CN108493452B - Water-based binder for inhibiting expansion of pole piece material, lithium ion battery negative electrode material based on water-based binder and preparation method - Google Patents
Water-based binder for inhibiting expansion of pole piece material, lithium ion battery negative electrode material based on water-based binder and preparation method Download PDFInfo
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- 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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- H01M4/386—Silicon or alloys based on silicon
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Abstract
The invention discloses a water-based binder for inhibiting expansion of a pole piece material, a lithium ion battery negative electrode material based on the water-based binder and a preparation method of the lithium ion battery negative electrode material, and belongs to the technical field of electrochemistry and new energy materials. The binder is dissolved in a dispersion medium to form a solution with the concentration of 0.5-3.0%, wherein the dispersion medium is deionized water, and the binder is a compound of galactomannan and fulvic acid. The lithium ion battery negative electrode slurry using the aqueous binder consists of an active material, a conductive agent and a binder, wherein the mass ratio of the components is (50-80): (10-30): (10-20). The aqueous binder can be coated on the surfaces of an active substance and a conductive agent to form a high-elasticity space, adapts to volume change in the charge-discharge process of an electrode, improves the cycle performance of a battery, has wide raw material sources, and is a green and environment-friendly composite binder.
Description
Technical Field
The invention belongs to the technical field of electrochemistry and new energy materials, and particularly relates to a water-based binder for inhibiting expansion of a pole piece material, a binder for a lithium ion battery negative electrode material based on the water-based binder, and a preparation method of the binder.
Background
The silicon material has the theoretical specific capacity up to 4200mAh/g, has lower lithium intercalation/deintercalation potential and good safety performance, and is expected to replace graphite materials to become a new generation of cathode materials. However, in the process of charge and discharge cycle of silicon material, the volume change generated by silicon particles is as high as 300-400%, which causes the cycle stability of the electrode to be greatly reduced.
Currently, the main binders for lithium ion battery electrode materials in the market mainly include polyvinylidene fluoride (PVDF), Styrene Butadiene Rubber (SBR)/sodium carboxymethylcellulose (CMC), and the like. When the PVDF is used, N-methyl pyrrolidone (NMP) needs to be added and dissolved to prepare slurry, in the process of preparing the pole piece, the volatilization of a solvent pollutes the environment and harms the health of workers, the binding power and the flexibility are poor, the effect of inhibiting the expansion of the pole piece is very limited, the capacity and the rate characteristic of the battery are difficult to improve, in addition, the price of the PVDF and the solvent is high, and the cost of the lithium ion battery is increased. The SBR/CMC water-based binder is applied on a large scale in the market, but is difficult to be applied to the preparation of the positive pole piece due to the self reason, and is slightly high in price, so that the use is limited within a certain range.
Disclosure of Invention
The invention aims to provide a water-based binder for inhibiting expansion of a pole piece material, a binder for a lithium ion battery negative electrode material based on the water-based binder, and a preparation method of the binder.
The invention is realized by the following technical scheme:
the invention discloses a water-based binder for inhibiting expansion of a pole piece material, which is prepared by mixing galactomannan and fulvic acid according to the weight ratio of (6-16): (1-4) dispersing in deionized water to prepare a solution with the mass concentration of 0.5-3.0%.
Preferably, the galactomannan comprises fenugreek gum, tara gum or locust bean gum.
Preferably, the fulvic acid has the formula:
wherein n is 50-100.
Preferably, the viscosity of the aqueous binder ranges from 200 to 1200 mPa.s.
The invention also discloses a lithium ion battery cathode material, which comprises the following components in percentage by mass: 50-80% of active material, 10-30% of conductive agent and 10-20% of water-based binder;
the aqueous binder is prepared by mixing galactomannan and fulvic acid according to the weight ratio of (6-16): (1-4) dispersing in deionized water to prepare a solution with the mass concentration of 0.5-3.0%.
Preferably, the galactomannan comprises fenugreek gum, tara gum or locust bean gum;
the structural formula of the fulvic acid is shown as follows:
wherein n is 50-100.
Preferably, the active material is selected from a silicon anode material, a graphite anode material or a sulfide; the conductive agent is selected from acetylene black or superconducting carbon black.
The invention also discloses a preparation method of the lithium ion battery cathode material, which comprises the following steps:
1) fully and uniformly grinding the active material and the conductive agent, then dropwise adding the aqueous binder, and continuously grinding until the aqueous binder is uniformly mixed in the active material and the conductive agent to prepare a mixture;
2) placing the product prepared in the step 1) on a Cu sheet and uniformly coating;
3) drying the Cu sheet treated in the step 2) to prepare a pole piece, and drying the pole piece in vacuum;
4) and weighing the pole piece slide glass after vacuum drying to obtain the lithium ion battery negative electrode material for assembling the battery.
Preferably, in the step 1), the active material and the conductive agent are put into a mortar to be ground for 5-10 min, and then the aqueous binder is dripped into the mortar to be ground uniformly.
Compared with the prior art, the invention has the following beneficial technical effects:
the aqueous binder for inhibiting the expansion of the pole piece material is prepared from a compound of galactomannan and fulvic acid, wherein the galactomannan contains a large number of polar hydroxyl groups, so that the interaction force between the galactomannan and silicon particles is enhanced, an effective transmission channel is provided for the conduction of lithium ions in the charge-discharge cycle process, and the stability of a silicon negative electrode in the cycle process is ensured. On the other hand, the lone pair electrons of the ether bond in the galactomannan can form a complexing point with lithium ions, and the lithium ions can move between the complexing points of the galactomannan, so that the effective transfer of the lithium ions is realized, and the high rate performance and the cycle stability performance of the lithium ion battery negative electrode material are improved. The fulvic acid is extracted from low-grade coal (peat, brown coal and weathered coal), mainly consists of aromatic hydroxycarboxylic acid substances, can enhance the adhesion between the fulvic acid and a negative electrode material through the action of hydrogen bonds, and buffers the volume change in the charging and discharging processes of the battery, thereby improving the cycle performance of the battery. Therefore, the aqueous binder for inhibiting the expansion of the pole piece material can improve the high-rate performance and the cycle stability of the lithium ion battery negative electrode material and prolong the service life of the battery.
According to the lithium ion battery cathode material prepared based on the aqueous binder for inhibiting the expansion of the pole piece material, the aqueous binder can be coated on the surfaces of the active substance and the conductive agent to form a high-elasticity space, so that the volume change of the electrode in the charging and discharging processes is buffered, the slurry dispersibility is improved, the electrode forms a good conductive network, and the battery cycle performance is improved. In view of the good electrochemical performance of the silicon negative electrode, the application of the aqueous binder for inhibiting the expansion of the pole piece material undoubtedly plays an important role in implementing a sustainable development strategy and promoting the commercialization process of the silicon negative electrode.
The preparation method disclosed by the invention is simple to operate, has low requirements on equipment, and is easy for large-scale production.
Detailed Description
The present invention will now be described in further detail with reference to specific examples, which are intended to be illustrative, but not limiting, of the invention.
The aqueous binder used for inhibiting the expansion of the pole piece material is usually prepared into 0.5-3.0 wt% of solution for preparing the electrode material of the lithium ion battery, and deionized water is used as a diluent to prepare the thickness of slurry in the preparation process.
The mass ratio of the galactomannan to the fulvic acid in the aqueous binder for inhibiting the expansion of the pole piece material is (6-16) to (1-4).
The invention discloses a negative electrode material of a lithium ion battery, which comprises the following components in percentage by mass: conductive agent: the binder is 50-80:10-30: 10-20.
The lithium ion battery negative electrode active material comprises a silicon negative electrode, a graphite negative electrode and a sulfide, and the conductive agent is preferably acetylene black or superconducting carbon black.
The preparation method comprises mixing the slurry for at least 30 min, coating with a thickness of 100-200 μm (preferably 100nm), and baking at 60-80 deg.C.
The preparation method of the lithium ion battery negative electrode material comprises the following steps:
step 1: preparing a galactomannan and fulvic acid complex into a 0.5-3 wt% aqueous solution;
step 2: grinding the active substance and the conductive agent in a mortar for 5-10 minutes;
and step 3: dropwise adding the binder prepared in the step 1 into the mixture obtained in the step 2, wherein the mass ratio of the binder to the mixture is 1:10-1:5, and grinding until the binder is uniformly mixed with the active substance and the conductive agent;
and 4, step 4: dropwise adding deionized water into the mixture obtained in the step 3, and then fully grinding for 20-30 minutes;
and 5: pouring the mixture obtained in the step (4) on a Cu sheet, and uniformly coating;
step 6: rapidly drying the copper sheet obtained in the step 5 by air blowing to remove solvent water to obtain a pole piece, and drying the pole piece in vacuum;
and 7: and weighing the vacuum-dried pole piece cut pieces, and assembling the battery.
The raw materials used in the invention are all commercial products, and the fulvic acid is purchased from Shandong Yousio chemical technology Co., Ltd, a product number of 059415001200.
Example 1
The fenugreek gum and the fulvic acid compound (FG/HA) with the viscosity of 200mPa are prepared into 0.5 wt% aqueous solution, wherein the mass ratio of the fenugreek gum to the fulvic acid is 4: 1.
60.0mg of nano Si and 30.0mg of acetylene black are weighed and put in a mortar, ground for 10 minutes, and then 2.0g of 0.5 wt% aqueous solution of fenugreek gum and fulvic acid compound is added dropwise. Grinding for 5 minutes until the binder is uniformly mixed with the Si powder and the carbon powder, then dripping 1mL of deionized water, and fully grinding for 15-10 minutes to obtain a pasty mixture, namely the binder for the lithium ion battery negative electrode material.
The lithium ion battery negative electrode material is placed on a Cu sheet by using a binder, uniformly coated by using a scraper with the thickness of 100 mu m, quickly placed in a forced air drying oven with the temperature of 60 ℃, and taken out after five minutes. And then putting the pole piece into a vacuum drying oven, and carrying out vacuum drying for 6h at the constant temperature of 80 ℃. Weighing the vacuum-dried pole piece cut pieces, assembling the pole piece cut pieces in a glove box in a 2032 battery case, taking a lithium piece as a positive electrode, taking a polyethylene film as a diaphragm and taking 1mol/L LiPF6EC/DMC/DEC (v/v/v-1/1/1) was used for constant current charge and discharge test of the assembled battery.
Example 2
Firstly, preparing the tala gum and the fulvic acid compound (TG/HA) into 2.0 wt% aqueous solution with the viscosity of 650mPa.s, wherein the mass ratio of the tala gum to the fulvic acid is 6: 1. 80.0mg of nano Si and 10.0mg of acetylene black were weighed and put in a mortar, ground for 10 minutes, and then 1.0g of 2.0 wt% aqueous solution of tala gum and fulvic acid complex was added dropwise. Grinding for 5 minutes until the binder is uniformly mixed with the Si powder and the carbon powder, then dripping 1mL of deionized water, and then fully grinding for 15-10 minutes. The pasty mixture was placed on a Cu sheet, uniformly coated with a 100 μm doctor blade, quickly placed in a forced air drying cabinet at 60 ℃ and taken out after five minutes. And then putting the pole piece into a vacuum drying oven, and carrying out vacuum drying for 6h at the constant temperature of 80 ℃. After weighing the pole piece cut pieces dried in vacuum, assembling the pole piece cut pieces in a glove box in a 2032 battery case, assembling the battery by using a lithium piece as a positive electrode, a polyethylene film as a diaphragm and 1mol/L LiPF6EC/DMC/DEC (v/v/v is 1/1/1) as electrolyte, and performing constant current charge and discharge tests.
Example 3
Preparing 3.0 wt% aqueous solution of locust bean and fulvic acid compound (LG/HA) with the viscosity of 1200mPa.s, wherein the mass ratio of the locust bean to the fulvic acid is 6: 1. 50.0mg of nano Si and 20.0mg of acetylene black were weighed out in a mortar, ground for 10 minutes, and then 0.67g of a 3.0 wt% aqueous solution of Robinia pseudoacacia L and fulvic acid complex was added dropwise. Grinding for 5 minutes until the binder is uniformly mixed with the Si powder and the carbon powder, then dripping 1mL of deionized water, and then fully grinding for 15-10 minutes. The pasty mixture was placed on a Cu sheet, uniformly coated with a 100 μm doctor blade, quickly placed in a forced air drying cabinet at 60 ℃ and taken out after five minutes. And then putting the pole piece into a vacuum drying oven, and carrying out vacuum drying for 6h at the constant temperature of 80 ℃. After weighing the pole piece cut pieces dried in vacuum, assembling the pole piece cut pieces in a glove box in a 2032 battery case, assembling the battery by using a lithium piece as a positive electrode, a polyethylene film as a diaphragm and 1mol/L LiPF6EC/DMC/DEC (v/v/v is 1/1/1) as electrolyte, and performing constant current charge and discharge tests.
Comparative example 1
In contrast to example 2, using PVDF as binder and N-methyl pyrrolidone (NMP) as diluent solvent, the corresponding film baking temperature was raised to 120 deg.C (vacuum drying).
Comparative example 2
In contrast to example 2, carboxymethyl cellulose (CMC) having a viscosity of 650mpa.s was used as a binder, and distilled water was used as a dispersion solvent.
The electrochemical performance of the silicon anode material of the composite binder provided by the invention is tested through charge-discharge cycles. Table 1 shows the cycle performance of the silicon electrodes of the examples of the present invention and the comparative examples at a charge/discharge current density of 100 mA/g.
TABLE 1
Table 1 shows the corresponding capacity and charge-discharge efficiency. As can be seen from Table 1, the first discharge capacities of both the galactomannan and the fulvic acid binder were greater than 2600 mAh/g. The first efficiency of PVDF and CMC as binders was below 80%. At the 200 th cycle, the electrode discharge capacities of PVDF and CMC as binders were lower than 60 mAh/g. And the discharge capacity of the electrode of the galactomannan and fulvic acid composite binder is higher than 1800 mAh/g.
Claims (3)
1. The lithium ion battery negative electrode material is characterized by comprising the following components in percentage by mass: 50% -80% of active materials, 10% -30% of conductive agents and 10% -20% of water-based binders;
the aqueous binder is prepared by mixing galactomannan and fulvic acid according to the weight ratio of 6:1 or 4:1, dispersing in deionized water to prepare a solution with the mass concentration of 0.5-3.0%, wherein the galactomannan comprises fenugreek gum, tara gum or locust bean gum, and the viscosity of the aqueous binder is 200-1200 mPa.s;
wherein the fulvic acid has the structural formula shown as follows:
wherein n = 50-100;
the active material is selected from silicon negative electrode materials;
the conductive agent is selected from acetylene black or superconducting carbon black.
2. The preparation method of the lithium ion battery negative electrode material of claim 1, characterized by comprising the following steps:
1) fully and uniformly grinding the active material and the conductive agent, then dropwise adding the aqueous binder, and continuously grinding until the aqueous binder is uniformly mixed in the active material and the conductive agent to prepare a mixture;
2) placing the product prepared in the step 1) on a Cu sheet and uniformly coating;
3) drying the Cu sheet treated in the step 2) to prepare a pole piece, and drying the pole piece in vacuum;
4) and weighing the pole piece slide glass after vacuum drying to obtain the lithium ion battery negative electrode material for assembling the battery.
3. The preparation method of the lithium ion battery anode material according to claim 2, wherein in the step 1), the active material and the conductive agent are put in a mortar to be ground for 5-10 min, and then the active material and the conductive agent are continuously and uniformly ground after dropwise adding the aqueous binder.
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| CN111769282B (en) * | 2020-06-22 | 2021-10-22 | 上海交通大学 | Application method of water-based binder in magnesium-sulfur battery |
| CN114914444A (en) * | 2021-02-10 | 2022-08-16 | 中国石油化工股份有限公司 | Silicon-carbon negative electrode plate, preparation method thereof and lithium ion battery |
| CN114824224A (en) * | 2022-05-11 | 2022-07-29 | 常州硅源新能材料有限公司 | Silicon-based negative electrode material, preparation method thereof and lithium ion battery |
| CN116515349B (en) * | 2022-12-08 | 2024-02-13 | 广西至善新材料科技有限公司 | Tara adhesive conductive coating and preparation method thereof |
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| CN106887594A (en) * | 2017-04-01 | 2017-06-23 | 陕西科技大学 | Hydrophobically modified natural plant polyose water-based binder and its application in lithium ion battery negative |
| CN107017408A (en) * | 2017-04-01 | 2017-08-04 | 陕西科技大学 | Trigonella bean gum water-based binder and its application in negative electrode of lithium ion battery |
| CN107359351A (en) * | 2017-06-29 | 2017-11-17 | 郑州大学 | A kind of method that lithium ion battery prepares electrode slice with humic acid base water-based binder and using the binding agent |
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| CN106887594A (en) * | 2017-04-01 | 2017-06-23 | 陕西科技大学 | Hydrophobically modified natural plant polyose water-based binder and its application in lithium ion battery negative |
| CN107017408A (en) * | 2017-04-01 | 2017-08-04 | 陕西科技大学 | Trigonella bean gum water-based binder and its application in negative electrode of lithium ion battery |
| CN107359351A (en) * | 2017-06-29 | 2017-11-17 | 郑州大学 | A kind of method that lithium ion battery prepares electrode slice with humic acid base water-based binder and using the binding agent |
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