CN111952576A - Composite negative electrode material, negative electrode, lithium ion battery and preparation method - Google Patents

Composite negative electrode material, negative electrode, lithium ion battery and preparation method Download PDF

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Publication number
CN111952576A
CN111952576A CN202010861903.4A CN202010861903A CN111952576A CN 111952576 A CN111952576 A CN 111952576A CN 202010861903 A CN202010861903 A CN 202010861903A CN 111952576 A CN111952576 A CN 111952576A
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lithium
negative electrode
composite
matrix
electrode material
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CN111952576B (en
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王秋君
张迪
王波
李文
李昭进
孙会兰
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Hebei University of Science and Technology
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Hebei University of Science and Technology
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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
    • H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
    • H01M4/381—Alkaline or alkaline earth metals elements
    • H01M4/382—Lithium
    • 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
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • H01M4/624—Electric conductive fillers
    • H01M4/625—Carbon or graphite
    • 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
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • H01M4/628—Inhibitors, e.g. gassing inhibitors, corrosion inhibitors
    • 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
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

Abstract

The invention particularly discloses a composite negative electrode material, a negative electrode, a lithium ion battery and a preparation method. According to the preparation method, the foamed resin of melamine or derivatives thereof is carbonized to be used as a matrix, and then the matrix is immersed into molten lithium to obtain the composite negative electrode material. The foam carbon matrix provided by the invention is uniformly distributed with nitrogen-containing functional groups, has strong binding energy to lithium, can homogenize lithium ion flow in the lithium ion deposition process, is beneficial to uniform deposition of metal lithium, and avoids forming nucleation sites for growth of lithium dendrites; meanwhile, the foam carbon matrix with the three-dimensional reticular structure also has a higher specific surface area, so that the local current density is favorably reduced, the deposition uniformity of the metal lithium in the matrix is further improved, the hollow structure of the foam carbon matrix is used as an ion transmission channel, the aggregation of a carrier and dispersed lithium ions/electrons is provided in the lithium deposition process, the continuous growth of lithium dendrites is favorably relieved, and the effects of inhibiting the lithium dendrites and buffering the volume expansion are achieved.

Description

Composite negative electrode material, negative electrode, lithium ion battery and preparation method
Technical Field
The invention relates to the technical field of electrochemical materials, in particular to a composite negative electrode material, a negative electrode, a lithium ion battery and a preparation method.
Background
Compared with the graphite negative electrode which is commercially used at present, the metallic lithium has extremely high capacity (3860mA/g) and lower potential (-3.040V vs. standard hydrogen electrode). Thus, the metallic lithium anode is considered as a key anode material of next generation high energy density. The battery constructed by adopting the metal lithium as the negative electrode can greatly improve the endurance mileage of the new energy automobile.
Then, lithium batteries are highly susceptible to the formation of lithium metal dendrites and the resulting volumetric changes during charging and discharging. The existing research finds that lithium metal foil is used as the negative electrode of the lithium battery, lithium dendrite is gradually formed on the surface of the lithium metal foil along with the increase of the cycle number, partial lithium and electrolyte are consumed by the large specific surface area of the dendrite, the dendrite continuously grows to form dead lithium, the volume of an electrode is changed due to the accumulation of the dendrite and the dead lithium, the circulating coulombic efficiency of the electrode is reduced, and even internal short circuit, thermal failure of the battery or explosion occur, so that the safety problem of the use of the lithium battery is caused. Lithium dendrites and volume changes of lithium metal have not been effectively addressed for many years. Therefore, the development of a negative electrode material capable of improving the cycle performance of the lithium ion battery and improving the first-time reproduction capacity of the lithium ion battery is of great significance to the development of the lithium ion battery.
Disclosure of Invention
Aiming at the problem that the initial charge-discharge capacity and the cycle performance of the cathode material in the conventional lithium ion battery are poor, the invention provides a composite cathode material, a cathode, a lithium ion battery and a preparation method thereof.
In order to solve the technical problems, the technical scheme provided by the invention is as follows:
a preparation method of the composite anode material comprises the following steps:
step one, under the protection of inert atmosphere, carbonizing melamine or melamine derivative foam resin at the temperature of 1000-1300 ℃ to obtain a foam carbon matrix;
melting the metal lithium foil to obtain molten lithium; and (3) immersing the foam carbon matrix into molten lithium for 2-6min, taking out and cooling to obtain the composite negative electrode material.
Compared with the prior art, the preparation method of the composite cathode material provided by the invention has the advantages that the melamine or melamine derivative foamed resin is selected to be converted into the hollow and interconnected three-dimensional reticulated foam carbon material through the high-temperature carbonization pyrolysis process, and the hollow and interconnected three-dimensional reticulated foam carbon material is used as a matrix to load lithium metal through an impregnation method to form the composite cathode material, wherein nitrogen-containing functional groups are uniformly distributed in the formed foam carbon matrix, have strong binding energy to lithium, improve the lithium affinity of the matrix material, facilitate the wetting of molten lithium, homogenize the lithium ion flow in the lithium ion deposition process, facilitate the uniform deposition of metal lithium, and avoid the formation of nucleation sites for the growth of lithium dendrites, so that the lithium dendrites are not generated in the charge-discharge cycle process of the lithium battery; meanwhile, the foam carbon matrix with the three-dimensional network structure also has a higher specific surface area, which is beneficial to reducing the local current density and further improving the deposition uniformity of the metal lithium in the matrix; in addition, the hollow structure of the foam carbon matrix is used as an ion transmission channel, and provides a carrier and disperse lithium ion/electron aggregation in the lithium deposition process, so that the continuous growth of lithium dendrites is favorably relieved, and the effects of inhibiting the lithium dendrites and relieving volume expansion are achieved.
The composite lithium cathode material prepared by the invention has the advantages of good voltage platform stability, no dendritic crystal after multiple cycles, and small electrode volume change, is light and flexible, can meet the requirements of certain special devices, effectively improves the energy density of the whole battery, provides an excellent composite cathode material for a lithium ion battery, has wide raw material sources and low price in the preparation method, can be produced in a large scale, is simple and feasible in the preparation process, opens up a new way for the structural design and optimization of the safe lithium cathode material, and has wide application prospects.
The inert gas in the present invention is an inert gas which is conventional in the art, such as argon, nitrogen, and the like.
Preferably, in the first step, the temperature of the carbonization is 1200 ℃.
The optimal carbonization temperature can avoid the structural collapse and deformation of the melamine or melamine derivative foamed resin in the carbonization treatment process, so that the prepared carbon foam substrate has a large number of holes and also has high conductivity.
Preferably, in the step one, the temperature of the carbonization is raised to 1000-1300 ℃ by adopting a temperature programming manner, and the temperature raising rate is 4-6 ℃/min.
Preferably, in the step one, the carbonization time is 2-4 h.
The preferable temperature rise speed and carbonization time are beneficial to maintaining the three-dimensional network structure of the melamine or melamine derivative foam resin and enabling the prepared foam carbon matrix to have higher conductivity.
Preferably, in the second step, the melting temperature is 180-500 ℃.
The invention also provides a composite negative electrode material which is prepared by the preparation method of any one of the composite negative electrode materials.
The invention also provides a negative electrode comprising the composite negative electrode material.
The invention also provides a lithium ion battery which comprises the cathode.
The composite negative electrode material prepared by the invention can solve the problem of lithium dendrite in the lithium metal circulation process, can effectively relieve volume expansion, and has excellent circulation stability and first charge and discharge performance. The cathode material is applied to the lithium ion battery, and the lithium ion battery with stable structure and excellent capacity and cycle performance can be obtained.
Drawings
FIG. 1 is an SEM photograph of a melamine foam resin in example 1 of the present invention;
FIG. 2 is an SEM photograph of a carbon foam matrix prepared in example 1 of the present invention;
fig. 3 is an SEM image of the composite anode material prepared in example 1 of the present invention;
fig. 4 is a cycle voltage stability chart of a lithium negative electrode symmetric battery prepared from the composite negative electrode material prepared in example 1 in an application example of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
In order to better illustrate the invention, the following examples are given by way of further illustration.
Example 1
A preparation method of the composite negative electrode material comprises the following steps:
cutting commercial melamine foam resin into a shape of 5cm multiplied by 3cm, putting the cut commercial melamine foam resin into a tubular furnace, carbonizing the commercial melamine foam resin for 2 hours at 1200 ℃ under the protection of nitrogen atmosphere, cooling the commercial melamine foam resin, washing the commercial melamine foam resin with absolute ethyl alcohol, drying the commercial melamine foam resin at 60 ℃, and then cutting the commercial melamine foam resin to obtain a foam carbon matrix of 5cm multiplied by 0.1 cm;
putting the metal lithium foil into a crucible, and heating to 250 ℃ to completely melt the metal lithium foil to obtain molten lithium; and immersing the foam carbon matrix into molten lithium for 2min, taking out and naturally cooling to obtain the composite negative electrode material.
Fig. 1 is an SEM image of the melamine resin foam, and fig. 2 is an SEM image of the carbonized carbon foam substrate, and it can be seen from the images that the prepared carbon foam substrate has a high open area ratio, the open area ratio can reach 99%, and the holes are uniformly distributed, and it can be seen from the fracture of the carbon skeleton that the interior of the skeleton is a hollow structure and is connected with each other to form a three-dimensional network structure.
Fig. 3 is an SEM image of the prepared composite negative electrode material, and it can be seen from the SEM image that the composite electrode material can still maintain a good three-dimensional network structure after loading with lithium metal, and still has a high porosity, which is beneficial to deposition of lithium metal and alleviation of volume expansion.
The content of C, N, O elements in the carbon foam matrix is tested by XPS (X-ray electron spectroscopy), the atomic ratio of C, N, O elements in the carbon foam matrix is shown in Table 1, the atomic ratio of N element is 3.6%, the high nitrogen content is favorable for wetting molten lithium, and the carbon content can reach 94.2%, which proves that the carbon foam matrix has high conductivity.
TABLE 1 atomic ratio of C, N, O elements in the carbon foam matrix
Sample (I) C N O N-6 N-5 N-Q
Foam carbon matrix 94.2％ 2.2％ 3.6％ 53.40％ 14.15％ 32.45％
Note: n-6, N-5 and N-Q represent N elements in different states, wherein N-6 represents pyridine nitrogen, N-5 represents pyrrole nitrogen and N-Q represents quaternary nitrogen.
Example 2
A preparation method of the composite negative electrode material comprises the following steps:
cutting commercial melamine foam resin into a shape of 5cm multiplied by 3cm, putting the cut commercial melamine foam resin into a tubular furnace, carbonizing the commercial melamine foam resin for 4 hours at 1000 ℃ under the protection of nitrogen atmosphere, washing the commercial melamine foam resin with absolute ethyl alcohol after cooling, drying the commercial melamine foam resin at 60 ℃, and then cutting the commercial melamine foam resin to obtain a foam carbon substrate of 5cm multiplied by 0.1 cm;
putting the metal lithium foil into a crucible, and heating to 180 ℃ to completely melt the metal lithium foil to obtain molten lithium; and immersing the foam carbon matrix into molten lithium for 4min, taking out and naturally cooling to obtain the composite negative electrode material.
Example 3
A preparation method of the composite negative electrode material comprises the following steps:
cutting commercial melamine foam resin into a shape of 5cm multiplied by 3cm, putting the cut commercial melamine foam resin into a tubular furnace, carbonizing the commercial melamine foam resin for 3 hours at 1300 ℃ under the protection of nitrogen atmosphere, washing the commercial melamine foam resin with absolute ethyl alcohol after cooling, drying the commercial melamine foam resin at 60 ℃, and then cutting the commercial melamine foam resin to obtain a foam carbon substrate of 5cm multiplied by 0.1 cm;
putting the metal lithium foil into a crucible, and heating to 500 ℃ to completely melt the metal lithium foil to obtain molten lithium; and immersing the foam carbon matrix into molten lithium for 6min, taking out and naturally cooling to obtain the composite negative electrode material.
Application examples
The composite cathode material prepared in the example 1 is assembled into a symmetrical battery at 5.0mA/cm2The polarization voltage after 60h cycling at the current density of (2) was less than 10mV, showing good cycling stability, as shown in FIG. 4.
The composite anode material prepared in example 1 was assembled into a pair of batteries at 5.0mA/cm2The polarization voltage after 1000h of circulation under the current density of (1) is lower than 28mV, and the good circulation stability is also shown.
With LiCoO2The composite cathode material prepared in example 1 was used as a cathode, a CR2032 button cell was assembled, and the charge-discharge voltage plateau was3.0-4.2V, 0.1C (1C ═ 135mA · g)-1) The first discharge capacity is 133.6mAh g-1The capacity retention after 100 cycles was 95.8%.
With LiNi0.8Co0.1Mn0.1O2The composite negative electrode material prepared in the example 1 is used as a negative electrode to assemble a CR2032 button cell as a positive electrode, the charge-discharge voltage platform is 2.8-4.3V, and the first discharge capacity is 213.4 mAh.g-1And the capacity retention rate after 100 cycles is 94.3%.
The composite negative electrode materials prepared in examples 2 to 3 all achieved substantially the same effects as in example 1.
Comparative example 1
This comparative example provides a method of preparing a composite anode material, which is identical to the method of example 1 except that the carbonization temperature in step one is 700 ℃.
The composite cathode material prepared in the example 1 is assembled into a symmetrical battery at 5.0mA/cm2The polarization voltage after cycling for 60h was below 15 mV.
The composite anode material prepared in example 1 was assembled into a pair of batteries at 5.0mA/cm2The polarization voltage after 1000h of cycling at the current density of (1) is lower than 36 mV.
With LiCoO2A CR2032 coin cell was assembled with the composite negative electrode material obtained in example 1 as a negative electrode as a positive electrode, and the charge/discharge voltage plateau was 3.0 to 4.2V at 0.1C (1C ═ 135mA · g)-1) The first discharge capacity is 125.8 mAh.g-1The capacity retention after 100 cycles was 90.1%.
With LiNi0.8Co0.1Mn0.1O2The composite negative electrode material prepared in the example 1 is used as a negative electrode to assemble a CR2032 button cell as a positive electrode, the charge-discharge voltage platform is 2.8-4.3V, and the first discharge capacity is 205.3 mAh.g-1And the capacity retention rate after 100 cycles is 90.4%.
Comparative example 2
This comparative example provides a method of preparing a composite anode material, which is identical to the method of example 1 except that the dipping time in step two was replaced with 8 min.
The composite cathode material prepared in the example 1 is assembled into a symmetrical battery at 5.0mA/cm2Is less than 17mV after cycling for 60 h.
The composite anode material prepared in example 1 was assembled into a pair of batteries at 5.0mA/cm2The polarization voltage after 1000h of cycling at the current density of (1) is less than 33 mV.
With LiCoO2A CR2032 coin cell was assembled with the composite negative electrode material obtained in example 1 as a negative electrode as a positive electrode, and the charge/discharge voltage plateau was 3.0 to 4.2V at 0.1C (1C ═ 135mA · g)-1) The first discharge capacity is 122.5mAh g-1The capacity retention after 100 cycles was 91.7%.
With LiNi0.8Co0.1Mn0.1O2The composite negative electrode material prepared in the example 1 is used as a negative electrode to assemble a CR2032 button cell as a positive electrode, the charge-discharge voltage platform is 2.8-4.3V, and the first discharge capacity is 206.3 mAh.g-1And the capacity retention rate after 100 cycles is 90.9%.
Comparative example 3
This comparative example provides a method of preparing a composite anode material, which is identical to the method of example 1, except that the melamine foam resin in step one was replaced with polystyrene.
The composite cathode material prepared in the example 1 is assembled into a symmetrical battery at 5.0mA/cm2Is less than 19mV after cycling for 60 h.
The composite anode material prepared in example 1 was assembled into a pair of batteries at 5.0mA/cm2The polarization voltage after 1000h of cycling at the current density of (1) is lower than 36 mV.
With LiCoO2A CR2032 coin cell was assembled with the composite negative electrode material obtained in example 1 as a negative electrode as a positive electrode, and the charge/discharge voltage plateau was 3.0 to 4.2V at 0.1C (1C ═ 135mA · g)-1) The first discharge capacity is 119.6mAh g-1The capacity retention after 100 cycles was 87.7%.
With LiNi0.8Co0.1Mn0.1O2The composite negative electrode material prepared in the example 1 is used as a negative electrode to assemble a CR2032 button cell as a positive electrode, the charge-discharge voltage platform is 2.8-4.3V, and the first discharge capacity is 201.5 mAh.g-1And the capacity retention rate after 100 cycles is 88.4%.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents or improvements made within the spirit and principle of the present invention should be included in the scope of the present invention.

Claims (8)

1. The preparation method of the composite anode material is characterized by comprising the following steps of:
step one, under the protection of inert atmosphere, carbonizing melamine or melamine derivative foam resin at the temperature of 1000-1300 ℃ to obtain a foam carbon matrix;
melting the metal lithium foil to obtain molten lithium; and (3) immersing the foam carbon matrix into molten lithium for 2-6min, taking out and cooling to obtain the composite negative electrode material.
2. The method of preparing a composite anode material according to claim 1, wherein in the first step, the temperature of the carbonization is 1200 ℃.
3. The method for preparing the composite anode material of claim 1, wherein in the first step, the temperature is raised to 1000-1300 ℃ in a temperature programming manner, and the temperature raising rate is 4-6 ℃/min.
4. The method for preparing a composite anode material according to claim 1, wherein in the first step, the carbonization time is 2 to 4 hours.
5. The method for preparing the composite anode material of claim 1, wherein in the second step, the melting temperature is 180-500 ℃.
6. A composite anode material, characterized by being produced by the method for producing a composite anode material according to any one of claims 1 to 5.
7. A negative electrode comprising the composite negative electrode material according to claim 6.
8. A lithium ion battery comprising the negative electrode according to claim 7.
CN202010861903.4A 2020-08-25 2020-08-25 Composite negative electrode material, negative electrode, lithium ion battery and preparation method Active CN111952576B (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112750987A (en) * 2021-01-04 2021-05-04 北京航空航天大学 Lithium metal negative electrode preparation method based on lithium-philic three-dimensional carbon-based current collector

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106784635A (en) * 2017-01-13 2017-05-31 北京科技大学 A kind of solid state battery preparation method for being combined cathode of lithium
CN107799736A (en) * 2017-09-22 2018-03-13 山东大学 A kind of lithium metal composite negative pole of three-dimensional self-supporting parent lithium carrier encapsulation and preparation method thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106784635A (en) * 2017-01-13 2017-05-31 北京科技大学 A kind of solid state battery preparation method for being combined cathode of lithium
CN107799736A (en) * 2017-09-22 2018-03-13 山东大学 A kind of lithium metal composite negative pole of three-dimensional self-supporting parent lithium carrier encapsulation and preparation method thereof

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112750987A (en) * 2021-01-04 2021-05-04 北京航空航天大学 Lithium metal negative electrode preparation method based on lithium-philic three-dimensional carbon-based current collector
CN112750987B (en) * 2021-01-04 2022-06-21 北京航空航天大学 Lithium metal negative electrode preparation method based on lithium-philic three-dimensional carbon-based current collector

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