CN108232109B - Application of konjac glucomannan in adhesive - Google Patents

Application of konjac glucomannan in adhesive Download PDF

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CN108232109B
CN108232109B CN201711435284.7A CN201711435284A CN108232109B CN 108232109 B CN108232109 B CN 108232109B CN 201711435284 A CN201711435284 A CN 201711435284A CN 108232109 B CN108232109 B CN 108232109B
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silicon
negative electrode
lithium ion
ion battery
binder
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CN108232109A (en
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胡先罗
郭松涛
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Huazhong 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
    • H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
    • H01M4/139—Processes of manufacture
    • 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
    • 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
    • H01M4/621—Binders
    • H01M4/622—Binders being polymers
    • 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

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  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Materials Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Battery Electrode And Active Subsutance (AREA)
  • Secondary Cells (AREA)
  • Silicon Compounds (AREA)

Abstract

The invention discloses application of konjac glucomannan as a binder, wherein the binder is used for preparing a silicon-based negative electrode plate of a lithium ion battery. Because konjac glucomannan molecules have more hydroxyl groups, the konjac glucomannan molecules have stronger cohesive force with silicon-based materials, show better mechanical properties, can powerfully resist the expansion and deformation of silicon-based materials, avoid the structural damage of electrodes, enhance the structural stability and are beneficial to prolonging the cycle life of the silicon-based negative electrodes. By modifying the functional group on the surface of the silicon-based material, the interaction force between the silicon-based material and the binder can be further enhanced, and the electrochemical performance of the silicon-based negative electrode is obviously improved.

Description

Application of konjac glucomannan in adhesive
Technical Field
The invention relates to the field of lithium ion batteries, in particular to application of konjac glucomannan to a binder.
Background
Lithium ion batteries have become the best choice for people because of their advantages such as long life, flexible design, portability, etc. The commercial negative electrode material graphite has low specific capacity (372mAh/g) and cannot meet the increasing demand of people. Silicon has a theoretical specific capacity as high as 4200mAh/g, and is a candidate for the next generation of high specific energy lithium ion battery cathode. However, silicon suffers from a large volume change (about 400%) during charging and discharging, resulting in disintegration of the electrode and rapid capacity fade.
The design of the nano-structure silicon-carbon composite material is expected to improve the problem. But the problem of deformation of the electrode film still remains due to the large volume change inherent in silicon itself. Therefore, the binder with strong binding power and excellent mechanical property is the basic requirement of the application of the silicon-based negative electrode material. The main functions of the binder in the lithium ion electrode are to bind active materials, conductive agents and current collectors, maintain the structural stability of the electrode, ensure a complete conductive network and enable the lithium ion battery to normally operate. Currently, binders commonly used in silicon-based negative electrode materials include sodium alginate, sodium carboxymethylcellulose, polyacrylic acid, and the like. At present, the viscosity and the mechanical property of the adhesive still do not reach the ideal target, so that the electrode structure is easy to be pulverized and fall off after the silicon-based negative electrode is cycled, and the capacity is quickly attenuated.
Disclosure of Invention
The invention aims to provide a silicon-based negative electrode material water-based binder which is low in price and excellent in performance. And the surface of the silicon-based material can be modified with functional groups to enhance the binding power with a water-based binder, so that the electrochemical performance of the silicon-based cathode is remarkably improved.
According to a first aspect of the present invention, there is provided the use of konjac glucomannan as a binder.
Preferably, the adhesive is used for preparing a silicon-based negative electrode plate of the lithium ion battery. According to another aspect of the invention, a preparation method of a silicon-based negative electrode piece of a lithium ion battery is provided, wherein a silicon-based material, the binder of claim 1 and a conductive agent are uniformly dispersed into water to obtain a mixed slurry, the mass ratio of the silicon-based material to the binder of claim 1 to the conductive agent is (4-8) - (1-3), the mixed slurry is coated on the surface layer of a current collector after being fully and uniformly mixed, and the current collector is dried and pressed into a sheet to obtain the silicon-based negative electrode piece of the lithium ion battery.
Preferably, the temperature of the drying is 30 ℃ to 60 ℃.
Preferably, the silicon-based material is a silicon nanoparticle, a silicon nanowire or a silicon carbon composite.
Preferably, the surface of the silicon-based material is modified by a functional group.
Preferably, the silicon-based material is modified with a hydroxyl group or an amino group.
Preferably, the method for modifying the surface of the silicon-based material by the functional group comprises the following steps: putting the silicon-based material into an oxidant or a solution containing a modified functional group, fully reacting and centrifuging; and cleaning and drying the precipitate obtained by centrifugation to obtain the silicon-based material with the surface modified by the functional group.
Preferably, the oxidizing agent is a mixed solution of hydrogen peroxide and sulfuric acid, a sodium peroxide solution or a sodium persulfate solution; the solution containing the modified functional group is 3-aminopropyltriethoxysilane, aminopropyltrimethoxysilane or dopamine hydrochloride solution.
According to another aspect of the invention, the silicon-based negative electrode plate of the lithium ion battery is prepared by the method of any one of claims 3 to 9.
Generally, compared with the prior art, the technical scheme of the invention mainly has the following beneficial effects:
(1) compared with the binder molecules in the prior art, the konjac glucomannan molecules have more hydroxyl groups, have stronger binding power with silicon-based materials, and effectively improve the specific capacity of the silicon-based negative electrode.
(2) The konjac glucomannan has better mechanical property, can powerfully resist the expansion deformation of the silicon-based material cathode, avoids the structural damage of the electrode, enhances the structural stability and slows down the problem of rapid capacity attenuation caused by the expansion of the silicon-based cathode. Compared with the traditional binder, the konjac glucomannan effectively prolongs the cycle life of the silicon-based negative electrode.
(3) By modifying functional groups such as hydroxyl, amino and the like on the surface of the silicon-based material, the interaction force between the silicon-based material and the binder can be further enhanced, so that the electrochemical performance of the silicon-based negative electrode is further improved.
Drawings
Fig. 1 is a graph of the cycle performance of the battery of example 1.
Fig. 2 is a graph of the cycle performance of the battery of example 2.
Fig. 3 is an SEM image of a silicon negative electrode after 50 cycles of the cell in example 2.
Fig. 4 is a graph of the cycle performance of the battery in example 3.
Fig. 5 is a graph showing cycle performance of the battery in comparative example 1.
Fig. 6 is a graph showing the cycle performance of the battery in comparative example 2.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and 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 addition, the technical features involved in the embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.
Example 1
Silicon nanoparticles do not do anythingDispersing silicon nanoparticles (0.05g), konjac glucomannan (0.025g) and a conductive agent (Super P, 0.025g) into 4ml of water, stirring for 12 hours, uniformly coating the blended slurry on copper foil, drying at 45 ℃ for 24 hours under a vacuum condition, cutting the dried pole piece, transferring the cut pole piece into a glove box, and assembling a 2032 button cell by taking a lithium piece as a counter electrode, wherein the electrolyte is 1M L iPF6PC/EC (volume ratio 1:1) solution as electrolyte, and 5% of FEC additive by mass fraction. And finally, carrying out constant-current charge and discharge test on the button cell, wherein the current density is 2A/g, and the voltage window is 0.01-2V. Fig. 1 shows that the battery using konjac glucomannan as a binder and silicon nanoparticles without any treatment as an active material shows excellent cycle performance, and the specific capacity is retained to 814mAh/g after 1000 charge-discharge cycles.
Example 2
The preparation method comprises the following steps of putting silicon nanoparticles (2g) into a hydrogen peroxide/sulfuric acid mixed solution (100ml, volume ratio of 3:7), stirring for 2 hours at 80 ℃, centrifuging a stirred product at 10000 r/min, centrifuging and cleaning obtained precipitates for 10 times at 10000 r/min by using water, drying at 80 ℃ to obtain hydroxyl-modified silicon nanoparticles, dispersing hydroxyl-modified silicon nanoparticles (0.05g), konjac glucomannan (0.025g) and a conductive agent (Super P, 0.025g) into 4ml of water, stirring for 12 hours, uniformly coating the well-blended slurry on copper foil, drying for 24 hours at 45 ℃ under a vacuum condition, cutting a dried pole piece, transferring the cut pole piece into a glove box, and assembling a button type 2032 battery by using a lithium piece as a counter electrode, wherein an electrolyte is 1M L iPF6PC/EC (volume ratio 1:1) solution as electrolyte, and 5% of FEC additive by mass fraction. And finally, carrying out constant-current charge and discharge test on the button cell, wherein the current density is 2A/g, and the voltage window is 0.01-2V. Fig. 2 shows that the battery shows excellent cycle performance when konjac glucomannan is used as a binder and silicon nanoparticles modified by hydroxyl are used as active materials, and the specific capacity is retained by 1278mAh/g after 1000 charge-discharge cycles. FIG. 3 also shows the Scanning Electron Microscope (SEM) image of the electrode plate after 50 charge-discharge cycles, the structure remains intact without rupture, which shows that the konjac glucomannan binder can effectively maintain the battery structureAnd (4) stability.
Example 3
Ultrasonically dispersing silicon nano particles (0.3g) in ethanol (360ml) for 1 hour, sequentially adding concentrated ammonia water (6ml), water (30ml) and 3-aminopropyltriethoxysilane (0.3ml), stirring at room temperature for 1.5 hours, centrifuging the stirred product at 10000 r/min, centrifugally cleaning the obtained precipitate with ethanol at 10000 r/min for 6 times, drying at 80 ℃ to obtain amino-modified silicon nano particles, dispersing the amino-modified silicon nano particles (0.05g), konjac glucomannan (0.025g) and a conductive agent (Super P, 0.025g) in 4ml of water, stirring for 12 hours, uniformly coating the well-mixed slurry on copper foil, drying at 45 ℃ for 24 hours under a vacuum condition, transferring the dried and cut silicon nano particles into a glove box, and assembling a 2032 battery by using a lithium sheet as a counter electrode, wherein the button electrolyte is 1M L iPF6PC/EC (volume ratio 1:1) solution as electrolyte, and 5% of FEC additive by mass fraction. And finally, carrying out constant-current charge and discharge test on the button cell, wherein the current density is 2A/g, and the voltage window is 0.01-2V. Fig. 4 shows that the battery shows excellent cycling stability when konjac glucomannan is used as a binder and silicon nanoparticles modified by amino groups are used as active materials, and the specific capacity is kept at 1803mAh/g after 300 charge-discharge cycles.
Example 4
Dispersing silicon nanoparticles (0.05g), konjac glucomannan (0.025g) and a conductive agent (Super P, 0.025g) into 4ml of water, stirring for 12 hours, uniformly coating the blended slurry on a copper foil, drying for 24 hours at 30 ℃ under a vacuum condition, cutting the dried pole piece, transferring the cut pole piece into a glove box, and assembling a 2032 button cell by taking a lithium piece as a counter electrode, wherein the electrolyte is 1M L iPF6PC/EC (volume ratio 1:1) solution as electrolyte, and 5% of FEC additive by mass fraction. And finally, carrying out constant current charge and discharge test on the button cell. The battery exhibited excellent cycle performance using konjac glucomannan as a binder and silicon nanoparticles without any treatment as an active material, similar to example 1.
Example 5
Silicon nanoparticles were left untreatedDispersing silicon nanoparticles (0.05g), konjac glucomannan (0.025g) and a conductive agent (Super P, 0.025g) into 4ml of water, stirring for 12 hours, uniformly coating the blended slurry on copper foil, drying at 60 ℃ for 24 hours under a vacuum condition, cutting the dried pole piece, transferring the cut pole piece into a glove box, and assembling a 2032 button cell by taking a lithium piece as a counter electrode, wherein the electrolyte is 1M L iPF6PC/EC (volume ratio 1:1) solution as electrolyte, and 5% of FEC additive by mass fraction. And finally, carrying out constant current charge and discharge test on the button cell. The battery exhibited excellent cycle performance using konjac glucomannan as a binder and silicon nanoparticles without any treatment as an active material, similar to example 1.
Example 6
Dispersing silicon nanoparticles (0.08g), konjac glucomannan (0.01g) and a conductive agent (Super P, 0.01g) into 4ml of water, stirring for 12 hours, uniformly coating the blended slurry on copper foil, drying for 24 hours at 45 ℃ under a vacuum condition, cutting the dried pole piece, transferring the cut pole piece into a glove box, and assembling a 2032 button cell by taking a lithium piece as a counter electrode, wherein the electrolyte is 1M L iPF6PC/EC (volume ratio 1:1) solution as electrolyte, and 5% of FEC additive by mass fraction. And finally, carrying out constant current charge and discharge test on the button cell. The content of silicon nano particles in the pole piece is increased, the capacity is reduced, and better cycle stability is still maintained.
Example 7
Dispersing a silicon-carbon composite material (0.05g), konjac glucomannan (0.025g) and a conductive agent (SuperP, 0.025g) into 4ml of water, stirring for 12 hours, uniformly coating the blended slurry on copper foil, drying for 24 hours at 45 ℃ under a vacuum condition, cutting the dried pole piece, transferring the cut pole piece into a glove box, and assembling a 2032 button cell by taking a lithium piece as a counter electrode, wherein the electrolyte is 1M L iPF6PC/EC (volume ratio 1:1) solution as electrolyte, and 5% of FEC additive by mass fraction. And finally, carrying out constant current charge and discharge test on the button cell. When the konjac glucomannan is used as a binder and the silicon-carbon composite material is used as an active material, the battery shows excellent cycle performance.
Comparative example 1
Dispersing silicon nanoparticles (0.05g), sodium alginate (0.025g) and a conductive agent (SuperP, 0.025g) into 4ml of water, stirring for 12 hours, uniformly coating the blended slurry on copper foil, drying for 12 hours at 80 ℃ under a vacuum condition, cutting the dried pole piece, transferring the cut pole piece into a glove box, and assembling a 2032 button cell by taking a lithium piece as a counter electrode, wherein the electrolyte is a PC/EC (volume ratio of 1:1) solution with 1M L iPF6 as an electrolyte, and adding an FEC additive with the mass fraction of 5%.
Comparative example 2
A2032 button cell is assembled by using a lithium sheet as a counter electrode, wherein the electrolyte is a PC/EC (volume ratio 1:1) solution with 1M L iPF6 as an electrolyte, and an FEC additive with the mass fraction of 5% is added, and finally the button cell is subjected to constant current charge and discharge test, as shown in FIG. 6, the cell shows poor cycle stability when the sodium carboxymethyl cellulose is used as a binder and the untreated silicon nanoparticles are used as an active material, and the specific capacity is only 129mAh/g after 90 charge and discharge cycles.
It will be understood by those skilled in the art that the foregoing is only a preferred embodiment of the present invention, and is not intended to limit the invention, and that any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the scope of the present invention.

Claims (6)

1. A preparation method of a silicon-based negative electrode piece of a lithium ion battery is characterized by uniformly dispersing a silicon-based material, a binder and a conductive agent into water to obtain a mixed slurry, wherein the mass ratio of the silicon-based material to the binder to the conductive agent is (4-8) to (1-3), fully and uniformly mixing, coating the mixed slurry on the surface layer of a current collector, drying the current collector and tabletting to obtain the silicon-based negative electrode piece of the lithium ion battery, wherein the binder is konjac glucomannan; the surface of the silicon-based material is modified by hydroxyl or amino.
2. The method for preparing the silicon-based negative electrode plate of the lithium ion battery according to claim 1, wherein the drying temperature is 30-60 ℃.
3. The method for preparing the silicon-based negative electrode plate of the lithium ion battery as claimed in claim 1, wherein the silicon-based material is silicon nanoparticles, silicon nanowires or a silicon-carbon composite.
4. The preparation method of the silicon-based negative electrode plate of the lithium ion battery as claimed in claim 1, wherein the method for modifying the surface of the silicon-based material by the functional group comprises the following steps: putting the silicon-based material into an oxidant or a solution containing a modified functional group, fully reacting and centrifuging; and cleaning and drying the precipitate obtained by centrifugation to obtain the silicon-based material with the surface modified by the functional group.
5. The method for preparing the silicon-based negative electrode plate of the lithium ion battery as claimed in claim 4, wherein the oxidant is a mixed solution of hydrogen peroxide and sulfuric acid, a sodium peroxide solution or a sodium persulfate solution; the solution containing the modified functional group is 3-aminopropyltriethoxysilane, aminopropyltrimethoxysilane or dopamine hydrochloride solution.
6. The silicon-based negative electrode plate of the lithium ion battery prepared by the method of any one of claims 1 to 5.
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CN113024898A (en) * 2021-03-16 2021-06-25 广东工业大学 Compound gum of kappa-carrageenan and konjac glucomannan as well as preparation method and application thereof
CN113555524B (en) * 2021-08-04 2022-09-13 蜂巢能源科技有限公司 Lithium ion battery cathode, preparation method thereof and lithium ion battery
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