CN115295800A - Lithium battery negative electrode material and sintering preparation method thereof - Google Patents

Lithium battery negative electrode material and sintering preparation method thereof Download PDF

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CN115295800A
CN115295800A CN202211224001.5A CN202211224001A CN115295800A CN 115295800 A CN115295800 A CN 115295800A CN 202211224001 A CN202211224001 A CN 202211224001A CN 115295800 A CN115295800 A CN 115295800A
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parts
water
lithium
negative electrode
electrode
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车小林
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Qingdao Longdi Carbon Material Technology Co ltd
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Qingdao Longdi Carbon Material Technology Co ltd
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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
    • 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
    • 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
    • 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
    • H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/485—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
    • 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
    • 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
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • H01M4/624—Electric conductive fillers
    • H01M4/625—Carbon or graphite
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
    • H01M2004/027—Negative electrodes
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

Abstract

The invention relates to the technical field of lithium batteries, in particular to a lithium battery cathode material and a sintering preparation method thereof. The feed comprises the following raw materials in parts by weight: 39-57 parts of lithium carbonate, 25-36 parts of graphite, 27-35 parts of titanate, 9-14 parts of a conductive agent, 3-9 parts of an antioxidant and 5-11 parts of an adhesive; the adhesive comprises styrene butadiene rubber, natural rubber and sodium carboxymethyl cellulose. According to the invention, by adding the lithium titanate, the lattice constant and the volume change are very small when the crystal of the lithium titanate is inserted or removed with lithium ions, the structural damage caused by multiple charging and discharging can be avoided, the cycle performance and the service life of the electrode are improved, the antioxidant is coated on the surface of the electrode to form the antioxidant coating, the ineffective loss of the electrode caused by oxidation can be avoided, and by adding the adhesive, the strong adhesive force can be provided, so that the structural integrity of the electrode is maintained, and the reduction of the battery capacity is avoided.

Description

Lithium battery negative electrode material and sintering preparation method thereof
Technical Field
The invention relates to the technical field of lithium batteries, in particular to a lithium battery cathode material and a sintering preparation method thereof.
Background
Lithium metal batteries generally use manganese dioxide as a positive electrode material, metal lithium or an alloy metal thereof as a negative electrode material, and a nonaqueous electrolyte solution, compared with lead-acid batteries, lithium batteries have a longer service life, and have a larger battery capacity under the same volume, lead-acid batteries pollute the environment, and lithium batteries can be recycled and are more environment-friendly.
The performance of a negative electrode material of a lithium battery directly determines the charge-discharge efficiency, the cycle performance and the like of the lithium battery, and in order to improve the charge-discharge performance of the lithium battery, the negative electrode material of the lithium battery needs to be improved, and the negative electrode material is generally spheroidized and subjected to surface modification so as to facilitate the insertion and extraction of lithium ions in the negative electrode of the lithium battery.
Disclosure of Invention
The invention aims to provide a lithium battery negative electrode material and a sintering preparation method thereof, which aim to solve the problems in the background technology.
In order to achieve the above object, in one aspect, the present invention provides a negative electrode material for a lithium battery, including the following raw materials in parts by weight: 39-57 parts of lithium carbonate, 25-36 parts of graphite, 27-35 parts of titanate, 9-14 parts of a conductive agent, 3-9 parts of an antioxidant and 5-11 parts of an adhesive;
the adhesive comprises styrene butadiene rubber, natural rubber and sodium carboxymethyl cellulose.
As a further improvement of the technical scheme, the titanate is lithium titanate, and the conductive agent is carbon fiber.
As a further improvement of the technical scheme, the antioxidant comprises silicon dioxide, aluminum oxide, phosphorus pentoxide and boron trioxide.
On the other hand, the invention also provides a sintering preparation method of the lithium battery negative electrode material, which comprises the following steps:
s1, adding lithium carbonate into water, filling carbon dioxide gas into the water to form a suspension, and adding titanate and a conductive agent into the water to form a hydrolysate;
s2, mixing the suspension with the hydrolysate, adding graphite and an adhesive to form a mixed solution, heating the mixed solution to remove water to form a paste, and sintering and drying the paste to form an electrode blank;
s3, adding an antioxidant into water, uniformly stirring to form a protective solution, coating the protective solution on the surface of the electrode blank, drying, and forming a protective coating on the surface of the electrode blank;
and S4, after the electrode blank is rolled by a compression roller, removing redundant parts of the electrode blank by a die milling cutter to produce the lithium battery cathode material meeting the requirements.
As a further improvement of the technical scheme, in the S1, when lithium carbonate is put into water, the water temperature is 10-25 ℃.
As a further improvement of the technical scheme, in the step S2, the mixed solution is stirred for 18-32min at the rotating speed of 5-15rpm/min before being heated.
As a further improvement of the technical scheme, in the step S2, the step of sintering and drying the paste includes three stages, namely, a temperature rise stage, a temperature preservation stage and a temperature reduction stage, wherein the heating temperature in the temperature rise stage is 50-1050 ℃, the heating temperature in the temperature preservation stage is 1050-1350 ℃, and the temperature reduction stage reduces the temperature to the normal temperature.
In a further improvement of this embodiment, in S3, the viscosity of the protective solution at room temperature is 2 to 10mPa · S.
As a further improvement of the technical scheme, in the S3, the thickness of the protective coating is 8-22 μm.
As a further improvement of the technical scheme, when the S4 middle die milling cutter cuts off redundant blanks, water-soluble cutting fluid is poured on the cutter body.
According to the invention, lithium titanate with small crystal constant and volume change during lithium ion insertion and extraction is used as titanate, a firmer electrode structure is provided, titanate is added as a charge and discharge material, xLi + + xe- + 6C ⇔ LixC6 during charge and discharge is used for inserting lithium ions during charge and extracting lithium ions during discharge, adhesive force is provided by adding adhesive and using styrene butadiene rubber, natural rubber and sodium carboxymethyl cellulose in the adhesive to maintain the integrity of the electrode structure, the styrene butadiene rubber and the natural rubber have good compatibility due to the similarity of molecular structures of the styrene butadiene rubber and the natural rubber, the problem of low elasticity of rubber materials caused by the fact that a trans-structure is too much and the structure is not regular in the styrene butadiene rubber and a benzene ring structure is carried on a side group can be solved by mixing the natural rubber, invalid loss caused by electrode oxidation can be avoided by coating the coating formed by an antioxidant on the surface of the electrode, the service life of the electrode is ensured, in addition, silicon dioxide in the antioxidant reacts with the sodium carboxymethyl cellulose in the adhesive, the carboxymethyl cellulose can be connected with silicon through chemical bonds and the like, and the connecting force of the silicon particles can be kept stronger, the solid phase connection between the silicon particles can be prevented from being connected after a plurality of the electrolyte is formed, and the electrolyte film is reduced.
Compared with the prior art, the invention has the beneficial effects that:
according to the lithium battery cathode material and the sintering preparation method thereof, due to the addition of the lithium titanate, the lattice constant and the volume change of crystals are very small when the lithium ions are inserted or removed, the structural damage caused by repeated charging and discharging can be avoided, the cycle performance and the service life of an electrode are improved, the antioxidant is coated on the surface of the electrode to form the antioxidant coating, the ineffective loss of the electrode caused by oxidation can be avoided, and the adhesive is added to provide strong adhesive force so as to keep the integrity of the electrode structure and avoid the reduction of the battery capacity.
Drawings
FIG. 1 is a flow chart of the preparation of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In one aspect, an object of this embodiment is to provide a negative electrode material for a lithium battery, including the following raw materials in parts by weight: 39-57 parts of lithium carbonate, 25-36 parts of graphite, 27-35 parts of titanate, 9-14 parts of a conductive agent, 3-9 parts of an antioxidant and 5-11 parts of an adhesive;
the adhesive comprises styrene butadiene rubber, natural rubber and sodium carboxymethyl cellulose, the styrene butadiene rubber, the natural rubber and the sodium carboxymethyl cellulose are added as the adhesive, so that strong adhesive force can be provided, the styrene butadiene rubber and the natural rubber are dissolved together, the problem of low elasticity of the adhesive can be solved, and the electrode is adhered to keep the integrity of the electrode structure.
On the basis, in the embodiment of the invention, titanate is lithium titanate, the conductive agent is carbon fiber, and by adding lithium titanate, the crystal has small lattice constant and volume change when lithium ions are inserted or removed, so that in multiple charge-discharge cycles, the structural damage caused by the back-and-forth expansion of an electrode material can be avoided, the cycle performance and the service life of the electrode are improved, the specific capacity attenuation caused by the structural damage is reduced, and by adding carbon fiber, a good conductive network can be formed in the electrode due to the linear structure of the carbon fiber, the internal resistance of the battery can be reduced, and the performance of the battery can be improved.
Furthermore, the antioxidant comprises silicon dioxide, aluminum oxide, phosphorus pentoxide and boron trioxide, and the antioxidant is coated on the surface of the electrode, so that the micro-nano ceramic powder forms an antioxidant coating on the surface of the electrode, the ineffective loss of the electrode caused by oxidation can be avoided, and the service life of the electrode is prolonged.
According to the invention, lithium titanate with small crystal constant and volume change during lithium ion insertion and extraction is used as titanate, a firmer electrode structure is provided, titanate is added as a charge and discharge material, xLi + + xe- + 6C ⇔ LixC6 during charge and discharge is used for inserting lithium ions during charge and extracting lithium ions during discharge, adhesive force is provided by adding adhesive and using styrene butadiene rubber, natural rubber and sodium carboxymethyl cellulose in the adhesive to maintain the integrity of the electrode structure, the styrene butadiene rubber and the natural rubber have good compatibility due to the similarity of molecular structures of the styrene butadiene rubber and the natural rubber, the problem of low elasticity of rubber materials caused by the fact that a trans-structure is too much and the structure is not regular in the styrene butadiene rubber and a benzene ring structure is carried on a side group can be solved by mixing the natural rubber, invalid loss caused by electrode oxidation can be avoided by coating the coating formed by an antioxidant on the surface of the electrode, the service life of the electrode is ensured, in addition, silicon dioxide in the antioxidant reacts with the sodium carboxymethyl cellulose in the adhesive, the carboxymethyl cellulose can be connected with silicon through chemical bonds and the like, and the connecting force of the silicon particles can be kept stronger, the solid phase connection between the silicon particles can be prevented from being connected after a plurality of the electrolyte is formed, and the electrolyte film is reduced.
Referring to fig. 1, an embodiment of the present invention further provides a sintering preparation method of a negative electrode material of a lithium battery, which includes the following specific steps:
1. 39-57 parts of lithium carbonate is put into water with the water temperature of 10-25 ℃, then carbon dioxide gas is filled into the water to form suspension, 27-35 parts of titanate and 9-14 parts of conductive agent are added into the water to form hydrolysate, inorganic matters of the lithium carbonate are slightly soluble in the water, the higher the temperature is, the lower the solubility is, the lithium carbonate can be converted into bicarbonate by filling the carbon dioxide gas, and thus the lithium ions can be dissolved conveniently;
2. mixing the suspension with the hydrolysate, adding 25-36 parts of graphite and 5-11 parts of an adhesive to form a mixed solution, stirring the mixed solution at a rotating speed of 5-15rpm/min for 18-32min, heating the mixed solution to remove water to form a paste, and sintering and drying the paste to form an electrode blank in three stages, wherein the three stages are a heating stage, a heat preservation stage and a cooling stage, the heating temperature in the heating stage is 50-1050 ℃, the heating temperature in the heat preservation stage is 1050-1350 ℃, the temperature in the cooling stage is reduced to the normal temperature, the mixed solution is stirred to facilitate uniform distribution of components in the subsequently formed paste and ensure the quality of the prepared electrode material, the heating stage is mainly used for evaporation of water in the paste, and the heat preservation stage is used for keeping the distribution state of lithium ions at high temperature;
3. 3-9 parts of antioxidant is put into water at room temperature and stirred uniformly to form a protective solution with the viscosity of 2-10mPa & s, the protective solution is coated on the surface of an electrode blank and dried, a protective coating with the thickness of 8-22 mu m is formed on the surface of the electrode blank, the quality of the protective coating is determined by the viscosity, the performance of the electrode is further influenced, the oxidation resistance of the electrode is inconvenient when the thickness of the protective coating is thin, and the utilization effect of substances in a battery is influenced when the thickness of the protective coating is thick, namely the charging and discharging performance of the battery is influenced;
4. after the electrode blank is rolled by the compression roller, redundant parts of the electrode blank are removed by the die milling cutter, and when the die milling cutter cuts off redundant blanks, water-soluble cutting fluid is poured on the cutter body to generate a lithium battery negative electrode material meeting requirements, so that the milling cutter can be prevented from being worn and dust can be prevented from flying by pouring the water-soluble cutting fluid.
According to the amount of different raw materials and different process parameters in the lithium battery negative electrode material, the lithium battery negative electrode material provided by the present invention is further illustrated by the following specific examples.
Example 1
1. 39 parts of lithium carbonate is added into water with the water temperature of 10 ℃, then carbon dioxide gas is filled into the water to form suspension, 27 parts of titanate and 9 parts of conductive agent are added into the water to form hydrolysate, lithium carbonate inorganic matter is slightly dissolved in the water, the solubility is lower when the temperature is higher, and the lithium carbonate can be converted into bicarbonate by filling the carbon dioxide gas, so that the lithium ions can be dissolved conveniently;
2. mixing the suspension with the hydrolysate, adding 25 parts of graphite and 5 parts of an adhesive to form a mixed solution, stirring the mixed solution at a rotating speed of 5rpm/min for 18min, heating and dehydrating the mixed solution to form paste, and sintering and drying the paste in three stages to form an electrode blank, wherein the three stages comprise a heating stage, a heat preservation stage and a cooling stage, the heating temperature in the heating stage is 50 ℃, the heating temperature in the heat preservation stage is 1050 ℃, the temperature is reduced to normal temperature in the cooling stage, the mixed solution is stirred to facilitate uniform distribution of components in the paste formed subsequently, the quality of the prepared electrode material is ensured, the heating stage is mainly used for evaporation of water in the paste, and the heat preservation stage is used for keeping the distribution state of lithium ions at high temperature;
3. 3 parts of antioxidant is put into water at room temperature and stirred uniformly to form a protective solution with the viscosity of 2mPa & s, the protective solution is coated on the surface of an electrode blank and dried, a protective coating with the thickness of 8 mu m is formed on the surface of the electrode blank, the quality of the protective coating is determined by the viscosity, the performance of the electrode is further influenced, the electrode is inconvenient to resist oxidation when the thickness of the protective coating is thin, and the utilization effect of substances in a battery, namely the charging and discharging performance of the battery is influenced when the thickness of the protective coating is thick;
4. after the electrode blank is rolled by the compression roller, redundant parts of the electrode blank are removed by the die milling cutter, and when the die milling cutter cuts off redundant blanks, water-soluble cutting fluid is poured on the cutter body to generate a lithium battery negative electrode material meeting requirements, so that the milling cutter can be prevented from being worn and dust can be prevented from flying by pouring the water-soluble cutting fluid.
Example 2
1. Adding 44 parts of lithium carbonate into water with the water temperature of 15 ℃, then filling carbon dioxide gas into the water to form a suspension, adding 29 parts of titanate and 10 parts of conductive agent into the water to form a hydrolysate, wherein lithium carbonate inorganic matter is slightly dissolved in the water, and the higher the temperature is, the lower the solubility is, the lithium carbonate can be converted into bicarbonate by filling the carbon dioxide gas, so that the lithium ions can be dissolved conveniently;
2. mixing the suspension with the hydrolysate, adding 29 parts of graphite and 6 parts of an adhesive to form a mixed solution, stirring the mixed solution at a rotating speed of 7rpm/min for 21min, heating the mixed solution to remove water to form paste, and sintering and drying the paste in three stages to form an electrode blank, wherein the three stages comprise a heating stage, a heat preservation stage and a cooling stage, the heating temperature in the heating stage is 350 ℃, the heating temperature in the heat preservation stage is 1150 ℃, the temperature is reduced to normal temperature in the cooling stage, the mixed solution is stirred to facilitate uniform distribution of components in the paste formed subsequently, the quality of the prepared electrode material is ensured, the heating stage is mainly used for evaporation of water in the paste, and the heat preservation stage is used for keeping the distribution state of lithium ions at high temperature;
3. 4 parts of antioxidant is put into water at room temperature and stirred uniformly to form a protective solution with the viscosity of 3mPa & s, the protective solution is coated on the surface of an electrode blank and dried, a protective coating with the thickness of 11 mu m is formed on the surface of the electrode blank, the quality of the protective coating is determined by the viscosity, the performance of the electrode is further influenced, the electrode is inconvenient to resist oxidation when the thickness of the protective coating is thin, and the utilization effect of substances in a battery, namely the charging and discharging performance of the battery is influenced when the thickness of the protective coating is thick;
4. after the electrode blank is rolled by the compression roller, redundant parts of the electrode blank are removed by the die milling cutter, and when the die milling cutter cuts off redundant blanks, water-soluble cutting fluid is poured on the cutter body to generate a lithium battery negative electrode material meeting requirements, so that the milling cutter can be prevented from being worn and dust can be prevented from flying by pouring the water-soluble cutting fluid.
Example 3
1. Adding 51 parts of lithium carbonate into water with the water temperature of 15 ℃, then filling carbon dioxide gas into the water to form a suspension, adding 31 parts of titanate and 11 parts of conductive agent into the water to form a hydrolysate, wherein inorganic matters of the lithium carbonate are slightly soluble in the water, and the higher the temperature is, the lower the solubility is, the lithium carbonate can be converted into acid carbonate by filling the carbon dioxide gas, so that the lithium ions can be dissolved conveniently;
2. mixing the suspension with the hydrolysate, adding 31 parts of graphite and 8 parts of an adhesive to form a mixed solution, stirring the mixed solution at a rotating speed of 9rpm/min for 24min, heating the mixed solution to remove water to form a paste, and sintering and drying the paste to form an electrode blank in three stages, wherein the three stages are a heating stage, a heat preservation stage and a cooling stage, the heating temperature in the heating stage is 600 ℃, the heating temperature in the heat preservation stage is 1200 ℃, the temperature in the cooling stage is reduced to the normal temperature, the mixed solution is stirred to facilitate uniform distribution of components in the paste formed subsequently, the quality of the prepared electrode material is ensured, the mixed solution is mainly used for evaporation of water in the paste in the heating stage, and the distribution state of lithium ions is maintained at a high temperature in the heat preservation stage;
3. 6 parts of antioxidant is put into water at room temperature and stirred uniformly to form a protective solution with the viscosity of 5mPa & s, the protective solution is coated on the surface of an electrode blank and dried, a protective coating with the thickness of 14 mu m is formed on the surface of the electrode blank, the quality of the protective coating is determined by the viscosity, the performance of the electrode is further influenced, the electrode is inconvenient to resist oxidation when the thickness of the protective coating is thin, and the utilization effect of substances in a battery, namely the charging and discharging performance of the battery is influenced when the thickness of the protective coating is thick;
4. after the electrode blank is rolled by the compression roller, redundant parts of the electrode blank are removed by the die milling cutter, and when the die milling cutter cuts off redundant blanks, water-soluble cutting fluid is poured on the cutter body to generate a lithium battery negative electrode material meeting requirements, so that the milling cutter can be prevented from being worn and dust can be prevented from flying by pouring the water-soluble cutting fluid.
Example 4
1. 55 parts of lithium carbonate is put into water with the water temperature of 20 ℃, then carbon dioxide gas is filled into the water to form suspension, 33 parts of titanate and 13 parts of conductive agent are added into the water to form hydrolysate, inorganic matters of the lithium carbonate are slightly dissolved in the water, the higher the temperature is, the lower the solubility is, the lithium carbonate can be converted into acid carbonate by filling the carbon dioxide gas, and thus, the lithium ions can be dissolved conveniently;
2. mixing the suspension with the hydrolysate, adding 34 parts of graphite and 9 parts of an adhesive to form a mixed solution, stirring the mixed solution at a rotating speed of 12rpm/min for 29min, heating and dehydrating the mixed solution to form paste, and sintering and drying the paste in three stages to form an electrode blank, wherein the three stages comprise a heating stage, a heat preservation stage and a cooling stage, the heating temperature in the heating stage is 900 ℃, the heating temperature in the heat preservation stage is 1250 ℃, the temperature is reduced to normal temperature in the cooling stage, the mixed solution is stirred to facilitate uniform distribution of components in the paste formed subsequently, the quality of the prepared electrode material is ensured, the heating stage is mainly used for evaporation of water in the paste, and the heat preservation stage is used for keeping the distribution state of lithium ions at high temperature;
3. adding 8 parts of antioxidant into water at room temperature, stirring uniformly to form a protective solution with the viscosity of 9mPa & s, coating the protective solution on the surface of an electrode blank, drying, forming a protective coating with the thickness of 18 mu m on the surface of the electrode blank, wherein the viscosity determines the quality of the protective coating, so that the performance of the electrode is influenced, the oxidation resistance of the electrode is not facilitated when the thickness of the protective coating is thin, and the utilization effect of substances in a battery, namely the charging and discharging performance of the battery is influenced when the thickness of the protective coating is thick;
4. after the electrode blank is rolled by the compression roller, redundant parts of the electrode blank are removed by the die milling cutter, and when the die milling cutter cuts off redundant blanks, water-soluble cutting fluid is poured on the cutter body to generate a lithium battery negative electrode material meeting requirements, so that the milling cutter can be prevented from being worn and dust can be prevented from flying by pouring the water-soluble cutting fluid.
Example 5
1. Adding 57 parts of lithium carbonate into water with the water temperature of 25 ℃, then filling carbon dioxide gas into the water to form a suspension, adding 35 parts of titanate and 14 parts of conductive agent into the water to form a hydrolysate, wherein inorganic matters of the lithium carbonate are slightly soluble in the water, and the higher the temperature is, the lower the solubility is, the lithium carbonate can be converted into acid carbonate by filling the carbon dioxide gas, so that the lithium ions can be dissolved conveniently;
2. mixing the suspension with the hydrolysate, adding 36 parts of graphite and 11 parts of an adhesive to form a mixed solution, stirring the mixed solution at a rotating speed of 15rpm/min for 32min, heating the mixed solution to remove water to form paste, and sintering and drying the paste to form an electrode blank in three stages, wherein the three stages are a heating stage, a heat preservation stage and a cooling stage, the heating temperature in the heating stage is 1050 ℃, the heating temperature in the heat preservation stage is 1350 ℃, the temperature in the cooling stage is reduced to the normal temperature, the mixed solution is stirred to facilitate uniform distribution of components in the paste formed subsequently, the quality of the prepared electrode material is ensured, the mixed solution is mainly used for evaporation of water in the paste in the heating stage, and the distribution state of lithium ions is maintained at a high temperature in the heat preservation stage;
3. 9 parts of antioxidant is put into water at room temperature and stirred uniformly to form a protective solution with the viscosity of 10mPa & s, the protective solution is coated on the surface of an electrode blank and dried, a protective coating with the thickness of 22 mu m is formed on the surface of the electrode blank, the quality of the protective coating is determined by the viscosity, the performance of the electrode is further influenced, the electrode is inconvenient to resist oxidation when the thickness of the protective coating is thin, and the utilization effect of substances in a battery, namely the charging and discharging performance of the battery is influenced when the thickness of the protective coating is thick;
4. after the electrode blank is rolled by the compression roller, redundant parts of the electrode blank are removed by the die milling cutter, and when the die milling cutter cuts off redundant blanks, water-soluble cutting fluid is poured on the cutter body to generate a lithium battery negative electrode material meeting requirements, so that the milling cutter can be prevented from being worn and dust can be prevented from flying by pouring the water-soluble cutting fluid.
Example 6
1. Adding 45 parts of lithium carbonate into water with the water temperature of 15 ℃, then filling carbon dioxide gas into the water to form a suspension, adding 30 parts of titanate and 9 parts of conductive agent into the water to form a hydrolysate, wherein lithium carbonate inorganic matter is slightly dissolved in the water, and the higher the temperature is, the lower the solubility is, the lithium carbonate can be converted into bicarbonate by filling the carbon dioxide gas, so that the lithium ions can be dissolved conveniently;
2. mixing the suspension with the hydrolysate, adding 33 parts of graphite and 8 parts of adhesive to form a mixed solution, stirring the mixed solution at the rotating speed of 10rpm/min for 25min, heating the mixed solution to remove water to form paste, and sintering and drying the paste to form an electrode blank in three stages, wherein the three stages are a heating stage, a heat preservation stage and a cooling stage, the heating temperature in the heating stage is 800 ℃, the heating temperature in the heat preservation stage is 1250 ℃, the temperature in the cooling stage is reduced to normal temperature, the mixed solution is stirred to facilitate uniform distribution of components in the paste formed subsequently, the quality of the prepared electrode material is ensured, the heating stage is mainly used for evaporation of water in the paste, and the heat preservation stage is used for keeping the distribution state of lithium ions at high temperature;
3. adding 7 parts of antioxidant into water at room temperature, stirring uniformly to form a protective solution with viscosity of 8mPa & s, coating the protective solution on the surface of an electrode blank, drying, forming a protective coating with the thickness of 20 mu m on the surface of the electrode blank, wherein the viscosity determines the quality of the protective coating, and further influences the performance of the electrode, when the thickness of the protective coating is thinner, the oxidation resistance of the electrode is inconvenient, and when the thickness of the protective coating is thicker, the utilization effect of substances in the battery is influenced, namely the charging and discharging performance of the battery is influenced;
4. after the electrode blank is rolled by the compression roller, redundant parts of the electrode blank are removed by the die milling cutter, and when the die milling cutter cuts off redundant blanks, water-soluble cutting fluid is poured on the cutter body to generate a lithium battery negative electrode material meeting requirements, so that the milling cutter can be prevented from being worn and dust can be prevented from flying by pouring the water-soluble cutting fluid.
Example 7
1. Adding 42 parts of lithium carbonate into water with the water temperature of 15 ℃, then filling carbon dioxide gas into the water to form a suspension, adding 35 parts of titanate and 12 parts of conductive agent into the water to form a hydrolysate, wherein inorganic matters of the lithium carbonate are slightly dissolved in the water, and the higher the temperature is, the lower the solubility is, the lithium carbonate can be converted into bicarbonate by filling the carbon dioxide gas, so that the lithium ions can be dissolved conveniently;
2. mixing the suspension with the hydrolysate, adding 26 parts of graphite and 7 parts of an adhesive to form a mixed solution, stirring the mixed solution at the rotating speed of 8rpm/min for 22min, heating the mixed solution to remove water to form paste, and sintering and drying the paste to form an electrode blank in three stages, wherein the three stages are a heating stage, a heat preservation stage and a cooling stage, the heating temperature in the heating stage is 450 ℃, the heating temperature in the heat preservation stage is 1200 ℃, the temperature in the cooling stage is reduced to the normal temperature, the mixed solution is stirred to facilitate uniform distribution of components in the paste formed subsequently, the quality of the prepared electrode material is ensured, the mixed solution is mainly used for evaporation of water in the paste in the heating stage, and the distribution state of lithium ions is maintained at high temperature in the heat preservation stage;
3. 5 parts of antioxidant is put into water at room temperature and stirred uniformly to form a protective solution with the viscosity of 5mPa & s, the protective solution is coated on the surface of an electrode blank and dried, a protective coating with the thickness of 8 mu m is formed on the surface of the electrode blank, the quality of the protective coating is determined by the viscosity, the performance of the electrode is further influenced, the electrode is inconvenient to resist oxidation when the thickness of the protective coating is thin, and the utilization effect of substances in a battery, namely the charging and discharging performance of the battery is influenced when the thickness of the protective coating is thick;
4. after the electrode blank is rolled by the compression roller, redundant parts of the electrode blank are removed by the die milling cutter, and when the die milling cutter cuts off redundant blanks, water-soluble cutting fluid is poured on the cutter body to generate a lithium battery negative electrode material meeting requirements, so that the milling cutter can be prevented from being worn and dust can be prevented from flying by pouring the water-soluble cutting fluid.
Example 8
1. 50 parts of lithium carbonate is put into water with the water temperature of 10 ℃, then carbon dioxide gas is filled into the water to form suspension, 35 parts of titanate and 10 parts of conductive agent are added into the water to form hydrolysis liquid, inorganic matters of the lithium carbonate are slightly soluble in the water, the higher the temperature is, the lower the solubility is, the lithium carbonate can be converted into acid carbonate by filling the carbon dioxide gas, and thus, the lithium ions can be dissolved conveniently;
2. mixing the suspension with the hydrolysate, adding 25 parts of graphite and 5 parts of an adhesive to form a mixed solution, stirring the mixed solution at the rotating speed of 10rpm/min for 25min, heating the mixed solution to remove water to form paste, and sintering and drying the paste to form an electrode blank in three stages, wherein the three stages are a heating stage, a heat preservation stage and a cooling stage, the heating temperature in the heating stage is 1050 ℃, the heating temperature in the heat preservation stage is 1150 ℃, the temperature in the cooling stage is reduced to normal temperature, the mixed solution is stirred to facilitate uniform distribution of components in the paste formed subsequently, the quality of the prepared electrode material is ensured, the mixed solution is mainly used for evaporation of water in the paste in the heating stage, and the distribution state of lithium ions is maintained at high temperature in the heat preservation stage;
3. 5 parts of antioxidant is put into water at room temperature and stirred uniformly to form a protective solution with the viscosity of 10mPa & s, the protective solution is coated on the surface of an electrode blank and dried, a protective coating with the thickness of 15 mu m is formed on the surface of the electrode blank, the quality of the protective coating is determined by the viscosity, the performance of the electrode is further influenced, the electrode is inconvenient to resist oxidation when the thickness of the protective coating is thin, and the utilization effect of substances in a battery, namely the charging and discharging performance of the battery is influenced when the thickness of the protective coating is thick;
4. after the electrode blank is rolled by the compression roller, redundant parts of the electrode blank are removed by the die milling cutter, and when the die milling cutter cuts off redundant blanks, water-soluble cutting fluid is poured on the cutter body to generate a lithium battery negative electrode material meeting requirements, so that the milling cutter can be prevented from being worn and dust can be prevented from flying by pouring the water-soluble cutting fluid.
TABLE 1 comparison of the amounts of the raw materials used in examples 1-8
Figure 469224DEST_PATH_IMAGE001
Table 2 comparison of process parameters in examples 1-8
Figure 682031DEST_PATH_IMAGE002
Comparative example 1
The comparative example, using the process of example 1, only lacks the binder and the remainder is unchanged, the specific steps are as follows:
1. 39 parts of lithium carbonate is added into water with the water temperature of 10 ℃, then carbon dioxide gas is filled into the water to form suspension, 27 parts of titanate and 9 parts of conductive agent are added into the water to form hydrolysate, lithium carbonate inorganic matter is slightly dissolved in the water, the solubility is lower when the temperature is higher, and the lithium carbonate can be converted into bicarbonate by filling the carbon dioxide gas, so that the lithium ions can be dissolved conveniently;
2. mixing the suspension with the hydrolysate and adding 25 parts of graphite to form a mixed solution, stirring the mixed solution at a rotating speed of 5rpm/min for 18min, heating the mixed solution to remove water to form a paste, and sintering and drying the paste to form an electrode blank in three stages, wherein the three stages are a heating stage, a heat preservation stage and a cooling stage, the heating temperature in the heating stage is 50 ℃, the heating temperature in the heat preservation stage is 1050 ℃, the temperature in the cooling stage is reduced to normal temperature, the mixed solution is stirred to facilitate uniform distribution of components in the paste formed subsequently and ensure the quality of the prepared electrode material, the heating stage is mainly used for evaporation of water in the paste, and the heat preservation stage is used for keeping the distribution state of lithium ions at high temperature;
3. 3 parts of antioxidant is put into water at room temperature and stirred uniformly to form a protective solution with the viscosity of 2mPa & s, the protective solution is coated on the surface of an electrode blank and dried, a protective coating with the thickness of 8 mu m is formed on the surface of the electrode blank, the quality of the protective coating is determined by the viscosity, the performance of the electrode is further influenced, the electrode is inconvenient to resist oxidation when the thickness of the protective coating is thin, and the utilization effect of substances in a battery, namely the charging and discharging performance of the battery is influenced when the thickness of the protective coating is thick;
4. after the electrode blank is rolled by a compression roller, redundant parts of the electrode blank are removed by a die milling cutter, and when the die milling cutter cuts off redundant blanks, water-soluble cutting fluid is poured on the cutter body to generate a lithium battery cathode material meeting the requirements, so that the milling cutter can be prevented from being worn and dust can be prevented from flying.
Comparative example 2
The process of example 2 is adopted in the comparative example, only the adhesive is lacked, the rest is unchanged, the specific steps are similar to those of comparative example 1, and the detailed description of the comparative example is omitted.
Comparative example 3
The process of example 3 is adopted in the comparative example, only the adhesive is lacked, the rest is unchanged, the specific steps are similar to those of comparative example 1, and the detailed description of the comparative example is omitted.
Comparative example 4
The process of example 4 is adopted in the comparative example, only the adhesive is lacked, the rest is unchanged, the specific steps are similar to those of comparative example 1, and the description of the comparative example is omitted.
Comparative example 5
The process of example 5 is adopted in the comparative example, only the adhesive is lacked, the rest is unchanged, the specific steps are similar to those of comparative example 1, and the detailed description of the comparative example is omitted.
TABLE 3 comparison of the amounts of starting materials in comparative examples 1 to 5
Figure 528764DEST_PATH_IMAGE003
TABLE 4 comparison of Process parameters in comparative examples 1-5
Figure 831307DEST_PATH_IMAGE004
Comparative example 6
In the comparative example, on the basis of the comparative example 1, the antioxidant is lacked, the rest is unchanged, the specific steps are similar to those of the example 1, and the details of the comparative example are not repeated.
Comparative example 7
In the comparative example, on the basis of the comparative example 2, the conductive agent is lacked, the rest is unchanged, the specific steps are similar to those in the example 2, and the detailed description of the comparative example is omitted.
Comparative example 8
In the comparative example, on the basis of the comparative example 3, the water temperature is changed to 30 ℃, the rest is not changed, the specific steps are similar to those in the example 3, and the comparative example is not repeated.
Comparative example 9
In the comparative example, on the basis of the comparative example 4, the stirring speed is changed to 25rpm/min, the rest is not changed, the specific steps are similar to those in the example 4, and the details of the comparative example are not repeated.
Comparative example 10
In the comparative example, on the basis of the comparative example 5, the stirring time is changed to 15min, the rest is not changed, the specific steps are similar to those in the example 5, and the details of the comparative example are not repeated.
Comparative example 11
In the comparative example, on the basis of the comparative example 1, the temperature rise temperature is changed to 1100 ℃, and the rest is not changed, the specific steps are similar to those in the example 1, and the detailed description of the comparative example is omitted.
Comparative example 12
In the comparative example, on the basis of the comparative example 2, the heat preservation temperature is changed to 900 ℃, the rest is not changed, the specific steps are similar to those in the example 2, and the detailed description of the comparative example is omitted.
Comparative example 13
In the comparative example, on the basis of the comparative example 3, the viscosity is changed to 15 mPas, the rest is not changed, the specific steps are similar to those in the example 3, and the details of the comparative example are not repeated.
Comparative example 14
In the comparative example, on the basis of the comparative example 4, the thickness is changed to 30 μm, the rest is not changed, the specific steps are similar to those in the example 4, and the details of the comparative example are not repeated.
Comparative example 15
In the comparative example, on the basis of the comparative example 5, the thickness is changed to 5 μm, the rest is not changed, the specific steps are similar to those in the example 5, and the detailed description of the comparative example is omitted.
TABLE 5 comparison of the amounts of the raw materials in comparative examples 6 to 15
Figure 763491DEST_PATH_IMAGE005
TABLE 6 comparison of Process parameters in comparative examples 6-15
Figure 45568DEST_PATH_IMAGE006
Test example 1
The lithium battery negative electrode materials prepared in examples 1 to 8 and the lithium battery negative electrode materials prepared in comparative examples 1 to 15 were subjected to charge-discharge tests, the average value of the electric quantity of the charge-discharge for a plurality of times was divided by the weight of the electrode itself to obtain a specific discharge capacity, the percentage of the battery capacity after 30 charge-discharge cycles to the battery capacity of the primary battery was detected, and the specific discharge capacity and the battery capacity ratio data were filled in table 7
TABLE 7 comparison of battery performance of negative electrode materials for lithium batteries prepared in examples and comparative examples
Figure 746808DEST_PATH_IMAGE007
As shown in table 7, compared with the negative electrode materials of the lithium batteries prepared in comparative examples 1 to 15, the negative electrode materials of the lithium batteries prepared in examples 1 to 8 have better discharge specific capacity and battery capacity ratio than those of the negative electrode materials of the lithium batteries prepared in comparative examples 1 to 15, the negative electrode materials of the lithium batteries in examples 1 to 8 have discharge specific capacity higher than 1879mAh/g and battery capacity ratio higher than 98.1, and when the compositions are reduced differently and the process conditions are changed in comparative examples 1 to 15, the discharge specific capacity and the battery capacity ratio of the negative electrode materials of the lithium batteries are reduced to different extents, so that it can be shown that the negative electrode materials of the lithium batteries prepared in the invention have good charge and discharge performance.
The foregoing shows and describes the general principles, principal features, and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, and the preferred embodiments of the present invention are described in the above embodiments and the description, and are not intended to limit the present invention. The scope of the invention is defined by the appended claims and equivalents thereof.

Claims (10)

1. The lithium battery negative electrode material is characterized by comprising the following raw materials in parts by weight: 39-57 parts of lithium carbonate, 25-36 parts of graphite, 27-35 parts of titanate, 9-14 parts of a conductive agent, 3-9 parts of an antioxidant and 5-11 parts of an adhesive;
the adhesive comprises styrene butadiene rubber, natural rubber and sodium carboxymethyl cellulose.
2. The negative electrode material for a lithium battery as claimed in claim 1, wherein: the titanate is lithium titanate, and the conductive agent is carbon fiber.
3. The negative electrode material for a lithium battery as claimed in claim 1, wherein: the antioxidant comprises silicon dioxide, aluminum oxide, phosphorus pentoxide and boron trioxide.
4. A method for preparing a negative electrode material for a lithium battery according to any of claims 1 to 3 by sintering, comprising the steps of:
s1, adding lithium carbonate into water, filling carbon dioxide gas into the water to form a suspension, and adding titanate and a conductive agent into the water to form a hydrolysate;
s2, mixing the suspension with the hydrolysate, adding graphite and an adhesive to form a mixed solution, heating the mixed solution to remove water to form a paste, and sintering and drying the paste to form an electrode blank;
s3, adding an antioxidant into water, uniformly stirring to form a protective solution, coating the protective solution on the surface of the electrode blank, drying, and forming a protective coating on the surface of the electrode blank;
and S4, after the electrode blank is rolled by a compression roller, removing the redundant part of the electrode blank by a die milling cutter to generate the lithium battery cathode material meeting the requirements.
5. The sintering preparation method of the negative electrode material for a lithium battery as claimed in claim 4, wherein: in the S1, when lithium carbonate is put into water, the water temperature is 10-25 ℃.
6. The sintering preparation method of the negative electrode material for lithium batteries according to claim 4, characterized in that: in the S2, the mixed solution is stirred for 18-32min at the rotating speed of 5-15rpm/min before being heated.
7. The sintering production method of the negative electrode material for a lithium battery as claimed in claim 6, characterized in that: in the S2, the sintering and drying of the paste comprise three stages, namely a heating stage, a heat preservation stage and a cooling stage, wherein the heating temperature in the heating stage is 50-1050 ℃, the heating temperature in the heat preservation stage is 1050-1350 ℃, and the temperature in the cooling stage is reduced to the normal temperature.
8. The sintering preparation method of the negative electrode material for lithium batteries according to claim 4, characterized in that: in S3, the viscosity of the protective solution at room temperature is 2-10mPa · S.
9. The sintering preparation method of the negative electrode material for lithium batteries according to claim 4, characterized in that: in S3, the thickness of the protective coating is 8-22 μm.
10. The sintering preparation method of the negative electrode material for a lithium battery as claimed in claim 4, wherein: and in the S4, when the die milling cutter cuts off redundant blanks, water-soluble cutting fluid is poured into the cutter body.
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