CN103022476A - Preparation method of high-nickel-content anode material for lithium ion battery - Google Patents
Preparation method of high-nickel-content anode material for lithium ion battery Download PDFInfo
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- CN103022476A CN103022476A CN2012105651601A CN201210565160A CN103022476A CN 103022476 A CN103022476 A CN 103022476A CN 2012105651601 A CN2012105651601 A CN 2012105651601A CN 201210565160 A CN201210565160 A CN 201210565160A CN 103022476 A CN103022476 A CN 103022476A
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- 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
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- 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
Abstract
The invention discloses a preparation method of a high-nickel-content anode material for a lithium ion battery. The method comprises the steps of calcining a synthesized high-nickel precursor, supplying non-reducing gas during calcining, obtaining high-valence nickel oxide, mixing high-valence nickel oxide with a lithium source in a wet mixing or dry mixing mode, obtaining a mixture, conducting segmented sintering on the mixture at an oxygen atmosphere, and obtaining the high-nickel-content anode material for the lithium ion battery. The high-nickel-content anode material for the lithium ion battery prepared with the method has the characteristic of high capacity, and also has good cycling stability and processability. The preparation method is high in production automation degree, avoids pollution to the environment, and has a very wide market prospect.
Description
Technical field
The present invention relates to a kind of preparation method of cell positive material, relate in particular to a kind of preparation method of high nickel content anode material for lithium-ion batteries.
Background technology
The energy, resources and environment etc. are the major issues of facing mankind.Along with industrial expansion, the home that the mankind depend on for existence---tellurian resource is day by day exhausted, and energy crisis is day by day serious.Lithium ion battery fast development under the background of protection of the environment and saving non-renewable energy resources has now related to the every field such as daily life, industrial production, military and national defense, Aero-Space.
Along with the progress of science and technology, people are also more and more higher to the requirement of lithium ion battery.On the one hand, people need the lithium rechargeable battery that service time is longer, size is less, weight is lighter, thereby when guaranteeing its fail safe and high energy ratio, can reduce cost again, in order to satisfy the fast development of equipment such as mobile phone, notebook computer, number " gadget ".But, the cobalt of maturation acid lithium, LiMn2O4 and nickel manganese cobalt (532) ternary material are difficult to satisfy its requirement at present, gram volume such as cobalt acid lithium has reached 150mAh/g, the gram volume of nickel manganese cobalt (532) ternary material has also reached 157mAh/g, all near its limiting performance, the possibility that continues its capacity of increase is very little.LiFePO4 not only can produce the problem of intellectual property dispute, and the consistency problem in its manufacturing process is difficult to the bottleneck gone beyond especially.On the other hand, electric automobile has proposed the requirement of the aspects such as high-energy-density, high security, long-life, low cost to lithium ion battery.For this situation, be necessary to develop than more suitable lithium ion anode materials such as LiMn2O4, LiFePO4, nickel manganese cobalt (532) and cobalt acid lithiums, to satisfy the needs of the development such as electric automobile.
High-nickel material is the most possible material that becomes to take as the leading factor anode material for lithium-ion batteries market.Its cost ratio cobalt acid lithium is much lower, but have the capacity characteristic more much higher than above-mentioned positive electrode, and principal component is nickel, other precious metal element content is low, if only replace cobalt acid lithium with it in the application of cobalt acid lithium, just can greatly save material cost and strategic resources cobalt, Social benefit and economic benefit is remarkable.But the high-nickel material synthesis condition is harsh, and not only strict to synthetic atmosphere, the synthesis temperature scope is narrow, is difficult to all obtain having the α-NaFeO of electro-chemical activity when synthetic
2The nickel-base anode material of type layered crystal structure.When synthetic, nickelous is difficult to be oxidized to nickelic and the material that generates stoichiometric proportion, usually all can have a small amount of nickelous to occupy niccolic lattice-site, simultaneously for replenishing charge balance, the nickelous of equivalent also can enter the lithium layer, causes cationic mixing, and capacitance and stability are reduced.Therefore, all difficulties of synthetic high-nickel material have restricted its development speed, up to the present also do not have production and the application of scale.
Summary of the invention
The technical problem to be solved in the present invention is to overcome the deficiencies in the prior art, provide a kind of low for equipment requirements, automaticity is high, the preparation method of simple to operate, environmentally friendly, the high nickel content anode material for lithium-ion batteries that is fit to suitability for industrialized production.
For solving the problems of the technologies described above, the technical scheme that the present invention proposes is a kind of preparation method of high nickel content anode material for lithium-ion batteries, may further comprise the steps:
(1) presoma preliminary treatment: the nickelic presoma that will synthesize (existing method) is calcined, passing into non-reducing gas in the calcination process (generally is dry gas, preferred dry air or oxygen), get the oxide of high price nickel, this step mainly be for presoma is dewatered, removal of impurities and pre-oxidation treatment, make its oxide that generates high price nickel, remove wherein water and other impurity, and each main metal is evenly distributed by High temperature diffusion;
(2) batch mixing: carry out batch mixing with following a or any one mode of b:
A. material by wet type mixing: carry out spray drying after oxide that will high price nickel and lithium source solution (the normally lithium source aqueous solution) are sized mixing, then vacuum treatment (vacuum treated main purpose is dehydration, removal of impurities etc.) gets compound;
B. dry method batch mixing: mix with the oxide of nickel at high price after lithium source vacuum powder processed, get compound;
(3) sintering: compound under oxygen atmosphere (other gases that the pure oxygen atom can be provided and not bring other foreign atoms into all can) is carried out multi-steps sintering, get the high nickel content anode material for lithium-ion batteries.
In the said method, in the oxide of described high price nickel in total metal molar amount and the described lithium source ratio of the mole of lithium be 1: 1.0～1.3.
In the said method, described calcination condition is preferably: temperature is 200 ℃～700 ℃, and the time is 5h～15h.
In the said method, preferred, the pressure during described spray drying in the spray tower is-80kPa～-50kPa, inlet temperature is 300 ℃～400 ℃, outlet temperature is 110 ℃～150 ℃.
In the said method, the granularity of lithium source powder is preferably below 150 μ m in the described dry method batch mixing.
In the said method, preferred, vacuum treated temperature is 50 ℃～300 ℃ in described material by wet type mixing or the dry method batch mixing, and the time is 3h～15h, vacuum degree is-and 100kPa～-50kPa.
In the said method, preferred, described multi-steps sintering comprises once sintered and double sintering, and described once sintered temperature is 350 ℃～650 ℃, and temperature retention time is 3h～15h, and the temperature of described double sintering is 650 ℃～850 ℃, and temperature retention time is 10h～35h.
In the said method, described lithium source is preferably one or more in lithium carbonate, lithium hydroxide, the lithium nitrate.
In the said method, the mole of nickel accounts for the ratio of total metal molar amount in the described nickelic presoma preferred 〉=70%.
Compared with prior art, the invention has the advantages that: the high nickel content anode material for lithium-ion batteries neutral and alkali content of material of the inventive method preparation is low, good processability, tap density is high, stable cycle performance, particularly specific capacity can be up to 180mAh/g～205mAh/g.Preparation method of the present invention is less demanding to synthesis device, and is simple to operate, can realize increasingly automatedly, and waste of raw materials is few, and is environmentally friendly, is fit to very much suitability for industrialized production.
Embodiment
Embodiment 1:
A kind of preparation method of high nickel content anode material for lithium-ion batteries of the present invention may further comprise the steps:
(1) presoma preliminary treatment: 80% the nickel cobalt aluminium hydroxide presoma that nickel content is accounted for total metal molar amount is calcined in the atmosphere Muffle furnace, calcining heat is 550 ℃, duration is 10h, in Muffle furnace, pass into dry air during calcining, after finishing, calcining with the stove cooling, gets the oxide of high price nickel;
(2) material by wet type mixing: the oxide of inciting somebody to action high price nickel mixes with lithium hydroxide aqueous solution sizes mixing, in the oxide of high price nickel in total metal molar amount and the lithium hydroxide ratio of the mole of lithium be 1: 1.03, size mixing and carry out spray drying after finishing, pressure in the spray tower is-60kPa, inlet temperature is 340 ℃, and outlet temperature is 125 ℃, will export the gained material at 180 ℃ of lower vacuum treatment 5h, vacuum degree is-50kPa, gets compound;
(3) sintering: compound is carried out twice sintering under oxygen atmosphere, once sintered is 550 ℃ of lower insulation 10h, and programming rate is 2 ℃/min; Double sintering is 730 ℃ of lower insulation 20h, and programming rate is 4 ℃/min, and products therefrom is rear broken with the stove cooling, namely obtains the high nickel content anode material for lithium-ion batteries.
After testing, the tap density of the high nickel content anode material for lithium-ion batteries of the method for present embodiment preparation is 2.84g/cm
3, this positive electrode processing characteristics is good, and when being made into battery, capacity is 189mAh/g, and 500 all 1C, 2.8V～4.2V charge/discharge capacity conservation rate is 82.5%, and battery performance is good, without disadvantageous changes such as bulging.
Embodiment 2:
A kind of preparation method of high nickel content anode material for lithium-ion batteries of the present invention compares with the step of embodiment 1, and the ratio of the mole of lithium is that other step is all identical 1: 1.08 in total metal molar amount and the lithium hydroxide in the oxide of high price nickel.
After testing, the tap density of the high nickel content anode material for lithium-ion batteries of the method for present embodiment preparation is 2.81g/cm
3, this positive electrode processing characteristics is good, and when being made into battery, capacity is 197mAh/g, and 500 all 1C, 2.8V～4.2V charge/discharge capacity conservation rate is 81.1%, and battery performance is good, without disadvantageous changes such as bulging.
Embodiment 3:
A kind of preparation method of high nickel content anode material for lithium-ion batteries of the present invention may further comprise the steps:
(1) presoma preliminary treatment: identical with the step (1) of embodiment 1;
(2) dry method batch mixing: be that the lithium hydroxide of-150 μ m is at 180 ℃ of lower vacuum treatment 5h with granularity, vacuum degree is-50kPa, then oxide that will high price nickel mixes (in the oxide of high price nickel always in metal molar amount and the lithium hydroxide ratio of the mole of lithium be 1: 1.08) with lithium hydroxide after the vacuum treatment, get compound;
(3) sintering: identical with the step (3) of embodiment 1.
After testing, the tap density of the high nickel content anode material for lithium-ion batteries of the method for present embodiment preparation is 2.90g/cm
3, this positive electrode processing characteristics is good, and when being made into battery, capacity is 202mAh/g, and 500 all 1C, 2.8V～4.2V charge/discharge capacity conservation rate is 81.7%, and battery performance is good, without disadvantageous changes such as bulging.
Embodiment 4:
A kind of preparation method of high nickel content anode material for lithium-ion batteries of the present invention compares with embodiment 3 steps, and calcining heat is 700 ℃ during except the presoma preliminary treatment, and other step is identical.
After testing, the tap density of the high nickel content anode material for lithium-ion batteries of the method for present embodiment preparation is 2.86g/cm
3, this positive electrode processing characteristics is good, and when being made into battery, capacity is 200mAh/g, and 500 all 1C, 2.8V～4.2V charge/discharge capacity conservation rate is 81.3%, and battery performance is good, without disadvantageous changes such as bulging.
Embodiment 5:
A kind of preparation method of high nickel content anode material for lithium-ion batteries of the present invention may further comprise the steps:
(1) presoma preliminary treatment: it is that 80% nickel cobalt manganese hydroxide presoma is calcined in the atmosphere Muffle furnace that nickel content is accounted for total metal molar amount, calcining heat is 450 ℃, duration is 10h, in Muffle furnace, pass into dry air during calcining, after finishing, calcining with the stove cooling, gets the oxide of high price nickel;
(2) dry method batch mixing: identical with the step (2) of embodiment 3;
(3) sintering: identical with the step (3) of embodiment 3.
After testing, the tap density 2.76g/cm of the high nickel content anode material for lithium-ion batteries of the method for present embodiment preparation
3, this positive electrode processing characteristics is good, and when being made into battery, capacity is 192mAh/g, and 500 all 1C, 2.8V～4.2V charge/discharge capacity conservation rate is 80.7%, and battery performance is good, without disadvantageous changes such as bulging.
By above each embodiment as can be known, the high nickel content anode material for lithium-ion batteries of the present invention's preparation has the characteristics of capacity height, good cycling stability and good processability.
The above only is preferred implementation of the present invention, and protection scope of the present invention also not only is confined to above-described embodiment.All technical schemes that belongs under the thinking of the present invention all belong to protection scope of the present invention.Be noted that for those skilled in the art in the improvements and modifications that do not break away under the principle of the invention prerequisite, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (10)
1. the preparation method of a high nickel content anode material for lithium-ion batteries is characterized in that, may further comprise the steps:
(1) presoma preliminary treatment: the nickelic presoma that will synthesize is calcined, and passes into non-reducing gas in the calcination process, gets the oxide of high price nickel;
(2) batch mixing: carry out batch mixing with following a or any one mode of b:
A. material by wet type mixing: carry out spray drying after oxide that will high price nickel and lithium source solution are sized mixing, then vacuum treatment gets compound;
B. dry method batch mixing: mix with the oxide of nickel at high price after lithium source vacuum powder processed, get compound;
(3) sintering: compound is carried out multi-steps sintering under oxygen atmosphere, get the high nickel content anode material for lithium-ion batteries.
2. the preparation method of high nickel content anode material for lithium-ion batteries according to claim 1 is characterized in that, in the oxide of described high price nickel in total metal molar amount and the described lithium source ratio of the mole of lithium be 1: 1.0～1.3.
3. the preparation method of high nickel content anode material for lithium-ion batteries according to claim 1 is characterized in that, described calcination condition is: temperature is 200 ℃～700 ℃, and the time is 5h～15h.
4. the preparation method of high nickel content anode material for lithium-ion batteries according to claim 1, it is characterized in that, pressure during described spray drying in the spray tower is-80kPa～-50kPa, inlet temperature is 300 ℃～400 ℃, outlet temperature is 110 ℃～150 ℃.
5. the preparation method of high nickel content anode material for lithium-ion batteries according to claim 1 is characterized in that, the granularity of lithium source powder is below 150 μ m in the described dry method batch mixing.
6. the preparation method of each described high nickel content anode material for lithium-ion batteries according to claim 1～5, it is characterized in that, vacuum treated temperature is 50 ℃～300 ℃ in described material by wet type mixing or the dry method batch mixing, and the time is 3h～15h, vacuum degree is-and 100kPa～-50kPa.
7. the preparation method of each described high nickel content anode material for lithium-ion batteries according to claim 1～5, it is characterized in that, described multi-steps sintering comprises once sintered and double sintering, described once sintered temperature is 350 ℃～650 ℃, temperature retention time is 3h～15h, the temperature of described double sintering is 650 ℃～850 ℃, and temperature retention time is 10h～35h.
8. the preparation method of each described high nickel content anode material for lithium-ion batteries is characterized in that according to claim 1～5, and described lithium source is one or more in lithium carbonate, lithium hydroxide, the lithium nitrate.
9. the preparation method of each described high nickel content anode material for lithium-ion batteries is characterized in that according to claim 1～5, and the mole of nickel accounts for the ratio of total metal molar amount 〉=70% in the described nickelic presoma.
10. the preparation method of each described high nickel content anode material for lithium-ion batteries is characterized in that according to claim 1～5, and described non-reducing gas comprises dry air or oxygen.
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103825016A (en) * | 2014-02-13 | 2014-05-28 | 宁波金和新材料股份有限公司 | Nickelic cathode material rich in lithium and preparation method thereof |
| CN104157843A (en) * | 2014-07-30 | 2014-11-19 | 深圳市贝特瑞新能源材料股份有限公司 | Positive electrode material of high-nickel lithium ion battery, preparation method of positive electrode material and lithium ion battery comprising positive electrode material |
| CN104157871A (en) * | 2014-08-18 | 2014-11-19 | 宁波金和新材料股份有限公司 | Preparation method of high-capacity lithium battery ternary positive electrode material |
| CN105439088A (en) * | 2015-12-15 | 2016-03-30 | 哈尔滨工业大学 | Spray drying method for purifying LiAlH4 |
| CN105870409A (en) * | 2016-04-08 | 2016-08-17 | 浙江新时代海创锂电科技有限公司 | Preparation method of nickel-cobalt-manganese ternary positive electrode material and lithium-ion battery |
| CN108832121A (en) * | 2018-06-04 | 2018-11-16 | 安徽潜川动力锂电科技有限公司 | A kind of nickelic positive electrode and preparation method thereof |
| CN109019703A (en) * | 2017-05-25 | 2018-12-18 | 宁波工程学院 | A kind of plasma fortified oxidizing roasting method of the nickelic positive electrode of lithium ion battery |
| CN110137488A (en) * | 2019-05-28 | 2019-08-16 | 郑州中科新兴产业技术研究院 | A kind of nickelic positive electrode of secondary lithium batteries and preparation method thereof |
| CN112186171A (en) * | 2019-07-05 | 2021-01-05 | 西北工业大学 | Pre-oxidation method and application of lithium nickelate positive electrode material precursor for lithium ion battery |
| CN112357968A (en) * | 2020-11-09 | 2021-02-12 | 中南大学 | Method for continuously preparing lithium ion battery anode material by shaft furnace |
| CN113060777A (en) * | 2021-04-01 | 2021-07-02 | 南通瑞翔新材料有限公司 | Preparation method of high-compaction ternary single crystal material |
| CN114388747A (en) * | 2020-10-19 | 2022-04-22 | 天津国安盟固利新材料科技股份有限公司 | Nano single crystal ternary material and preparation method thereof |
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| CN103825016A (en) * | 2014-02-13 | 2014-05-28 | 宁波金和新材料股份有限公司 | Nickelic cathode material rich in lithium and preparation method thereof |
| CN103825016B (en) * | 2014-02-13 | 2016-09-07 | 宁波金和锂电材料有限公司 | A kind of rich nickelic positive electrode of lithium and preparation method thereof |
| CN104157843A (en) * | 2014-07-30 | 2014-11-19 | 深圳市贝特瑞新能源材料股份有限公司 | Positive electrode material of high-nickel lithium ion battery, preparation method of positive electrode material and lithium ion battery comprising positive electrode material |
| CN104157843B (en) * | 2014-07-30 | 2018-11-02 | 深圳市贝特瑞新能源材料股份有限公司 | A kind of nickelic anode material for lithium-ion batteries and preparation method thereof and include its lithium ion battery |
| CN104157871A (en) * | 2014-08-18 | 2014-11-19 | 宁波金和新材料股份有限公司 | Preparation method of high-capacity lithium battery ternary positive electrode material |
| CN105439088A (en) * | 2015-12-15 | 2016-03-30 | 哈尔滨工业大学 | Spray drying method for purifying LiAlH4 |
| CN105870409A (en) * | 2016-04-08 | 2016-08-17 | 浙江新时代海创锂电科技有限公司 | Preparation method of nickel-cobalt-manganese ternary positive electrode material and lithium-ion battery |
| CN105870409B (en) * | 2016-04-08 | 2019-06-28 | 浙江美都海创锂电科技有限公司 | A kind of preparation method and lithium ion battery of nickel-cobalt-manganternary ternary anode material |
| CN109019703A (en) * | 2017-05-25 | 2018-12-18 | 宁波工程学院 | A kind of plasma fortified oxidizing roasting method of the nickelic positive electrode of lithium ion battery |
| CN109019703B (en) * | 2017-05-25 | 2020-11-06 | 宁波工程学院 | Plasma enhanced oxidation roasting method for high-nickel cathode material of lithium ion battery |
| CN108832121A (en) * | 2018-06-04 | 2018-11-16 | 安徽潜川动力锂电科技有限公司 | A kind of nickelic positive electrode and preparation method thereof |
| CN108832121B (en) * | 2018-06-04 | 2020-12-04 | 安徽潜川动力锂电科技有限公司 | High-nickel positive electrode material and preparation method thereof |
| CN110137488A (en) * | 2019-05-28 | 2019-08-16 | 郑州中科新兴产业技术研究院 | A kind of nickelic positive electrode of secondary lithium batteries and preparation method thereof |
| CN112186171A (en) * | 2019-07-05 | 2021-01-05 | 西北工业大学 | Pre-oxidation method and application of lithium nickelate positive electrode material precursor for lithium ion battery |
| CN114388747A (en) * | 2020-10-19 | 2022-04-22 | 天津国安盟固利新材料科技股份有限公司 | Nano single crystal ternary material and preparation method thereof |
| CN112357968A (en) * | 2020-11-09 | 2021-02-12 | 中南大学 | Method for continuously preparing lithium ion battery anode material by shaft furnace |
| CN113060777A (en) * | 2021-04-01 | 2021-07-02 | 南通瑞翔新材料有限公司 | Preparation method of high-compaction ternary single crystal material |
| CN113060777B (en) * | 2021-04-01 | 2023-05-02 | 南通瑞翔新材料有限公司 | Preparation method of high-compaction ternary monocrystal material |
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