CN115332512A - Lithium ion battery negative electrode material beta-SnSb/HCS/C and preparation method thereof - Google Patents

Lithium ion battery negative electrode material beta-SnSb/HCS/C and preparation method thereof Download PDF

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CN115332512A
CN115332512A CN202211031331.2A CN202211031331A CN115332512A CN 115332512 A CN115332512 A CN 115332512A CN 202211031331 A CN202211031331 A CN 202211031331A CN 115332512 A CN115332512 A CN 115332512A
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史鑫磊
林少雄
蔡桂凡
王叶
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Hefei Gotion High Tech Power Energy Co Ltd
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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
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
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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
    • 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
    • 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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    • 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
    • H01M4/387—Tin or alloys based on tin
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
    • H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
    • H01M4/587—Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
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Abstract

The invention discloses a lithium ion battery negative electrode material beta-SnSb/HCS/C and a preparation method thereof, relating to the technical field of lithium ion battery materials, wherein the negative electrode material is obtained by blending beta-SnSb alloy and spherical hard carbon and then coating a carbon layer on the surface of the beta-SnSb alloy and the spherical hard carbon; the preparation method comprises the following steps: preparing a carbon source aqueous solution, adding a dehydrating agent, stirring for reaction, continuously adding the dehydrating agent after a jelly appears in the solution, heating, stirring for reaction, filtering, and carbonizing to obtain HCS; to alkaline NaBH 4 Dropwise adding a metal ion solution containing tin and antimony into the solution, and carrying out water bath reaction to obtain a beta-SnSb alloy; under an inert atmosphere, mixing and grinding HCS and beta-SnSb to obtain a beta-SnSb/HCS composite material; bag for packingAnd mixing the carbon-coated source with the beta-SnSb/HCS composite material, and carrying out a carbonization reaction in an inert atmosphere to obtain the beta-SnSb/HCS/C composite material. The invention has simple preparation and stable performance, shows excellent electrochemical performance when being applied to the lithium ion battery, and has the advantages of high specific capacity, high first charge-discharge efficiency, excellent rate performance and good cycle performance.

Description

Lithium ion battery negative electrode material beta-SnSb/HCS/C and preparation method thereof
Technical Field
The invention relates to the technical field of lithium ion batteries, in particular to a lithium ion battery cathode material beta-SnSb/HCS/C and a preparation method thereof.
Background
Compared with other secondary batteries, the lithium ion battery has the advantages of high specific capacity, high charging efficiency, good temperature characteristic, low self-discharge rate, small charging heat effect, no memory effect and the like, is widely applied to the fields of various portable electronic products, electric automobiles and the like, receives wide attention in the current society, and has very bright application prospect. The performance of a lithium ion battery is determined by the performance of its electrode material, electrolyte performance, battery structure, and other factors, wherein the electrode material directly determines the capacity and cycle life of the lithium battery. Although the graphite negative electrode material currently in widespread use is close to the theoretical specific capacity (372 mAh/g), the material still cannot meet the increasing demand of the human society for high energy density and environment-friendly secondary batteries. The existing low-capacity cathode material has gradually become one of the limiting factors for improving the energy density of the lithium ion battery.
The silicon-based, tin-based and antimony-based negative electrode materials have higher charge-discharge specific capacities. The theoretical specific capacity of lithium embedded by tin is 994mAh/g, which is 3 times of the theoretical specific capacity of the commercial graphite carbon material. Sn and Li alloyed final product Li 22 Sn 5 The lithium intercalation potential is between 0.3 and 0.6V, so that the generation of lithium dendrites is avoided, but because the simple substance of the metallic Sn has a relatively obvious volume effect in the lithium intercalation/lithium deintercalation process, and simultaneously, the toughness of the Sn and lithium after forming an alloy becomes poor, so that lithium ions are difficult to deintercalate, and in the lithium intercalation/lithium deintercalation process, active substances are easy to be pulverized and shed, and finally lose electrical contact with a current collector to be inactivated, so that the metallic Sn is directly used as the negative electrode material of the lithium ion battery and is greatly limited. The theoretical specific capacity of the metallic antimony is 660mAh/g, the lithium insertion/removal voltage platform is about 0.8V, relatively stable working voltage and higher charge-discharge specific capacity can be provided, and the antimony metal serving as a lithium ion battery cathode material also faces serious volume expansion problem, has large irreversible capacity, and is firstly usedLow efficiency and poor cycle stability, and also limits the application of the lithium ion battery cathode material.
The tin-antimony alloy has the advantages of both tin-based negative electrode material and antimony-based negative electrode material, and has high specific capacity of the former and stable voltage platform of the latter. Different lithium intercalation/deintercalation potentials enable the two materials to be mutually buffer matrixes in the charging and discharging processes, so that the charging and discharging specific capacity of the materials is improved, and the cycling stability of the materials is enhanced. However, in the preparation process of the alloy material, tin oxide and antimony oxide are generated to increase irreversible capacity, so that the first effect is reduced.
The hard carbon material shows a high specific capacity of 200-600mAh/g in a voltage interval of 1.5-0V, and the potential of the hard carbon mainly consists of two states: a ramp state having a specific capacity of about 150 to 250mAh/g at 1.0 to 0.1V, and a plateau region having a specific capacity of about 100 to 400 mAh/g. Moreover, the hard carbon material has no obvious lithium intercalation/deintercalation potential, so that the condition that the negative electrode separates lithium in the process of charging and discharging does not occur. From a microscopic viewpoint, lithium ions, when entering hard carbon, are mainly stored in the pore structure of the hard carbon, and are not in a graphite-like layered structure. The hard carbon material has excellent rate performance and has the defects of low first effect and low tap density. Therefore, the preparation of the ideal hard carbon material with high initial efficiency and high tap density is of great significance. Among them, spherical hard carbon materials are desirable. However, spherical hard carbon materials are difficult to prepare by direct pyrolysis of organic or polymeric precursors.
Disclosure of Invention
Based on the technical problems in the background art, the invention provides a lithium ion battery negative electrode material beta-SnSb/HCS/C and a preparation method thereof.
The invention provides a beta-SnSb/HCS/C lithium ion battery cathode material, which is obtained by blending a beta-SnSb alloy and spherical hard carbon and then coating a carbon layer on the surface of the beta-SnSb alloy and the spherical hard carbon.
Preferably, the mass ratio of the beta-SnSb alloy to the spherical hard carbon is 1:5-10.
The invention also provides a preparation method of the lithium ion battery negative electrode material beta-SnSb/HCS/C, which comprises the following steps:
s1, HCS preparation: preparing a carbon source aqueous solution, adding a dehydrating agent into the aqueous solution, stirring for reaction, continuing to add the dehydrating agent into the aqueous solution after a jelly appears in the aqueous solution, heating the aqueous solution, stirring for reaction, cooling the aqueous solution to room temperature, filtering the aqueous solution, drying the aqueous solution in vacuum, and carbonizing the aqueous solution to obtain a spherical hard carbon material HCS;
s2, preparing beta-SnSb: reacting NaBH 4 Dissolving in NaOH solution to obtain alkaline NaBH 4 A solution; dissolving tin source and antimony source in water to obtain metal ion solution, ultrasonic dispersing, and adding alkali NaBH 4 Stirring in the solution, carrying out water bath reaction, filtering, washing and drying to obtain a beta-SnSb alloy;
s3, preparation of beta-SnSb/HCS: mixing and grinding the spherical hard carbon material HCS and the beta-SnSb alloy in an inert atmosphere to obtain a beta-SnSb/HCS composite material;
s4, preparation of beta-SnSb/HCS/C: and mixing the coated carbon source with the beta-SnSb/HCS composite material, carrying out high-temperature carbonization reaction in an inert atmosphere, and coating a carbon layer on the surface of the beta-SnSb/HCS composite material to obtain the beta-SnSb/HCS/C composite material.
Preferably, in S1, the carbon source is one or more of glucose, sucrose, fructose and lactose; the dehydrating agent is one or more of ethanol, acetone, glycerol, n-butanol, and tert-butanol.
Preferably, in S1, the addition amount of the dehydrating agent is 12-18vt% of the volume of the carbon source aqueous solution; the mass ratio of the dehydrating agent added in the two times is 1:1.8-2.5; adding the dehydrating agent for the second time, heating to 380-420 ℃, and stirring for reaction for 1-2h.
Preferably, in S1, the carbonization treatment is carried out at 2-3 ℃/min to 800-1000 ℃ under inert atmosphere, and the temperature is kept for 12-20h.
Preferably, in S2, the tin source is SnCl 2 ·2H 2 O, antimony source is SbCl 3 The concentration of the metal ion solution is 0.07-0.15mol/L, n Sn ：n Sb =1:1; alkaline NaBH 4 The pH of the solution is 9-12, naBH in the solution 4 The concentration of (A) is 0.07-0.15mol/L; preferably, the reaction temperature of the water bath reaction is 80-90 ℃ and the reaction time is 4-6h.
Preferably, in S3, the mass ratio of HCS to beta-SnSb is 5-10:1.
preferably, in S4, the coating carbon source is one or more of coal pitch, petroleum residual pitch, mesophase pitch, polyacrylonitrile, epoxy resin, and phenolic resin; preferably, the addition amount of the coating carbon source is 5-8wt% of the mass of the beta-SnSb/HCS composite material.
Preferably, in S4, the carbonization reaction is carried out at the temperature of 2-3 ℃/min to 1000-1200 ℃ under the inert atmosphere, and the temperature is kept for 10-20h.
Has the beneficial effects that: according to the invention, a hydrothermal method is used for preparing nano-scale spherical hard carbon HCS, a chemical reduction coprecipitation method is used for preparing a beta-SnSb nano alloy material, HCS and beta-SnSb are mixed through grinding, finally carbon coating is carried out, and a layer of carbon shell is coated on the surface of the material, thus obtaining the composite cathode material beta-SnSb/HCS/C. Although Sn and Sb have higher capacities in the prior art, the cycle performance is poor due to material pulverization in the cycle process, the beta-SnSb prepared by the method relieves the problem of material pulverization, oxides generated by reaction reduce the first efficiency of the material, the HCS and carbon coating can be used for effectively improving the first efficiency of the material, and the problem of poor cycle caused by volume expansion and pulverization of the material can be also inhibited. The invention has simple preparation, stable performance and better application prospect. The beta-SnSb/HCS/C composite negative electrode material is applied to a lithium ion battery, shows excellent electrochemical performance, and has the advantages of high specific capacity, high first charge-discharge efficiency, excellent rate performance and good cycle performance.
Drawings
Fig. 1 is a first charge-discharge graph of lithium ion batteries using anode materials prepared in example 1 and comparative example 1, respectively;
fig. 2 is a graph showing cycle retention ratios of lithium ion batteries using the anode materials prepared in example 1 and comparative example 2, respectively.
Detailed Description
The technical solution of the present invention will be described in detail below with reference to specific examples.
Example 1
1) Preparation of lithium ion battery negative electrode material beta-SnSb/HCS/C
1.1 ) hydrothermal preparation of spherical hard carbon HCS: adding glucose into deionized water, stirring to prepare 1mol/L glucose solution, adding 50mL of ethanol solution with the mass fraction of more than 90% into 1L of glucose solution, dehydrating, stirring, reacting for 30min, continuously adding 100mL of ethanol solution after a jelly appears in the solution, heating to 400 ℃, reacting for 1.5h, cooling to room temperature, stirring, filtering, precipitating, vacuum drying, heating to 900 ℃ at the speed of 2.5 ℃/min under an inert atmosphere, keeping for 15h, and carbonizing to prepare the required spherical hard carbon material HCS.
1.2 B) preparing beta-SnSb by a chemical reduction coprecipitation method: respectively weighing SnCl according to the molar ratio of 1 2 ·2H 2 O、SbCl 3 Respectively dissolved in deionized water to prepare 0.1mol/L solution and 0.1mol/L alkaline NaBH 4 Solution (pH adjusted to 11 by addition of NaOH); snCl 2 ·2H 2 O、SbCl 3 The mixed solution is added into NaBH drop by drop after being ultrasonically oscillated for 40min 4 Stirring the solution to form suspension, continuously stirring for 20-40min to generate black precipitate, putting the mixed solution in a thermostatic water bath at 85 ℃ for 5h, filtering the precipitate, washing the precipitate for multiple times by using deionized water and an ethanol solution, and drying the black precipitate in vacuum at 105 ℃ for 10h to obtain a target product beta-SnSb.
1.3 Grinding, mixing, coating and carbonizing: the prepared HCS sample and the beta-SnSb sample are mixed according to the mass ratio of 10:1, putting the mixture into a mortar, putting the mortar into a glove box, grinding and uniformly mixing the mixture in an inert environment, taking a uniformly mixed beta-SnSb/HCS sample, mixing the uniformly mixed beta-SnSb/HCS sample with epoxy resin according to a ratio of 100:5, carbonizing and cooling at 1050 ℃ to obtain the required beta-SnSb/HCS/C composite negative electrode material.
2) Preparation of battery cathode and assembly test of half-cell
2.1 Mixing the prepared beta-SnSb/HCS/C composite negative electrode material with conductive carbon black according to the proportion of 8;
2.2 Taking a binder into a slurry mixing tank, and adding the mixed powder ground in 2.1) into the slurry mixing tank for slurry mixing;
2.3 Uniformly coating the slurry on a copper foil, drying at 80 ℃ for 12 hours, and preparing a negative plate by using a tablet press;
2.4 The negative electrode sheet obtained in (2.3) was used to perform half-cell assembly with a metallic lithium sheet, a nickel foam, a separator, and positive and negative electrode cases in a glove box under an argon atmosphere.
2.5 Analysis of electrochemical properties of the assembled half-cells to obtain the charge-discharge curve of the resulting material
The material obtained by the implementation has the first charging capacity of 441mAh/g and the first efficiency of 89% under the condition of 0.1C multiplying power, and the reversible capacity is up to 439mAh/g after 100 cycles.
Example 2
1) Preparation of lithium ion battery negative electrode material beta-SnSb/HCS/C
Compared with example 1, the difference is only that in step 1.3), the mass ratio of the HCS sample to the β -SnSb sample is 5:1.
2) Preparation of battery negative electrode and assembly test of half cell: the same as in example 1.
Compared with the material obtained in the embodiment 1, the material obtained in the embodiment has the first charge capacity of 591mAh/g and the first efficiency of 85% at the rate of 0.1C, and the reversible capacity of 576mAh/g after 100 cycles.
Example 3
1) Compared with example 1, the difference is only that in step 1.3), the mass ratio of the HCS sample to the β -SnSb sample is 8:1; the carbon source is coal pitch, the mass ratio of the beta-SnSb/HCS sample to the coal pitch is 100:5.
2) Preparation of battery negative electrode and assembly test of half cell: the same as in example 1.
Example 4
1) Compared with the example 1, the difference is only that in the step 1.3), the coating carbon source is phenolic resin, the mass ratio of the beta-SnSb/HCS sample to the phenolic resin is 100:8.
2) Preparation of battery negative electrode and assembly test of half cell: the same as in example 1.
Comparative example 1
1) Compared with the example 1, the difference is only that the step 1.2) is not included), and the specific steps are that the spherical hard carbon material HCS prepared in the step 1.1) is mixed with the epoxy resin in a ratio of 100:5, carbonizing and cooling at 1050 ℃ to obtain the required HCS/C composite negative electrode material.
2) Preparation of battery negative electrode and assembly test of half cell: the same as in example 1.
Comparative example 2
1) Compared with example 1-only in the absence of step 1.1), the specific procedure is to mix the β -SnSb prepared in step 1.2) with an epoxy resin in a ratio of 100:5, and carbonizing and cooling at 1050 ℃ to obtain the required HCS/C composite negative electrode material.
2) Preparation of battery negative electrode and assembly test of half cell: the same as in example 1.
The raw material ratios and the electrochemical performance test results in examples 1 to 4 and comparative examples 1 to 2 are shown in table 1; the first charge and discharge curves of the lithium ion batteries of the negative electrode materials prepared in example 1 and comparative example 1 are shown in fig. 1, and the cycle retention curves of the lithium ion batteries of example 1 and comparative example 2 are shown in fig. 2.
Table 1 raw material ratios and electrochemical performance test results in examples and comparative examples
Figure BDA0003817533680000071
From the electrochemical performance test results in table 1 and fig. 1-2: the single spherical hard carbon HCS has excellent cycle performance but has the defect of low capacity; the SnSb composite negative electrode material has high gram capacity but poor cycle performance. The spherical hard carbon HCS and the beta-SnSb are compounded, and the surface of the material is modified by a coating method, so that the prepared beta-SnSb/HCS/C has the characteristics of high capacity and excellent cycle performance.
The above description is only for the preferred embodiment 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 to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.

Claims (10)

1. The lithium ion battery negative electrode material beta-SnSb/HCS/C is characterized in that the negative electrode material is obtained by mixing beta-SnSb alloy and spherical hard carbon and then coating a carbon layer on the surface of the mixture.
2. The lithium ion battery anode material beta-SnSb/HCS/C according to claim 1, wherein the mass ratio of the beta-SnSb alloy to the spherical hard carbon is 1:5-10.
3. The preparation method of the beta-SnSb/HCS/C lithium ion battery negative electrode material of claim 1 or 2, which is characterized by comprising the following steps:
s1, HCS preparation: preparing a carbon source aqueous solution, adding a dehydrating agent into the aqueous solution, stirring for reaction, continuing to add the dehydrating agent into the aqueous solution after a jelly appears in the aqueous solution, heating the aqueous solution, stirring for reaction, cooling the aqueous solution to room temperature, filtering the aqueous solution, drying the aqueous solution in vacuum, and carbonizing the aqueous solution to obtain a spherical hard carbon material HCS;
s2, preparing beta-SnSb: reacting NaBH 4 Dissolving in NaOH solution to obtain alkaline NaBH 4 A solution; dissolving tin source and antimony source in water to obtain metal ion solution, ultrasonic dispersing, and adding alkali NaBH 4 Stirring the solution, carrying out water bath reaction, filtering, washing and drying to obtain a beta-SnSb alloy;
s3, preparation of beta-SnSb/HCS: mixing and grinding the spherical hard carbon material HCS and the beta-SnSb alloy in an inert atmosphere to obtain a beta-SnSb/HCS composite material;
s4, preparation of beta-SnSb/HCS/C: and mixing the coated carbon source with the beta-SnSb/HCS composite material, carrying out high-temperature carbonization reaction in an inert atmosphere, and coating a carbon layer on the surface of the beta-SnSb/HCS composite material to obtain the beta-SnSb/HCS/C composite material.
4. The preparation method of the beta-SnSb/HCS/C of the lithium ion battery anode material according to claim 3, wherein in S1, the carbon source is one or more of glucose, sucrose, fructose and lactose; the dehydrating agent is one or more of ethanol, acetone, glycerol, n-butanol, and tert-butanol.
5. The preparation method of the beta-SnSb/HCS/C of the lithium ion battery cathode material according to the claim 3 or 4, characterized in that in S1, the addition amount of the dehydrating agent is 12-18vt% of the volume of the carbon source water solution; the mass ratio of the dehydrating agent added in the two times is 1:1.8-2.5; adding the dehydrating agent for the second time, heating to 380-420 ℃, and stirring for reaction for 1-2h.
6. The preparation method of the beta-SnSb/HCS/C lithium ion battery negative electrode material according to any one of claims 3 to 5, wherein in the step S1, the carbonization treatment is carried out by raising the temperature to 800-1000 ℃ at 2-3 ℃/min under an inert atmosphere and keeping the temperature for 12-20h.
7. The preparation method of the beta-SnSb/HCS/C lithium ion battery anode material according to any one of claims 3 to 6, wherein in S2, the Sn source is SnCl 2 ·2H 2 O, antimony source is SbCl 3 The concentration of the metal ion solution is 0.07-0.15mol/L, n Sn ：n Sb =1:1; alkaline NaBH 4 The pH of the solution is 9-12, and NaBH is contained in the solution 4 The concentration of (A) is 0.07-0.15mol/L; preferably, the reaction temperature of the water bath reaction is 80-90 ℃ and the reaction time is 4-6h.
8. The preparation method of the beta-SnSb/HCS/C lithium ion battery anode material according to any one of claims 3 to 7, wherein in S3, the mass ratio of HCS to beta-SnSb is 5-10:1.
9. the preparation method of the lithium ion battery anode material beta-SnSb/HCS/C according to any one of claims 3 to 8, characterized in that in S4, the coating carbon source is one or more of coal pitch, petroleum residual pitch, mesophase pitch, polyacrylonitrile, epoxy resin and phenolic resin; preferably, the addition amount of the coating carbon source is 5-8wt% of the mass of the beta-SnSb/HCS composite material.
10. The preparation method of the beta-SnSb/HCS/C lithium ion battery negative electrode material according to any one of claims 3 to 9, wherein in S4, the carbonization reaction is carried out under inert atmosphere, the temperature is raised to 1000-1200 ℃ at 2-3 ℃/min, and the temperature is kept for 10-20h.
CN202211031331.2A 2022-08-26 2022-08-26 Lithium ion battery negative electrode material beta-SnSb/HCS/C and preparation method thereof Pending CN115332512A (en)

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