CN109935793B - Preparation method of lithium ion battery composite graphene negative electrode material - Google Patents
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Abstract
The invention discloses a preparation method of a composite graphene anode material of a lithium ion battery, which adopts secondary graphite particles prepared by coating, bonding and graphitizing graphene, because the inner core is made of graphene, the capacity is high, the multiplying power performance is good, after artificial graphite is compounded outside, the capacity is high, the charge and discharge performance is good, and the surfaces of the particles are arranged towards all directions, the composite graphene anode material has the characteristic of high isotropy, and meanwhile, the secondary particle structure can increase the internal pores of graphite; the lithium ion can move towards a plurality of directions, so that the lithium ion is beneficial to the infiltration of the electrolyte, more lithium ion migration channels are formed, the migration path is shorter, the high-current charge-discharge performance of the graphite is improved, and the cycle and low-temperature performance is better.
Description
Technical Field
The invention relates to the technical field of lithium ion batteries, in particular to a preparation method of a lithium ion battery composite graphene negative electrode material.
Background
The lithium ion battery has the characteristics of high voltage, high specific energy, no memory effect, long cycle life, no environmental pollution and the like, and is widely applied to mobile phones, notebook computers and other portable electronic equipment. The negative electrode material of the lithium ion battery plays a key role in the performance of the whole battery, and thus the negative electrode material has become a research hotspot in recent years.
Most of the negative electrode materials of commercial lithium ion batteries are graphite materials. Graphite has a crystalline layered structure and is susceptible to intercalation/deintercalation of lithium ions therein to form an intercalation compound LiC6It is a negative electrode material with stable performance. However, the theoretical specific capacity of the graphite cathode is only 372mAh/g, so in order to realize high specific energy of the lithium ion battery, research and development of a high-capacity cathode material graphene (graphene) which is a novel carbon nano material must be carried out, and a two-dimensional honeycomb structure is formed by tightly stacking single-layer s carbon atoms. Recent research shows that graphene has a series of special properties such as excellent electrical, thermal, optical and mechanical properties, high theoretical specific surface area and never-disappearing electrical conductivity. The large specific surface area and the good electrical properties of graphene determine the great potential of graphene in the field of lithium ion batteries, and a small amount of reports are made on the use of graphene as a lithium ion battery cathode material at present. Because graphene is formed by closely arranging single-layer carbon atoms, lithium ions can be stored in two layers of graphene sheetsAnd the graphene can be stored at the edge and in the hole of the graphene sheet layer, and the theoretical capacity of the graphene sheet layer is 740-780 mAh/g, which is more than 2 times of that of the traditional graphite material. The graphene is used as the lithium ion battery cathode material, so that the lithium storage capacity of the battery is greatly improved, and the energy density is further improved. In addition, when the graphene is used as the lithium ion battery cathode material, the diffusion path of lithium ions in the graphene material is short, the conductivity is high, and the rate capability of the lithium ion battery can be improved to a great extent. Therefore, the graphene has a good application prospect as a lithium ion battery cathode material. However, graphene used only as a negative electrode has many problems in processing due to its small particle size, low tap, large specific surface area, and the like.
Disclosure of Invention
In view of the above, the present invention provides a method for preparing a composite graphene negative electrode material for a lithium ion battery, which is characterized in that a layer of artificial graphite is coated and bonded on the surface of graphene, and the composite graphene negative electrode material has the characteristics of high capacity, good compaction performance and good rate performance, and improves the high-current charge and discharge performance of the battery negative electrode.
In order to achieve the purpose, the invention adopts the following technical scheme:
the preparation method of the composite graphene negative electrode material of the lithium ion battery comprises the following steps
Step (1), reducing graphene and a pore-forming agent according to a mass ratio of 1: (10-30) after uniformly mixing, soaking in a water solvent, drying, activating for 0.1-0.4 h at the temperature of 1000-3000 ℃ in an inert atmosphere, cleaning, and welding to obtain porous graphene;
step (2), feeding: feeding porous graphene, adhesive and graphitization catalyst into a roller microwave heating furnace, wherein during feeding, the roller in the roller microwave heating furnace is required to rotate and feed materials, the rotating speed of the roller is controlled to be 10-20 r/min, and a vibrator is added in the roller microwave heating furnace, and the vibration frequency is 80-100 Hz; wherein the mass ratio of the materials is as follows: 30-94 parts of porous graphene, 5-30 parts of adhesive and 1-5 parts of graphitization catalyst;
step (3), low-temperature integrated coating, bonding and carbonization: adjusting the rotation speed of a roller microwave heating furnace to 90-120 r/min, heating in the furnace for primary heating, raising the temperature from normal temperature to 200 ℃, keeping the constant temperature for 1.5-2 hours, realizing low-temperature coating and bonding, then heating in the furnace for secondary heating, raising the temperature to 400 ℃, keeping the constant temperature for 1-1.5 hours, then heating in the furnace for tertiary heating, raising the temperature to 600 ℃, keeping the constant temperature for 1-1.5 hours, finally heating in the furnace for quaternary heating, raising the temperature to 800 ℃, keeping the constant temperature for 1-1.5 hours, and sequentially carbonizing the graphitized catalyst from the outer layer to the inner layer step by step;
and (4) cooling: quenching with dry method and using cold inert gas N2Carrying out heat exchange with red coke in a coke oven, cooling the red coke in a dry quenching furnace by inert circulating gas, removing coarse-particle coke powder from the high-temperature circulating gas which absorbs the heat of the red coke by a primary dust remover, then feeding the high-temperature circulating gas into a boiler, absorbing heat by the boiler to generate steam, removing fine-particle coke powder from the cooled inert circulating gas by a secondary dust remover, and blowing the cooled inert circulating gas into the dry quenching furnace by a circulating fan to continuously cool the red coke until the coke is cooled to normal temperature;
step (5), purification graphitization treatment: adopting a carbon electrode rod containing a platinum catalyst as an anode, a high-purity carbon electrode rod as a cathode, and realizing arc discharge between the anode and the cathode in helium with the air pressure of 900-1500 Torr, wherein the discharge current is 300-350A; during discharging, the distance between the anode and the cathode is 1-1.5 mm, and a crude product of the composite graphene negative electrode material is prepared; carrying out high-temperature heat treatment on the prepared crude product in air, controlling the temperature of the air atmosphere at 300-500 ℃ and the treatment time at 0.5-1.0 hour to remove most impurities;
and (6) grinding and sieving to obtain the secondary particles with the core-shell structure, which are coated and bonded by using the artificial graphite and take the graphene as an inner core.
Preferably, in the step (1), the specific surface area of the porous graphene is 3.5-5m2(ii) g, tap density of 0.8-1.0g/cm3The pore diameter is 2-10nm, and the particle size is 5-15 μm.
Preferably, in the step (2), the binder is one of or a mixture of asphalt, coal tar and polymer resin.
Preferably, in the step (2), the adhesive is a polymer resin containing, by weight, 60 to 90 parts of butadiene, 5 to 15 parts of Rn-CH ═ C-CN, and CH3And (2) polymerizing monomer emulsion of-C-CH-COORm 1-5 parts, and purifying the product to obtain emulsion with the gel content of 35-55%.
In a preferable embodiment, in the step (2), the graphitization catalyst is an oxide or carbide containing silicon, iron, and tin.
Preferably, in step (2), the graphitization catalyst is SiO2、SiC、Fe2O3、SnO2Or a mixture thereof.
As a preferable scheme, in the step (5), the anode and cathode arc discharge is realized by introducing adjustable pulse direct current to electrodes at two ends, and the current density is adjusted to be 5-15 mA/cm2The retention time is 20-30 min.
Preferably, in the step (6), the artificial graphite coated on the inner core and the outer core of the graphene is in a dusty rock structure, and the dusty rocks are closely arranged to each other to form a conductive network.
As a preferable scheme, in the step (2), the organic carbon source substance can be further added during the feeding.
Preferably, the organic carbon source is selected from one or a mixture of two or more of glucose, sucrose, ascorbic acid, polyvinyl alcohol, citric acid, starch, agarose, polyethylene glycol and beta-cyclodextrin.
Compared with the prior art, the method has obvious advantages and beneficial effects, and concretely, according to the technical scheme, the secondary graphite particles are prepared by coating, bonding and graphitizing graphene, as the inner core is made of graphene, the capacity is high, the rate capability is good, and after the artificial graphite is compounded outside, the capacity is high, the charge and discharge performance is good, and the particle surfaces are arranged towards all directions, so that the method has the characteristic of high isotropy, and meanwhile, the secondary particle structure can increase the internal pores of the graphite; the lithium ion can move towards a plurality of directions, so that the lithium ion is beneficial to the infiltration of the electrolyte, more lithium ion migration channels are formed, the migration path is shorter, the high-current charge-discharge performance of the graphite is improved, and the cycle and low-temperature performance is better.
The present invention will be described in detail with reference to specific embodiments in order to more clearly illustrate the structural features and effects of the present invention.
Detailed Description
The invention provides a negative electrode material, which is particularly suitable for a lithium ion secondary battery with high capacity, large current, fast charging and fast discharging requirements.
Step (1), reducing graphene and a pore-forming agent according to a mass ratio of 1: (10-30), soaking in a water solvent, drying, activating for 0.1-0.4 h at the temperature of 1000-3000 ℃ in an inert atmosphere, cleaning, and welding to obtain the porous graphene. After the process, the specific surface area of the porous graphene is 3.5-5m2(ii) g, tap density of 0.8-1.0g/cm3The pore diameter is 2-10nm, and the particle size is 5-15 μm.
Step (2), feeding: feeding porous graphene, adhesive and graphitization catalyst into a roller microwave heating furnace, wherein during feeding, the roller in the roller microwave heating furnace is required to rotate and feed materials, the rotating speed of the roller is controlled to be 10-20 r/min, and a vibrator is added in the roller microwave heating furnace, and the vibration frequency is 80-100 Hz; wherein the mass ratio of the materials is as follows: 30-94 parts of porous graphene, 5-30 parts of adhesive and 1-5 parts of graphitization catalyst. By the aid of the roller in the roller microwave heating furnace, the mixing effect of the graphene, the adhesive and the graphitization catalyst can be improved while the roller rotates for feeding, the three are fully mixed, the coating of the adhesive and the graphitization catalyst on the graphene is facilitated, and the coating of the adhesive and the graphitization catalyst is more uniform and effective.
Wherein, the adhesive is one or a mixture of asphalt, coal tar and high molecular resin. The binder may have a particle size of100um or less, preferably 15um or less. In this embodiment, the adhesive is a polymer resin, and comprises, by weight, 60 to 90 parts of butadiene, 5 to 15 parts of Rn-CH ═ C-CN, and CH3And (2) polymerizing 1-5 parts of-C-CH-COORm monomer emulsion to obtain a product, and purifying the product to obtain an emulsion containing 35-55% of the rubber. The graphitization catalyst is an oxide or carbide containing silicon, iron and tin. In this embodiment, the graphitization catalyst is SiO2、SiC、Fe2O3、SnO2Or a mixture thereof.
In addition, organic carbon source substances can be further added during feeding, for example, the fed materials are as follows by mass ratio: 82 parts of porous graphene, 29 parts of adhesive, 5 parts of graphitization catalyst and 8 parts of organic carbon source. In this embodiment, the organic carbon source is selected from one or a mixture of two or more of glucose, sucrose, ascorbic acid, polyvinyl alcohol, citric acid, starch, agarose, polyethylene glycol, and β -cyclodextrin.
Step (3), low-temperature integrated coating, bonding and carbonization: regulating the rotation speed of a roller microwave heating furnace to 90-120 r/min, heating in the furnace for primary heating, raising the temperature from normal temperature to 200 ℃, keeping the constant temperature for 1.5-2 hours, realizing low-temperature coating and bonding, then heating in the furnace for secondary heating, raising the temperature to 400 ℃, keeping the constant temperature for 1-1.5 hours, then heating in the furnace for tertiary heating, raising the temperature to 600 ℃, keeping the constant temperature for 1-1.5 hours, finally heating in the furnace for quaternary heating, raising the temperature to 800 ℃, keeping the constant temperature for 1-1.5 hours, and gradually carbonizing the graphitized catalyst from an outer layer to an inner layer in sequence. Because the device of a roller microwave heating furnace is adopted, the heating temperature does not need to be very high due to the microwave property, and compared with the carbonization temperature of the traditional heating furnace above 2000 ℃, the highest carbonization temperature of the invention only needs to be adjusted to 800 ℃, so the device is called low-temperature carbonization. After low-temperature integrated coating, bonding and carbonization processes, the core-shell structure primary particles with smaller particle sizes are arranged on the surface of the bonded composite graphite particles in all directions, so that the composite graphite particles have the characteristic of high isotropy and increase the internal pores of graphite; the lithium ions can move towards a plurality of directions, so that the lithium ion battery is beneficial to soaking of the electrolyte, more lithium ion migration channels are formed, the migration path is shorter, and the high-current charging and discharging and low-temperature performance of the graphite are improved.
And (4) cooling: quenching with dry method and using cold inert gas N2The heat exchange is carried out between the inert circulating gas and the red coke in the coke oven, after the inert circulating gas cools the red coke in the dry quenching furnace, the high-temperature circulating gas absorbing the heat of the red coke enters a boiler after coarse particle coke powder is removed by a primary dust remover, the boiler absorbs heat to generate steam, the cooled inert circulating gas removes fine particle coke powder by a secondary dust remover, and then the inert circulating gas is blown into the dry quenching furnace by a circulating fan to continuously cool the red coke in a circulating manner until the coke is cooled to the normal temperature. The cooling method shortens the cooling time by more than 50 times compared with the natural cooling time.
Step (5), purification graphitization treatment: adopting a carbon electrode rod containing a platinum catalyst as an anode, a high-purity carbon electrode rod as a cathode, and realizing arc discharge between the anode and the cathode in helium with the air pressure of 900-1500 Torr, wherein the discharge current is 300-350A; during discharging, the distance between the anode and the cathode is 1-1.5 mm, and a crude product of the composite graphene negative electrode material is prepared; and (3) carrying out high-temperature heat treatment on the prepared crude product in air, wherein the temperature of the air atmosphere is controlled to be 300-500 ℃, and the treatment time is 0.5-1.0 hour, so as to remove most impurities. In the embodiment, the anode and cathode arc discharge is realized by introducing adjustable pulse direct current to electrodes at two ends, and the current density is adjusted to be 5-15 mA/cm2The retention time is 20-30 min. By adopting purification and graphitization treatment, impurities can be more fully removed, and the prepared graphite has higher purity.
And (6) grinding and sieving to obtain the secondary particles with the core-shell structure, which are coated and bonded by using the artificial graphite and take the graphene as an inner core. The artificial graphite coated outside the graphene inner core is in a dust spar structure, and the dust spars are closely arranged with each other to form a conductive network. The specific surface area of the artificial graphite of the composite secondary particle is 1000-3000m2(ii) g, tap density of 3-5g/cm3The pore diameter is 30-38nm, the particle size is 7-11 μm, and the capacity is more than 350 mAh/g.
In summary, the design of the present invention is characterized in that the core-shell structure secondary particles, which are formed by coating and bonding the core-shell structure secondary particles with the artificial graphite, have the characteristics of high capacity, good compaction performance and good rate capability. The process comprises the following steps: mixing according to a specific proportion, adding an adhesive for coating and bonding, and finally heating and carbonizing by a program to obtain the composite graphite material. The lithium ion secondary battery has the characteristics of high capacity, high compaction and high rate, and is suitable for the requirements of high-capacity quick charge or high-capacity heavy-current discharge.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the technical scope of the present invention, so that any minor modifications, equivalent changes and modifications made to the above embodiment according to the technical spirit of the present invention are within the technical scope of the present invention.
Claims (10)
1. A preparation method of a lithium ion battery composite graphene negative electrode material is characterized by comprising the following steps: comprises the following steps
Step (1), reducing graphene and a pore-forming agent according to a mass ratio of 1: (10-30) after uniformly mixing, soaking in a water solvent, drying, activating for 0.1-0.4 h at the temperature of 1000-3000 ℃ in an inert atmosphere, cleaning, and welding to obtain porous graphene;
step (2), feeding: feeding porous graphene, adhesive and graphitization catalyst into a roller microwave heating furnace, wherein during feeding, the roller in the roller microwave heating furnace is required to rotate and feed materials, the rotating speed of the roller is controlled to be 10-20 r/min, and a vibrator is added in the roller microwave heating furnace, and the vibration frequency is 80-100 Hz; wherein the mass ratio of the materials is as follows: 30-94 parts of porous graphene, 5-30 parts of adhesive and 1-5 parts of graphitization catalyst;
step (3), low-temperature integrated coating, bonding and carbonization: adjusting the rotation speed of a roller microwave heating furnace to 90-120 r/min, heating in the furnace for primary heating, raising the temperature from normal temperature to 200 ℃, keeping the constant temperature for 1.5-2 hours, realizing low-temperature coating and bonding, then heating in the furnace for secondary heating, raising the temperature to 400 ℃, keeping the constant temperature for 1-1.5 hours, then heating in the furnace for tertiary heating, raising the temperature to 600 ℃, keeping the constant temperature for 1-1.5 hours, finally heating in the furnace for quaternary heating, raising the temperature to 800 ℃, keeping the constant temperature for 1-1.5 hours, and sequentially carbonizing the graphitized catalyst from the outer layer to the inner layer step by step;
and (4) cooling: quenching with dry method and using cold inert gas N2Carrying out heat exchange with red coke in a coke oven, cooling the red coke in a dry quenching furnace by inert circulating gas, removing coarse-particle coke powder from the high-temperature circulating gas which absorbs the heat of the red coke by a primary dust remover, then feeding the high-temperature circulating gas into a boiler, absorbing heat by the boiler to generate steam, removing fine-particle coke powder from the cooled inert circulating gas by a secondary dust remover, and blowing the cooled inert circulating gas into the dry quenching furnace by a circulating fan to continuously cool the red coke until the coke is cooled to normal temperature;
step (5), purification graphitization treatment: adopting a carbon electrode rod containing a platinum catalyst as an anode, a high-purity carbon electrode rod as a cathode, and realizing arc discharge between the anode and the cathode in helium with the air pressure of 900-1500 Torr, wherein the discharge current is 300-350A; during discharging, the distance between the anode and the cathode is 1-1.5 mm, and a crude product of the composite graphene negative electrode material is prepared; carrying out high-temperature heat treatment on the prepared crude product in air, controlling the temperature of the air atmosphere at 300-500 ℃ and the treatment time at 0.5-1.0 hour to remove most impurities;
and (6) grinding and sieving to obtain the secondary particles with the core-shell structure, which are coated and bonded by using the artificial graphite and take the graphene as an inner core.
2. The preparation method of the lithium ion battery composite graphene negative electrode material according to claim 1, characterized in that: in the step (1), the specific surface area of the porous graphene is 3.5-5m2(ii) g, tap density of 0.8-1.0g/cm3The pore diameter is 2-10nm, and the particle size is 5-15 μm.
3. The preparation method of the lithium ion battery composite graphene negative electrode material according to claim 1, characterized in that: in the step (2), the adhesive is one or a mixture of asphalt, coal tar and polymer resin.
4. The preparation method of the lithium ion battery composite graphene negative electrode material according to claim 2, characterized by comprising the following steps: in the step (2), the adhesive is a polymer resin, and comprises, by weight, 60 to 90 parts of butadiene, 5 to 15 parts of Rn-CH ═ C-CN, and CH3And (2) 1-5 parts of-C-CH-COORm, polymerizing the monomer emulsion of the-C-CH-COORm and the monomer emulsion of the-C-COORm, and purifying the product to obtain the emulsion with the gel content of 35-55%.
5. The preparation method of the lithium ion battery composite graphene negative electrode material according to claim 1, characterized in that: in the step (2), the graphitization catalyst is an oxide or carbide containing silicon, iron and tin.
6. The preparation method of the lithium ion battery composite graphene negative electrode material according to claim 5, characterized in that: in the step (2), the graphitization catalyst is SiO2、SiC、Fe2O3、SnO2Or a mixture thereof.
7. The preparation method of the lithium ion battery composite graphene negative electrode material according to claim 1, characterized in that: in the step (5), the anode and cathode arc discharge is realized by introducing adjustable pulse direct current to the electrodes at two ends, and the current density is adjusted to be 5-15 mA/cm2The retention time is 20-30 min.
8. The preparation method of the lithium ion battery composite graphene negative electrode material according to claim 1, characterized in that: in the step (6), the artificial graphite coated outside the graphene inner core is in a dust crystal structure, and the dust crystals are closely arranged to form a conductive network.
9. The preparation method of the lithium ion battery composite graphene negative electrode material according to claim 1, characterized in that: in the step (2), organic carbon source substances can be further added during feeding.
10. The preparation method of the lithium ion battery composite graphene negative electrode material according to claim 9, characterized in that: the organic carbon source is selected from one or a mixture of more than two of glucose, sucrose, ascorbic acid, polyvinyl alcohol, citric acid, starch, agarose, polyethylene glycol and beta-cyclodextrin.
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| CN103241731A (en) * | 2013-04-01 | 2013-08-14 | 东莞市凯金电池材料有限公司 | Preparation method of compound graphite material for lithium ion secondary battery |
| CN106450176A (en) * | 2016-08-24 | 2017-02-22 | 上海颐行高分子材料有限公司 | Preparation method of high-capacity negative electrode material |
| WO2017029692A1 (en) * | 2015-08-18 | 2017-02-23 | Nec Corporation | Porous Graphene Coated Oxygen-Containing Carbon Material for High Capacity and Fast Chargeable Anode of Lithium Ion Battery |
| CN106981657A (en) * | 2017-05-26 | 2017-07-25 | 成都海成远创科技有限公司 | A kind of graphite cathode material and preparation method thereof |
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| CN103241731A (en) * | 2013-04-01 | 2013-08-14 | 东莞市凯金电池材料有限公司 | Preparation method of compound graphite material for lithium ion secondary battery |
| WO2017029692A1 (en) * | 2015-08-18 | 2017-02-23 | Nec Corporation | Porous Graphene Coated Oxygen-Containing Carbon Material for High Capacity and Fast Chargeable Anode of Lithium Ion Battery |
| CN106450176A (en) * | 2016-08-24 | 2017-02-22 | 上海颐行高分子材料有限公司 | Preparation method of high-capacity negative electrode material |
| CN106981657A (en) * | 2017-05-26 | 2017-07-25 | 成都海成远创科技有限公司 | A kind of graphite cathode material and preparation method thereof |
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