CN101630736A - Improvement method of cycle performance of lithium battery tertiary cathode material - Google Patents
Improvement method of cycle performance of lithium battery tertiary cathode material Download PDFInfo
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- CN101630736A CN101630736A CN200910109331A CN200910109331A CN101630736A CN 101630736 A CN101630736 A CN 101630736A CN 200910109331 A CN200910109331 A CN 200910109331A CN 200910109331 A CN200910109331 A CN 200910109331A CN 101630736 A CN101630736 A CN 101630736A
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- lithium battery
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- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention relates to an improvement method of the cycle performance of a lithium battery tertiary cathode material. The improvement method comprises the following steps: checking: checking and analyzing the lithium battery tertiary cathode material to obtain the content of lithium carbonate; and proportioning reaction: adding titanium dioxide in a proportion of a chemical reaction formula: TiO2+Li2CO3=Li2TiO3+1/2CO2 according to the content of the lithium carbonate, uniformly mixing and sintering so as to obtain a new lithium battery tertiary cathode material containing the Li2TiO3. The corrective method of the cycle performance of the lithium battery tertiary cathode material adds the titanium dioxide in the proportion of the chemical reaction formula of the Li2TiO3 according to the content of the lithium carbonate in the prior lithium battery tertiary cathode material and sinters the titanium dioxide to obtain the lithium battery tertiary cathode material containing the Li2TiO3. Compared with the prior lithium battery tertiary cathode material, the lithium battery tertiary cathode material has better cycle performance.
Description
Technical field
The present invention relates to the lithium battery field, more particularly, relate to improving one's methods of a kind of cycle performance of lithium battery tertiary cathode material.
Background technology
Energy problem is the key issue that is related to whole world sustainable development, seeks and develop the important state basic policy that alternative secondary energy sources are countries in the world.Lithium ion battery is a kind of high-energy battery of getting up of fast development during the last ten years recently, has become the first-selection of secondary energy sources.Compare with other battery, therefore advantage such as lithium ion battery has voltage height, specific energy height, cycle period is long, environmental pollution is little has broad application prospects.
Positive electrode is the important component part of lithium ion battery, also is the highest part of cost in the lithium ion battery.Positive electrode commonly used at present is cobalt acid lithium (LiCoO
2), yet the annual requirement of cobalt acid lithium surpasses 10,000 tons, thus cause the cobalt valency unprecedented soaring, and the cobalt resource shortage has begun to restrict industry development.
New type lithium ion positive electrode-tertiary cathode material nickle cobalt lithium manganate [Li (Ni
xCo
yMn
1-x-y) O
2] be the higher material of a kind of cost performance, its manufacture method is with a certain proportion of nickel salt, manganese salt, cobalt salt mixed dissolution, a certain proportion of dissolution of sodium hydroxide, certain flow and the pH value reaction of salt and alkali control generates precursor then, with the precursor drying, mix with a certain proportion of lithium carbonate, sintering forms.With cobalt acid lithium relatively, ternary material has identical bound voltage, and is good with the compatibility of electrolyte, and fail safe is also better relatively, becomes the focus of anode material for lithium-ion batteries research in recent years, also is the positive electrode that liked by vast electric core producer.In order to make tertiary cathode material have more superiority, along with the development of technology, the cycle performance of ternary material also need continue to improve.
Summary of the invention
The technical problem to be solved in the present invention is, the problem of improving at the performance need of existing lithium battery tertiary cathode material, improving one's methods of a kind of cycle performance of lithium battery tertiary cathode material is provided, cycle performance of lithium battery tertiary cathode material is effectively improved.
The technical solution adopted for the present invention to solve the technical problems is: improving one's methods of a kind of cycle performance of lithium battery tertiary cathode material is provided, comprises the steps:
Detect: lithium battery tertiary cathode material is carried out check and analysis, obtain the content of lithium carbonate;
Proportioning reaction: according to the content of lithium carbonate, according to chemical equation: TiO
2+ Li
2CO
3==Li
2TiO
3+ 1/2CO
2Proportioning add titanium dioxide, obtain containing Li behind the sintering
2TiO
3Lithium battery tertiary cathode material.
In the improving one's methods of cycle performance of lithium battery tertiary cathode material of the present invention, also comprise preparation process before the described detection step: the preparation lithium battery tertiary cathode material.
In the improving one's methods of cycle performance of lithium battery tertiary cathode material of the present invention, in the proportioning reactions steps, described lithium carbonate and titanium dioxide by wet ball grinding batch mixing, drying after, carry out sintering again.
In the improving one's methods of cycle performance of lithium battery tertiary cathode material of the present invention, in the proportioning reactions steps, sintering temperature is less than 900 ℃.
In the improving one's methods of cycle performance of lithium battery tertiary cathode material of the present invention, the percentage composition of described titanium dioxide is less than 1%.
Implement the present invention, have following beneficial effect: according to the content of lithium carbonate in the existing lithium battery tertiary cathode material, according to Li
2TiO
3The proportioning of chemical equation adds titanium dioxide, obtains the new Li that contains behind the sintering
2TiO
3Lithium battery tertiary cathode material, have better cycle performance compared to existing lithium battery tertiary cathode material.
Description of drawings
The invention will be further described below in conjunction with drawings and Examples, in the accompanying drawing:
Fig. 1 is the XRD figure of the existing lithium battery tertiary cathode material among the embodiment 2;
Fig. 2 is the Li that contains among the embodiment 2
2TiO
3The XRD figure of lithium battery tertiary cathode material;
Fig. 3 is the Li that contains among the embodiment 2
4Ti
5O
12The XRD figure of lithium battery tertiary cathode material;
Fig. 4 be among the embodiment 2 three kinds of different finished products at 42～44 ° of peakedness ratios of locating;
Fig. 5 is the cyclic curve figure of three kinds of different finished products among the embodiment 1;
Fig. 6 is the cyclic curve figure of three kinds of different finished products among the embodiment 2;
Fig. 7 is the cyclic curve figure of three kinds of different finished products among the embodiment 3.
Embodiment
Improving one's methods of cycle performance of lithium battery tertiary cathode material of the present invention comprises the steps:
Step 1: prepare existing lithium battery tertiary cathode material, this step can be passed through existing techniques in realizing.
Step 2: existing lithium battery tertiary cathode material is carried out check and analysis, obtain the content of lithium carbonate;
Step 3: the content according to lithium carbonate in the finished product material, add a certain proportion of titanium dioxide according to an amount of chemical equation, obtain the required Li that contains behind the sintering
2TiO
3Lithium battery tertiary cathode material.
An amount of chemical equation is: TiO
2+ Li
2CO
3==Li
2TiO
3+ 1/2CO
2
In this step, if the titanium dioxide that adds is excessive, then may react to generate by excessive chemical equation contains Li
4Ti
5O
12Lithium battery tertiary cathode material.
Excessive chemical equation is: 5TiO
2+ 2Li
2CO
3+ 2O
2==Li
4Ti
5O
12+ 4CO
2
Below come improving one's methods of cycle performance of lithium battery tertiary cathode material of the present invention described and test confirmation by specific embodiment:
Embodiment 1:
Comparative example 1.1: prepare existing lithium battery tertiary cathode material
The adding mol ratio is 0.4: 0.4: 0.2 a nickel, manganese, the sulfate liquor 16L of cobalt (comprises nickelous sulfate 3420g, manganese sulfate 2138g, cobaltous sulfate 1851g, pure water 14.5L) the NaOH 16L with 4mol/L reacts, and regulating mixing speed is 200 commentaries on classics/min, and the salting liquid flow is 10ml/min, regulate the aqueous slkali flow, pH value is remained between the 10-11, carry out the ageing reaction, after reaction finishes, continue to stir half an hour, then slurry is put in the centrifuge, after anhydrating, puts into oven drying then, after drying finishes, weighing 1Kg precursor, the 0.446Kg lithium carbonate mixes in blender, then at 1000 degree sintering 15h, the finished product material that sintering obtains is pulverized, carried out classification after finishing and handle, prepare existing lithium battery tertiary cathode material.
Embodiment 1.2: preparation contains Li
2TiO
3Lithium battery tertiary cathode material
1), the finished product material of the lithium battery tertiary cathode material in the comparative example 1.1 carried out chemical detection after, obtaining lithium carbonate content is about 1400ppm.
2), take by weighing the finished product material 100g in the comparative example 1.1, the content (about 1400ppm) according to lithium carbonate in the finished product material according to an amount of chemical equation, takes by weighing titanium dioxide 0.2g, wet ball grinding batch mixing, drying, 800 degree sintering 4 hours obtain the required Li that contains
2TiO
3Lithium battery tertiary cathode material.
Comparative example 1.3: preparation contains Li
4Ti
5O
12Lithium battery tertiary cathode material
1), take by weighing the finished product material 100g in the comparative example 1.1, the content (about 1400ppm) according to lithium carbonate in the finished product material according to excessive chemical equation, takes by weighing titanium dioxide 0.5g, wet ball grinding batch mixing, drying, 800 degree sintering 4 hours obtain the required Li that contains
4Ti
5O
12Lithium battery tertiary cathode material.
As shown in Figure 5, be the cyclic curve figure of three kinds of different finished products among the embodiment 1, illustrated abscissa is a cycle period, the ordinate in the diagram is a capacity.As can be seen, embodiment 1.2 prepares contains Li from diagram
2TiO
3The cycle performance of lithium battery tertiary cathode material be better than the Li that contains that existing lithium battery tertiary cathode material that comparative example 1.1 prepares and comparative example 1.3 prepare
4Ti
5O
12The cycle performance of lithium battery tertiary cathode material.
Embodiment 2:
Comparative example 2.1: prepare existing lithium battery tertiary cathode material
The adding mol ratio is 0.5: 0.3: 0.2 a nickel, manganese, the sulfate liquor 16L of cobalt (comprises nickelous sulfate 4276g, manganese sulfate 1604g, cobaltous sulfate 1851g, pure water 14.5L) the NaOH 16L with 4mol/L reacts, and regulating mixing speed is 200 commentaries on classics/min, and the salting liquid flow is 10ml/min, regulate the aqueous slkali flow, pH value is remained between the 10-11, carry out the ageing reaction, after reaction finishes, continue to stir half an hour, then slurry is put in the centrifuge, after anhydrating, puts into oven drying then, after drying finishes, weighing 1Kg precursor, the 0.446Kg lithium carbonate mixes in blender, then at 900 degree sintering 15h, the finished product material that sintering obtains is pulverized, carried out classification after finishing and handle, prepare existing lithium battery tertiary cathode material.
Embodiment 2.2: preparation contains Li
2TiO
3Lithium battery tertiary cathode material
1), the finished product material of the lithium battery tertiary cathode material in the comparative example 1.1 carried out chemical detection after, obtaining lithium carbonate content is about 2400ppm.
2), take by weighing the finished product material 100g in the comparative example 1.1, the content (about 2400ppm) according to lithium carbonate in the finished product material according to an amount of chemical equation, takes by weighing titanium dioxide 0.35g, wet ball grinding batch mixing, drying, 800 degree sintering 4 hours obtain the required Li that contains
2TiO
3Lithium battery tertiary cathode material.
Comparative example 2.3: preparation contains Li
4Ti
5O
12Lithium battery tertiary cathode material
1), take by weighing the finished product material 100g in the comparative example 1.1, the content (about 2400ppm) according to lithium carbonate in the finished product material according to excessive chemical equation, takes by weighing titanium dioxide 0.88g, wet ball grinding batch mixing, drying, 800 degree sintering 4 hours obtain the required Li that contains
4Ti
5O
12Lithium battery tertiary cathode material.
As shown in Figure 6, be the cyclic curve figure of three kinds of different finished products among the embodiment 2, illustrated abscissa is a cycle period, the ordinate in the diagram is a capacity.As can be seen, embodiment 2.2 prepares contains Li from diagram
2TiO
3The cycle performance of lithium battery tertiary cathode material be better than the Li that contains that existing lithium battery tertiary cathode material that comparative example 2.1 prepares and comparative example 2.3 prepare
4Ti
5O
12The cycle performance of lithium battery tertiary cathode material.
As Figure 1-3, be the XRD figure of three kinds of different finished products of embodiment 2, XRD figure adopts Japanese Rigaku D/max of science 2550 full-automatic X-ray diffractometers, and testing conditions is: radiographic source: CuK α; Voltage: 40KV; Electric current: 250mA; Sweep speed: 8 °/min; Filtering mode: graphite monochromator.Figure 1 shows that existing lithium battery tertiary cathode material; Figure 2 shows that and contain Li
2TiO
3The XRD figure of lithium battery tertiary cathode material; Figure 3 shows that and contain Li
4Ti
5O
12The XRD figure of lithium battery tertiary cathode material, Fig. 3 and Fig. 1 and Fig. 2 relatively near 43.6 degree, a small peak occurred, amplify as shown in Figure 4, do not have the feature small peak near 31.5 degree, so be the characteristic peak of lithium titanate.The titanium dioxide percentage composition is too low owing to joining according to an amount of chemical equation, so there is not Li among the XRD
2TiO
3Characteristic peak occurs.
Embodiment 3:
Comparative example 3.1: prepare existing lithium battery tertiary cathode material
The adding mol ratio is 0.7: 0.15: 0.15 a nickel, manganese, the sulfate liquor 16L of cobalt (comprises nickelous sulfate 5985g, manganese sulfate 802g, cobaltous sulfate 1388g, pure water 14.5L) the NaOH 16L with 4mol/L reacts, and regulating mixing speed is 200 commentaries on classics/min, and the salting liquid flow is 10ml/min, regulate the aqueous slkali flow, pH value is remained between the 10-11, carry out the ageing reaction, after reaction finishes, continue to stir half an hour, then slurry is put in the centrifuge, after anhydrating, puts into oven drying then, after drying finishes, weighing 1Kg precursor, the 0.446Kg lithium carbonate mixes in blender, then at 800 degree sintering 15h, the finished product material that sintering obtains is pulverized, carried out classification then and handle, prepare existing lithium battery tertiary cathode material.
Embodiment 3.2: preparation contains Li
2TiO
3Lithium battery tertiary cathode material
1), the finished product material of the lithium battery tertiary cathode material in the comparative example 1.1 carried out chemical detection after, obtaining lithium carbonate content is about 6000ppm.
2), take by weighing the finished product material 100g in the comparative example 1.1, the content (about 6000ppm) according to lithium carbonate in the finished product material according to an amount of chemical equation, takes by weighing titanium dioxide 0.6g, wet ball grinding batch mixing, drying, 780 degree sintering 4 hours obtain the required Li that contains
2TiO
3Lithium battery tertiary cathode material.
Comparative example 3.3: preparation contains Li
4Ti
5O
12Lithium battery tertiary cathode material
1), take by weighing the finished product material 100g in the comparative example 1.1, the content (about 6000ppm) according to lithium carbonate in the finished product material according to excessive chemical equation, takes by weighing titanium dioxide 1.5g, wet ball grinding batch mixing, drying, 800 degree sintering 4 hours obtain the required Li that contains
4Ti
5O
12Lithium battery tertiary cathode material.
As shown in Figure 7, be the cyclic curve figure of three kinds of different finished products among the embodiment 3, illustrated abscissa is a cycle period, the ordinate in the diagram is a capacity.As can be seen, embodiment 3.2 prepares contains Li from diagram
2TiO
3The cycle performance of lithium battery tertiary cathode material be better than the Li that contains that existing lithium battery tertiary cathode material that comparative example 3.1 prepares and comparative example 3.3 prepare
4Ti
5O
12The cycle performance of lithium battery tertiary cathode material.
In sum, can know according to Fig. 5-7, the cycle performance of embodiment 1.2 is better than comparative example 1.1, comparative example 1.3, the cycle performance of embodiment 2.2 is better than comparative example 2.1, comparative example 2.3, the cycle performance of embodiment 3.2 is better than comparative example 3.1, comparative example 3.3, thereby draw following conclusion: according to the content of lithium carbonate in the existing lithium battery tertiary cathode material, according to Li
2TiO
3The proportioning of chemical equation adds titanium dioxide, obtains containing Li behind the sintering
2TiO
3Lithium battery tertiary cathode material, contain Li compared to what existing lithium battery tertiary cathode material and titanium dioxide excessive response obtained
4Ti
5O
12Lithium battery tertiary cathode material compare, have better cycle performance.
The above; only for the preferable embodiment of the present invention, but protection scope of the present invention is not limited thereto, and anyly is familiar with those skilled in the art in the technical scope that the present invention discloses; the variation that can expect easily or replacement all should be encompassed within protection scope of the present invention.Therefore, protection scope of the present invention should be as the criterion with the protection range of claim.
Claims (5)
1, improving one's methods of a kind of cycle performance of lithium battery tertiary cathode material is characterized in that, comprises the steps:
Detect: lithium battery tertiary cathode material is carried out check and analysis, obtain the content of lithium carbonate;
Proportioning reaction: according to the content of lithium carbonate, according to chemical equation: TiO
2+ Li
2CO
3==Li
2TiO
3+ 1/2CO
2Proportioning add titanium dioxide, obtain containing Li behind the sintering
2TiO
3Lithium battery tertiary cathode material.
2, improving one's methods of cycle performance of lithium battery tertiary cathode material as claimed in claim 1 is characterized in that, also comprises preparation process before the described detection step: the preparation lithium battery tertiary cathode material.
3, improving one's methods of cycle performance of lithium battery tertiary cathode material as claimed in claim 1 is characterized in that, in the proportioning reactions steps, described lithium carbonate and titanium dioxide carry out sintering after passing through wet ball grinding batch mixing, drying again.
4, improving one's methods of cycle performance of lithium battery tertiary cathode material as claimed in claim 1 is characterized in that, in the proportioning reactions steps, sintering temperature is less than 900 ℃.
5, improving one's methods of cycle performance of lithium battery tertiary cathode material as claimed in claim 1 is characterized in that, the percentage composition of described titanium dioxide is less than 1%.
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| CN112042015A (en) * | 2018-05-04 | 2020-12-04 | 尤米科尔公司 | Ni-based lithium ion secondary battery comprising fluorinated electrolyte |
| CN111178270A (en) * | 2019-12-30 | 2020-05-19 | 上海交通大学 | XRD-based ternary combined material chip structure analysis system and method |
| CN111178270B (en) * | 2019-12-30 | 2023-04-18 | 上海交通大学 | XRD-based ternary combined material chip structure analysis system and method |
| CN113690419A (en) * | 2021-08-25 | 2021-11-23 | 蜂巢能源科技有限公司 | Ternary positive electrode composite material, preparation method thereof and lithium ion battery |
| CN114725357A (en) * | 2022-05-06 | 2022-07-08 | 蜂巢能源科技股份有限公司 | Method for reducing residual sodium content of sodium ion cathode material |
| CN114725357B (en) * | 2022-05-06 | 2024-02-20 | 蜂巢能源科技股份有限公司 | Method for reducing residual sodium content of sodium ion positive electrode material |
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