CN111244452A - Novel lithium ion battery based on biomass porous carbon material as negative electrode material - Google Patents

Novel lithium ion battery based on biomass porous carbon material as negative electrode material Download PDF

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CN111244452A
CN111244452A CN202010062600.6A CN202010062600A CN111244452A CN 111244452 A CN111244452 A CN 111244452A CN 202010062600 A CN202010062600 A CN 202010062600A CN 111244452 A CN111244452 A CN 111244452A
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lithium ion
ion battery
porous carbon
carbon material
negative electrode
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葛昊
尚婷婷
修忠海
郭欣
张诏
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Liaoning University
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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
    • H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
    • H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
    • H01M4/587—Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/30—Active carbon
    • C01B32/312—Preparation
    • C01B32/318—Preparation characterised by the starting materials
    • C01B32/324—Preparation characterised by the starting materials from waste materials, e.g. tyres or spent sulfite pulp liquor
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/30—Active carbon
    • C01B32/312—Preparation
    • C01B32/342—Preparation characterised by non-gaseous activating agents
    • C01B32/348—Metallic compounds
    • 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
    • H01M10/04—Construction or manufacture in general
    • H01M10/0422—Cells or battery with cylindrical casing
    • H01M10/0427—Button cells
    • 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
    • H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
    • H01M4/134—Electrodes based on metals, Si or alloys
    • 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
    • H01M2004/021—Physical characteristics, e.g. porosity, surface area
    • 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
    • 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
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
    • Y02P70/50—Manufacturing or production processes characterised by the final manufactured product

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  • Chemical Kinetics & Catalysis (AREA)
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  • General Chemical & Material Sciences (AREA)
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  • Inorganic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Environmental & Geological Engineering (AREA)
  • Battery Electrode And Active Subsutance (AREA)

Abstract

The invention discloses a novel lithium ion battery based on a biomass porous carbon material as a negative electrode material. The biomass porous carbon material is used as a negative electrode material, a proper amount of conductive agent, binder and the biomass porous carbon material are uniformly mixed to form paste, the paste is uniformly coated on a copper foil to be used as a negative electrode, and a lithium sheet is used as a positive electrode to assemble the lithium ion battery. The biomass porous carbon material is carbonized tangerine leaves. The carbonized orange leaves are applied to the lithium ion battery cathode material, on one hand, the raw material is easy to obtain and is green and environment-friendly, and on the other hand, the carbonized orange leaves have a porous structure, so that the active sites of the reaction are increased, the electronegativity of the material can be improved, and the electrochemical performance of the material is improved.

Description

Novel lithium ion battery based on biomass porous carbon material as negative electrode material
Technical Field
The invention relates to the technical field of lithium ion batteries, in particular to a novel lithium ion battery based on a biomass porous carbon material as a negative electrode material.
Background
With the increasing severity of environmental pollution and energy crisis, clean and sustainable energy use and storage become hot spots for research. Lithium ion batteries are the most promising energy storage devices due to their inherent characteristics of high energy density, high cycling stability, no memory effect, etc. The electrode active material is the core of the battery and plays a decisive role in the battery performance.
Since the first use of coke as a negative electrode material for Lithium Ion Batteries (LIBs) by Sony corporation in the early 1990's, carbon materials have been considered as the most commercially valuable negative electrode material in LIBs. The carbon material selected for the negative electrode of the current commercial rechargeable lithium battery is generally graphite, and the graphite is widely applied due to low price, high conductivity, excellent cycling stability and low lithium intercalation potential. However, the lower theoretical capacity and diffusion coefficient of lithium ions of graphite limit its application in power sources with high energy and power density requirements, such as electric vehicles. To solve these problems, wang et al have studied carbon nanotubes and other carbonaceous materials that have higher performance by creating additional lithium ion sites. However, their large-scale application is limited by the non-regenerability and high cost of carbon precursors and the complex manufacturing techniques. The energy shortage and growing market demand still drives us to find inexhaustible, effective resources for the production of high performance carbonaceous materials.
In recent years, the biomass porous carbon material has attracted extensive attention of researchers due to the advantages of low cost, abundant microstructure, reproducibility, environmental friendliness and the like. In addition, as an electrode material of a lithium ion battery, the lithium ion battery should have a high capacity, excellent rate capability and good cycle stability.
At present, research on biomass porous carbon materials has attracted more and more attention from scientific researchers and industrial circles at home and abroad. The negative electrode material of the lithium ion battery based on the biomass porous carbon material is also a subject of continuous research and development in the field.
Disclosure of Invention
The invention aims to provide a novel lithium ion battery which can improve electrochemical performance and takes a biomass porous carbon material as a negative electrode material.
The technical scheme provided by the invention is as follows: a novel lithium ion battery based on a biomass porous carbon material as a negative electrode material is prepared by taking the biomass porous carbon material as the negative electrode material, uniformly mixing a proper amount of conductive agent, a binder and the biomass porous carbon material into paste, uniformly coating the paste on a copper foil to serve as a negative electrode, and taking a lithium sheet as a positive electrode to assemble the lithium ion battery.
Furthermore, according to the novel lithium ion battery, the lithium ion battery is a lithium ion button battery.
Further, in the novel lithium ion battery, the biomass porous carbon material is carbonized tangerine leaves, and the preparation method comprises the following steps: cutting folium Citri Gangerinae into 0.2cm pieces2Adding the large and small fragments into a reaction kettle, and carrying out hydrothermal treatment at 130 ℃ for 8 h; vacuum drying the orange leaf fragments subjected to the hydrothermal treatment at 80 ℃ for 12h, then placing the dried orange leaf fragments in a tube furnace, and calcining the orange leaf fragments at 900 ℃ for 1-3h in an argon atmosphere; and (3) centrifuging and washing the obtained product to be neutral by using hydrochloric acid and distilled water in sequence, drying the product for 12 hours in vacuum at the temperature of 80 ℃, and grinding the product to obtain the target product carbonized tangerine leaves.
Further, in the novel lithium ion battery, the activator solution is a potassium hydroxide solution.
Further, according to the preparation method, the weight ratio of the orange leaf fragments to the potassium hydroxide is 1: 1-3.
Further, in the novel lithium ion battery, the conductive agent is acetylene black.
Furthermore, in the novel lithium ion battery, the binder is PVDF (polyvinylidene fluoride).
Furthermore, according to the novel lithium ion battery, the biomass porous carbon material comprises acetylene black, PVDF (polyvinylidene fluoride) (6-8), PVDF (3-1) and 1 in a weight ratio.
Furthermore, according to the novel lithium ion battery, the biomass porous carbon material, acetylene black and PVDF are 6:3:1, 7:2:1 and 8:1:1 in weight ratio.
The invention has the beneficial effects that:
1. the method takes waste biomass orange leaves as a raw material, takes potassium hydroxide as an activating agent, carries out hydrothermal treatment in a reaction kettle, carries out vacuum drying, and carries out high-temperature calcination to obtain carbonized orange leaves, and the synthesis process conditions are easy to control, the operation is simple, and the industrial production is easy to realize.
2. The carbonized tangerine leaves prepared by the method have the characteristics of easily obtained raw materials, environmental protection, sustainability and the like, and the prepared material has a relatively uniform spongy porous structure. The formation of the pore structure not only increases the lithium ion storage capacity but also reduces the resistance to lithium ion migration and accelerates the migration speed during charge and discharge thereof. And can make the material more compatible with the electrolyte.
3. The method adopts the waste biomass orange leaves as the raw material to prepare the three-dimensional porous carbon material, uses the three-dimensional porous carbon material as an electrode material for energy storage equipment, greatly reduces the cost after improving the capacity, and can create a green environment.
4. The invention prepares the three-dimensional porous carbon material by a chemical activation method, and the simple and economic preparation method provides a foundation for further industrial application of the waste biomass.
Drawings
FIG. 1 is an SEM image of carbonized cotyledons of oranges prepared by the present invention.
FIG. 2 is an XRD pattern of carbonized cotyledons of citrus prepared according to the present invention.
FIG. 3 is a Raman image of carbonized cotyledons prepared according to the present invention.
Detailed Description
The invention is further explained below with reference to specific embodiments, but is not intended to limit the scope of protection of the invention.
In order to improve the electrochemical performance of the lithium ion battery and find a suitable substitute for the negative electrode material graphite, the invention provides the lithium ion battery taking the biomass porous carbon material as the negative electrode material. The technical scheme is as follows:
preparation of biomass porous carbon material-carbonized tangerine leaf
1) Dissolving potassium hydroxide in distilled water at room temperature to prepare a potassium hydroxide solution;
preferably, the concentration of the potassium hydroxide solution is 60-80 mg/mL.
More preferably, the concentration of the potassium hydroxide solution is 70 mg/mL.
2) Cutting folium Citri Gangerinae into 0.2cm pieces2Adding the large and small fragments into a reaction kettle, and carrying out hydrothermal treatment at 130 ℃ for 8 h; and (3) drying the orange leaf fragments subjected to the hydrothermal treatment at 80 ℃ for 12h in vacuum.
Preferably, the weight ratio of the orange leaf fragments to the potassium hydroxide is 1: 1-3.
3) Placing the dried orange leaf fragments obtained in the step 2) in a tube furnace, and calcining for 1-3h at the temperature of 900 ℃ in an argon atmosphere; and (3) centrifuging and washing the obtained product to be neutral by using hydrochloric acid and distilled water in sequence, drying the product for 12 hours in vacuum at the temperature of 80 ℃, and grinding the product to obtain the target product carbonized tangerine leaves.
Preferably, the calcination temperature is 800 ℃ and the calcination time is 2 h.
Wherein the potassium hydroxide activating solution is prepared to enrich K in the solution+. Subjecting the leaves of Citrus reticulata to hydrothermal treatment in potassium hydroxide solution to obtain K+Entering the surface of the orange leaves to better prepare the porous carbonized orange leaf material.
(II) lithium ion button cell
Carbonized tangerine leaves are used as a negative electrode material, a proper amount of conductive agent, binder and carbonized tangerine leaves are uniformly mixed to form paste, the paste is uniformly coated on a copper foil to be used as a negative electrode, a lithium sheet is used as a positive electrode, and the lithium ion battery is assembled.
Preferably, the conductive agent is acetylene black.
Preferably, the binder is PVDF (polyvinylidene fluoride).
Preferably, the carbonized tangerine leaves comprise acetylene black and PVDF (6-8) and PVDF (3-1) in weight ratio of 1.
EXAMPLE 1 lithium ion Battery
Preparation of biomass porous carbon material-carbonized tangerine leaf
1) A potassium hydroxide solution having a concentration of 70mg/mL was prepared by dissolving 3.5g of potassium hydroxide in 50mL of distilled water at room temperature.
2) Cutting folium Citri Gangerinae into 0.2cm pieces2Adding 2g of orange leaf fragments and the potassium hydroxide solution with the concentration of 70mg/mL obtained in the step 1) into a reaction kettle for large and small fragments, and carrying out hydrothermal treatment at 130 ℃ for 8 h; and (3) drying the orange leaf fragments subjected to the hydrothermal treatment at 80 ℃ for 12h in vacuum.
3) Placing the dried orange leaf fragments obtained in the step 2) in a tube furnace, and calcining for 2h at 800 ℃ in an argon atmosphere; and (3) centrifuging and washing the obtained product to be neutral by using hydrochloric acid and distilled water in sequence, drying the product for 12 hours in vacuum at the temperature of 80 ℃, and grinding the product to obtain the target product carbonized tangerine leaves.
Fig. 1 is an SEM image of the carbonized cotyledon of the orange prepared in this example, and it can be seen from fig. 1 that the carbonized cotyledon material prepared has a spongy porous structure.
Fig. 2 is an XRD pattern of the carbonized tangerine leaves prepared in this example, and it can be seen from fig. 2 that there is a peak at 26 ° 2 θ, which is consistent with XRD pattern of graphite carbon material reported in literature.
FIG. 3 shows a Raman spectrum of the leaves of the carbonized tangerine prepared in this example. As can be seen in FIG. 3, the carbonized cotyledons were found to be 1350cm in length-1、1595cm-1There are D and G peaks, consistent with the Raman spectrum of the graphitic carbon material.
As can be seen from fig. 1, 2 and 3, the carbonized orange leaf material obtained in this embodiment has a graphene-like porous sponge-like material and a uniform pore structure.
Assembling of lithium ion battery
1) Common acetylene black bought from the market is taken as a conductive agent material, PVDF is taken as a binder, and carbonized tangerine leaves are taken as a negative electrode material, the materials are mixed and pasted according to the mass ratio of 6:3:1, the mixture is uniformly coated on copper foil to be taken as a negative electrode, and a lithium sheet is taken as a positive electrode to assemble the button cell-1.
2) Common acetylene black purchased from the market is taken as a conductive agent material, PVDF is taken as a binder, and carbonized tangerine leaves are taken as a negative electrode material, the materials are mixed and pasted according to the mass ratio of 7:2:1, the mixture is uniformly coated on copper foil to be taken as a negative electrode, and a (lithium sheet) is taken as a positive electrode to assemble the button cell-2.
3) Common acetylene black purchased from the market is taken as a conductive agent material, PVDF is taken as a binder, and carbonized tangerine leaves are taken as a negative electrode material, the materials are mixed and pasted according to the mass ratio of 8:1:1, the mixture is uniformly coated on copper foil to be taken as a negative electrode, and a (lithium sheet) is taken as a positive electrode to assemble the button cell-3.
Comparative example: common acetylene black purchased from the market is taken as a conductive agent material, PVDF is taken as a binder, graphite is taken as a negative electrode material, the materials are mixed and pasted according to the mass ratio of 8:1:1, the mixture is uniformly coated on copper foil to be taken as a negative electrode, and a (lithium sheet) is taken as a positive electrode to assemble the button cell-4.
And (3) electrochemical performance testing: electrochemical tests were carried out on button cells prepared with different amounts of negative electrode materials, and the results are shown in table 1.
TABLE 1 comparison of electrochemical Performance of batteries made with different negative electrode materials (Current Density 0.1A/g)
Figure BDA0002374974760000041
As can be seen from table 1, compared with a graphite negative electrode material, the electrochemical performance of the carbonized tangerine leaf negative electrode material synthesized by the method is obviously improved, along with the increase of the quality of the carbonized tangerine leaf, the electrochemical performance of the conductive agent material synthesized by the method is firstly weakened and then improved, and the electrochemical performance of the battery material prepared by using the carbonized tangerine leaf, acetylene black and PVDF in a mass ratio of 8:1:1 is obviously far higher than that of the material obtained under other conditions.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (9)

1. A novel lithium ion battery based on a biomass porous carbon material as a negative electrode material is characterized in that the biomass porous carbon material is used as the negative electrode material, a proper amount of conductive agent, binder and the biomass porous carbon material are uniformly mixed to form paste, the paste is uniformly coated on a copper foil to serve as a negative electrode, a lithium sheet serves as a positive electrode, and the lithium ion battery is assembled.
2. The novel lithium ion battery according to claim 1, wherein the lithium ion battery is a lithium ion button cell.
3. The novel lithium ion battery as claimed in claim 1 or 2, wherein the biomass porous carbon material is carbonized tangerine leaves, and the preparation method comprises the following steps: cutting folium Citri Gangerinae into 0.2cm pieces2Adding the large and small fragments into a reaction kettle, and carrying out hydrothermal treatment at 130 ℃ for 8 h; vacuum drying the orange leaf fragments subjected to the hydrothermal treatment at 80 ℃ for 12h, then placing the orange leaf fragments in a tube furnace, calcining the orange leaf fragments at 900 ℃ for 1-3h in an argon atmosphere, sequentially and centrifugally washing the obtained product with hydrochloric acid and distilled water to neutrality, vacuum drying at 80 ℃ for 12h, and grinding to obtain the target product carbonized orange leaves.
4. The novel lithium ion battery of claim 3, wherein the activator solution is a potassium hydroxide solution.
5. The novel lithium ion battery according to claim 3, wherein the weight ratio of the orange leaf fragments to the potassium hydroxide is 1: 1-3.
6. The novel lithium ion battery according to claim 1 or 2, characterized in that the conductive agent is acetylene black.
7. The novel lithium ion battery of claim 1 or 2, characterized in that the binder is PVDF.
8. The novel lithium ion battery according to claim 1 or 2, wherein the weight ratio of the biomass porous carbon material to the acetylene black to the PVDF is (6-8) to (3-1) to 1.
9. The novel lithium ion battery of claim 8, wherein the weight ratio of the biomass porous carbon material to the acetylene black to the PVDF is 6:3:1, 7:2:1, and 8:1: 1.
CN202010062600.6A 2020-01-20 2020-01-20 Novel lithium ion battery based on biomass porous carbon material as negative electrode material Pending CN111244452A (en)

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CN112736243A (en) * 2021-01-15 2021-04-30 辽宁大学 Preparation method and application of novel lithium ion battery negative electrode material carbonized grape skin

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