CN103151517B - Preparation method of lithium cobalt oxide - Google Patents
Preparation method of lithium cobalt oxide Download PDFInfo
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- CN103151517B CN103151517B CN201310023936.1A CN201310023936A CN103151517B CN 103151517 B CN103151517 B CN 103151517B CN 201310023936 A CN201310023936 A CN 201310023936A CN 103151517 B CN103151517 B CN 103151517B
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Abstract
The invention discloses a preparation method of lithium cobalt oxide. The preparation method of the lithium cobalt oxide solves the problems that an existing preparation method of the lithium cobalt oxide is high in temperature, the lithium cobalt oxide obtained through the existing preparation method is uneven in particle, the agglomeration phenomenon exists, the high temperature process causes uneven content of cobalt and lithium in materials and leads to the lithium element to be separated out. The preparation method of the lithium cobalt oxide includes the following steps of weighting out a certain amount of lithium salt, measuring water-solubility organics based on the molar weight of the lithium salt according to the ratio that the total molar weight of the water-solubility organics is 50%-70% of the molar weight of the lithium salt, mixing the water-solubility organics and the lithium salt, adding water to mixture, conducting ball-milling, obtaining pre-reaction slurry, adding materials with cobalt and water to the pre-reaction slurry wherein the molar ratio of the lithium to the cobalt is 0.95-1.2: 1, conducting the ball-milling, obtaining reaction slurry, drying the reaction slurry, calcining the slurry, and obtaining the lithium cobalt oxide. The preparation method of the lithium cobalt oxide has the advantages that the lithium cobalt oxide obtained through the preparation method is good in evenness, small in crystal particle, even in particle size, and less in agglomeration. In addition, the preparation method of the lithium cobalt oxide has the advantages of being simple in technology process, appropriate for large batch production, low in calcination temperature and the like.
Description
Technical field
The present invention relates to anode material for lithium-ion batteries technical field, especially relate to the preparation method of a kind of cobalt acid lithium.
Background technology
In current commercial anode material for lithium-ion batteries, cobalt acid lithium (LiCoO
2) due to chemical property comparatively stable, good cycle, voltage platform is higher, good with the compatibility of electrolyte, and the compacted density of positive pole diaphragm of its composition can reach 4.1g/cm
3, and do not affect battery performance and by the positive active material widely as lithium ion battery.
Cobalt acid lithium batch preparation traditional at present adopts the simple high temperature solid-state technique of technique, diffuses to form LiCoO by material under high temperature
2crystal, the temperature of needs is high, and the particle diameter of product is large, and particle is uneven and have agglomeration, and the electrical property of product also affects by the pattern of material, and electrical property and the lot stability of material all have much room for improvement.
Such as, publication number CN1412121A, the Chinese patent in publication date on April 23rd, 2003, disclose the preparation method of a kind of anode active material of lithium ion battery cobalt acid lithium, the method is the raw material heat treatment stage by stage lithium, cobalt stoichiometrically mixed, the water washing of cobalt acid lithium containing precipitation reagent after crushing and screening, the solid phase after Separation of Solid and Liquid obtains required sample after drying.The method mainly reduces the alkalescence of cobalt acid lithium to improve the processing characteristics of cobalt acid lithium, but the method is still diffuse to form LiCoO by material under high temperature
2crystal, the temperatures as high more than 800 DEG C needed, not only energy consumption is high, the particle diameter obtaining product is large, particle is uneven, and having agglomeration, the electrical property of product is poor, simultaneously, because heat treated temperature is higher, high temperature sintering causes liquid lithium carbonate to be easily gathered in material top, makes material there is lamination, causes cobalt, middle level that lithium concentrates on material, and the upper and lower layer cobalt of material, lithium content are few, therefore the cobalt acid lithium uniformity obtained and poor electrical performance, high temperature also may cause the precipitation of elemental lithium, reduces the electrical property of cobalt acid lithium further.
Summary of the invention
The present invention is that the cobalt acid lithium preparation method temperature in order to solve prior art is high, the particle diameter obtaining cobalt acid lithium is large, particle is uneven, and have agglomeration, and in pyroprocess, easily cause cobalt in material, problem that lithium content skewness even causes elemental lithium to be separated out, provide a kind of processing step simple, preparation temperature is low, obtained cobalt acid lithium particle diameter is little, uniform particles, can effectively avoid cobalt in preparation process, lithium content skewness and elemental lithium to separate out the preparation method of the cobalt acid lithium of phenomenon, the cobalt acid lithium cyclical stability obtained by the method is good.
To achieve these goals, the present invention is by the following technical solutions:
A preparation method for cobalt acid lithium, comprises the following steps:
(1) taking a certain amount of lithium salts, with lithium salts integral molar quantity for benchmark, is that lithium salts rubs the ratio metering water soluble organic substance of your amount 50 ~ 70% total in water soluble organic substance integral molar quantity.Lithium salts integral molar quantity and water soluble organic substance integral molar quantity all refer to the mole sum of wherein each material here, be added and obtain after namely calculating respective mole according to the quality of each material and the molal weight of correspondence.
(2) after being mixed with lithium salts by water soluble organic substance, be incorporated as the water of water soluble organic substance gross mass 10 ~ 20%, with the rotating speed ball milling 2 ~ 5h of 100 ~ 300rpm, obtain pre-reaction slurry.Ball milling speed when preparing pre-reaction slurry in the present invention is 100 ~ 300rpm, and Ball-milling Time is 2 ~ 5h, to make soluble organism and lithium salts energy Quick uniform disperse.
(3) in pre-reaction slurry, add cobalt-containing materials and the water for water soluble organic substance gross mass 30 ~ 50%, wherein, the mol ratio of Li:Co is 0.95 ~ 1.2:1, to obtain reaction paste after the rotating speed ball milling 6 ~ 12h of 50 ~ 80rpm.The particle diameter of cobalt-containing materials is larger, after adding cobalt-containing materials in pre-reaction slurry, each component can be reunited, rotational speed of ball-mill reduces, Ball-milling Time extends, fully to open the particle of reunion, make each component dispersed, form the little and uniform particle of particle diameter, so last obtained cobalt acid lithium granularity thinner evenly, reunite few, be conducive to the raising of electrical property, simultaneously, utilize the energy that ball milling produces, water soluble organic substance can with lithium salts, cobalt-containing materials generation complexing, make lithium ion and cobalt ions can remain dispersed, in roasting process, in material, each component can remain and be uniformly distributed, lamination can not be caused, and water soluble organic substance also can avoid the precipitation of elemental lithium, the cobalt acid lithium component finally obtained is stablized, homogeneous, the electrical property of cobalt acid lithium is good, in addition, water soluble organic substance can also reduce the one-tenth phase difficulty of product cobalt acid lithium greatly, thus be greatly lowered into phase temperature, namely sintering temperature, reduce energy consumption, in addition, water soluble organic substance can play sterically hindered effect in heat treatment process, not only effectively can prevent the precipitation of elemental lithium, and the excessive grain growth of cobalt acid lithium can also be inhibit, reduce the generation of product agglomeration, make the cobalt acid lithium grain after last sintering little, epigranular, reunite few.
(4) reaction paste is dried.
(5) by the reaction paste roasting under air atmosphere after oven dry, cobalt acid lithium is obtained.
As preferably, lithium salts is one or both in lithium carbonate, lithium hydroxide.Lithium salts also can be lithium oxalate, lithium acetate etc., preferred lithium carbonate, lithium hydroxide, obtains that cobalt acid lithium productive rate is high and purity good.
As preferably, described water soluble organic substance is one or more in citric acid, glucose, sucrose, acrylic acid, oxalic acid and ascorbic acid.
As preferably, cobalt-containing materials is one or more in cobalt carbonate, cobalt oxide, cobalt acetate.Cobalt-containing materials also can be the cobalt-containing materials such as cobalt oxalate, three cobalt oxides or cobaltosic oxide, preferred cobalt carbonate, cobalt oxide, cobalt acetate, the cobalt acid lithium productive rate obtained is high and purity good, and cobalt-containing materials can proportioning arbitrarily, as long as the mol ratio meeting Li:Co is 0.95 ~ 1.2:1.
As preferably, the condition of drying in step (4) is: temperature 100 ~ 300 DEG C, time 3 ~ 8h.
As preferably, in step (5), the concrete steps of roasting are: in step (5), the concrete steps of roasting are: by the reaction paste after oven dry under air atmosphere, first with the temperature calcination 2 ~ 3h of 400 ~ 600 DEG C, then after being cooled to 200 ~ 300 DEG C of maintenance 1 ~ 2h, be warming up to 400 ~ 600 DEG C of continuation roasting 2 ~ 3h.Adding due to water soluble organic substance in the present invention, sintering temperature only needs 400 ~ 600 DEG C, much smaller than traditional sintering temperature being greater than 800 DEG C, energy consumption of reaction can be greatly reduced, and carry out in roasting process lowering the temperature with lower temperature calcination 1 ~ 2h, not only be conducive to cobalt, the sufficient crystallising of elemental lithium, cobalt acid lithium is made to keep good crystal structure, and be conducive to cobalt, being uniformly distributed of elemental lithium, thus effectively can avoid cobalt, the lamination of elemental lithium in material, intermediate temperature drop also helps the shaping of material particles simultaneously, the cobalt acid lithium particle making to obtain is more even, this step continues to remain calcined state in cooling or temperature-rise period.
As preferably, rate of temperature fall is 200 ~ 300 DEG C/h.
As preferably, the heating rate after cooling is 100 ~ 200 DEG C/h.
Therefore, the present invention has following beneficial effect:
(1) water soluble organic substance is added in preparation process, in roasting process, in material, each component can remain and is uniformly distributed, lamination can not be caused, also can avoid the precipitation of elemental lithium, suppress the excessive grain growth of cobalt acid lithium, reduce product agglomeration, make the cobalt acid lithium component that finally obtains stable, homogeneous, uniform particles, electrical property is good;
(2) be lowered into phase difficulty, sintering temperature is low, greatly reduces energy consumption;
(3) adopt cooling roasting in roasting process, be conducive to cobalt, elemental lithium sufficient crystallising be uniformly distributed, effectively can avoid cobalt, the elemental lithium lamination in material, also help the shaping of material particles simultaneously, the cobalt that obtains acid lithium particle is more even;
(4) obtained cobalt acid lithium uniformity is good, crystal grain is little, epigranular, reunion are few;
(5) processing step is simple, is applicable to producing in enormous quantities.
Accompanying drawing explanation
Fig. 1 is the Electronic Speculum figure of cobalt acid lithium obtained in embodiment 1.
Fig. 2 is the XRD figure of cobalt acid lithium obtained in embodiment 1.
Fig. 3 is the first charge-discharge curve chart of half-cell under 1C that cobalt acid lithium obtained in embodiment 1 is made.
Fig. 4 be in embodiment 1 capacity be the lithium ion battery of 1500mAh at 20 ± 5 DEG C, with the loop test figure of 1C/1C charge-discharge magnification in the voltage range of 3.0 ~ 4.2V.
Embodiment
Below in conjunction with the drawings and specific embodiments, the present invention will be further described.
In the present invention, all devices and raw material all can be buied from market or the industry is conventional, and the method in following embodiment, if no special instructions, is this area conventional method.
Embodiment 1
(1) a certain amount of lithium salts is taken and with lithium salts integral molar quantity for benchmark, lithium salts is lithium carbonate (M
lithium carbonate: 74 g/mol), take 74g(1mol), be the ratio metering water soluble organic substance of lithium salts integral molar quantity 50% in water soluble organic substance integral molar quantity, water soluble organic substance is citric acid (M
citric acid: 192 g/mol), measure to obtain 96 g.
(2), after being mixed with lithium carbonate by citric acid, be incorporated as citric acid quality 10%(9.6g) water, with the rotating speed ball milling 5h of 100rpm, obtain pre-reaction slurry.
(3) with the mol ratio of the Li:Co ratio that is 0.95:1 in pre-reaction slurry, add cobalt-containing materials and for citric acid quality 30%(57.6 g) water, with after the rotating speed ball milling 12h of 50rpm reaction paste, wherein, cobalt-containing materials is cobalt carbonate (M
cobalt carbonate: 119 g/mol), addition is 251 g.
(4) dried by reaction paste, drying condition is: temperature 100 DEG C, time 8h.
(5) by the reaction paste roasting under air atmosphere after oven dry, obtain cobalt acid lithium, the concrete steps of roasting are: by the reaction paste after oven dry under air atmosphere, first with the temperature calcination 3h of 400 DEG C, maintaining after 2h for being cooled to 200 DEG C with the rate of temperature fall of 200 DEG C/h again, being warming up to 400 DEG C with the heating rate of 100 DEG C/h and continuing roasting 3h.
one, Micro-Structure Analysis
The cobalt acid lithium utilizing electron microscope observation obtained, the microscopic pattern obtained as shown in Figure 1.
Carry out X-ray diffraction to the cobalt acid lithium obtained, the spectrogram obtained as shown in Figure 2.
two, electrochemical property test
With the cobalt obtained acid lithium for positive pole, pure lithium is that negative pole makes half-cell, and at 20 ± 5 DEG C, 1C, carries out half-cell test under the condition of 3.0 ~ 4.2 V, and the first charge-discharge curve obtained as shown in Figure 3.
Using obtain cobalt acid lithium as positive electrode, making model is 495148, and nominal capacity is the lithium ion battery of 1500mAh, at 20 ± 5 DEG C, in the voltage range of 3.0 ~ 4.2V, carry out loop test with 1C/1C charge-discharge magnification, the loop test figure obtained as shown in Figure 4.
Embodiment 2
(1) a certain amount of lithium salts is taken and with lithium salts integral molar quantity for benchmark, lithium salts is lithium hydroxide (M
lithium hydroxide: 24 g/mol), take 24g(1mol), be the ratio metering water soluble organic substance of lithium salts integral molar quantity 60% in water soluble organic substance integral molar quantity, water soluble organic substance is citric acid and glucose (M
citric acid: 192 g/mol, M
glucose: 180 g/mol), the mole of citric acid and glucose is respectively 0.3 mol, measures 111.6g altogether.
(2), after citric acid, glucose being mixed with lithium hydroxide, be incorporated as citric acid and glucose gross mass 15%(16.74g) water, with the rotating speed ball milling 3h of 200rpm, obtain pre-reaction slurry.
(3) with the mol ratio of the Li:Co ratio that is 1:1 in pre-reaction slurry, add cobalt-containing materials and for citric acid and glucose gross mass 40%(44.64 g) water, to obtain reaction paste after the rotating speed ball milling 8h of 70rpm, wherein, cobalt-containing materials is cobalt oxide (M
cobalt oxide: 166 g/mol), addition is 83g.
(4) dried by reaction paste, drying condition is: temperature 200 DEG C, time 5h.
(5) by the reaction paste roasting under air atmosphere after oven dry, obtain cobalt acid lithium, the concrete steps of roasting are: by the reaction paste after oven dry under air atmosphere, first with the temperature calcination 2.5h of 500 DEG C, maintaining after 1.5h for being cooled to 250 DEG C with the rate of temperature fall of 250 DEG C/h again, being warming up to 500 DEG C with the heating rate of 150 DEG C/h and continuing roasting 2.5h.
In the present embodiment, the cobalt acid Micro-Structure Analysis of lithium is identical with embodiment 1 with the method for electrochemical property test, and the result obtained is similar, therefore does not repeat at this and enumerate.
Embodiment 3
(1) a certain amount of lithium salts is taken and with lithium salts integral molar quantity for benchmark, lithium salts is lithium carbonate and lithium hydroxide (M
lithium carbonate: 74 g, M
lithium hydroxide: 24 g/mol), take 74 g lithium carbonates, 24 g lithium hydroxides, integral molar quantity 2mol, be the ratio metering water soluble organic substance of lithium salts integral molar quantity 70% in water soluble organic substance integral molar quantity, water soluble organic substance is citric acid, glucose and oxalic acid (M
citric acid: 192 g/mol, M
glucose: 180 g/mol, M
oxalic acid: 90 g/mol), wherein, citric acid and glucose are respectively 0.5mol, and oxalic acid is 0.4mol, amount to 222 g.
(2), after citric acid, glucose, oxalic acid being mixed with lithium carbonate, lithium hydroxide, be incorporated as citric acid, glucose and oxalic acid gross mass 20%(44.4g) water, with the rotating speed ball milling 2h of 300rpm, obtain pre-reaction slurry.
(3) ratio being 1.2:1 with the mol ratio of Li:Co adds cobalt-containing materials and is citric acid, glucose and oxalic acid gross mass 50%(110.5 g in pre-reaction slurry) water, to obtain reaction paste after the rotating speed ball milling 6h of 80rpm, wherein, cobalt-containing materials is cobalt carbonate and cobalt acetate (M
cobalt carbonate: 119 g/mol, M
cobalt acetate: 249 g/mol), cobalt carbonate addition is 119 g(1mol), cobalt acetate addition is 373.5 g(1.5mol).
(4) dried by reaction paste, drying condition is: temperature 300 DEG C, time 3h.
(5) by the reaction paste roasting under air atmosphere after oven dry, obtain cobalt acid lithium, the concrete steps of roasting are: by the reaction paste after oven dry under air atmosphere, first with the temperature calcination 2h of 600 DEG C, maintaining after 1h for being cooled to 300 DEG C with the rate of temperature fall of 300 DEG C/h again, being warming up to 600 DEG C with the heating rate of 200 DEG C/h and continuing roasting 2h.
In the present embodiment, the cobalt acid Micro-Structure Analysis of lithium is identical with embodiment 1 with the method for electrochemical property test, and the result obtained is similar, therefore does not repeat at this and enumerate.
Can obviously find out from Fig. 1, the uniform particle sizes of cobalt acid lithium of the present invention, without obviously reuniting.
As can be seen from Figure 2, the XRD spectra of cobalt of the present invention acid lithium and the standard spectrogram of the sour lithium of cobalt can one_to_one corresponding, illustrate that the present invention separates out without Li element in roasting process, obtained cobalt acid lithium purity is high, good crystallinity, crystal structure is good, and cobalt acid lithium crystalline phase is single, complete.
As can be seen from Figure 3, cobalt acid lithium of the present invention is when first charge-discharge, initial charge specific capacity is 162 mAh/g, first discharge specific capacity is 155mAh/g, reverse efficiency can reach 95.7% first, with existing commercially available cobalt acid lithium first discharge specific capacity 140 mAh/g, first charge-discharge can reverse efficiency 90 ~ 93% be compared, specific capacity and first charge-discharge efficiency are obtained for raising, illustrate that cobalt of the present invention acid lithium has good chemical property.
As can be seen from Figure 4, battery is in the voltage range of 3.0 ~ 4.2V, about 89% of initial capacity can be remained on the capability retention after 1C circulation 300 times, illustrate that the cycle performance of battery is still good, namely positive electrode (the cobalt acid lithium obtained by the present invention) stability, good cycle.
The above embodiment is one of the present invention preferably scheme, not does any pro forma restriction to the present invention, also has other variant and remodeling under the prerequisite not exceeding the technical scheme described in claim.
Claims (7)
1. a preparation method for cobalt acid lithium, is characterized in that, comprise the following steps:
(1) a certain amount of lithium salts is taken, with lithium salts integral molar quantity for benchmark, in the ratio metering water soluble organic substance that water soluble organic substance integral molar quantity is lithium salts integral molar quantity 50 ~ 70%, wherein water soluble organic substance is one or more in citric acid, glucose and oxalic acid;
(2) after being mixed with lithium salts by water soluble organic substance, be incorporated as the water of water soluble organic substance gross mass 10 ~ 20%, with the rotating speed ball milling 2 ~ 5h of 100 ~ 300rpm, obtain pre-reaction slurry;
(3) in pre-reaction slurry, add cobalt-containing materials and the water for water soluble organic substance gross mass 30 ~ 50%, wherein, the mol ratio of Li:Co is 0.95 ~ 1.2:1, to obtain reaction paste after the rotating speed ball milling 6 ~ 12h of 50 ~ 80rpm;
(4) reaction paste is dried;
(5) by the reaction paste roasting under air atmosphere after oven dry, cobalt acid lithium is obtained.
2. the preparation method of a kind of cobalt acid lithium according to claim 1, is characterized in that, described lithium salts is one or both in lithium carbonate, lithium hydroxide.
3. the preparation method of a kind of cobalt acid lithium according to claim 1, is characterized in that, described cobalt-containing materials is one or more in cobalt carbonate, cobalt oxide, cobalt acetate.
4. the preparation method of a kind of cobalt acid lithium according to claim 1 or 2 or 3, it is characterized in that, the condition of drying in step (4) is: temperature 100 ~ 300 DEG C, time 3 ~ 8h.
5. the preparation method of a kind of cobalt acid lithium according to claim 4, it is characterized in that, in step (5), the concrete steps of roasting are: by the reaction paste after oven dry under air atmosphere, first with the temperature calcination 2 ~ 3h of 400 ~ 600 DEG C, be warming up to 400 ~ 600 DEG C again after being cooled to 200 ~ 300 DEG C of maintenance 1 ~ 2h and continue roasting 2 ~ 3h.
6. the preparation method of a kind of cobalt acid lithium according to claim 5, it is characterized in that, rate of temperature fall is 200 ~ 300 DEG C/h.
7. the preparation method of a kind of cobalt acid lithium according to claim 5, it is characterized in that, the heating rate after cooling is 100 ~ 200 DEG C/h.
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| CN104993148A (en) * | 2015-06-16 | 2015-10-21 | 田东 | Synthesizing method for lithium-ion positive electrode material of LiCoO2/C |
| CN108130450A (en) * | 2018-02-05 | 2018-06-08 | 南通鑫祥锌业有限公司 | A kind of alloy zinc belt and preparation method thereof |
| CN109231282A (en) * | 2018-09-28 | 2019-01-18 | 青岛大学 | A kind of preparation method and applications of cobalt acid lithium |
| CN112467104A (en) * | 2020-11-23 | 2021-03-09 | 复旦大学 | Preparation method of lithium cobaltate thick electrode |
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| CN1357933A (en) * | 2000-12-08 | 2002-07-10 | 兰州大学化学化工学院 | Prepn of LiCoC2 as nanometer positive electrode material for lithium ion cell |
| CN1412121A (en) * | 2002-12-13 | 2003-04-23 | 北大先行科技产业有限公司 | Method for preparing possitive active material lithium cobaltate of lithium ion cell |
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| CN1357933A (en) * | 2000-12-08 | 2002-07-10 | 兰州大学化学化工学院 | Prepn of LiCoC2 as nanometer positive electrode material for lithium ion cell |
| CN1412121A (en) * | 2002-12-13 | 2003-04-23 | 北大先行科技产业有限公司 | Method for preparing possitive active material lithium cobaltate of lithium ion cell |
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Address after: 315800 standard workshop No. 2 of the 0212 massif in the West Zone of the Ningbo Free Trade Zone, Zhejiang Patentee after: Ningbo Veken Battery Co., Ltd. Address before: No. 5, West Boulevard of Zhejiang Free Trade Zone, Ningbo, Zhejiang Patentee before: Ningbo Veken Battery Co., Ltd. |