CN110534818B - Suspending agent for lithium ion battery cathode, lithium ion battery cathode and lithium ion battery - Google Patents
Suspending agent for lithium ion battery cathode, lithium ion battery cathode and lithium ion battery Download PDFInfo
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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
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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
- H01M10/42—Methods or arrangements for servicing or maintenance of secondary cells or secondary half-cells
- H01M10/4235—Safety or regulating additives or arrangements in electrodes, separators or electrolyte
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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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
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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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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- Y02E60/10—Energy storage using batteries
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Abstract
The invention discloses a suspending agent for a lithium ion battery cathode, which comprises one of a compound shown in a general formula (I), a compound shown in a general formula 1c and a compound shown in a general formula 1 e:
wherein R is1is-CH2‑，R2Is selected from-CH2CN、‑CH2CH2CN、‑OCN、‑CH2NH2、‑OH、‑CH2OH、‑C(CH3)2OH、‑SO3H、‑CH2SO3H; or R1Is alkyl with 2-5 carbon atoms or alkenyl with 2-5 carbon atoms, R2Is a compound containing-CN, -COOH, -NH2、‑OCN、‑OH、‑CONHCH3、‑CON(CH3)2、‑SO3A group of H; x is Li+、Na+、K+、NH4+One of (1), m>0，n>0, and m + n equals 100%. Compared with the prior art, the suspending agent provided by the invention has the advantages that the multi-membered ring alpha-cellulose is copolymerized with polar monomers such as acrylonitrile/propionate/methyl propionate/butyrate/vinyl acetate/allyl acetate/propanesulfonic acid and the like, and the molecular chain contains a large amount of polar groups, so that more Li is easily accumulated on the surface of the active material+Is advantageous to Li+The lithium ion battery can conduct rapidly in a suspending agent, and the finally obtained lithium ion battery has good rate capability。
Description
Technical Field
The invention belongs to the field of lithium ion batteries, and particularly relates to a suspending agent for a lithium ion battery cathode, the lithium ion battery cathode and the lithium ion battery.
Background
The lithium ion battery has the advantages of high energy density, good cycle performance, low self-discharge rate, environmental protection, no pollution and the like, and becomes one of the secondary batteries which are applied and researched most widely in the world nowadays. At present, lithium ion batteries have been successfully applied to portable electronic devices such as mobile phones and notebooks, and have gradually developed into various fields such as aerospace, electric vehicles and energy storage systems. The new application provides higher requirements for the performances of the lithium ion battery, such as specific capacity, rate characteristic, cycle life and the like. The performance of lithium ion batteries depends to a large extent on the positive and negative electrode materials that make up the battery.
When the traditional cellulose suspending agent is used for preparing the battery cathode, the battery has low rate capability, short cycle life and high DCR value due to the fact that the traditional cellulose suspending agent does not have lithium ion transmission capability, and the requirement cannot be met.
In view of the above, it is necessary to provide a suspending agent for a lithium ion battery negative electrode, which helps to improve the lithium ion transport rate, and a lithium ion battery negative electrode and a lithium ion battery having the suspending agent.
Disclosure of Invention
The invention aims to: the suspending agent for the lithium ion battery cathode, the lithium ion battery cathode with the suspending agent and the lithium ion battery are beneficial to improving the lithium ion transmission rate.
In order to achieve the above object, the present invention provides a suspension for a negative electrode of a lithium ion battery, comprising one of a compound represented by general formula (I), a compound represented by general formula 1c, and a compound represented by general formula 1 e:
wherein R is1is-CH2-，R2Is selected from-CH2CN、-CH2CH2CN、-OCN、-CH2NH2、-OH、-CH2OH、-C(CH3)2OH、-SO3H、-CH2SO3H; or
R1Is alkyl with 2-5 carbon atoms or alkenyl with 2-5 carbon atoms, R2Is a compound containing-CN, -COOH, -NH2、-OCN、-OH、-CONHCH3、-CON(CH3)2、-SO3A group of H;
x is Li+、Na+、K+、NH4+One of (1);
m >0, n >0, and m + n is 100%.
As an improvement of the suspending agent for the negative electrode of the lithium ion battery, R is1When the alkyl group has 2 to 5 carbon atoms, R1Is selected from- (CH)2)2-、-(CH2)3-、-(CH2)4-、-(CH2)5-、-CH(CH3)-、-C(CH3)2-、-C(CH3)2CH2-、-C(CH3)2CH2CH2-、-CH(CH3)CH2-、-C(CH2CH3)CH2-、-C(CH2CH2CH3)CH2-、-CH(CH3)CH2CH2-、-CH(CH3)CH2CH2CH2-one of the above;
when R is1When the alkenyl group has 2 to 5 carbon atoms, R1Selected from-CH ═ CH-, -CH2-CH＝CH-、-CH2-CH2-CH＝CH-、-CH2-CH＝CH-CH2-CH2-、-CH2-CH2-CH2-CH-is one of CH-;
R2selected from-CN, -CH2CN、-CH2CH2CN、-OCN、-CH2NH2、-CONHCH3、-CON(CH3)2、-OH、-CH2OH、-C(CH3)2OH、-COOH、-C6H5COOH、-SO3H、-CH2SO3H、-C6H5SO3H、-C6H5CH2SO3H.
As an improvement of the suspending agent for the negative electrode of the lithium ion battery, the suspending agent for the negative electrode of the lithium ion battery is selected from one or more of the following compounds:
as an improvement of the suspending agent for the negative electrode of the lithium ion battery, the ratio of m to n in the general formula (I) is (50-80%) (20-50%). When the ratio is too small, the slurry is difficult to disperse and poor in stability, and when the ratio is too large, Li+The transmission is difficult, and the dynamics are not favorably promoted; meanwhile, the flexibility of the pole piece is not obviously improved, and drying cracking is easy to occur in coating.
As an improvement of the suspending agent for the negative electrode of the lithium ion battery, the ratio of m to n in the general formula (I) is (60-70%) (30-40%).
As an improvement of the suspending agent for the negative electrode of the lithium ion battery, the ratio of m to n in the general formula (I) is 65% to 35%.
As an improvement of the suspending agent for the negative electrode of the lithium ion battery, the number average molecular weight of the suspending agent for the negative electrode of the lithium ion battery is 300000-400000.
In order to achieve the above object, the present invention provides a lithium ion battery negative electrode, including a negative electrode current collector and a negative electrode active material layer coated on the negative electrode current collector, wherein the negative electrode active material layer includes a negative electrode active material and a suspending agent, and the suspending agent is the above suspending agent for the lithium ion battery negative electrode.
As an improvement of the lithium ion battery cathode, the suspending agent accounts for 2-5% of the total weight of the cathode active material layer. When the content is too small, the slurry is difficult to disperse and has poor stability, and when the content is too large, the amount of active materials is affected, and the capacity density of the battery is reduced.
As an improvement of the negative electrode of the lithium ion battery, the negative electrode active material is selected from one or more of soft carbon, hard carbon, artificial graphite, natural graphite, silicon-oxygen compound, silicon-carbon compound, lithium titanate and metal capable of forming an alloy with lithium.
In order to achieve the above object, the present invention provides a lithium ion battery, including a positive electrode, a negative electrode, a separator interposed between the positive electrode and the negative electrode, and an electrolyte, wherein the negative electrode is the above-mentioned negative electrode of the lithium ion battery.
As an improvement of the lithium ion battery of the present invention, the positive electrode includes a positive electrode active material selected from one or more of lithium cobalt oxide, lithium nickel oxide, lithium manganese oxide, lithium nickel cobalt aluminum oxide, and compounds obtained by adding other transition metals or non-transition metals to these oxides.
Compared with the prior art, the suspending agent for the lithium ion battery cathode provided by the invention is prepared by copolymerizing multi-membered ring alpha-cellulose and polar monomers such as acrylonitrile/propionate/methyl propionate/butyrate/vinyl acetate/allyl acetate/acrylic acid/propanesulfonic acid and the like, and a molecular chain of the suspending agent contains a large amount of polar groups such as-CN, -OCN, -COOH and-SO3H, etc., and the active material surface is easy to gather more Li due to the larger electronegativity+Is advantageous to Li+The lithium ion battery using the suspending agent has good dynamic performance. Simultaneously reacting-COOH and-SO on the molecular chain of the copolymer3And H and other groups are continuously subjected to ionization treatment, so that lithium ions are favorably extracted and inserted, the internal resistance is reduced, the lithium ion transmission efficiency is improved, and the finally obtained lithium ion battery has good rate capability, strong lithium precipitation capability and low DCR value.
Detailed Description
In order to make the objects, technical solutions and technical effects of the present invention more clear, the present invention will be described in further detail with reference to specific embodiments. It should be understood that the detailed description and specific examples, while indicating the preferred embodiment of the invention, are intended for purposes of illustration only and are not intended to limit the scope of the invention.
Example 1
1) The suspending agent is synthesized by adopting the following reaction conditions and steps:
wherein R is1is-CH2CH2-，R2is-COOH, X is Na+，
Structural formula is
The number average molecular weight is 300000-400000.
Preparation of the Battery
1) Preparation of positive plate
The positive active material LiNiCoMnO2And stirring the binder PVDF, the conductive agent SP and the solvent N-methyl pyrrolidone (NMP) at a high speed for 3 hours to obtain uniformly dispersed slurry. In the slurry, the solid content was 60 wt%, and 90 wt% of lithium nickel cobalt manganese oxide (LiNiCoMnO) was contained in the solid content2) 5.0 wt% of polyvinylidene fluoride and 5 wt% of conductive carbon black. And then, uniformly coating the slurry on two surfaces of the aluminum foil, and drying and compacting by a roller press to obtain the positive plate.
2) Preparation of negative plate
Mixing the artificial graphite serving as the negative electrode active material, the SBR emulsion serving as the binder, the suspending agent for the lithium ion battery negative electrode and the conductive carbon black serving as the conductive agent, adding deionized water serving as a solvent, and stirring at a high speed to obtain uniformly dispersed slurry. The slurry had a solid content of 40 wt%, and contained 90 wt% of artificial graphite, 2 wt% of a suspension for a negative electrode of a lithium ion battery (general formula Ia), 3 wt% of conductive carbon black, and 5 wt% of SBR as solid components. And then uniformly coating the slurry on two surfaces of the copper foil, and drying and compacting by a roller press to obtain the negative plate.
3) Preparation of the electrolyte
The electrolyte is prepared by mixing lithium hexafluorophosphate with the concentration of 1M as a lithium salt and ethylene carbonate, dimethyl carbonate and 1, 2-propylene carbonate as a solvent according to the volume ratio of 1:1: 1.
4) Preparation of lithium ion battery
And welding conductive tabs on the positive plate and the negative plate, spacing the positive plate and the negative plate by adopting a polypropylene/polyethylene composite isolating film with the thickness of 12 microns, then winding to form a naked electric core, and packaging by using an aluminum plastic film. And injecting electrolyte after packaging, and carrying out formation and aging on the battery cell to obtain the square flexible package lithium ion battery with the length, width and thickness of 130mm multiplied by 60mm multiplied by 4 mm.
Examples 2 to 21 are basically the same as example 1 except that the suspending agent for a negative electrode of a lithium ion battery has different substituents in the structural formula, and the relevant parameters of each example are shown in table 1.
Comparative example 1
Comparative example 1 is substantially the same as example 1 except that the suspending agent used in the negative electrode is a conventional suspending agent CMC (sodium carboxymethylcellulose) and the relevant parameters are shown in table 1.
Lithium ion battery performance testing
DCR testing of lithium ion batteries
The lithium ion batteries obtained in examples 1 to 21 and the lithium ion battery obtained in comparative example 1 were subjected to DCR testing according to the following procedures.
Internal resistance test of the battery corresponding to 50% capacity at 25 ℃:
1) standing the battery for 5min at 25 ℃;
2) charging the 1C constant current to 4.3V voltage, and charging the constant voltage 4.3V to 0.05C current;
3) then standing for 10 min;
4)1C0 discharge for 30min (extracted C0, adjusted to 50% capacity);
5) standing for 60 min;
6)4C discharge for 30s (sampling point interval 0.1 s);
7) standing for 10 min.
-internal resistance test of the cell at 25 ℃ for 50% capacity:
1) standing at 25 deg.C for 5 min;
2) charging to 4.3V at a constant current of 1C and charging to 0.05C at a constant voltage of 4.3V;
3) then standing for 10 min;
4)1C0 discharge for 30min (extracted C0, adjusted to 50% capacity);
5) adjusting the temperature to-25 ℃;
6) standing for 2 h;
7)0.36C discharge for 10s (0.1 s sampling point interval);
8) standing for 10 min.
The test results of examples 1 to 21 and comparative example 1 are shown in tables 1 and 2.
TABLE 1 internal resistance of examples 1 to 21 and comparative example 1 at 25 ℃ at 4C/30s for 50% capacity and at-25 ℃ at 0.36C/10s for 50% capacity
As can be seen from table 1, the DCR of the lithium ion batteries of examples 1 to 21 was significantly reduced compared to that of comparative example 1. Since the suspending agents used in examples 1 to 21 contain Li in the molecular chain+Conductive functional groups-COOH, -SO3H. CN, -OH, etc., these functional groups are strongly electronegative to Li having positive charge+Has a large attraction effect, and molecular chains actually become Li under the driving of an electric field+Favorable channels for transport, Li+The transmission resistance is reduced; at the same time, Li can be reduced+Desolvation energy barrier, Li, in positive and negative de-intercalation processes+Is advantageous in that the resistance to detachment and insertion is reducedThe dynamic performance of the battery is improved. In the general formula (I), R is represented by the following general formula (I) regardless of the structure of the examples1is-CH2An alkyl group having 2 to 5 carbon atoms or an alkenyl group having 2 to 5 carbon atoms, R2Is a compound containing-CN, -COOH, -NH2、-OCN、-OH、-CONHCH3、-CON(CH3)2、-SO3A group of H; x is Li+、Na+、K+、NH4+The DCR of the obtained lithium ion battery is obviously reduced, and the dynamic performance is obviously improved.
Rate capability test of lithium ion battery
The lithium ion batteries obtained in examples 1 to 21 and the lithium ion battery obtained in comparative example 1 were charged at a constant current of 0.5C to 4.3V and at a constant voltage to a cutoff voltage of 0.05C at room temperature, and then discharged at different discharge rates (0.5C, 1.0C, 2.0C, and 3.0C), respectively, and the test results are shown in table 2. The capacity obtained by 0.5C discharge was used as a reference value (100%).
TABLE 2 Rate Performance test results for examples 1-21 and comparative example 1
As can be seen from Table 2, the rate performance of the lithium ion batteries of examples 1 to 21 was significantly improved at (1.0C, 2.0C, 3.0C) compared to comparative example 1, because the molecular chains of the suspending agents used in examples 1 to 21 contain Li-utilizing compounds+Conductive functional groups-COOH, -SO3H. CN, -OH, etc., these functional groups are strongly electronegative to Li having positive charge+Has a large attraction effect, and molecular chains actually become Li under the driving of an electric field+Favorable channels for transport, Li+The transmission resistance is reduced; at the same time, Li can be reduced+Desolvation energy barrier, Li, in positive and negative de-intercalation processes+The de-intercalation resistance is reduced, and the rate capability of the battery is improved. In the general formula (I), R is represented by the following general formula (I) regardless of the structure of the examples1is-CH2An alkyl group having 2 to 5 carbon atoms or an alkenyl group having 2 to 5 carbon atoms, R2Is a compound containing-CN, -COOH, -NH2、-OCN、-OH、-CONHCH3、-CON(CH3)2、-SO3A group of H; x is Li+、Na+、K+、NH4+The rate capability of the obtained lithium ion battery is obviously improved.
Negative pole lithium separating performance test of lithium ion battery
Respectively charging the lithium ion batteries obtained in the examples 1-21 and the lithium ion battery obtained in the comparative example 1 at 25 ℃ by using a 3C constant current to 4.3V, charging at a constant voltage to a cut-off voltage of 0.05C, discharging at 1C to 2.8V, and completing the test process after circulating for 10 circles; charging to 4.3V at-20 deg.C under constant current of 0.1C, charging to cut-off voltage of 0.05C under constant voltage, discharging to 2.8V under 0.33C, and circulating for 10 circles. The lithium deposition from the negative electrode is shown in table 3.
TABLE 3 negative electrode lithium deposition test results of examples 1 to 21 and comparative example 1
0 means no lithium precipitation, 1 means slight lithium precipitation, 4 means more severe lithium precipitation, 5 means severe lithium precipitation, and data from 0 to 5 means more and more severe lithium precipitation.
As can be seen from table 3, compared to comparative example 1, the lithium deposition of the negative electrodes of the lithium ion batteries of examples 1 to 21 is significantly improved, substantially no lithium deposition occurs, and the lithium deposition of comparative example 1 is very serious. This is because the suspending agents used in examples 1 to 21 contain Li in the molecular chain+Conductive functional groups-CN, -OCN, -COOH, -SO3H, etc., of these functional groupsHas strong electronegativity and is suitable for Li with positive charge+Has a larger attraction effect, on one hand, under the driving of an electric field, the molecular chain is actually changed into Li+Favorable channels for transport, Li+The transmission resistance is reduced; on the other hand, Li can be reduced+Desolvation energy in positive and negative de-intercalation process, Li+The de-intercalation resistance is reduced, so that the de-intercalation resistance is favorable for de-intercalation and intercalation of lithium ions, the internal resistance is reduced, the lithium ion transmission efficiency is improved, and the dynamic performance of the battery is favorably improved. In the general formula (I), R is represented by the following general formula (I) regardless of the structure of the examples1is-CH2An alkyl group having 2 to 5 carbon atoms or an alkenyl group having 2 to 5 carbon atoms, R2Is a compound containing-CN, -COOH, -NH2、-OCN、-OH、-CONHCH3、-CON(CH3)2、-SO3A group of H; x is Li+、Na+、K+、NH4+The lithium ion battery obtained has obviously improved negative pole lithium separation condition and obviously improved dynamic performance.
Compared with the prior art, the suspending agent for the lithium ion battery cathode provided by the invention is prepared by copolymerizing multi-membered ring alpha-cellulose and polar monomers such as acrylonitrile/propionate/methyl propionate/butyrate/vinyl acetate/allyl acetate/acrylic acid/propanesulfonic acid and the like, and a molecular chain of the suspending agent contains a large amount of polar groups such as-CN, -OCN, -COOH and-SO3H, etc., and the active material surface is easy to gather more Li due to the larger electronegativity+Is advantageous to Li+The lithium ion battery using the suspending agent has good dynamic performance. Simultaneously reacting-COOH and-SO on the molecular chain of the copolymer3And H and other groups are continuously subjected to ionization treatment, so that lithium ions are favorably extracted and inserted, the internal resistance is reduced, the lithium ion transmission efficiency is improved, and the finally obtained lithium ion battery has good rate capability, strong lithium precipitation capability and low DCR value.
The present invention can be modified and adapted appropriately from the above-described embodiments, according to the principles described above. Therefore, the present invention is not limited to the specific embodiments disclosed and described above, and some modifications and variations of the present invention should fall within the scope of the claims of the present invention. Furthermore, although specific terms are employed herein, they are used in a generic and descriptive sense only and not for purposes of limitation.
Claims (10)
1. A suspending agent for a negative electrode of a lithium ion battery, comprising one of a compound represented by general formula (I), a compound represented by general formula 1c, and a compound represented by general formula 1 e:
wherein R is1is-CH2-，R2Is selected from-CH2CN、-CH2CH2CN、-OCN、-CH2NH2、-OH、-CH2OH、-C(CH3)2OH、-SO3H、-CH2SO3H; or
R1Is alkyl with 2-5 carbon atoms or alkenyl with 2-5 carbon atoms, R2Is a compound containing-CN, -COOH, -NH2、-OCN、-OH、-CONHCH3、-CON(CH3)2、-SO3A group of H;
x is Li+、Na+、K+、NH4+One of (1);
m >0, n >0, and m + n is 100%.
2. The suspension for a negative electrode of a lithium ion battery according to claim 1, wherein R is the number of moles of the compound represented by formula (I)1When the alkyl group has 2 to 5 carbon atoms, R1Is selected from- (CH)2)2-、-(CH2)3-、-(CH2)4-、-(CH2)5-、-CH(CH3)-、-C(CH3)2-、-C(CH3)2CH2-、-C(CH3)2CH2CH2-、-CH(CH3)CH2-、-C(CH2CH3)CH2-、-C(CH2CH2CH3)CH2-、-CH(CH3)CH2CH2-、-CH(CH3)CH2CH2CH2-one of the above;
when R is1When the alkenyl group has 2 to 5 carbon atoms, R1Selected from-CH ═ CH-, -CH2-CH＝CH-、-CH2-CH2-CH＝CH-、-CH2-CH＝CH-CH2-CH2-、-CH2-CH2-CH2-CH-is one of CH-;
R2selected from-CN, -CH2CN、-CH2CH2CN、-OCN、-CH2NH2、-CONHCH3、-CON(CH3)2、-OH、-CH2OH、-C(CH3)2OH、-COOH、-C6H5COOH、-SO3H、-CH2SO3H、-C6H5SO3H、-C6H5CH2SO3H.
3. The suspending agent for the negative electrode of the lithium ion battery according to claim 1, wherein the suspending agent for the negative electrode of the lithium ion battery is one or more selected from the following compounds:
4. the suspending agent for the negative electrode of the lithium ion battery as claimed in claim 1, wherein the ratio of m to n in the general formula (I) is (50-80%) (20-50%).
5. The suspending agent for the negative electrode of the lithium ion battery as claimed in claim 1, wherein the ratio of m to n in the general formula (I) is (60-70%) (30-40%).
6. The suspending agent for a negative electrode of a lithium ion battery according to claim 1, wherein the number average molecular weight of the suspending agent for a negative electrode of a lithium ion battery is 300000 to 400000.
7. A lithium ion battery negative electrode, comprising a negative electrode current collector and a negative electrode active material layer coated on the negative electrode current collector, wherein the negative electrode active material layer comprises a negative electrode active material and a suspending agent, and the suspending agent is the suspending agent for the lithium ion battery negative electrode in any one of claims 1 to 6.
8. The negative electrode for lithium ion batteries according to claim 7, wherein the suspension agent is present in an amount of 2 to 5 wt% based on the total weight of the negative electrode active material layer.
9. The negative electrode of claim 7, wherein the negative active material is selected from one or more of soft carbon, hard carbon, artificial graphite, natural graphite, silicon-oxygen compound, silicon-carbon composite, lithium titanate, and metals capable of forming an alloy with lithium.
10. A lithium ion battery comprising a positive electrode, a negative electrode, a separator interposed between the positive electrode and the negative electrode, and an electrolyte, wherein the negative electrode is the negative electrode of claim 7.
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