CN103219510A - Lithium battery negative electrode material preparation method and its product - Google Patents
Lithium battery negative electrode material preparation method and its product Download PDFInfo
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- CN103219510A CN103219510A CN2013100916511A CN201310091651A CN103219510A CN 103219510 A CN103219510 A CN 103219510A CN 2013100916511 A CN2013100916511 A CN 2013100916511A CN 201310091651 A CN201310091651 A CN 201310091651A CN 103219510 A CN103219510 A CN 103219510A
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Abstract
The invention discloses a preparation method of a lithium battery negative electrode material. The method includes: (a) taking water, alcohol or an alcohol-water mixture as a solvent, and dissolving the metal precursor of at least one material selected from Co3O4, Fe3O4, NiO or a doped compound thereof in the solvent so as to obtain a precursor solution; (b) adding carbon into the obtained precursor solution, and then performing a concentration treatment until obtaining a slurry mixture; (c) subjecting the slurry mixture to baking drying and grinding, and then carrying out a reduction reaction, thereby obtaining nanoparticles of a carbon loaded metal material; and (d) conducting a heating oxidation treatment on the obtained nanoparticles to obtain the needed lithium battery electrode material. The invention also discloses the corresponding lithium battery negative electrode material and a lithium battery product. By the method provided in the invention, the negative electrode material that has a hollow structure and is suitable for lithium batteries can be obtained through a simple process at a low cost, and the quality is easy to control. The obtained lithium battery product has the characteristics of high capacity, good cycling performance and the like.
Description
Technical field
The invention belongs to field of nano material preparation, more specifically, relate to preparation method of a kind of lithium cell cathode material and products thereof.
Background technology
Lithium ion battery with its voltage height, specific energy height, have extended cycle life, advantage such as memory-less effect, be widely used in the military and civilian electronic equipment, as mobile phone, notebook computer, camera etc.Though jumbo lithium ion battery is also to electric automobile, field of power tools expansion, yet present lithium ion battery does not also possess needed high power in electric automobile field and long life.For lithium battery, the character of its electrode material is the key factor of decision lithium battery performance quality.Present commercial lithium cell cathode material mainly is a material with carbon element, and is growing to lithium battery high-energy-density, high-power requirement but its lower specific capacity and specific energy can not satisfy.
Transition metal oxide such as Co
3O
4, Fe
3O
4, NiO etc., caused researcher's very big interest with its higher specific capacity.For example, disclose a kind of employing surfactant among the CN102280635A and prepared micron order Co
3O
4The method of-C composite material, this composite material is graininess, and each particle comprises the hemisphere layer of a plurality of stacked expansion, and battery performance test shows that this composite material has higher specific discharge capacity and high rate performance.In addition, a kind of lithium ion battery electrode material and preparation method thereof is disclosed among the CN10187689A, wherein adopting polymer is template, by the particle size of control synthesis temperature, sintering time, polymer template, thereby makes submicron order material applicable to electrode of lithium cell.
Yet, further studies show that above-mentioned preparation method's following defective or the deficiency of still existence: at first, owing in the material preparation process, need to add surfactant or template, not only operating process is loaded down with trivial details, is difficult to control, and has increased the preparation cost of material; Secondly, according to above-mentioned process, prepared material is micron or sub-micron rank, and particle is relatively large, is unfavorable for the rapid diffusion of lithium ion, thereby influences the performance and the life-span of battery in actual motion.Therefore, seek new cathode of lithium battery preparation method and replace structure needing badly in association area, growing to meet to lithium battery high-energy-density, high-power requirement.
Summary of the invention
Above defective or improvement demand at prior art, the object of the present invention is to provide preparation method of a kind of lithium cell cathode material and products thereof, the mode by taking transition metal oxide nanoization and its preparation technology studied and improve wherein, can be simple with technology, cost is low, be convenient to the negative material product that quality control ground obtains to be applicable to lithium battery, and prepared lithium battery possesses characteristics such as capacity height, good cycle.
According to one aspect of the present invention, a kind of method that is used to prepare lithium cell cathode material is provided, it is characterized in that this method comprises the following steps:
(a) be solvent with water, alcohol or alcohol-water mixture, will be selected from Co
3O
4, Fe
3O
4, in NiO or its doped compound at least a material the metal precursor dissolving wherein, obtain precursor solution thus;
(b) add carbon in the precursor solution that is obtained, wherein the mass ratio of metal ion is controlled to be 4:1～1:4 in carbon and the precursor solution, carries out concentration then until the mixture that obtains to be pulpous state;
(c) paste mixture that step (b) is obtained is carried out and is cured drying and grinding, carries out reduction reaction then, obtains the nano particle of carbon-supported metal material thus;
(d) nano particle that step (c) is obtained is carried out the heated oxide processing, obtains required electrode material of lithium battery thus.
Transition metal oxide such as Co
3O
4, Fe
3O
4, though NiO etc. possesses higher specific capacity, but lithium to take off in the embedding process change in volume bigger, cause higher irreversible capacity loss easily, it is relatively poor to add the transition metal oxide self-conductive, can make the specific capacity of electrode material reduce, and cycle performance become bad.By above design, can mode simple with technology, that be convenient to quality control obtain the carbon-supported metal material of nanometer, thereby effectively remedy above deficiency; Especially, prepared carbon-supported metal material presents the special appearance of hollow structure, change in volume is less in charge and discharge process, and possesses bigger specific area, make the contact area of itself and electrolyte big and reduced lithium ion and electron diffusion path, thereby bigger specific capacity can be provided and improve cycle characteristics.
As further preferably, in step (a), described metal precursor is metal chloride or nitrate.
As further preferably, in step (a), the concentration of described metal precursor is controlled as 10mg/mL～100mg/mL, and described alcohol is selected from least a in methyl alcohol, ethanol or the propyl alcohol.
As further preferably, in step (b), by ultrasonic dispersion with add the mode that thermal agitation replaces, carry out concentration until the mixture that obtains to be pulpous state.
As further preferably, in step (c), under the temperature conditions of 40～100 degree, dried is cured in described paste mixture execution, and be ground into Powdered.
As further preferably, in step (c), described reduction reaction is carried out in hydrogen atmosphere, and its reduction temperature scope is 300～1000 ℃, and the recovery time is 2～10 hours.
As further preferably, in step (d), the heating-up temperature that described heated oxide is handled is 250～400 ℃, and heat treatment time is 5～20 hours.
As further preferably, described carbon is acetylene black, carbon black, Vulcan XC-72, carbon nano-tube, graphite, Graphene, various meso-porous carbon materials etc.
According to another aspect of the present invention, also provide corresponding electrode material of lithium battery product.
As further preferably, described electrode material of lithium battery is made of the metal oxide nano-material that possesses hollow structure that carbon carries, and wherein said metal oxide is selected from Co
3O
4, Fe
3O
4, at least a in NiO or its doped compound.
As further preferably, the specific area of described electrode material of lithium battery is 50m
2More than/the g.
According to another aspect of the present invention, also provide corresponding lithium battery product.
In general, according to electrode material of lithium battery preparation method of the present invention and products thereof compared with prior art, mainly possess following technological merit:
1, by design to key reaction thing and reaction condition, can mode simple with technology, that be convenient to quality control obtain the carbon-supported metal material of nanometer, and need not surfactant or template in the course of reaction, reduced manufacturing cost;
2, according to process of the present invention, prepared lithium cell cathode material directly but be loaded on the high carbon carrier of conductivity, has overcome the shortcoming of transition metal oxide poorly conductive in building-up process; In addition, this transition metal oxide presents the nano particle that possesses hollow structure, possesses bigger specific area, helps increasing the contact area of electrode material and electrolyte, shortens lithium ion and electron diffusion path, thereby shows excellent chemical property;
3, the economic environmental protection of whole preparation method, and be convenient to quality control, and can be used for the large-scale industrialization batch process, therefore be particularly useful for making purposes such as lithium ion battery negative, ultracapacitor.
Description of drawings
Fig. 1 is the method flow diagram that is used to prepare lithium cell cathode material according to the present invention;
Fig. 2 a is according to the embodiment of the invention 1 prepared Co
3O
4The transmission electron microscope photo of-C sample;
Fig. 2 b is according to the embodiment of the invention 1 prepared Co
3O
4The XRD figure spectrum of-C sample;
Fig. 2 c is according to the embodiment of the invention 1 prepared Co
3O
4When-C sample is used for lithium battery as negative material, the cycle performance figure that under the 100mA/g condition, discharges.
Embodiment
In order to make purpose of the present invention, technical scheme and advantage clearer,, the present invention is further elaborated below in conjunction with drawings and Examples.Should be appreciated that specific embodiment described herein only in order to explanation the present invention, and be not used in qualification the present invention.
Specify the method flow that is used to prepare lithium cell cathode material according to the present invention with reference to Fig. 1 below.
At first, be solvent with water, alcohol or alcohol-water mixture, will be selected from Co
3O
4, Fe
3O
4, the metal precursor of at least a material in NiO or its doped compound, for example dissolving such as metal chloride or nitrate wherein obtains precursor solution thus.Wherein, the concentration of described metal precursor is controlled as 10mg/mL～100mg/mL, and described alcohol is selected from least a in methyl alcohol, ethanol or the propyl alcohol.
Then, in the precursor solution that is obtained, add all kinds of carbon that for example are selected from acetylene black, carbon black, Vulcan XC-72, carbon nano-tube, graphite, Graphene, various meso-porous carbon materials etc., wherein the mass ratio of metal ion is controlled to be 4:1～1:4 in carbon and the precursor solution, carries out concentration then until the mixture that obtains to be pulpous state.In this process,, carry out concentration until the mixture that obtains to be pulpous state preferably by ultrasonic dispersion with add the mode that thermal agitation replaces.
Then, drying and grinding are cured in the paste mixture execution under the temperature conditions of 40～100 degree that is obtained, carry out reduction reaction then, obtain the nano particle of carbon-supported metal material thus; Reduction reaction is preferably carried out in hydrogen atmosphere, and its reduction temperature scope is 300～1000 ℃, and the recovery time is 2～10 hours.
At last, the nano particle that is obtained is carried out heated oxide to be handled, obtain required electrode material of lithium battery thus, wherein more contrast test shows, the heating-up temperature that heated oxide is handled can be set at 250～400 ℃, heat treatment time is set at 5～20 hours, can obtain the more uniform nanometer product of particle.
Embodiment 1
At first, with the CoCl of 1.61g
26H
2O is dissolved in the 50mL water and forms precursor solution, then adds the Vulcan XC-72 carbon black of 0.6g in precursor solution, adopts ultrasonic dispersion repeatedly and adds the mode that thermal agitation replaces, and carries out concentration until obtaining to be pulpous state carbon mud.
After this pulpous state carbon mud placed 12 hours, place baking oven to cure drying with the temperature conditions of 60 degree, grind then and place porcelain boat to be placed in the tube furnace, in the hydrogen atmosphere of 350 degree, carried out reduction reaction 5 hours, be cooled to room temperature then, the carbon that promptly obtains 40wt%Co content carries Co(Co-C) nano particle.
The carbon that obtains is carried the Co nano particle places tube furnace, in air atmosphere with 1 the degree/minute programming rate be heated to 400 the degree, then under this temperature the insulation 10 hours, be cooled to room temperature, promptly obtain required carbon and carry Co
3O
4The lithium cell cathode material product.
Embodiment 2
At first, with the CoCl of 0.8g
26H
2O is dissolved in the 50mL methyl alcohol and forms precursor solution, then adds the acetylene black of 0.8g in precursor solution, adopts ultrasonic dispersion repeatedly and adds the mode that thermal agitation replaces, and carries out concentration until obtaining to be pulpous state carbon mud.
After this pulpous state carbon mud placed 12 hours, place baking oven to cure drying with the temperature conditions of 50 degree, grind then and place porcelain boat to be placed in the tube furnace, in the hydrogen atmosphere of 300 degree, carried out reduction reaction 10 hours, be cooled to room temperature then, the carbon that promptly obtains 20wt%Co content carries Co(Co-C) nano particle.
The carbon that obtains is carried the Co nano particle places tube furnace, in air atmosphere with 1 the degree/minute programming rate be heated to 350 the degree, then under this temperature the insulation 5 hours, be cooled to room temperature, promptly obtain required carbon and carry Co
3O
4The lithium cell cathode material product.
Embodiment 3
At first, with the CoCl of 3.22g
26H
2O is dissolved in the 50mL ethanol and forms precursor solution, then adds the mesoporous carbon of 0.2g in precursor solution, adopts ultrasonic dispersion repeatedly and adds the mode that thermal agitation replaces, and carries out concentration until obtaining to be pulpous state carbon mud.
After this pulpous state carbon mud placed 12 hours, place baking oven to cure drying with the temperature conditions of 40 degree, grind then and place porcelain boat to be placed in the tube furnace, in the hydrogen atmosphere of 400 degree, carried out reduction reaction 5 hours, be cooled to room temperature then, the carbon that promptly obtains 80wt%Co content carries Co(Co-C) nano particle.
The carbon that obtains is carried the Co nano particle places tube furnace, in air atmosphere with 1 the degree/minute programming rate be heated to 350 the degree, then under this temperature the insulation 15 hours, be cooled to room temperature, promptly obtain required carbon and carry Co
3O
4The lithium cell cathode material product.
Embodiment 4
At first, with the FeCl of 2.14g
2Be dissolved in the 50mL propyl alcohol and form precursor solution, then in precursor solution, add the acetylene black of 0.4g, adopt ultrasonic dispersion repeatedly and add the mode that thermal agitation replaces, carry out concentration until obtaining to be pulpous state carbon mud.
After this pulpous state carbon mud placed 12 hours, place baking oven to cure drying with the temperature conditions of 60 degree, grind then and place porcelain boat to be placed in the tube furnace, in the hydrogen atmosphere of 300 degree, carried out reduction reaction 10 hours, be cooled to room temperature then, the carbon that promptly obtains 60wt%Co content carries Fe(Fe-C) nano particle.
The carbon that obtains is carried the Fe nano particle places tube furnace, in air atmosphere with 1 the degree/minute programming rate be heated to 350 the degree, then under this temperature the insulation 10 hours, be cooled to room temperature, promptly obtain required carbon and carry Fe
3O
4The lithium cell cathode material product.
Embodiment 5
At first, with the NiCl of 3.24g
26H
2O is dissolved in the 50mL water and forms precursor solution, then adds the Graphene of 0.2g in precursor solution, adopts ultrasonic dispersion repeatedly and adds the mode that thermal agitation replaces, and carries out concentration until obtaining to be pulpous state carbon mud.
After this pulpous state carbon mud placed 12 hours, place baking oven to cure drying with the temperature conditions of 40 degree, grind then and place porcelain boat to be placed in the tube furnace, in the hydrogen atmosphere of 400 degree, carried out reduction reaction 5 hours, be cooled to room temperature then, the carbon that promptly obtains 80wt%Co content carries Ni(Ni-C) nano particle.
The carbon that obtains is carried the Ni nano particle places tube furnace, in air atmosphere with 1 the degree/minute programming rate be heated to 250 the degree, then under this temperature the insulation 10 hours, be cooled to room temperature, promptly obtain required carbon and carry NiO lithium cell cathode material product.
Embodiment 6
At first, Fe (NO3) 39H2O of 5.71g is dissolved in the 50mL water forms precursor solution, then in precursor solution, add the Graphene of 0.2g, adopt ultrasonic dispersion repeatedly and add the mode that thermal agitation replaces, carry out concentration until obtaining to be pulpous state carbon mud.
After this pulpous state carbon mud placed 12 hours, place baking oven to cure drying with the temperature conditions of 100 degree, grind then and place porcelain boat to be placed in the tube furnace, in the hydrogen atmosphere of 1000 degree, carried out reduction reaction 2 hours, be cooled to room temperature then, the carbon that promptly obtains 80wt%Co content carries Fe(Fe-C) nano particle.
The carbon that obtains is carried the Fe nano particle places tube furnace, in air atmosphere with 1 the degree/minute programming rate be heated to 250 the degree, then under this temperature the insulation 20 hours, be cooled to room temperature, promptly obtain required carbon and carry Fe
3O
4The lithium cell cathode material product.
To be example with embodiment 1 prepared sample below, introduce analyzing according to the negative material product that the present invention obtained and the process of Performance Detection.The prepared sample of other embodiment after tested, its aspect of performance and embodiment 1 obtained sample performance basically identical.
Fig. 2 a is according to the embodiment of the invention 1 prepared Co
3O
4The transmission electron microscope photo of-C sample, Fig. 2 b are according to the embodiment of the invention 1 prepared Co-C and Co
3O
4The XRD figure spectrum of-C sample.As can be seen, the nano transition metal oxides of this lithium cell cathode material presents hollow structure from Fig. 2 a, and its average diameter of particles is about 50nm, and transition metal oxide is dispersed on the surface of carbon carrier.The XRD of Fig. 2 b test has proved that formed metallic cobalt after cobalt precursor is reduced containing that carbon carries in hydrogen atmosphere, its principal character be in 2 θ=41.7,44.5 and 47.5 degree places have occurred corresponding to (100), (002) and the characteristic diffraction peak of (101) crystal face, consistent with the metallic cobalt standard diagram (JCPDS card No.05-0727) of hexagonal closs packing.With prepared Co/C in oxidizing atmosphere after the heat treatment, the XRD diffraction maximum changes, in 2 θ=31.3,36.9,44.9,59.4 and 65.4 the degree occurred corresponding to (220), (311), (400), (511) and the characteristic diffraction peak of (440) crystal face, all consistent with the Co3O4 standard diagram (JCPDS card No.42-1467) of spinel-type.The wide characteristic diffraction peak of carrier carbon appears in these external 2 θ=25 degree places.
Fig. 2 c is according to the embodiment of the invention 1 prepared Co
3O
4When-C sample is used for lithium battery as negative material, the cycle performance figure that under the 100mA/g condition, discharges.As can be seen, its discharge capacity remains on 880mAh/g except irreversible loss first from Fig. 2 c, approaching theoretical capacity, and discharge and recharge after 50 times, capacity substantially and does not lose, and illustrates that prepared electrode material has charge-discharge performance and stability preferably.
Those skilled in the art will readily understand; the above only is preferred embodiment of the present invention; not in order to restriction the present invention, all any modifications of being done within the spirit and principles in the present invention, be equal to and replace and improvement etc., all should be included within protection scope of the present invention.
Claims (10)
1. a method that is used to prepare lithium cell cathode material is characterized in that, this method comprises the following steps:
(a) be solvent with water, alcohol or alcohol-water mixture, will be selected from Co
3O
4, Fe
3O
4, in NiO or its doped compound at least a material the metal precursor dissolving wherein, obtain precursor solution thus;
(b) add carbon in the precursor solution that is obtained, wherein the mass ratio of metal ion is controlled to be 4:1～1:4 in carbon and the precursor solution, carries out concentration then until the mixture that obtains to be pulpous state;
(c) paste mixture that step (b) is obtained is carried out and is cured drying and grinding, carries out reduction reaction then, obtains the nano particle of carbon-supported metal material thus;
(d) nano particle that step (c) is obtained is carried out the heated oxide processing, obtains required electrode material of lithium battery thus.
2. the method for claim 1 is characterized in that, in step (a), the concentration of described metal precursor is controlled as 10mg/mL～100mg/mL, and described alcohol is selected from least a in methyl alcohol, ethanol or the propyl alcohol.
3. method as claimed in claim 1 or 2 is characterized in that, in step (b), by ultrasonic dispersion with add the mode that thermal agitation replaces, carries out concentration until the mixture that obtains to be pulpous state.
4. as any described method of claim 1-3, it is characterized in that, in step (c), under the temperature conditions of 40～100 degree, dried is cured in described paste mixture execution, and be ground into Powdered.
5. method as claimed in claim 4 is characterized in that, in step (c), described reduction reaction is carried out in hydrogen atmosphere, and its reduction temperature scope is 300～1000 ℃, and the recovery time is 2～10 hours.
6. as any described method of claim 1-5, it is characterized in that in step (d), the heating-up temperature that described heated oxide is handled is preferably 250～400 ℃, heat treatment time is preferably 5～20 hours.
7. the lithium cell cathode material product that makes as any described method of claim 1-6.
8. lithium cell cathode material product as claimed in claim 7 is characterized in that, this lithium cell cathode material is made of the metal oxide nano-material that possesses hollow structure that carbon carries, and wherein said metal oxide is selected from Co
3O
4, Fe
3O
4, at least a in NiO or its doped compound.
9. lithium cell cathode material product as claimed in claim 8 is characterized in that, the specific area of described electrode material of lithium battery is 50m
2More than/the g.
10. a lithium battery is characterized in that, its negative pole is by constituting as any described negative material of claim 7-9.
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| CN105118962A (en) * | 2015-07-20 | 2015-12-02 | 上海交通大学 | Carbon sphere/ferroferric oxide composite material, preparation and application method thereof |
| CN105845895A (en) * | 2016-05-09 | 2016-08-10 | 上海交通大学 | Preparation method for negative electrode material of lithium ion battery |
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| CN105118962A (en) * | 2015-07-20 | 2015-12-02 | 上海交通大学 | Carbon sphere/ferroferric oxide composite material, preparation and application method thereof |
| CN105845895A (en) * | 2016-05-09 | 2016-08-10 | 上海交通大学 | Preparation method for negative electrode material of lithium ion battery |
| CN106067549A (en) * | 2016-07-29 | 2016-11-02 | 昆明理工大学 | A kind of preparation method of lithium ion battery negative material |
| CN107946548A (en) * | 2016-10-13 | 2018-04-20 | 内蒙古欣源石墨烯科技有限公司 | Store up the preparation method of oxide/lithium ferrite and the compound lithium ion battery negative material of carbon |
| CN107946548B (en) * | 2016-10-13 | 2023-09-19 | 内蒙古欣源石墨烯科技股份有限公司 | Preparation method of lithium-iron oxide and carbon composite lithium ion battery anode material |
| CN106972166A (en) * | 2017-05-17 | 2017-07-21 | 江西南氏锂电新材料有限公司 | A kind of lithium ion battery negative material and preparation method thereof |
| CN108417799A (en) * | 2018-02-11 | 2018-08-17 | 合肥国轩高科动力能源有限公司 | A kind of preparation method and applications of hollow structure copper oxide/multi-wall carbon nano-tube composite material |
| CN108511706A (en) * | 2018-03-13 | 2018-09-07 | 合肥国轩高科动力能源有限公司 | A kind of preparation method of lithium battery Two-dimensional Inorganic perovskite negative material |
| CN109754897A (en) * | 2019-03-28 | 2019-05-14 | 山东华冠智能卡有限公司 | Graphene-based electrocondution slurry and preparation method thereof |
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