CN103137974A - Lithium ion battery anode active material, preparation method of the lithium ion battery anode active material, and lithium ion battery - Google Patents
Lithium ion battery anode active material, preparation method of the lithium ion battery anode active material, and lithium ion battery Download PDFInfo
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- CN103137974A CN103137974A CN201110378050XA CN201110378050A CN103137974A CN 103137974 A CN103137974 A CN 103137974A CN 201110378050X A CN201110378050X A CN 201110378050XA CN 201110378050 A CN201110378050 A CN 201110378050A CN 103137974 A CN103137974 A CN 103137974A
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Abstract
The invention provides a lithium ion battery anode active material, a preparation method of the lithium ion battery anode active material, and a lithium ion battery. The lithium ion battery anode active material is a lithium hydroxy group-containing carbon material subjected to surface modification, has small internal resistance, can fast discharge at a large electric current, improves a lithium ion battery rate capability, and can satisfy development demands of large-power electronic apparatuses such as a hybrid car and various roll boosters. The preparation method comprises the following steps that a carbon material and an oxidizing agent are mixed and then undergo a reaction in an oil bath pan at a temperature of 80 to 140 DEG C for 0.5 to 5 hours to produce an oxidized carbon material; and the oxidized carbon material and a lithium salt are mixed and then are dried to form the lithium hydroxy group-containing carbon material subjected to surface modification. The preparation method is simple, can be operated easily and is suitable for industrial production. The lithium ion battery has a high rate capability and utilizes the lithium hydroxy group-containing carbon material subjected to surface modification as the lithium ion battery anode active material.
Description
Technical field
The present invention relates to electrochemical field, relate in particular to anode active material of lithium ion battery and preparation method thereof and high multiplying power lithium ion battery and lithium ion battery.
Background technology
Lithium ion battery has been widely used in the small-power electronic utensils such as mobile phone, notebook computer, video camera and digital camera because having the advantages such as high-energy-density.Development along with hybrid electric vehicle and various boost motors etc., the appearance of various great-power electronic utensils is had higher requirement to the battery product performance, namely the lithium ion battery as great-power electronic utensil power supply is required to have high-rate charge-discharge capability, needed current value in the time of can charging and discharging at short notice its rated capacity (equal the multiple of battery rated capacity on data value, usually represent with letter C).High multiplying power lithium ion battery even is required sometimes can be at the above multiplying power discharging of 10C.But the commodity lithium ion battery of general conventional design can only be emitted 80% left and right of its nominal capacity when the 2C multiplying power discharging, and at all can not be at the 10C multiplying power discharging.Therefore, a kind of energy of exploitation seems very important for the high multiplying power lithium ion battery of above-mentioned great-power electronic utensil.
Lithium ion battery is by positive plate, negative plate, electrolyte and prevent that between between positive/negative plate the barrier film of its short circuit from forming, and passes through Li
+Embed and deviate from the positive and negative electrode material and carry out energy exchange.The charge-discharge magnification of lithium ion battery is relevant with the positive and negative pole material of battery and preparation technology.The positive electrode active materials of conventional lithium ion battery (for example, LiFePO4 and cobalt acid lithium etc.) be lithium is stored in positive electrode body mutually in, Li
+Need to be inner to positive electrode through the positive electrode bulk diffusion from positive electrode surface, cause internal resistance excessive, thereby required to discharge and recharge the time longer.
Summary of the invention
For addressing the above problem, the present invention aims to provide a kind of anode active material of lithium ion battery and its preparation method and application.This anode active material of lithium ion battery internal resistance is less, can repid discharge under large electric current, thus satisfy the growth requirement of the great-power electronic utensils such as hybrid electric vehicle and various boost motors.The preparation method of this anode active material of lithium ion battery is simple, is suitable for suitability for industrialized production.The present invention aims to provide the application of above-mentioned anode active material of lithium ion battery in the high multiplying power lithium ion battery preparation simultaneously.
First aspect the invention provides a kind of anode active material of lithium ion battery, and described positive electrode active materials is that the surface is through including the material with carbon element of hydroxyl lithium after modifying.
Preferably, material with carbon element is selected from one or more in active carbon, carbon aerogels, carbon nano-tube, Graphene and carbon fiber, and specific area is 100～3000m
2/ g.
Li in this anode active material of lithium ion battery
+Be stored in the surface of material with carbon element, the activity of materials site is all on the surface, Li
+Not need to from the diffusion into the surface to the material bodies mutually inside react, thereby shortened the time of discharging and recharging.Anode active material of lithium ion battery internal resistance of the present invention is less, can repid discharge under large electric current, improved the doubly forthright of lithium ion battery, and can satisfy the growth requirement of the great-power electronic utensils such as hybrid electric vehicle and various boost motors.
Second aspect, the invention provides a kind of preparation method of anode active material of lithium ion battery, comprise the following steps: material with carbon element is mixed with oxidant, react 0.5～5h at 80～140 ℃ of temperature in oil bath pan, obtain the material with carbon element after oxidation, the material with carbon element after oxidation is mixed with lithium salts, drying obtains the surface and include the material with carbon element of hydroxyl lithium as anode active material of lithium ion battery after modifying again.
Preferably, material with carbon element is selected from one or more in active carbon, carbon aerogels, carbon nano-tube, Graphene and carbon fiber, and specific area is 100～3000m
2/ g.
Preferably, oxidant is selected from the solution that 68% nitric acid, 68% nitric acid and 98% sulfuric acid mixes by 1: 3 volume ratio, a kind of (by the mass fraction) in 20% liquor potassic permanganate.Preferably, the consumption of oxidant is the oxidizing agent solution that the 1g material with carbon element adds 20～80ml.
Preferably, the temperature of reacting in oil bath pan is 80～100 ℃, and the reaction time is 3～5 hours.
The result of oxidation also makes carbon-carbon double bond be oxidized to the oxygen-containing functional groups such as hydroxyl, carbonyl, and the carbon material surface after oxidation contains a large amount of polar groups, and the good hydrophily of material with carbon element, adsorptivity and ion exchangeable are given in the existence of a large amount of oxy radicals.
Material with carbon element after oxidation mixes with lithium salts, drying.Preferably, the mass ratio of the material with carbon element after oxidation and lithium salts is 1: 2.Preferably, the material with carbon element after oxidation with after excessive lithium salts mixes 80 ℃ of vacuumizes.In this process, the hydroxyl Li of carbon material surface
+Be connected to the surface of material with carbon element.The surface of material with carbon element includes a large amount of hydroxyl lithiums after modifying, be the material with carbon element that the surface includes the hydroxyl lithium.
Preferably, lithium salts is selected from one or more in lithium hydroxide, lithium carbonate and lithium acetate.
The preparation method of this anode active material of lithium ion battery passes through Li
+Be stored in the surface of active material, the activity of materials site is all on the surface, Li
+Not need to from the diffusion into the surface to the material bodies mutually inside react, thereby shortened the time of discharging and recharging.This preparation method is simple, is suitable for suitability for industrialized production.
The third aspect the invention provides a kind of lithium ion battery, and anode active material of lithium ion battery is that the surface is through including the material with carbon element of hydroxyl lithium after modifying.
Lithium ion battery of the present invention comprises positive plate, negative plate, the barrier film between positive plate and negative plate and electrolyte, and wherein, the active material that is coated with on positive plate is that the surface is through including the material with carbon element of hydroxyl lithium after modifying.
Negative plate is conventional negative plate.Negative active core-shell material adopts can embed Li
+Active material.Preferably, negative active core-shell material is selected from one or more in commercial graphite, silicon-carbon cathode, Graphene, soft charcoal and hard charcoal.
Preferably, electrolyte is for being dissolved with LiPF
6Solution Deng aprotic organic solvent.
The high multiplying power lithium ion battery assembling mode is according to the lithium ion battery assembling mode assembling of routine.
The present invention has following beneficial effect:
(1) anode active material of lithium ion battery internal resistance of the present invention is less, can repid discharge under large electric current, improved the doubly forthright of lithium ion battery, and can satisfy the growth requirement of the great-power electronic utensils such as hybrid electric vehicle and various boost motors;
(2) preparation method of anode active material of lithium ion battery of the present invention is simple, is suitable for suitability for industrialized production;
(3) lithium ion battery of the present invention has high-rate discharge capacity.
Description of drawings
Fig. 1 is the SEM Electronic Speculum picture of anode active material of lithium ion battery.
Embodiment
The following stated is the preferred embodiment of the present invention; should be pointed out that for those skilled in the art, under the prerequisite that does not break away from the principle of the invention; can also make some improvements and modifications, these improvements and modifications also are considered as protection scope of the present invention.
Embodiment one
A kind of preparation method of anode active material of lithium ion battery comprises the following steps: (Graphene, specific area are 3000m with the 10g material with carbon element
2/ g) mix with 150ml oxidant (68% nitric acid), react 5h at 80 ℃ of temperature in oil bath pan, obtain the material with carbon element (graphene oxide) after oxidation, again the material with carbon element after the 10g oxidation (graphene oxide) is mixed with 20g lithium salts (lithium hydroxide), drying obtains the surface and includes the Graphene of hydroxyl lithium as anode active material of lithium ion battery.
Embodiment two
A kind of preparation method of anode active material of lithium ion battery comprises the following steps: (Graphene, specific area are 2000m with 10 material with carbon elements
2/ g) mix with 100ml oxidant (solution that 68% nitric acid and 98% sulfuric acid mix by 1: 3 volume ratio), react 3h at 110 ℃ of temperature in oil bath pan, obtain the material with carbon element (graphene oxide) after oxidation, again the material with carbon element after the 20g oxidation (graphene oxide) is mixed with 40g lithium salts (lithium carbonate), drying obtains the surface and includes the Graphene of hydroxyl lithium as anode active material of lithium ion battery.Fig. 1 is the SEM Electronic Speculum picture of the present embodiment anode active material of lithium ion battery.
Embodiment three
A kind of preparation method of anode active material of lithium ion battery comprises the following steps: (Graphene, specific area are 100m with the 10g material with carbon element
2/ g) mix with 200ml oxidant (20% liquor potassic permanganate), react 0.5h at 140 ℃ of temperature in oil bath pan, obtain the material with carbon element (graphene oxide) after oxidation, again the material with carbon element after the 30g oxidation (graphene oxide) is mixed with 60 lithium salts (lithium acetate), drying obtains the surface and includes the Graphene of hydroxyl lithium as anode active material of lithium ion battery.
Embodiment four
A kind of preparation method of anode active material of lithium ion battery comprises the following steps: (active carbon, specific area are 1000m with 10 material with carbon elements
2/ g) mix with 180ml oxidant (68% nitric acid), react 2h at 120 ℃ of temperature in oil bath pan, obtain the material with carbon element after oxidation, again the material with carbon element after the 15g oxidation is mixed with 30g lithium salts (lithium carbonate), drying obtains the surface and includes the active carbon of hydroxyl lithium as anode active material of lithium ion battery.
Embodiment five
A kind of preparation method of anode active material of lithium ion battery comprises the following steps: (carbon aerogels, specific area are 100m with the 10g material with carbon element
2/ g) mix with 120ml oxidant (68% nitric acid), react 0.5h at 140 ℃ of temperature in oil bath pan, obtain the material with carbon element after oxidation, again the material with carbon element after the 25g oxidation is mixed with 50g lithium salts (lithium acetate), drying obtains the surface and includes the carbon aerogels of hydroxyl lithium as anode active material of lithium ion battery.
Embodiment six
A kind of preparation method of anode active material of lithium ion battery comprises the following steps: (carbon nano-tube, specific area are 500m with the 10g material with carbon element
2/ g) mix with 130ml oxidant (solution that 68% nitric acid and 98% sulfuric acid mix by 1: 3 volume ratio), react 3h at 100 ℃ of temperature in oil bath pan, obtain the material with carbon element after oxidation, again the material with carbon element after the 20g oxidation is mixed with 40g lithium salts (lithium carbonate), drying obtains the surface and includes the carbon nano-tube of hydroxyl lithium as anode active material of lithium ion battery.
Embodiment seven
A kind of preparation method of anode active material of lithium ion battery comprises the following steps: (carbon fiber, specific area are 300m with the 10g material with carbon element
2/ g) mix with 190ml oxidant (20% liquor potassic permanganate), react 1h at 120 ℃ of temperature in oil bath pan, obtain the material with carbon element after oxidation, again the material with carbon element after the 10g oxidation is mixed with 20g lithium salts (lithium acetate), drying obtains the surface and includes the carbon fiber of hydroxyl lithium as anode active material of lithium ion battery.
Embodiment eight
A kind of high multiplying power lithium ion battery comprises positive plate, negative plate, the barrier film between positive plate and negative plate and electrolyte, and wherein, the active material that is coated with on positive plate includes the Graphene of hydroxyl lithium for the surface.
Positive electrode active materials and binding agent (Kynoar PVDF), conductive agent (conductive black Super P) are done in mass ratio form slurry and are coated on aluminium foil as anodal at 85: 5: 10; Negative active core-shell material is done in mass ratio form slurry with graphite and binding agent (Kynoar PVDF), conductive agent (conductive black Super P) and is coated on Copper Foil as negative pole at 85: 5: 10, through super-dry, roll film, cut and be made into high multiplying power lithium ion battery positive plate and negative plate.Positive plate, negative plate and barrier film are assembled by the mode of lamination, inject electrolyte, obtain high multiplying power lithium ion battery after sealing.
Embodiment nine～12
A kind of high multiplying power lithium ion battery, comprise positive plate, negative plate, the barrier film between positive plate and negative plate and electrolyte, its assemble method is with embodiment eight, difference only is that the active material that is coated with on positive plate is different, and positive electrode active materials is respectively the surface and includes the active carbon (embodiment nine) of hydroxyl lithium, the carbon aerogels (embodiment ten) that the surface includes the hydroxyl lithium, carbon nano-tube (embodiment 11) and the surperficial carbon fiber (embodiment 12) that includes the hydroxyl lithium that the surface includes the hydroxyl lithium.
Effect embodiment
For beneficial effect of the present invention is verified explanation, provide test experience data such as following table 1.
The doubly forthright experiment of table 1. embodiment eight～12
Table 1 is the doubly forthright experiment of embodiment eight～12, carries out under the constant current of 1C, 5C, 20C, 50C respectively, and under each multiplying power, volume percent is take 1C as 100% standard.Experimental data shows: this kind material can discharge under the multiplying power of 50C, has well doubly forthright.
To sum up, anode active material of lithium ion battery internal resistance of the present invention is less, can repid discharge under large electric current, improved the doubly forthright of lithium ion battery, and can satisfy the growth requirement of the great-power electronic utensils such as hybrid electric vehicle and various boost motors; The preparation method is simple, is suitable for suitability for industrialized production; High multiplying power lithium ion battery has high-rate discharge capacity.
Claims (10)
1. an anode active material of lithium ion battery, is characterized in that, described positive electrode active materials is that the surface is through including the material with carbon element of hydroxyl lithium after modifying.
2. positive electrode active materials as claimed in claim 1, is characterized in that, described material with carbon element is selected from one or more in active carbon, carbon aerogels, carbon nano-tube, Graphene and carbon fiber, and specific area is 100～3000m
2/ g.
3. the preparation method of an anode active material of lithium ion battery, it is characterized in that, comprise the following steps: material with carbon element is mixed with oxidant, react 0.5～5h at 80～140 ℃ of temperature in oil bath pan, obtain the material with carbon element after oxidation, the material with carbon element after oxidation is mixed with lithium salts, drying obtains the surface and include the material with carbon element of hydroxyl lithium as anode active material of lithium ion battery after modifying again.
4. preparation method as claimed in claim 3, is characterized in that, described material with carbon element is selected from one or more in active carbon, carbon aerogels, carbon nano-tube, Graphene and carbon fiber, and specific area is 100～3000m
2/ g.
5. preparation method as claimed in claim 3, is characterized in that, a kind of in the described oxidant solution that to be 68% nitric acid, 68% nitric acid mix by 1: 3～5 volume ratios with 98% sulfuric acid, 20% liquor potassic permanganate.
6. preparation method as claimed in claim 3, is characterized in that, the consumption of described oxidant is the oxidizing agent solution that the 1g material with carbon element adds 20～80ml.
7. preparation method as claimed in claim 3, is characterized in that, described temperature of reacting in oil bath pan is 80～100 ℃, and the reaction time is 3～5 hours.
8. preparation method as claimed in claim 3, is characterized in that, described lithium salts is selected from one or more in lithium hydroxide, lithium carbonate and lithium acetate.
9. preparation method as claimed in claim 3, is characterized in that, the material with carbon element after described oxidation mixes rear 80 ℃ of vacuumizes with lithium salts.
10. a lithium ion battery, is characterized in that, described anode active material of lithium ion battery is that the surface is through including the material with carbon element of hydroxyl lithium after modifying.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107108225A (en) * | 2014-10-10 | 2017-08-29 | 东丽株式会社 | Graphene powder, lithium ion battery are with electrode paste and lithium ion battery electrode |
| CN108550848A (en) * | 2018-04-20 | 2018-09-18 | 苏州缘聚新材料技术服务合伙企业（有限合伙） | Rich lithium carbon material, preparation method and application |
| CN109786127A (en) * | 2018-12-26 | 2019-05-21 | 中国电子科技集团公司第十八研究所 | Modification method of graphene-based lithium ion capacitor positive electrode material |
| CN115070056A (en) * | 2022-06-24 | 2022-09-20 | 哈尔滨工程大学 | Method for uniformly growing superfine aluminum nanocrystals on surface of carbon fiber |
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| CN102201275A (en) * | 2010-03-25 | 2011-09-28 | 海洋王照明科技股份有限公司 | Lithium salt and graphene composite material as well as preparation method and application thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107108225A (en) * | 2014-10-10 | 2017-08-29 | 东丽株式会社 | Graphene powder, lithium ion battery are with electrode paste and lithium ion battery electrode |
| CN108550848A (en) * | 2018-04-20 | 2018-09-18 | 苏州缘聚新材料技术服务合伙企业（有限合伙） | Rich lithium carbon material, preparation method and application |
| CN109786127A (en) * | 2018-12-26 | 2019-05-21 | 中国电子科技集团公司第十八研究所 | Modification method of graphene-based lithium ion capacitor positive electrode material |
| CN115070056A (en) * | 2022-06-24 | 2022-09-20 | 哈尔滨工程大学 | Method for uniformly growing superfine aluminum nanocrystals on surface of carbon fiber |
| CN115070056B (en) * | 2022-06-24 | 2024-03-19 | 哈尔滨工程大学 | Method for uniformly growing ultrafine aluminum nanocrystalline on carbon fiber surface |
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Application publication date: 20130605 |