CN102903898A - Graphite and transitional metallic oxide composite cathode material and preparation method thereof - Google Patents
Graphite and transitional metallic oxide composite cathode material and preparation method thereof Download PDFInfo
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- CN102903898A CN102903898A CN201210398479XA CN201210398479A CN102903898A CN 102903898 A CN102903898 A CN 102903898A CN 201210398479X A CN201210398479X A CN 201210398479XA CN 201210398479 A CN201210398479 A CN 201210398479A CN 102903898 A CN102903898 A CN 102903898A
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Abstract
The invention discloses a graphite and transitional metallic oxide composite cathode material. The technical problem caused by using graphite and transitional metallic oxide as cathode materials of lithium ion batteries is solved. The graphite and transitional metallic oxide composite cathode material is prepared by using graphite and transitional metallic oxide, and the mass ratio of the graphite to the transitional metallic oxide is 3-9: 1-7. The preparation method comprises the following steps of: weighing the graphite and the transitional metallic oxide; sufficiently grinding the graphite and the transitional metallic oxide; uniformly mixing the graphite and the transitional metallic oxide so as to obtain the graphite and transitional metallic oxide composite cathode material; and coating carbon on the surface of the graphite and transitional metallic oxide composite cathode material in the nitrogen atmosphere to obtain a composite cathode material with the surface coated with the carbon. The electrochemical performance of the composite cathode material with the surface coated with the carbon is high. The graphite and transitional metallic oxide composite cathode material has high conductivity; the capacity of the graphite and transitional metallic oxide composite cathode material is higher than that of a graphite cathode material; the rate capability of the graphite and transitional metallic oxide composite cathode material is higher than that of graphite; the change of the size of the transitional metallic oxide in charging and discharging processes can be effectively buffered owing to a loose graphite structure; and the graphite and transitional metallic oxide composite cathode material has good cycle performance and rate capability even if the surface of the graphite and transitional metallic oxide composite cathode material is not coated with the carbon.
Description
Technical field
The present invention relates to a kind of graphite and transition metal oxide composite cathode material and preparation method thereof, belong to technical field of inorganic nonmetallic materials.
Background technology
Graphite has layer structure, and lithium ion easily is combined with carbon atom at interlayer and is formed intercalation compound Li
xC
6(x≤1), thus can repeatedly carry out the embedding of lithium and deviate from, and corresponding theoretical specific capacity is 372mAh/g, is the main flow negative material of present commercial li-ion battery.Graphite is that electron conduction is good as the major advantage of negative material, charge and discharge potential is low, security performance is high, shortcoming is actual capacity lower (being about 300-330mAh/g), high rate performance is relatively poor, the battery of its assembling can not satisfy current actual demand far away, especially the needs of electrokinetic cell.Although graphite is carried out doping vario-property or surface treatment, storing up the lithium ability low is the basic reason that causes its actual capacity to be difficult to improve.In order to satisfy the demand of high-energy power supply, exploration has high power capacity, long-life Novel cathode material for lithium ion battery, to substitute the graphite cathode material of present low capacity, has very important significance.
Transition metal oxide is as lithium ion battery negative material, in charging process, and transition metal oxide and lithium metal reaction and the transition metal that restores; In discharge process, the metallic element that restores again is oxidized to metal oxide and again lithium is restored simultaneously, and Mechanism of electrochemical behaviors of anhydrous can be expressed as:
Transition metal oxide negative material theoretical capacity is higher, generally about 700mAh/g, good rate capability, safe, abundant, cheap, the environmental friendliness of most of transition oxide raw material sources of while, preparation is simple, so transition metal oxide is the negative electrode of power lithium-ion battery material that a class has development potentiality very much.Yet because metal conductive oxide is poor, and change in volume is violent in the charge and discharge process, causes its cycle performance relatively poor, thereby has affected the actual practicality of transition metal oxide in lithium ion battery.At present, although taked the measures such as nanometer, porous, carbon coating to improve the cycle performance of transition metal oxide, but still be difficult to fundamentally overcome the deficiency that its aspect of performance exists.
In conjunction with the Mechanism of electrochemical behaviors of anhydrous of graphite and transition metal oxide, separately performance advantage and weakness, applicant of the present invention has proposed a kind ofly to form the technology that composite negative pole material improves the lithium ion battery negative material chemical property by graphite and transition metal oxide.
Summary of the invention
For above-mentioned prior art, the present invention provides a kind of and has formed the technology that composite negative pole material improves the lithium ion battery negative material chemical property by graphite and transition metal oxide for solving graphite and transition metal oxide as the existing technical problem of lithium ion battery negative material.Graphite and the transition metal oxide composite cathode material of the present invention's preparation have good conductivity, and its capacity is higher than graphite cathode material, and high rate performance also is better than graphite; Fluffy graphite-structure also can effectively cushion the change in volume that transition metal oxide occurs in charge and discharge process; Do not carry out surface bag carbon and can have good cycle performance and high rate performance yet.
The present invention is achieved by the following technical solutions:
A kind of graphite and transition metal oxide composite cathode material, be to be (3～9) by mass ratio: graphite and the transition metal oxide of (1～7) are made.
Described transition metal oxide is the binary oxide of the elements such as Fe, Mn, Co, Ni, Cu, Ti, W, Mo, V, Cr, and the ternary oxide and the multivariant oxide that comprise these elements, such as A
-xB
yO
z, wherein A=Mg, Ca, Na, K, Zn, Fe, Mn, Co, Ni, Cu, Ti, W, Mo, V, Cr etc., B=Fe, Mn, Co, Ni, Cu, Ti, W, Mo, V, Cr, Sn etc. also can be two or more mixtures in these oxides.
Preferably, the mass ratio of graphite and transition metal oxide is (1～4): 1.
The preparation method of described graphite and transition metal oxide composite cathode material is: take by weighing graphite, transition metal oxide, fully grind, mix, namely get composite negative pole material.
Preferably, the particle diameter of described graphite is 0.5～80 μ m.
Preferably, when the particle diameter of described transition metal oxide was 10～200nm, chemical property was better.
Preferably, after graphite and transition metal oxide ground and mixed were even, resulting composite negative pole material carried out material with carbon-coated surface again in nitrogen atmosphere, and the chemical property of the composite negative pole material of the surface that obtains bag carbon is better.
The described concrete grammar that carries out material with carbon-coated surface in nitrogen atmosphere is: after graphite and transition metal oxide ground and mixed are even, add in the aqueous solution of glucose, wherein the mass ratio of glucose and composite negative pole material is (0.2～0.4): 1, the addition of water was to cover the solid union material as good, after mixing, 100～120 ℃ of oven dry, then in nitrogen atmosphere, be heated to 500 ℃～600 ℃, be incubated 5～10 hours, namely get the composite negative pole material of surperficial bag carbon.
The present invention is for solving graphite and transition metal oxide as the existing technical problem of lithium ion battery negative material, in conjunction with the Mechanism of electrochemical behaviors of anhydrous of graphite and transition metal oxide, separately performance advantage and weakness, provide a kind of and formed the technology that composite negative pole material improves the lithium ion battery negative material chemical property by graphite and transition metal oxide.Graphite and the transition metal oxide composite cathode material of the present invention's preparation have good conductivity, and its capacity is higher than graphite cathode material, and high rate performance also is better than graphite; Fluffy graphite-structure also can effectively cushion the change in volume that transition metal oxide occurs in charge and discharge process; Do not carry out surface bag carbon and can have good cycle performance and high rate performance yet.
The invention has the beneficial effects as follows:
1, simple, the easily control of graphite and transition metal oxide composite cathode material preparation process, equipment investment is few, and energy consumption is low, and production efficiency is high.
2, graphite and the transition metal oxide composite cathode material of preparation have good chemical property, and not only capacity is higher than graphite, and high rate performance also is better than graphite.
3, the graphite of preparation can be adjusted according to the different proportionings of the two easily from the actual capacity of transition metal oxide composite cathode material.
4, graphite and the transition metal oxide composite cathode material of preparation do not carry out surface bag carbon and can have good cycle performance and high rate performance yet.
5, preparation graphite and transition metal oxide composite cathode material is to carry out at room temperature the air, and needing protection property atmosphere not can not change the composition and structure of oxide, has guaranteed the stability of graphite and metal oxide composite negative pole material.
Although 6 transition metal oxide negative materials in charge and discharge process larger change in volume can occur, fluffy graphite-structure can play effective cushioning effect.
Description of drawings
Fig. 1 is the x-ray diffraction pattern of carbon coated iron oxide/composite cathode material of silicon/carbon/graphite of making of embodiment 2.
Fig. 2 is the cycle performance of iron oxide/composite cathode material of silicon/carbon/graphite of making of embodiment 1.
Fig. 3 is the cycle performance of the carbon coated graphite that makes of embodiment 2/iron oxide composite negative pole material.
Fig. 4 is the high rate performance of the carbon coated graphite that makes of embodiment 4/iron oxide composite negative pole material.
Embodiment
The present invention is further illustrated below in conjunction with embodiment.
The preparation method is: weigh the iron oxide 0.6g that gets about particle diameter 20nm in the balance, graphite 2.4g about granularity 20 μ m, in mortar, fully grind evenly, get iron oxide/composite cathode material of silicon/carbon/graphite, after mixing with 10 milliliters of the aqueous solution of 0.9g glucose preparation, 105 ℃ of oven dry, then in nitrogen atmosphere, be heated to 500 ℃, be incubated 5 hours, obtain the composite negative pole material of surface bag carbon.
The cycle performance of iron oxide/composite cathode material of silicon/carbon/graphite that present embodiment obtains as shown in Figure 2, recording its capacity that discharges and recharges 85 times under the 0.1C multiplying power is 408.7mAh/g.
Embodiment 2 is by iron oxide and the standby iron oxide/composite cathode material of silicon/carbon/graphite of graphite-made
The preparation method is: weigh the iron oxide 0.9g that gets about particle diameter 20nm in the balance, graphite 2.1g about granularity 20 μ m, in mortar, fully grind evenly, get iron oxide/composite cathode material of silicon/carbon/graphite, after mixing with 10 milliliters of the aqueous solution of 0.9g glucose preparation, 120 ℃ of oven dry, then in nitrogen atmosphere, be heated to 550 ℃, be incubated the composite negative pole material that obtained surface bag carbon in about 5 hours.
The battery of the carbon coated iron oxide that present embodiment obtains/composite cathode material of silicon/carbon/graphite assembling, the cycle performance under the 0.1C multiplying power as shown in Figure 3, the capacity that discharges and recharges 30 times is 497mAh/g.
X-ray diffraction pattern such as Fig. 1 of carbon coated iron oxide/composite cathode material of silicon/carbon/graphite that present embodiment obtains only have two kinds of phases of graphite and iron oxide among the figure, do not have other impurity.
Embodiment 3 is by iron oxide and the standby iron oxide/composite cathode material of silicon/carbon/graphite of graphite-made
The preparation method is: weigh the iron oxide 1.2g that gets about particle diameter 20nm in the balance, graphite 1.8g about granularity 6 μ m, in mortar, fully grind evenly, get iron oxide/composite cathode material of silicon/carbon/graphite, after mixing with 10 milliliters of the aqueous solution of 0.9g glucose preparation, 105 ℃ of oven dry, then in nitrogen atmosphere, be heated to 550 ℃, be incubated 5 hours, obtain the composite negative pole material of surface bag carbon.Battery by this carbon coated iron oxide/composite cathode material of silicon/carbon/graphite assembling, recording its capacity that discharges and recharges 30 times under the 0.1C multiplying power is 483mAh/g, respectively carry out 10 times charge and discharge cycles under the discharge-rate of 0.1C, 0.2C, 0.5C, 1.0C, capacity can reach respectively 481.5,463.4,357.7,287.4mAh g
-1
Embodiment 4 is by iron oxide and the standby iron oxide/composite cathode material of silicon/carbon/graphite of graphite-made
The preparation method is: weigh the iron oxide 1.5g that gets about particle diameter 50nm in the balance, graphite 1.5g about granularity 6 μ m, in mortar, fully grind evenly, get iron oxide/composite cathode material of silicon/carbon/graphite, after mixing with 10 milliliters of the aqueous solution of 0.9g glucose preparation, 110 ℃ of oven dry, then in nitrogen atmosphere, be heated to 600 ℃, be incubated 5 hours, obtain the composite negative pole material of surface bag carbon.By the battery of carbon coated iron oxide/composite cathode material of silicon/carbon/graphite assembling, recording its capacity that discharges and recharges 30 times under the 0.1C multiplying power is 475mAh/g.
High rate performance such as Fig. 4 of carbon coated iron oxide/composite cathode material of silicon/carbon/graphite that present embodiment obtains, respectively carry out 10 times charge and discharge cycles under the discharge-rate of 0.1C, 0.2C, 0.5C, 1.0C, 2.0C, capacity can reach respectively 472.4,464,376,322.4,230mAh g
-1
Embodiment 5 is by manganese oxide and the standby manganese oxide/composite cathode material of silicon/carbon/graphite of graphite-made
The preparation method is: weigh the manganese oxide 1.5g that gets about particle diameter 50nm in the balance, the graphite 1.5g about granularity 20 μ m fully grinds evenly in mortar, and get final product.By the battery of this composite material assembling, the capacity of circulation 55 times is 452mAh/g under the 0.1C multiplying power.
The preparation method is: weigh the cupric oxide 1.5g that gets about particle diameter 30nm in the balance, the graphite 1.5g about granularity 20 μ m fully grinds evenly in mortar, and get final product.By the battery of this composite material assembling, the capacity of circulation 37 times is 472mAh/g under the 0.1C multiplying power.
Embodiment 7 is by cobalt oxide and the standby cobalt oxide/composite cathode material of silicon/carbon/graphite of graphite-made
The preparation method: weigh the cobalt oxide 1.2g that gets about particle diameter 60nm in the balance, the graphite 1.8g about granularity 20 μ m fully grinds evenly in mortar, and get final product.By the battery of this composite material assembling, the capacity of circulation 42 times is 552.4mAh/g under the 0.1C multiplying power.
Although above-mentionedly with accompanying drawing the specific embodiment of the present invention is described in conjunction with the embodiments; but be not limiting the scope of the invention; one of ordinary skill in the art should be understood that; on the basis of technical scheme of the present invention, those skilled in the art do not need to pay various modifications that creative work can make or distortion still in protection scope of the present invention.
Claims (9)
1. a graphite and transition metal oxide composite cathode material, it is characterized in that: be to be (3～9) by mass ratio: graphite and the transition metal oxide of (1～7) are made.
2. a kind of graphite according to claim 1 and transition metal oxide composite cathode material, it is characterized in that: described transition metal oxide is the binary oxide of the elements such as Fe, Mn, Co, Ni, Cu, Ti, W, Mo, V, Cr, and the ternary oxide and the multivariant oxide that comprise these elements, also can be two or more mixture in these oxides.
3. a kind of graphite according to claim 1 and 2 and transition metal oxide composite cathode material is characterized in that: the mass ratio of described graphite and transition metal oxide is (1～4): 1.
4. the preparation method of claim 1 or 2 or 3 described a kind of graphite and transition metal oxide composite cathode material is characterized in that: take by weighing graphite, transition metal oxide, fully grind, mix, namely get composite negative pole material.
5. the preparation method of a kind of graphite according to claim 4 and transition metal oxide composite cathode material, it is characterized in that: the particle diameter of described graphite is 0.5～80 μ m.
6. the preparation method of a kind of graphite according to claim 4 and transition metal oxide composite cathode material, it is characterized in that: the particle diameter of described transition metal oxide is 10～200nm.
7. the preparation method of a kind of graphite according to claim 4 and transition metal oxide composite cathode material, it is characterized in that: after described graphite and transition metal oxide ground and mixed are even, in nitrogen atmosphere, carry out again material with carbon-coated surface, namely obtain the composite negative pole material of surface bag carbon.
8. the preparation method of a kind of graphite according to claim 7 and transition metal oxide composite cathode material, it is characterized in that: the described concrete grammar that carries out material with carbon-coated surface in nitrogen atmosphere is: after graphite and transition metal oxide ground and mixed are even, add in the aqueous solution of glucose, wherein the mass ratio of glucose and composite negative pole material is (0.2～0.4): 1, the addition of water was to cover the solid union material as good, after mixing, 100～120 ℃ of oven dry, then in nitrogen atmosphere, be heated to 500 ℃～600 ℃, be incubated 5～10 hours, namely get the composite negative pole material of surperficial bag carbon.
9. the preparation method of each described a kind of graphite and transition metal oxide composite cathode material according to claim 4～8, it is characterized in that: described transition metal oxide is iron oxide, manganese oxide, cupric oxide or cobalt oxide.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105226242A (en) * | 2014-10-27 | 2016-01-06 | 湖南摩根海容新材料有限责任公司 | A kind of lithium ion battery cathode material and its preparation method |
| CN105591092A (en) * | 2014-11-18 | 2016-05-18 | 中国科学院兰州化学物理研究所 | Ni-Co-Mn composite oxide lithium ion battery anode material, preparation method and application thereof |
| CN105702938A (en) * | 2016-04-15 | 2016-06-22 | 华南师范大学 | Iron-based oxide lithium ion battery negative electrode material and preparation method and application thereof |
| CN105958069A (en) * | 2016-05-27 | 2016-09-21 | 雅安乾润锂电池材料有限公司 | Preparation method of graphite negative electrode material for lithium-ion battery |
| CN106663784A (en) * | 2014-09-01 | 2017-05-10 | 日立汽车***株式会社 | Lithium ion secondary battery |
| CN107017397A (en) * | 2017-06-01 | 2017-08-04 | 湖北工程学院 | Graphite composite material and application thereof, preparation method and lithium ion battery |
| CN109244392A (en) * | 2018-08-23 | 2019-01-18 | 武汉艾特米克超能新材料科技有限公司 | A kind of composite graphite negative electrode material and preparation method thereof and lithium ion battery |
| CN110931757A (en) * | 2019-12-16 | 2020-03-27 | 成都爱敏特新能源技术有限公司 | Graphite composite material and preparation method thereof |
| CN113258042A (en) * | 2021-04-22 | 2021-08-13 | 湖南镕锂新材料科技有限公司 | Graphite negative electrode material and preparation method and application thereof |
| CN113860351A (en) * | 2021-08-23 | 2021-12-31 | 中南大学 | Preparation method and application of CuO-graphite composite material prepared from waste graphite |
| CN114883537A (en) * | 2022-03-31 | 2022-08-09 | 格龙新材料科技(常州)有限公司 | High-capacity fast-charging negative electrode composite material and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106663784A (en) * | 2014-09-01 | 2017-05-10 | 日立汽车***株式会社 | Lithium ion secondary battery |
| US11011743B2 (en) | 2014-09-01 | 2021-05-18 | Vehicle Energy Japan Inc. | Lithium ion secondary battery |
| CN105226242B (en) * | 2014-10-27 | 2017-12-26 | 湖南摩根海容新材料有限责任公司 | A kind of lithium ion battery negative material and preparation method thereof |
| CN105226242A (en) * | 2014-10-27 | 2016-01-06 | 湖南摩根海容新材料有限责任公司 | A kind of lithium ion battery cathode material and its preparation method |
| CN105591092A (en) * | 2014-11-18 | 2016-05-18 | 中国科学院兰州化学物理研究所 | Ni-Co-Mn composite oxide lithium ion battery anode material, preparation method and application thereof |
| CN105702938A (en) * | 2016-04-15 | 2016-06-22 | 华南师范大学 | Iron-based oxide lithium ion battery negative electrode material and preparation method and application thereof |
| CN105958069A (en) * | 2016-05-27 | 2016-09-21 | 雅安乾润锂电池材料有限公司 | Preparation method of graphite negative electrode material for lithium-ion battery |
| CN107017397A (en) * | 2017-06-01 | 2017-08-04 | 湖北工程学院 | Graphite composite material and application thereof, preparation method and lithium ion battery |
| CN109244392A (en) * | 2018-08-23 | 2019-01-18 | 武汉艾特米克超能新材料科技有限公司 | A kind of composite graphite negative electrode material and preparation method thereof and lithium ion battery |
| CN110931757A (en) * | 2019-12-16 | 2020-03-27 | 成都爱敏特新能源技术有限公司 | Graphite composite material and preparation method thereof |
| CN113258042A (en) * | 2021-04-22 | 2021-08-13 | 湖南镕锂新材料科技有限公司 | Graphite negative electrode material and preparation method and application thereof |
| CN113860351A (en) * | 2021-08-23 | 2021-12-31 | 中南大学 | Preparation method and application of CuO-graphite composite material prepared from waste graphite |
| CN114883537A (en) * | 2022-03-31 | 2022-08-09 | 格龙新材料科技(常州)有限公司 | High-capacity fast-charging negative electrode composite material and preparation method thereof |
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