CN115632131B - Lithium ion battery anode material and preparation method thereof - Google Patents
Lithium ion battery anode material and preparation method thereof Download PDFInfo
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- CN115632131B CN115632131B CN202211442189.0A CN202211442189A CN115632131B CN 115632131 B CN115632131 B CN 115632131B CN 202211442189 A CN202211442189 A CN 202211442189A CN 115632131 B CN115632131 B CN 115632131B
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- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 title claims abstract description 25
- 229910001416 lithium ion Inorganic materials 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 239000010405 anode material Substances 0.000 title claims abstract description 9
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims abstract description 37
- 229910052744 lithium Inorganic materials 0.000 claims abstract description 37
- 229910003023 Mg-Al Inorganic materials 0.000 claims abstract description 32
- 238000005245 sintering Methods 0.000 claims abstract description 23
- 239000000463 material Substances 0.000 claims abstract description 21
- 239000007774 positive electrode material Substances 0.000 claims abstract description 19
- 239000002243 precursor Substances 0.000 claims abstract description 18
- 238000000034 method Methods 0.000 claims abstract description 17
- 238000003825 pressing Methods 0.000 claims abstract description 13
- 229910000625 lithium cobalt oxide Inorganic materials 0.000 claims abstract description 11
- BFZPBUKRYWOWDV-UHFFFAOYSA-N lithium;oxido(oxo)cobalt Chemical compound [Li+].[O-][Co]=O BFZPBUKRYWOWDV-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000000227 grinding Methods 0.000 claims abstract description 5
- 238000002156 mixing Methods 0.000 claims abstract description 5
- 238000000465 moulding Methods 0.000 claims description 7
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 claims description 6
- 229910021503 Cobalt(II) hydroxide Inorganic materials 0.000 claims description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 3
- 239000010406 cathode material Substances 0.000 claims description 3
- UBEWDCMIDFGDOO-UHFFFAOYSA-N cobalt(II,III) oxide Inorganic materials [O-2].[O-2].[O-2].[O-2].[Co+2].[Co+3].[Co+3] UBEWDCMIDFGDOO-UHFFFAOYSA-N 0.000 claims description 3
- 229910052593 corundum Inorganic materials 0.000 claims description 3
- 229910001845 yogo sapphire Inorganic materials 0.000 claims description 3
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims 1
- 239000002245 particle Substances 0.000 abstract description 13
- 238000009826 distribution Methods 0.000 abstract description 3
- 239000000843 powder Substances 0.000 description 10
- 229910032387 LiCoO2 Inorganic materials 0.000 description 5
- 239000004570 mortar (masonry) Substances 0.000 description 5
- 238000005056 compaction Methods 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
Classifications
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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
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
- H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—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
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/028—Positive 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
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Inorganic Chemistry (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention provides a lithium ion battery anode material and a preparation method thereof, wherein the preparation method comprises the following steps: mixing the precursor materials, and cold-pressing the precursor materials to form under a first pressure; performing first sintering treatment on the current precursor material to obtain Mg-Al co-doped lithium cobalt oxide; grinding the Mg-Al co-doped lithium cobalt oxide, and cold-pressing the current Mg-Al co-doped lithium cobalt oxide under a second pressure to form; and performing second sintering treatment on the Mg-Al co-doped lithium cobaltate after cold press forming to obtain a sample of the lithium ion battery positive electrode material. According to the preparation method of the lithium ion battery anode material, provided by the invention, the regulation and control of the size distribution of Mg-Al co-doped lithium cobaltate particles are realized by a cold pressing preforming method.
Description
Technical Field
The invention relates to the technical field of lithium battery preparation, in particular to a lithium ion battery anode material and a preparation method thereof.
Background
Lithium ion batteries are widely used in the fields of portable electronic devices, new energy automobiles, large-scale energy storage and the like due to the characteristics of high energy density, long cycle life and the like. Along with the development of portable electronic devices and the Internet of things, the electronic products have higher and higher requirements on the volume energy density of lithium ion batteries. Lithium cobaltate is considered as one of the lithium ion cathode materials with the highest volumetric energy density, attracting widespread interest to researchers.
The volumetric energy density of the positive electrode material of a lithium ion battery consists of three factors: the capacity of the electrode material, the potential of the discharge curve, and the density of the electrodes. Generally, the structure of the material can be stabilized by doping Mg, al and other elements between the layers of lithium cobaltate, so that the layered structure can be still kept stable when the number of lithium ions deintercalated is more than 0.5 per unit cell. Therefore, by doping Mg, al and other elements, the charge termination potential of the material can be increased from 4.2V to more than 4.6V, and the capacity and the discharge curve potential of the lithium cobaltate material can be greatly increased. For the density of the electrode, it is necessary to control the size of the Mg-Al co-doped lithium cobaltate particles.
However, the size of the Mg-Al co-doped lithium cobaltate particles is difficult to control at present.
Disclosure of Invention
The invention aims to solve the technical problem that in the prior art, the size of Mg-Al co-doped lithium cobaltate particles is difficult to effectively control in the preparation process of a lithium battery positive electrode material, and in view of the problem, the invention provides the lithium battery positive electrode material and a preparation method thereof.
The technical scheme adopted by the invention is that the preparation method of the lithium ion battery anode material comprises the following steps:
Mixing the precursor materials, and cold-pressing the precursor materials to form under a first pressure;
Performing first sintering treatment on the precursor material to obtain Mg-Al co-doped lithium cobaltate;
Grinding the Mg-Al co-doped lithium cobalt oxide, and cold-pressing and forming the Mg-Al co-doped lithium cobalt oxide at a second pressure;
And performing second sintering treatment on the Mg-Al co-doped lithium cobaltate after cold press molding to obtain a sample of the lithium ion battery positive electrode material.
In one embodiment, the first pressure is in the pressure range of 1 MPa to 10 Gpa.
In one embodiment, the first pressure is in the pressure range of 100 MPa to 2.1 GPa.
In one embodiment, the temperature of the first sintering process is 700-1200 o C.
In one embodiment, the temperature of the first sintering process is 800-1100 o C.
In one embodiment, the second pressure is in the pressure range of 1 MPa to 8 GPa,
In one embodiment, the temperature of the second sintering process is 800-1200 o C.
In one embodiment, the precursor material comprises: at least four of Li 2CO3、LiOH、Co3O4、Co(OH)2、Al2O3 and MgO.
The invention further provides a lithium battery positive electrode material, which is prepared by the preparation method of the lithium ion battery positive electrode material.
Another aspect of the present invention provides a lithium battery comprising a lithium battery cathode material as described above.
By adopting the technical scheme, the invention has at least the following advantages:
according to the preparation method of the lithium ion battery anode material, provided by the invention, the regulation and control of the size distribution of Mg-Al co-doped lithium cobaltate particles are realized by a cold pressing preforming method.
Drawings
Fig. 1 is a flowchart of a method for preparing a positive electrode material of a lithium ion battery according to an embodiment of the present invention;
FIG. 2 is a cylindrical Mg-Al co-doped lithium cobaltate sample subjected to secondary cold compaction according to a fourth embodiment of the invention;
FIG. 3 is a scanning electron microscope image of Mg-Al co-doped lithium cobaltate particles prepared at higher cold compaction pressures according to a fourth embodiment of the invention;
Fig. 4 is a scanning electron microscope image of Mg-Al co-doped lithium cobaltate particles prepared according to a fourth embodiment of the invention at a lower cold pressure.
Detailed Description
In order to further describe the technical means and effects adopted by the present invention for achieving the intended purpose, the following detailed description of the present invention is given with reference to the accompanying drawings and preferred embodiments.
In the drawings, the thickness, size and shape of the object have been slightly exaggerated for convenience of explanation. The figures are merely examples and are not drawn to scale.
It will be further understood that the terms "comprises," "comprising," "includes," "including," "having," "containing," and/or "including," when used in this specification, specify the presence of stated features, integers, steps, operations, elements, and/or components, but do not preclude the presence or addition of one or more other features, integers, steps, operations, elements, components, and/or groups thereof. Furthermore, when a statement such as "at least one of the following" appears after a list of features that are listed, the entire listed feature is modified instead of modifying a separate element in the list. Furthermore, when describing embodiments of the present application, the use of "may" means "one or more embodiments of the present application. Also, the term "exemplary" is intended to refer to an example or illustration.
As used herein, the terms "substantially," "about," and the like are used as terms of a table approximation, not as terms of a table level, and are intended to illustrate inherent deviations in measured or calculated values that would be recognized by one of ordinary skill in the art.
Unless otherwise defined, all terms (including technical and scientific terms) used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs. It will be further understood that terms, such as those defined in commonly used dictionaries, should be interpreted as having a meaning that is consistent with their meaning in the context of the relevant art and will not be interpreted in an idealized or overly formal sense unless expressly so defined herein.
It should be noted that, without conflict, the embodiments of the present application and features of the embodiments may be combined with each other. The application will be described in detail below with reference to the drawings in connection with embodiments.
The steps of the method flow described in the specification and the flow chart shown in the drawings of the specification are not necessarily strictly executed according to step numbers, and the execution order of the steps of the method may be changed. Moreover, some steps may be omitted, multiple steps may be combined into one step to be performed, and/or one step may be decomposed into multiple steps to be performed.
In a first embodiment of the present invention, as shown in fig. 1, a method for preparing a positive electrode material of a lithium ion battery includes the following specific steps:
step S1, mixing precursor materials, and cold-pressing the precursor materials to form under a first pressure;
s2, performing first sintering treatment on the current precursor material to obtain Mg-Al co-doped lithium cobaltate;
s3, grinding the Mg-Al co-doped lithium cobalt oxide, and cold-pressing the current Mg-Al co-doped lithium cobalt oxide under a second pressure to form;
And S4, performing second sintering treatment on the Mg-Al co-doped lithium cobaltate after cold press forming to obtain a sample of the positive electrode material of the lithium ion battery.
The method provided in this embodiment will be described in detail in steps.
Step S1, mixing the precursor materials, and cold-pressing the precursor materials at a first pressure to form.
In this embodiment, the precursor material includes: at least four of Li 2CO3、LiOH、Co3O4、Co(OH)2、Al2O3 and MgO.
In this embodiment, the first pressure may have a pressure in the range of 1 MPa to 10 Gpa.
Preferably, the first pressure may have a pressure in the range of 100 MPa to 2.1 GPa.
And S2, performing first sintering treatment on the current precursor material to obtain the Mg-Al co-doped lithium cobaltate.
In this embodiment, the temperature of the first sintering process may be 700-1200 o C.
Preferably, the temperature of the first sintering process may be 800-1100 o C.
And S3, grinding the Mg-Al co-doped lithium cobalt oxide, and cold-pressing and forming the current Mg-Al co-doped lithium cobalt oxide under a second pressure.
In this embodiment, the second pressure is in the pressure range of 1 MPa to 8 GPa.
And S4, performing second sintering treatment on the Mg-Al co-doped lithium cobaltate after cold press forming to obtain a sample of the positive electrode material of the lithium ion battery.
In this embodiment, the temperature of the second sintering process is 800-1200 o C.
It should be noted that, the parameters in the above process may be reasonably changed or appropriately adjusted according to the actual application, which will not be limited herein.
It can be appreciated that by adjusting the first pressure and the second pressure, the size of the Mg-Al co-doped lithium cobaltate particles (i.e., a sample of the positive electrode material of the lithium ion battery) can be effectively controlled.
In a second embodiment of the present invention, corresponding to the first embodiment, this embodiment describes a positive electrode material for a lithium battery, which is prepared by the preparation method described in the first embodiment.
In a third embodiment of the invention, a lithium battery comprises the positive electrode material of the lithium battery as described in the second embodiment.
A fourth embodiment of the present invention is to introduce an application example of the present invention on the basis of the above-described embodiment.
0.67 mmolCo3O4、1 mmolLi2CO3、0.369 mgAl2O3、0.326 mgMgO, Was mixed well in a mortar and subsequently the sample was transferred to a cold press mill, the pressure was slowly increased to 1.77 Gpa and maintained at 5.5 min. Subsequently, the obtained bulk sample was taken out, and as can be seen from fig. 2, the sample diameter after cold press molding was 20 mm. The bulk sample was transferred to a muffle furnace, which was warmed from ambient temperature to 1000 o C at a rate of 2 o C/min, and sample 10 h was sintered at that temperature.
After sintering was completed, the sample was taken out and ground into a powder. The resultant LiCoO2 powder was transferred to a cold press mill, the pressure was slowly increased to 1.77 Gpa, and the pressure was maintained at 5 min. Subsequently, the obtained bulk sample was taken out and transferred to a muffle furnace, which was warmed up from normal temperature to 900 o C at a speed of 2 o C/min, and at which temperature the sample 10 h was sintered. An SEM image of the obtained Mg-Al co-doped lithium cobaltate is shown in FIG. 3. The average particle size was found to be 5.77 microns, with the vast majority of particles being below 10 microns.
The same procedure was used, but the pressure of both cold presses was reduced to 0.374 GPa, and the SEM of the resulting Mg-Al co-doped lithium cobaltate was shown in fig. 4. The average size of the particles was found to be 12.37 microns, with a large range of particle sizes ranging from 5 microns to 20 microns.
A fifth embodiment of the present invention is to introduce an application example of the present invention on the basis of the above-described embodiment.
2 Mmole of Co (OH) 2、1 mmolLi2CO3、0.369 mgAl2O3, 0.326/mgMgO were taken and mixed well in a mortar, after which the sample was transferred to a cold press mill, the pressure was slowly increased to 1.77/Gpa, and the pressure was maintained at 5/min. Subsequently, the obtained bulk sample was taken out, and as can be seen from fig. 2, the sample diameter after cold press molding was 20 mm. The bulk sample was transferred to a muffle furnace, which was warmed from ambient temperature to 1000 o C at a rate of 2 o C/min, and sample 10h was sintered at that temperature.
After sintering was completed, the sample was taken out and ground into a powder. The resultant LiCoO2 powder was transferred to a cold press mill, the pressure was slowly increased to 1.77 Gpa, and the pressure was maintained at 5 min. Subsequently, the obtained bulk sample was taken out and transferred to a muffle furnace, which was warmed up from normal temperature to 900 o C at a speed of 2 o C/min, and at which temperature the sample 10 h was sintered.
A sixth embodiment of the present invention is to introduce an application example of the present invention on the basis of the above-described embodiment.
2 Mmole of Co (OH) 2、2mmolLiOH、0.369 mgAl2O3, 0.326/mgMgO were taken and mixed well in a mortar, after which the sample was transferred to a cold press mill, the pressure was slowly increased to 1.77/Gpa, and the pressure was maintained at 5/min. Subsequently, the obtained bulk sample was taken out, and as can be seen from fig. 2, the sample diameter after cold press molding was 20 mm. The bulk sample was transferred to a muffle furnace, which was warmed from ambient temperature to 1000 o C at a rate of 2 o C/min, and sample 10h was sintered at that temperature.
After sintering was completed, the sample was taken out and ground into a powder. The resultant LiCoO2 powder was transferred to a cold press mill, the pressure was slowly increased to 1.77 Gpa, and the pressure was maintained at 5 min. Subsequently, the obtained bulk sample was taken out and transferred to a muffle furnace, which was warmed up from normal temperature to 900 o C at a speed of 2 o C/min, and at which temperature the sample 10 h was sintered.
A seventh embodiment of the present invention is to introduce an application example of the present invention on the basis of the above-described embodiment.
0.67 MmolCo 3O4、2mmolLiOH、0.369 mgAl2O3, 0.326 and mgMgO were taken and mixed well in a mortar, after which the sample was transferred to a cold press mill, the pressure was slowly increased to 1.77 and Gpa, and maintained at 5 min. Subsequently, the obtained bulk sample was taken out, and as can be seen from fig. 2, the sample diameter after cold press molding was 20 mm. The bulk sample was transferred to a muffle furnace, which was warmed from ambient temperature to 1000 o C at a rate of 2 o C/min, and sample 10h was sintered at that temperature.
After sintering was completed, the sample was taken out and ground into a powder. The resultant LiCoO2 powder was transferred to a cold press mill, the pressure was slowly increased to 1.77 Gpa, and the pressure was maintained at 5 min. Subsequently, the obtained bulk sample was taken out and transferred to a muffle furnace, which was warmed up from normal temperature to 900 o C at a speed of 2 o C/min, and at which temperature the sample 10 h was sintered.
An eighth embodiment of the present invention is to introduce an application example of the present invention on the basis of the above-described embodiment.
0.67 mmolCo3O4、1 mmolLi2CO3、0.369 mgAl2O3、0.326 mgMgO, Was mixed well in a mortar and subsequently the sample was transferred to a cold press mill, the pressure was slowly increased to 1.77 Gpa and maintained at 5.5 min. Subsequently, the obtained bulk sample was taken out, and as can be seen from fig. 2, the sample diameter after cold press molding was 20 mm. The bulk sample was transferred to a muffle furnace, which was warmed from ambient temperature to 1000 o C at a rate of 2 o C/min, and sample 10 h was sintered at that temperature.
After sintering was completed, the sample was taken out and ground into a powder. The resultant LiCoO2 powder was transferred to a cold press mill, slowly increased to a pressure of 0.374 Gpa, and maintained at the pressure of 5 min. Subsequently, the obtained bulk sample was taken out and transferred to a muffle furnace, which was warmed up from normal temperature to 900 o C at a speed of 2 o C/min, and at which temperature the sample 10 h was sintered.
In conclusion, the preparation method of the lithium ion battery anode material provided by the invention realizes the regulation and control of the size distribution of Mg-Al co-doped lithium cobaltate particles by a cold pressing preforming method.
While the invention has been described in connection with specific embodiments thereof, it is to be understood that these drawings are included in the spirit and scope of the invention, it is not to be limited thereto.
Claims (4)
1. The preparation method of the lithium ion battery anode material is characterized by comprising the following steps:
mixing the precursor materials and cold-pressing the precursor materials to form at a first pressure, wherein the pressure of the first pressure ranges from 1.77GPa to 2.1GPa;
performing first sintering treatment on the precursor material to obtain Mg-Al co-doped lithium cobaltate, wherein the temperature of the first sintering treatment is 800-1100 o C; grinding the Mg-Al co-doped lithium cobalt oxide, and cold-pressing the current Mg-Al co-doped lithium cobalt oxide into shape under a second pressure, wherein the pressure of the second pressure ranges from 0.374GPa to 8GPa; and performing second sintering treatment on the Mg-Al co-doped lithium cobaltate after cold press molding to obtain a sample of the positive electrode material of the lithium ion battery, wherein the temperature of the second sintering treatment is 800-1200 o ℃.
2. The method for preparing a positive electrode material for a lithium ion battery according to claim 1, wherein the precursor material comprises: at least four of Li 2CO3、LiOH、Co3O4、Co(OH)2、Al2O3 and MgO.
3. A lithium battery positive electrode material, characterized in that the lithium battery positive electrode material is prepared by the preparation method of the lithium ion battery positive electrode material according to claim 1 or 2.
4. A lithium battery comprising the lithium battery cathode material of claim 3.
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2022
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| CN101219806A (en) * | 2008-01-25 | 2008-07-16 | 南京大学 | Anode material of lithium cell and solid-phase sintering production method at high temperature |
| CN101931073A (en) * | 2009-06-23 | 2010-12-29 | 中国科学院化学研究所 | Preparation method of lithium iron phosphate/carbon composite cathode material |
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