CN113942992A - Preparation method of amorphous carbon - Google Patents
Preparation method of amorphous carbon Download PDFInfo
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- CN113942992A CN113942992A CN202111152691.3A CN202111152691A CN113942992A CN 113942992 A CN113942992 A CN 113942992A CN 202111152691 A CN202111152691 A CN 202111152691A CN 113942992 A CN113942992 A CN 113942992A
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- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/05—Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30
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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
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- 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
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- 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 preparation of battery negative electrode materials, and discloses a preparation method of an amorphous carbon negative electrode material, wherein emulsion polymerization is adopted to coat a polymer on the surface of a hard carbon precursor, and a spherical hard carbon material is obtained through high-temperature sintering.
Description
Technical Field
The invention relates to the technical field of preparation of battery negative electrode materials, in particular to a preparation method of an amorphous carbon negative electrode material.
Background
The negative electrode refers to the end of the power supply where the potential (potential) is lower. In a galvanic cell, the electrode is the electrode that functions as an oxidation electrode, and physically, the electrode is the one from which electrons flow out of the circuit.
The cathode material refers to a raw material for forming a cathode in a battery, and currently, common cathode materials include a carbon cathode material, a tin-based cathode material, a lithium-containing transition metal nitride cathode material, an alloy cathode material and a nano cathode material.
The negative electrode of the lithium ion battery is formed by uniformly coating a paste adhesive prepared by mixing a negative electrode active material carbon material or a non-carbon material, a binder and an additive on two sides of a copper foil, drying and rolling, and the key point is whether the negative electrode material capable of reversibly releasing/embedding lithium ions can be prepared.
In general, the selection of a good anode material should follow the following principle: high specific energy, low electrode potential relative to lithium electrode, good reversibility of charge-discharge reaction, good compatibility with electrolyte and binder, and small specific surface area (<10m2(g) high true density>2.0g/cm3) Good size and mechanical stability in the process of lithium intercalation, rich resources, low price, stability in air and no toxic or side effect. At present, the negative electrode material that has been practically used in lithium ion batteries is generally a carbon material such as graphite, soft carbon (e.g., coke, etc.), hard carbon, and the like.
The carbon cathode material is widely applied to commercial lithium ion batteries, and the carbon material has the advantages of high specific capacity, low cost, long cycle life and the like. Carbon negative electrode materials which can be used for lithium ion batteries mainly comprise graphite and amorphous carbon, and artificially manufactured carbon materials have disordered structures with different degrees, wherein amorphous carbon materials prepared by low-temperature carbonization have low crystallinity and are generally divided into two types: soft carbon (graphitizable carbon) and hard carbon (non-graphitizable carbon).
Wherein, the crystallinity of the soft carbon is low, the grain size is small, and the compatibility with the electrolyte is good; the hard carbon has higher reversible specific capacity and good rapid charge and discharge performance. Compared with the traditional graphite negative electrode material, the amorphous carbon material has higher specific capacity and better quick charging performance, and is concerned by research workers as a novel material with the potential of replacing a graphite material in recent years.
Disclosure of Invention
The invention aims to provide a preparation method of an amorphous carbon negative electrode material with a core-shell structure, which comprises the steps of firstly preparing a soft carbon precursor with a polymer coated on the surface through emulsion polymerization, then obtaining the soft carbon precursor with the core-shell structure through stabilization, and finally obtaining the amorphous carbon negative electrode material with the core-shell structure through high-temperature carbonization.
The invention provides a preparation method of an amorphous carbon negative electrode material, which comprises the following steps:
step 1, weighing a predetermined amount of petroleum coke as a precursor A, adding the precursor A, a set amount of distilled water, a polymer monomer and Sodium Dodecyl Sulfate (SDS) as an emulsifier into a reaction kettle to form a mixed system, vacuumizing the reaction kettle, introducing nitrogen into the reaction kettle, stirring the mixed system, heating the mixed system to 60-70 ℃ after the mixed system is stirred for 30-120 minutes, adding an ammonium persulfate aqueous solution as an initiator at the temperature of 0.5g/min for reaction for 3-5 hours, continuing stirring and cooling the reacted mixed system after the reaction is finished, cooling to below 50 ℃, adding methanol for demulsification, and filtering to obtain a polymer/petroleum coke composite precursor B;
step 2, performing low-temperature pre-carbonization treatment on the precursor B obtained in the step 1 for 5-10 hours in a nitrogen environment to obtain a precursor C, wherein the roasting temperature of the low-temperature pre-carbonization treatment is not higher than 800 ℃;
and 3, carbonizing the precursor C obtained in the step 2 at a high temperature in a nitrogen environment to obtain the amorphous carbon anode material with the core-shell structure, wherein the roasting temperature of the high-temperature carbonization is not lower than 1000 ℃.
Preferably, the specific surface area of the petroleum coke is 2-10 m2/g。
Preferably, in the step 1, the amount of the precursor A is 200-1000 g per 1L of distilled water.
In the step 1, the polymer monomer (monomer) is a general name of a small molecule capable of polymerizing with the same kind or other molecules, is a simple compound capable of performing polymerization reaction or polycondensation reaction to form a high molecular compound, and is a low molecular raw material for synthesizing a polymer.
In the step 1, the input mass ratio of the precursor A to the polymer monomer is 100 (10-30).
In the step 1, the amount of Sodium Dodecyl Sulfate (SDS) added is 2 to 4g per 1L of distilled water.
In the step 1, the adding amount of the ammonium persulfate aqueous solution (10% concentration) is that 0.2-2 g of the ammonium persulfate aqueous solution is put into every 1L of distilled water.
In the step 2, the roasting temperature of the low-temperature pre-carbonization treatment is 400-800 ℃.
In the step 3, the roasting temperature of the high-temperature carbonization treatment is 1000-1400 ℃.
Compared with the prior art, the technical scheme of the invention at least has the following advantages:
1. the invention coats the poly-p-soft carbon precursor by emulsion, and finally, the product obtained by sintering is a mixture of soft carbon and hard carbon, and has the advantages of both the soft carbon and the hard carbon.
2. The emulsion polymerization process of the invention can prevent the agglomeration of the soft carbon precursor while coating the polymer, and the obtained product has uniform size and good processing performance.
3. The amorphous carbon anode material prepared by the invention has higher charge and discharge capacity.
Drawings
The foregoing and following detailed description of the invention will be apparent when read in conjunction with the following drawings, in which:
fig. 1 is a graph showing the first charge and discharge curves of an amorphous carbon anode material in example 4.
Detailed Description
The technical solutions for achieving the objects of the present invention are further illustrated by the following specific examples, and it should be noted that the technical solutions claimed in the present invention include, but are not limited to, the following examples.
Example 1
The embodiment provides a preparation method of an amorphous carbon anode material, which comprises the following steps:
step 1, weighing 200g of specific surface area of 3m2The precursor A is petroleum coke/g.
And 2, adding a precursor A and 1L of distilled water into a reaction kettle, adding 60g of monomer Methyl Methacrylate (MMA) and 2g of Sodium Dodecyl Sulfate (SDS) serving as an emulsifier to form a mixed system, vacuumizing the reaction kettle, introducing nitrogen and stirring, heating to 60 ℃ after the mixed system is stirred for 30 minutes, adding 2g of ammonium persulfate aqueous solution (10% concentration) serving as an initiator at the temperature at the rate of 0.5g/min, stopping heating after the reaction is carried out for 3 hours, continuing stirring after the reaction is finished, cooling, adding methanol to carry out demulsification, precipitating with a large amount of methanol, and filtering to obtain the PMMA (polymer)/petroleum coke composite precursor B. In the step, the less the precursor A is added, the more the polymer monomer amount is, and the more the coating amount is; the addition amount of the emulsifier is based on the full emulsification of the system; the more the initiator is added, the lower the molecular weight of the polymer is; the amount of methanol used was such that sufficient precipitation of the precursor was achieved.
And 3, roasting the precursor B obtained in the step 2 at 500 ℃ for 7 hours in a nitrogen environment to obtain a precursor C.
And 4, carbonizing the precursor C in the step 3 at 1000 ℃ in a nitrogen environment to obtain the amorphous carbon anode material with the core-shell structure.
Example 2
A preparation method of an amorphous carbon negative electrode material comprises the following steps:
step 1, weighing 400g of specific surface area of 5m2Adding the petroleum coke in an amount of/g as a precursor A into a reaction kettle.
And 2, adding 1L of distilled water into a reaction kettle, adding 60g of monomer Methyl Methacrylate (MMA) and 2.5g of Sodium Dodecyl Sulfate (SDS) serving as an emulsifier to form a mixed system, vacuumizing the reaction kettle, introducing nitrogen and stirring, heating to 60 ℃ after the mixed system is stirred for 90 minutes, adding 5g of ammonium persulfate aqueous solution (10% concentration) serving as an initiator at the temperature at the rate of 0.5g/min, stopping heating after the reaction is carried out for 3 hours, continuing stirring after the reaction is finished, cooling, adding methanol to carry out demulsification, precipitating with a large amount of methanol, and filtering to obtain the PMMA/petroleum coke composite precursor B. In the step, the less the precursor A is added, the more the polymer monomer amount is, and the more the coating amount is; the addition amount of the emulsifier is based on the full emulsification of the system; the more the initiator is added, the lower the molecular weight of the polymer is; the amount of methanol used was such that sufficient precipitation of the precursor was achieved.
And 3, roasting the precursor B obtained in the step 2 at 550 ℃ for 7 hours in a nitrogen environment to obtain a precursor C.
And 4, carbonizing the precursor C obtained in the step 3 at 1150 ℃ in a nitrogen environment to obtain the amorphous carbon anode material with the core-shell structure.
Example 3
A preparation method of an amorphous carbon negative electrode material comprises the following steps:
step 1, weighing 700g of specific surface area of 7m2The precursor A is petroleum coke/g.
And 2, adding the precursor A and 1L of distilled water into a reaction kettle, adding 70g of monomer Methyl Methacrylate (MMA) and 3g of Sodium Dodecyl Sulfate (SDS) serving as an emulsifier to form a mixed system, vacuumizing the reaction kettle, introducing nitrogen and stirring, heating to 70 ℃ after the mixed system is stirred for 30 minutes, adding 4g of ammonium persulfate aqueous solution (10% concentration) serving as an initiator at the temperature at the rate of 0.5g/min, stopping heating after the reaction is carried out for 4 hours, continuing stirring after the reaction is finished, cooling, adding methanol to carry out demulsification, precipitating with a large amount of methanol, and filtering to obtain the PMMA/petroleum coke composite precursor B. In the step, the less the precursor A is added, the more the polymer monomer amount is, and the more the coating amount is; the addition amount of the emulsifier is based on the full emulsification of the system; the more the initiator is added, the lower the molecular weight of the polymer is; the amount of methanol used was such that sufficient precipitation of the precursor was achieved.
And 3, roasting the precursor B obtained in the step 2 at 800 ℃ for 8 hours in a nitrogen environment to obtain a precursor C.
And 4, carbonizing the precursor C obtained in the step 3 at 1350 ℃ in a nitrogen environment to obtain the amorphous carbon anode material with the core-shell structure.
Example 4
A preparation method of an amorphous carbon negative electrode material comprises the following steps:
step 1, weighing 700g of specific surface area of 7m2The precursor A is petroleum coke/g.
And 2, adding a precursor A and 1L of distilled water into a reaction kettle, adding 140g of monomer Methyl Methacrylate (MMA) and 3g of Sodium Dodecyl Sulfate (SDS) serving as an emulsifier to form a mixed system, vacuumizing the reaction kettle, introducing nitrogen and stirring, heating to 70 ℃ after the mixed system is fully emulsified, adding 4g of ammonium persulfate aqueous solution (10% concentration) serving as an initiator at the temperature at the rate of 0.5g/min, stopping heating after reacting for 4 hours, continuing stirring after the reaction is finished, cooling, adding methanol to perform demulsification, precipitating with a large amount of methanol, and filtering to obtain the PMMA/petroleum coke composite precursor B. In the step, the less the precursor A is added, the more the polymer monomer amount is, and the more the coating amount is; the addition amount of the emulsifier is based on the full emulsification of the system; the more the initiator is added, the lower the molecular weight of the polymer is; the amount of methanol used was such that sufficient precipitation of the precursor was achieved.
And 3, roasting the precursor B obtained in the step 2 at the temperature of 750 ℃ for 8 hours in a nitrogen environment to obtain a precursor C.
And 4, carbonizing the precursor C obtained in the step 3 at 1250 ℃ in a nitrogen environment to obtain the amorphous carbon anode material with the core-shell structure.
And (3) mixing the amorphous carbon negative material obtained in the step (4) with conductive agent carbon black and adhesive polyvinylidene fluoride (PVDF) according to the mass ratio of 8:1:1, adding N-methyl pyrrolidone (NMP) to prepare slurry, uniformly coating the slurry on copper foil, drying the slurry in vacuum at 100 ℃ for 12 hours, and uniformly pressing the pole piece by using a tablet press to obtain the pole piece to be tested.
The lithium sheet is taken as a counter electrode, and the electrolyte is LiPF6Ethyl Carbonate (EC) and dimethyl carbonate (DMC) in a concentration of 1mol/L were reacted in a ratio of 1:1, a cell separator of the type celgard2325 was used, and the negative electrode materials of the above examples 1 to 4 were used in a glove box under an argon atmosphere to assemble a CR2032 type coin cell.
Through tests, the assembled battery is subjected to constant current charge and discharge tests in a voltage range of 0-2.5V, the first lithium intercalation specific capacity can reach 546.5mAh/g and the first lithium deintercalation specific capacity can reach 447.0mAh/g under the multiplying power of 0.1C. As a comparison, pure petroleum coke is sintered under the same conditions of the step 3 and the step 4 in the above examples 1 to 4, a button cell is manufactured under the same conditions, and a charge-discharge test is performed, so that the first lithium intercalation specific capacity can only reach 288.5mAh/g and the first lithium deintercalation specific capacity can only reach 237.9mAh/g under the multiplying power of 0.1C.
Namely, the amorphous carbon negative electrode material prepared by the invention enables the battery to have higher charge and discharge capacity.
Claims (9)
1. The preparation method of the amorphous carbon anode material is characterized by comprising the following steps of:
step 1, weighing a predetermined amount of petroleum coke as a precursor A, adding the precursor A, a set amount of distilled water, a polymer monomer and Sodium Dodecyl Sulfate (SDS) as an emulsifier into a reaction kettle to form a mixed system, vacuumizing the reaction kettle, introducing nitrogen into the reaction kettle, stirring the mixed system, heating the mixed system to 60-70 ℃ after the mixed system is stirred for 30-120 minutes, adding an ammonium persulfate aqueous solution as an initiator at the temperature of 0.5g/min for reaction for 3-5 hours, continuing stirring and cooling the reacted mixed system after the reaction is finished, adding methanol for demulsification after the mixed system is cooled to below 50 ℃, and filtering to obtain a polymer/petroleum coke composite precursor B;
step 2, carrying out low-temperature pre-carbonization treatment on the precursor B obtained in the step 1 for 5-10 hours in a nitrogen environment to obtain a precursor C, wherein the roasting temperature of the low-temperature pre-carbonization treatment is not higher than 800 ℃;
and 3, carbonizing the precursor C obtained in the step 2 at a high temperature in a nitrogen environment to obtain the amorphous carbon anode material with the core-shell structure, wherein the roasting temperature of the high-temperature carbonization is not lower than 1000 ℃.
2. The method of claim 1, wherein the method comprises the following steps: the specific surface area of the petroleum coke is 2-10 m2/g。
3. The method for preparing an amorphous carbon anode material according to claim 1 or 2, wherein: in the step 1, the feeding amount of the precursor A is 200-1000 g of the precursor A per 1L of distilled water.
4. The method of claim 3, wherein the method comprises the following steps: in the step 1, the polymer monomer is one or a mixture of several of methyl methacrylate, ethyl methacrylate and acrylate in any proportion.
5. The method for preparing an amorphous carbon anode material according to claim 1 or 2, wherein: in the step 1, the input mass ratio of the precursor A to the polymer monomer in the step 1 is 100 (10-30).
6. The method for preparing an amorphous carbon anode material according to claim 1 or 2, wherein: in the step 1, the amount of Sodium Dodecyl Sulfate (SDS) added is 2 to 4g per 1L of distilled water.
7. The method for preparing an amorphous carbon anode material according to claim 1 or 2, wherein: in the step 1, the adding amount of the ammonium persulfate aqueous solution is that 0.2-2 g of the ammonium persulfate aqueous solution is put into every 1L of distilled water.
8. The method of claim 1, wherein the method comprises the following steps: in the step 2, the roasting temperature of the low-temperature pre-carbonization treatment is 400-800 ℃.
9. The method of claim 1, wherein the method comprises the following steps: in the step 3, the roasting temperature of the high-temperature carbonization treatment is 1000-1400 ℃.
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