not easily dissolved in an electrolyte and has good rate capability and high capacity is a technical problem to be solved by the technical personnel in the field.
Disclosure of Invention
In view of the above, the invention provides a sodium ion battery negative electrode material, a preparation method thereof and a battery, which can effectively solve the technical defects of poor cycle performance, low rate performance and low capacity caused by the fact that an organic compound with electrochemical activity is easily dissolved in an organic electrolyte solution.
The invention provides a preparation method of a sodium-ion battery cathode material, which comprises the following preparation steps:
A. mixing 1, 4-bis (p-carboxyphenyl) -1, 3-butadiene with an ethanol solution of an alkaline compound of sodium to obtain a mixed solution;
B. and mixing the graphite load material with the mixed solution, and then freezing and drying to obtain the sodium-ion battery negative electrode material.
Preferably, the graphite support material comprises one or more of graphene oxide, reduced graphene, redox graphene, multi-walled carbon nanotubes and carbon nanotubes.
Preferably, the graphite supporting material accounts for 5-50% of the mass of the 1, 4-bis (p-carboxyphenyl) -1, 3-butadiene.
Preferably, the molar ratio of the sodium element to 1, 4-bis (p-carboxyphenyl) -1, 3-butadiene is 2: 1.
Wherein the sodium element is sodium element in ethanol solution of sodium alkaline compound.
Preferably, the alkaline compound is one or more of sodium hydroxide, sodium carbonate and sodium bicarbonate.
Preferably, the mixing of the graphite supporting material and the mixed solution is specifically: and mixing the graphite load material with the mixed solution for 6-12h under the ultrasonic condition.
Preferably, the freeze-drying time is 12-24 h.
The invention also discloses a sodium ion battery cathode material, which comprises the sodium ion battery cathode material prepared by the preparation method of the sodium ion battery cathode material.
The invention also discloses a sodium ion battery cathode, which comprises a cathode material, a conductive agent, a binder and a current collector;
and the mixture of the negative electrode material, the conductive agent and the binder is attached to the current collector, and the sodium-ion battery negative electrode is prepared by drying, rolling and punching.
The invention also provides a sodium ion battery which comprises a positive electrode, a negative electrode, electrolyte and a diaphragm, wherein the negative electrode is the negative electrode of the sodium ion battery.
Compared with the prior art, the invention has the advantages that: active substance (sodium salt) is generated by a liquid phase method by using an ethanol solution of 1, 4-bis (p-carboxyphenyl) -1, 3-butadiene and an alkaline compound of sodium, and the active substance (sodium salt) adopts a double-conjugated pi bond, so that the conductivity of the material is improved by a method for increasing the electron cloud density, and conjugated carbonyl sodium salt with a certain crystal form is synthesized, thereby reducing the solubility in organic electrolyte. The method comprises the steps of converting a small-polarity conjugated carbonyl compound into a large-polarity sodium salt with a certain crystal form by using a polarity inversion strategy, prolonging conjugated pi bonds to improve conductivity, activating by using a graphite load material, loading a reinforcing active substance, and drying to obtain the graphite material modified organic cathode material. The freeze drying treatment can keep the physical property and the chemical property of the negative electrode material of the sodium ion battery from being damaged, the graphite load material is used for activating and loading and reinforcing the active substance, the sodium salt can be inhibited from being dissolved in the electrolyte, and the mechanical property, the corrosion resistance and the conductivity of the organic material are improved. The invention utilizes the graphite load material to activate the organic electrode, the selected graphite load material can show excellent electrical, thermal and mechanical properties, especially mechanical properties, and the graphite load material is SP which is a carbon atom2Hybrid orbital or from carbon atoms with SP2And SP3The graphite load material is used for loading and reinforcing active substances, can lock the active substances to inhibit the active substances from being dissolved in electrolyte, has good mechanical property, electrochemical property and mechanical property, can improve the corrosion resistance and mechanical property of the cathode material, and further improves the negative pole materialThe conductivity of the electrode material is high, and meanwhile, the preparation method is simple and convenient, low in energy consumption and cost and environment-friendly.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below.
Fig. 1 shows a first charge-discharge diagram of a battery assembled with a negative electrode material for a sodium ion battery prepared in example 1 of the present invention;
fig. 2 shows a graph of rate performance at room temperature for cells assembled with the negative electrode material of sodium ion batteries prepared in example 2 of the present invention and at current densities of 0.1C, 0.2C, 0.5C, 1C, 2C;
fig. 3 shows a graph of the cycling performance and coulombic efficiency at room temperature and a current density of 0.1C (100mA/g) for a battery assembled from the negative electrode material of a sodium ion battery prepared in example 3 of the present invention.
Detailed Description
The invention provides a sodium ion battery cathode material, a preparation method thereof and a battery, which are used for overcoming the technical defects in the prior art.
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. 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.
The invention provides a preparation method of a sodium ion battery cathode material, a cathode pole piece and a sodium ion battery, which comprises the following preparation steps:
(1) mixing 1, 4-bis (p-carboxyphenyl) -1, 3-butadiene with a certain mass and an ethanol solution of an alkaline compound of sodium to obtain a mixed solution;
(2) mixing a graphite load material with the mixed solution, and then freezing and drying to obtain a sodium-ion battery negative electrode material;
(3) dissolving a sodium ion battery negative electrode material, a conductive agent and a binder in N-methyl pyrrolidone (NMP) according to a certain mass percentage, mixing into slurry, coating the slurry on a copper current collector, carrying out vacuum drying for 5-12h at the temperature of 80-120 ℃, rolling and punching to obtain a negative electrode piece.
(4) The negative plate and sodium are used as counter electrodes, the porous glass fiber is used as a diaphragm, and the electrolyte comprises the following components: (sodium perchlorate (NaClO4) with an EC to PC volume ratio of 1:1) the materials were assembled into sodium ion cells in a glove box filled with Ar and having a moisture content below 1 ppm.
Wherein the alkaline compound of sodium is one or more of sodium hydroxide, sodium carbonate and sodium bicarbonate, and the molar ratio of sodium element to 1, 4-bis (p-carboxyphenyl) -1, 3-butadiene is 2: 1.
The stirring time is 6-12 h.
The graphite support material comprises one or more of graphene oxide, reduced graphene, redox graphene, multi-walled carbon nanotubes and carbon nanotubes.
The graphite load material accounts for 5-50% of the mass of the 1, 4-bis (p-carboxyphenyl) -1, 3-butadiene.
The freeze drying time is 12-24 h.
In the step (3), the conductive agent is one or more of acetylene black, Super P, conductive graphite and carbon nanofiber.
And (4) in the step (3), the binder is polyvinylidene fluoride (PVDF).
In the step (3), the mass percentages of the active substance, the binder and the conductive agent of the sodium-ion battery are respectively 60-90%, 5-15% and 5-25%.
Wherein, the raw materials used in the following examples are commercially available or self-made.
Example 1
This example provides a specific embodiment, and a preparation method of a sodium ion battery anode material and a battery thereof are as follows:
(1) 2.943g of 1, 4-bis (p-carboxyphenyl) -1, 3-butadiene was added to an ethanol solution containing 8g of sodium hydroxide, and stirred at room temperature for 12 hours to obtain a mixed solution;
(2) 0.1472g of graphene oxide is added into the mixed solution, ultrasonic stirring is carried out for 12h at room temperature, and then freeze drying is carried out for 12h, so as to obtain the sodium salt of the 1, 4-bis (p-carboxyphenyl) -1, 3-butadiene modified by the graphene oxide.
(3) The prepared graphene oxide modified 1, 4-bis (p-carboxyphenyl) -1, 3-butadiene sodium salt is used as an active substance, Acetylene Black (AB) is used as a conductive agent, polyvinylidene fluoride (PVDF) is used as a binder, the active substance and the conductive agent are weighed and ground in proportion and then added into N-methylpyrrolidone (NMP) dissolved with the PVDF, wherein the mass percentages of the active substance, the PVDF (binder) and the AB (conductive agent) are 60%, 15% and 25% respectively. The slurry was uniformly coated on a current collector copper foil with a coater, and dried in a vacuum oven at 80 ℃ for 12 hours. Rolling, punching to obtain negative pole piece, and weighing.
(4) The negative pole piece and sodium are used as a counter electrode, the porous glass fiber is used as a diaphragm, and the electrolyte is 1mol/L sodium perchlorate (NaClO)4) Ethylene Carbonate (EC) -dimethyl carbonate (DMC) (where the volume ratio of EC to DMC is 1: 1). The battery was assembled in a glove box filled with an Ar atmosphere and having a moisture content of less than 1 ppm.
(5) The first charge and discharge performance test of the battery was carried out, and the results are shown in fig. 1. As can be seen from FIG. 1, the first discharge capacity was 384.5mAh/g, the first charge capacity was 273.5mAh/g, and the first effect was 71.13%. The first charging and discharging platforms are 0.78V and 0.38V respectively.
Graphene oxide is a compound consisting of carbon atoms and SP2The honeycomb lattice of the planar film of the honeycomb lattice composed of the hybrid tracks can be loaded with reinforcing active substances, so that the dissolution of the planar film in an electrolyte can be inhibited, and the specific capacity, the cycle performance and the coulombic efficiency of the planar film are improved.
Example 2
This example provides a specific embodiment, and a preparation method of a sodium ion battery anode material and a battery thereof are as follows:
(1) 0.8829g of 1, 4-bis (p-carboxyphenyl) -1, 3-butadiene was added to an ethanol solution containing 0.318g of sodium carbonate, and stirred at room temperature for 6 hours to obtain a mixed solution;
(2) and adding 0.0883g of redox graphene into the mixed solution, ultrasonically stirring at room temperature for 8h, and freeze-drying for 18h to obtain the sodium salt of the 1, 4-bis (p-carboxyphenyl) -1, 3-butadiene modified by the redox graphene.
(3) The prepared sodium salt of the oxidized graphene modified 1, 4-bis (P-carboxyphenyl) -1, 3-butadiene is used as an active substance, Super P is used as a conductive agent, polyvinylidene fluoride (PVDF) is used as a binder, the active substance and the conductive agent are weighed and ground in proportion and then added into N-methylpyrrolidone (NMP) dissolved with the PVDF, wherein the mass percentages of the active substance, the Super P (conductive agent) and the PVDF (binder) are respectively 80%, 10% and 10%. The slurry was uniformly coated on a current collector copper foil with a coater, and dried in a vacuum oven at 120 ℃ for 8 hours. Rolling, punching to obtain negative pole piece, and weighing.
(4) The negative pole piece and sodium are used as a counter electrode, the porous glass fiber is used as a diaphragm, and the electrolyte is 1mol/L sodium perchlorate (NaClO)4) Ethylene Carbonate (EC) -dimethyl carbonate (DMC) (where the volume ratio of EC to DMC is 1: 1). The battery was assembled in a glove box filled with an Ar atmosphere and having a moisture content of less than 1 ppm.
(5) The rate performance of the battery of step (4) was measured at room temperature and at current densities of 0.1C, 0.2C, 0.5C, 1C, and 2C, and the results are shown in fig. 2, and it can be seen from fig. 2 that the rate performance of the battery prepared in this example is good.
Example 3
This example provides a specific embodiment, and a preparation method of a sodium ion battery anode material and a battery thereof are as follows:
(1) 1.1772g of 1, 4-bis (p-carboxyphenyl) -1, 3-butadiene was added to an ethanol solution containing 0.672g of sodium bicarbonate, and stirred at room temperature for 8 hours to obtain a mixed solution;
(2) 0.5886g of multi-walled carbon nanotubes are added into the mixed solution, and after 12h of ultrasonic stirring at room temperature, the mixture is frozen and dried for 20h to obtain the sodium salt of the 1, 4-bis (p-carboxyphenyl) -1, 3-butadiene modified by the multi-walled carbon nanotubes.
(3) The prepared modified 1, 4-bis (P-carboxyphenyl) -1, 3-butadiene sodium salt is used as an active substance, Super P is used as a conductive agent, polyvinylidene fluoride (PVDF) is used as a binder, the active substance and the conductive agent are weighed and ground in proportion and then added into N-methylpyrrolidone (NMP) dissolved with the PVDF, wherein the mass percentages of the active substance, the Super P (conductive agent) and the PVDF (binder) are respectively 70%, 20% and 10%. The slurry was uniformly coated on a current collector copper foil with a coater, and dried in a vacuum oven at 100 ℃ for 5 hours. Rolling, punching to obtain negative pole piece, and weighing.
(4) The negative plate and sodium are used as a counter electrode, the porous glass fiber is used as a diaphragm, and the electrolyte is 1mol/L sodium perchlorate (NaClO)4) Ethylene Carbonate (EC) -dimethyl carbonate (DMC) (where the volume ratio of EC to DMC is 1: 1). The battery was assembled in a glove box filled with Ar and having a moisture content of less than 1 ppm.
(5) The cycle life test of the battery was performed at room temperature to obtain a cycle performance and coulombic efficiency graph, and as a result, as shown in fig. 3, it can be seen from fig. 3 that the current density was about 100mA/g, and after cycling to 100 times, the capacity maintained 81% of the initial capacity, which was about 170.3 mAh/g.
The multi-wall carbon nanotube is formed by carbon atoms and SP2And SP3The track hybridization can also be said to be formed by coiling graphene sheets, and small holes are distributed on the inner wall of the multi-wall carbon nano tube, so that the multi-wall carbon nano tube is loaded with a reinforcing active substance, the dissolution of the reinforcing active substance in an electrolyte can be inhibited, and the corrosion resistance is improved.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (8)
1. The sodium-ion battery negative electrode material is characterized by comprising 1, 4-bis (p-carboxyphenyl) -1, 3-butadiene disodium, which is loaded on a graphite load material;
the preparation method comprises the following preparation steps:
A. reacting 1, 4-bis (p-carboxyphenyl) -1, 3-butadiene with an alkaline compound solution of sodium to obtain disodium 1, 4-bis (p-carboxyphenyl) -1, 3-butadiene; the alkaline compound of sodium is one or more of sodium hydroxide, sodium carbonate and sodium bicarbonate;
B. mixing a graphite load material with the 1, 4-bis (p-carboxyphenyl) -1, 3-disodium butadiene, and freeze-drying to obtain a sodium-ion battery negative electrode material of which the 1, 4-bis (p-carboxyphenyl) -1, 3-disodium butadiene is loaded on the graphite load material; the graphite support material comprises one or more of graphene oxide, reduced graphene, graphene oxide and carbon nanotubes.
2. The preparation method of the negative electrode material of the sodium-ion battery is characterized by comprising the following preparation steps:
A. reacting 1, 4-bis (p-carboxyphenyl) -1, 3-butadiene with an alkaline compound solution of sodium to obtain disodium 1, 4-bis (p-carboxyphenyl) -1, 3-butadiene; the alkaline compound of sodium is one or more of sodium hydroxide, sodium carbonate and sodium bicarbonate;
B. mixing a graphite load material with the 1, 4-bis (p-carboxyphenyl) -1, 3-disodium butadiene, and freeze-drying to obtain a sodium-ion battery negative electrode material of which the 1, 4-bis (p-carboxyphenyl) -1, 3-disodium butadiene is loaded on the graphite load material; the graphite support material comprises one or more of graphene oxide, reduced graphene, graphene oxide and carbon nanotubes.
3. The method for preparing the negative electrode material of the sodium-ion battery according to claim 2, wherein the molar ratio of the sodium element in the alkaline compound solution of sodium to 1, 4-bis (p-carboxyphenyl) -1, 3-butadiene is 2: 1.
4. The preparation method of the negative electrode material of the sodium-ion battery as claimed in claim 2, wherein the graphite load material accounts for 5-50% of the mass of the 1, 4-bis (p-carboxyphenyl) -1, 3-butadiene.
5. The preparation method of the negative electrode material of the sodium-ion battery as claimed in claim 2, wherein the mixing of the graphite supporting material and the disodium 1, 4-bis (p-carboxyphenyl) -1, 3-butadiene is specifically as follows: under the ultrasonic condition, the graphite load material is mixed with the 1, 4-bis (p-carboxyphenyl) -1, 3-butadiene disodium for 6-12 h.
6. The method for preparing the negative electrode material of the sodium-ion battery as claimed in claim 2, wherein the freeze-drying time is 12-24 h.
7. A negative electrode of a sodium-ion battery, which is characterized by comprising the negative electrode material of the sodium-ion battery as claimed in claim 1 or the negative electrode material of the sodium-ion battery as claimed in any one of claims 2 to 6, a conductive agent, a binder and a current collector;
and the mixture of the sodium-ion battery negative electrode material, the conductive agent and the binder is attached to the current collector, and the sodium-ion battery negative electrode is prepared by drying, rolling and punching.
8. A sodium ion battery comprising a positive electrode, a negative electrode, an electrolyte and a separator, wherein the negative electrode is the negative electrode of the sodium ion battery according to claim 7.
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