CN115642232A - Preparation method of carbon-coated lithium-rich lithium ferrite, product obtained by preparation method and application of product - Google Patents
Preparation method of carbon-coated lithium-rich lithium ferrite, product obtained by preparation method and application of product Download PDFInfo
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Abstract
The invention provides a preparation method of carbon-coated lithium-rich lithium ferrite, and an obtained product and application thereof, belonging to the technical field of preparation of lithium supplement agents of lithium batteries, and the method comprises the following steps: 1) Mixing nano ferric oxide, soluble lithium salt, an organic carbon source and water to obtain mixed slurry; 2) Spray drying the mixed slurry to obtain a precursor; 3) And calcining the precursor in an inert gas atmosphere, and cooling to obtain the carbon-coated lithium-rich lithium ferrite. The preparation method of the carbon-coated lithium-rich lithium ferrite provided by the invention has the advantages that the carbon coating is carried out in situ, the process is simple, and the prepared carbon-coated lithium-rich lithium ferrite has good air stability and high capacity and conductivity.
Description
Technical Field
The invention belongs to the technical field of lithium supplement preparation of lithium batteries, and particularly relates to a preparation method of carbon-coated lithium-rich lithium ferrite, and an obtained product and application thereof.
Background
It is known that during the first cycle (formation) of a lithium ion battery, the negative electrode SEI film is formed to consume about 7-10% of active lithium, and the loss of lithium causes the battery capacity to be reduced, the coulombic efficiency to be reduced, and the cycle performance to be deteriorated. Especially in the case of adding part of the high-capacity silicon-based negative electrode material, the loss of active lithium is higher in the first cycle of the battery. Supplementation with active lithium is an effective means to solve this problem.
The existing lithium supplementing method is that the lithium is supplemented to the positive electrode and the lithium is supplemented to the negative electrode. The lithium supplement of the negative electrode involves the use of active metals such as lithium powder and lithium foil, so that the requirements on the operating environment and lithium supplement equipment are strict, and the real industrialization is not always realized for many years. The positive electrode lithium supplement is simple and easy to operate, a small amount of positive electrode lithium supplement agent can be added in the homogenizing process of the preparation of the positive electrode piece, the lithium supplement can be realized in the formation stage, the lithium supplement process is safe, and the compatibility with the existing battery manufacturing process is good, so that the lithium supplement method has wide commercial application prospect. The currently researched and reported positive electrode lithium supplement agents are various, and lithium iron oxide (Li) is rich in lithium 5 FeO 4 ) Because of the higher specific capacity (867 mAh/g theory) and the proper lithium removal voltage (3.5-4.7V), the lithium ion replenishing agent is considered to be the lithium replenishing agent with the best lithium replenishing effect at present. But the conductivity and the air stability of the material are extremely poor, and lithium compound impurities can be produced when a small amount of water in the air is contacted at normal temperature, so that the performance of the material is reduced, and the polarization is increased; and the material preparation cost is high, the difficulty is high, and the large-scale industrial production and application are increased.
To solve the problem of poor air stability, the common method is to use Li 5 FeO 4 Carbon coating is carried out, so that on one hand, a uniform carbon coating layer can be formed to isolate air; on one hand, the compact and uniform carbon layer can form a conductive network, so that the conductivity of the material is improved. The prior carbon coating generally prepares ferric hydroxide colloid precursor or Fe 2 O 3 C, sintering the precursor; or first preparing Li 5 FeO 4 And coating the active material with gas-phase or solid-phase carbon. The preparation processes of the technologies are complicated, the energy consumption is high, the use of acidic or alkaline reagents is involved, and the three-waste treatment cost is increased.
Disclosure of Invention
The invention provides a preparation method of carbon-coated lithium-rich lithium ferrite, and an obtained product and application thereof.
In order to achieve the aim, the invention provides a preparation method of carbon-coated lithium-rich lithium ferrite, which comprises the following steps:
1) Mixing nano ferric oxide, soluble lithium salt, an organic carbon source and water to obtain mixed slurry;
2) Spray drying the mixed slurry to obtain a precursor;
3) And calcining the precursor in an inert gas atmosphere, and cooling to obtain the carbon-coated lithium-rich lithium ferrite.
Preferably, the molar ratio of Li to nano iron oxide in the soluble lithium source is 5.0 to 6.0; the mass ratio of the organic carbon source to the nano ferric oxide is 0.2-3:1.
Preferably, the soluble lithium salt is one or more of lithium hydroxide, lithium oxalate, lithium acetate, lithium nitrate and lithium carbonate; the organic carbon source is one or more of polyvinylpyrrolidone (PVP), polyvinyl alcohol (PVA), polyethylene glycol (PEG) and polyacrylic acid (PAA).
Preferably, the nano iron oxide is spherical particles, and the particle size is 20-500nm.
Preferably, a dispersant is also added before mixing in the step 1); the dispersant is alkylphenol polyoxyethylene.
Preferably, the mass ratio of the dispersing agent to the organic carbon source is 0 to 1:1.
Preferably, the mixed sizing material is stirred all the time before spray drying; the air inlet temperature of the spray drying is 120-300 ℃, and the air outlet temperature is 60-150 ℃.
Preferably, the calcining temperature is 450-950 ℃; the time is 8 to 100 hours.
The invention also provides the carbon-coated lithium-rich lithium ferrite prepared by any one of the methods, the particle size of the carbon-coated lithium-rich lithium ferrite is 3-20 mu m, and the first-loop charging specific capacity of 0.05C is more than 650 mAh/g.
The invention also provides an application of the carbon-coated lithium-rich lithium ferrite in a lithium ion battery anode lithium supplement agent.
Compared with the prior art, the invention has the advantages and positive effects that:
(1) The invention carries out carbon coating in situ, does not need post treatment after preparation, does not contact air, and has high product purity, uniform particle size distribution and good air stability.
(2) The invention adopts the nano ferric oxide as the raw material, has no mixed discharge of cations in the preparation process, and has high material capacity compared with the material obtained by other liquid phase methods.
(3) According to the invention, the carbon source is added before sintering, and plays a role in blocking particles in the sintering process, so that the growth of primary particles is slowed down, the growth of large single crystal particles is avoided, and the improvement of the conductivity of the material is facilitated;
(4) The preparation method disclosed by the invention is green and pollution-free in preparation process, low in cost and suitable for industrialization.
Drawings
FIG. 1 is an SEM image of carbon-coated lithium-rich lithium iron oxide of example 1 of the present invention;
FIG. 2 is an SEM image of lithium-rich lithium iron oxide of comparative example 1 of the present invention;
fig. 3 is XRD patterns of lithium iron oxide rich lithium of example 1 of the present invention and comparative example 1;
fig. 4 is a charge profile of lithium-rich lithium iron oxides of example 1 of the present invention and comparative example 1.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention provides a preparation method of carbon-coated lithium-rich lithium ferrite, which comprises the following steps:
1) Mixing nano ferric oxide, soluble lithium salt, an organic carbon source and water to obtain mixed slurry;
2) Spray drying the mixed slurry to obtain a precursor;
3) And calcining the precursor in an inert gas atmosphere, and cooling to obtain the carbon-coated lithium-rich lithium ferrite.
The invention mixes nano ferric oxide, soluble lithium salt, organic carbon source and water to obtain mixed slurry. In the present invention, the nano iron oxide is preferably spherical particles, and the particle size is preferably 20 to 500nm. In the invention, the soluble lithium salt is preferably one or more of lithium hydroxide, lithium oxalate, lithium acetate, lithium nitrate and lithium carbonate; the organic carbon source is preferably one or more of polyvinylpyrrolidone (PVP), polyvinyl alcohol (PVA), polyethylene glycol (PEG) and polyacrylic acid (PAA). In the present invention, the molar ratio of Li to nano iron oxide in the soluble lithium source is preferably 5.0 to 6.0; the mass ratio of the organic carbon source to the nano iron oxide is preferably 0.2-3:1.
In the present invention, before the mixing is carried out, it is preferable to further add a dispersant; the dispersant is preferably alkylphenol polyoxyethylene ether, and is more preferably nonylphenol polyoxyethylene ether or octyl polyoxyethylene ether. The mass ratio of the dispersant to the organic carbon source is preferably 0 to 1:1, more preferably 0.01 to 0.1. In the invention, the dispersing agent is added before mixing to assist the sufficient dispersion and mixing of the nano iron oxide, the lithium salt and the organic carbonic acid, so that the sedimentation in the spray drying process is avoided.
After the mixed slurry is obtained, the mixed slurry is subjected to spray drying to obtain a precursor. In the present invention, the mixed gum is stirred all the time before spray drying in order to prevent the material from being uneven due to settling. In the present invention, the stirring is preferably magnetic stirring. In the invention, the air inlet temperature of the spray drying is preferably 120-300 ℃, and more preferably 140-180 ℃; the air outlet temperature is preferably 60 to 150 ℃, and more preferably 70 to 90 ℃.
After the precursor is obtained, the precursor is calcined in the inert gas atmosphere, and the carbon-coated lithium-rich lithium ferrite is obtained after cooling. In the present invention, the temperature of the calcination is preferably 450 to 950 ℃, more preferably 700 to 800 ℃; the time is preferably 8 to 100 hours, more preferably 10 to 30 hours.
In the invention, the nano iron oxide is used as a raw material, no cation is mixed in the preparation process, and the capacity of the material is higher compared with that obtained by other liquid phase methods. According to the invention, the nano iron oxide, the soluble lithium salt, the organic carbon source and the water are mixed, and the carbon coating is directly carried out in situ without contacting with air, so that the product has high purity, good air stability and uniform particle size distribution. The carbon source is added before sintering, and plays a role in blocking particles in the sintering process, so that the growth of primary particles is slowed down, the growth of large single crystal particles is avoided, and the improvement of the conductivity of the material is facilitated. The preparation process of the method is green and pollution-free, no post-treatment is needed after the preparation, the cost is low, and the method is suitable for industrialization.
The invention also provides carbon-coated lithium-rich lithium ferrite prepared by any one of the methods, wherein the particle size of the carbon-coated lithium-rich lithium ferrite is 3-20 mu m, and the first-loop charging specific capacity of 0.05C is more than 650 mAh/g. In the carbon-coated lithium-rich lithium iron oxide, the thickness of the carbon layer is 0.1-1000 nm, and the carbon content is 0.5-20 wt%.
The invention also provides an application of the carbon-coated lithium-rich lithium ferrite in a lithium ion battery anode lithium supplement agent.
In order to further illustrate the present invention, the following embodiments are described in detail, but they should not be construed as limiting the scope of the present invention.
Example 1
Weighing lithium hydroxide and nano iron oxide according to a molar ratio of 5.5, dissolving the lithium hydroxide and the nano iron oxide in deionized water, adding PVP-8000 according to a mass ratio of the PVP-8000 to the nano iron oxide of 1:1 into the solution, weighing nonylphenol polyoxyethylene ether accounting for 5% of the mass of the PVP, and stirring the solution at room temperature to form uniform slurry; the resulting slurry is then spray dried (in)The wind temperature is 165 ℃, the air outlet temperature is 80 ℃) to obtain precursor powder, the obtained precursor powder is subjected to heat preservation for 15 hours at 700 ℃ in the argon atmosphere, and the precursor powder is cooled along with the furnace to obtain the carbon-coated lithium iron oxide-rich Li 5 FeO 4 @ C. For Li obtained by preparation 5 FeO 4 @ C the results of electron microscopy and X-ray diffraction analysis are shown in FIGS. 1 and 3.
Example 2
Weighing lithium carbonate and nano iron oxide according to the molar ratio of lithium to nano iron oxide of 5.5; then spray drying the obtained slurry (the air inlet temperature is 140 ℃, the air outlet temperature is 75 ℃) to obtain precursor powder, preserving the temperature of the obtained precursor powder for 15h at 700 ℃ in the argon atmosphere, and cooling along with the furnace to obtain the carbon-coated lithium-rich lithium iron oxide-Li 5 FeO 4 @C。
Example 3
Weighing lithium nitrate and nano iron oxide according to the molar ratio of the lithium to the nano iron oxide of 6:1, dissolving the lithium nitrate and the nano iron oxide in deionized water, adding PVP-8000 according to the mass ratio of the PVP-8000 to the nano iron oxide of 2:1 into the solution, and stirring the solution at room temperature until the solution becomes uniform slurry; then spray drying the obtained slurry (the air inlet temperature is 165 ℃, the air outlet temperature is 80 ℃) to obtain precursor powder, preserving the temperature of the obtained precursor powder at 800 ℃ for 10h in an argon atmosphere, and cooling along with the furnace to obtain the carbon-coated lithium iron oxide-rich Li 5 FeO 4 @C。
Example 4
Weighing lithium hydroxide and nano iron oxide according to a molar ratio of 5.5; then spray drying the obtained slurry (the air inlet temperature is 165 ℃, the air outlet temperature is 80 ℃) to obtain precursor powder, preserving the temperature of the obtained precursor powder for 24 hours at 600 ℃ in an argon atmosphere, and cooling along with the furnace to obtain the carbon-coated lithium iron oxide-rich Li 5 FeO 4 @C。
Example 5
Weighing lithium hydroxide and nano-iron oxide according to a molar ratio of 5:1, dissolving the lithium hydroxide and the nano-iron oxide in deionized water, weighing PVA according to a mass ratio of the PVA to the nano-iron oxide of 3:1, adding the PVA into the solution, and stirring the mixture at room temperature until the solution becomes uniform slurry; then spray drying the obtained slurry (the air inlet temperature is 300 ℃, the air outlet temperature is 150 ℃) to obtain precursor powder, preserving the temperature of the obtained precursor powder for 50h at 450 ℃ in the argon atmosphere, and cooling along with the furnace to obtain the carbon-coated lithium-rich lithium iron oxide-Li 5 FeO 4 @C。
Example 6
Weighing lithium hydroxide and nano-iron oxide according to a molar ratio of 6:1, dissolving in deionized water, adding PAA according to a mass ratio of 0.5 to the nano-iron oxide, weighing the PAA and the nano-iron oxide, and stirring at room temperature until the solution becomes uniform slurry; then spray drying the obtained slurry (the air inlet temperature is 120 ℃, the air outlet temperature is 60 ℃) to obtain precursor powder, preserving the temperature of the obtained precursor powder at 800 ℃ for 10h in an argon atmosphere, and cooling along with the furnace to obtain the carbon-coated lithium iron oxide-rich lithium-Li 5 FeO 4 @C。
Comparative example 1
Weighing lithium hydroxide and ferric nitrate nonahydrate according to a molar ratio of 5.5, dissolving the lithium hydroxide and the ferric nitrate nonahydrate into deionized water, weighing PVP 8000 according to a mass ratio of PVP-8000 to ferric nitrate 1:1, adding the PVP 8000 into the solution, stirring at 70 ℃ to form sol, performing spray drying (165 ℃, the air outlet temperature of 80 ℃) on the sol to obtain precursor powder, preserving the temperature of the precursor powder at 700 ℃ in an argon atmosphere for 15 hours, and cooling along with a furnace to obtain the carbon-coated lithium-rich lithium iron oxide. For Li obtained by preparation 5 FeO 4 @ C the results of electron microscopy and X-ray diffraction analysis are shown in FIGS. 2 and 3.
Comparative example 2
Weighing lithium hydroxide and nano-iron oxide according to a molar ratio of 5.5, ball-milling and mixing, keeping the temperature of the mixture at 700 ℃ for 15h in an argon atmosphere, and cooling along with the furnace to obtain lithium-rich lithium iron oxide; and then weighing PVP-8000 and lithium-rich lithium ferrite according to the mass ratio of 0.5, mixing in a vacuum ball milling tank, uniformly mixing, preserving the temperature for 10 hours at 500 ℃ in an argon atmosphere, and cooling along with the furnace to obtain the carbon-containing lithium-rich lithium ferrite.
Performance testing
Taking the products in examples 1-6 and comparative examples 1-2 as positive electrode materials, weighing the positive electrode materials, SP and PVDF according to a ratio of 8; and then assembling the positive plate and the Li plate into a lithium ion battery, and respectively carrying out charge and discharge tests, wherein the specific capacity test method of the lithium supplement agent is that the lithium ion battery is used as a positive active material to prepare a button half cell and is tested under the voltage of 3.0-4.5V and the current of 0.05C, the specific results are shown in Table 1, and the charging curves of the embodiment 1 and the comparative example 1 are shown in FIG. 4.
TABLE 1 first discharge Capacity of lithium-rich lithium ferrite
As can be seen from Table 1, examples 1-6 all showed higher specific charge capacity and small and uniform particle size < 10 μm under the condition of 0.05C rate charging in the voltage range of 3.0-4.5V; this is because the organic carbon source is uniformly dispersed on the surface of the iron oxide, and carbonization occurs during sintering of the material to form a uniform carbon coating layer, which hinders the growth of particles, which is advantageous for improving the conductivity of the material. In comparative example 1, the agglomerate material having a uniform particle size was obtained, but the total particle size was too large (about 200 μm) and the conductivity of the material was reduced, so that the specific capacity was not satisfactory at the same magnification, and it was only 296.2mAh/g. This is because comparative example 1 uses iron salt and lithium salt as raw materials, has gone through the sol-gel process, in this process, ferric hydroxide gel is stable under acidic condition (pH is about 2-3), the strong alkaline condition destroys colloidal stability, causes to produce the ferric hydroxide precipitation of big granule easily, causes the precursor particle size too big (mum level), because ferric hydroxide colloid need decompose into ferric oxide first in the sintering process at the same time, just can accept the Li that diffuses as the skeleton, the effect of carbon barrier layer is weakened in the volatilization of a large amount of gaseous water, causes the granule to appear the secondary agglomeration. Comparative example 2, which employs a lithium-rich lithium iron oxide material prepared first and then carbon-coated after solid-phase mixing, shows that, although the material of this embodiment has a high carbon content, the carbon does not coat the surface of the material well, and thus there is no improvement in conductivity and gram-volume and almost no charge capacity.
In addition, from the capacity expressions of example 1 and example 4, the target material added with the dispersant group exerts better capacity, because the dispersant facilitates the uniform dispersion of the nano ferric trioxide and the lithium source to enable the reaction raw materials to be mixed more fully, which obviously facilitates the forward progress of the reaction process, and the product purity is higher.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. A preparation method of carbon-coated lithium-rich lithium ferrite is characterized by comprising the following steps:
1) Mixing nano ferric oxide, soluble lithium salt, an organic carbon source and water to obtain mixed slurry;
2) Spray drying the mixed slurry to obtain a precursor;
3) And calcining the precursor in an inert gas atmosphere, and cooling to obtain the carbon-coated lithium-rich lithium ferrite.
2. The method according to claim 1, wherein the molar ratio of Li to nano iron oxide in the soluble lithium source is 5.0 to 6.0; the mass ratio of the organic carbon source to the nano ferric oxide is 0.2-3:1.
3. The preparation method according to claim 1, wherein the soluble lithium salt is one or more of lithium hydroxide, lithium oxalate, lithium acetate, lithium nitrate and lithium carbonate; the organic carbon source is one or more of polyvinylpyrrolidone (PVP), polyvinyl alcohol (PVA), polyethylene glycol (PEG) and polyacrylic acid (PAA).
4. The method according to claim 1, wherein the nano iron oxide is in the form of spherical particles having a particle size of 20 to 500nm.
5. The method according to claim 1, wherein a dispersant is further added before the mixing in step 1); the dispersant is alkylphenol polyoxyethylene.
6. The method according to claim 5, wherein the mass ratio of the dispersant to the organic carbon source is 0 to 1:1.
7. The method of claim 1, wherein the mixed size is stirred at all times before spray drying; the air inlet temperature of the spray drying is 120-300 ℃, and the air outlet temperature is 60-150 ℃.
8. The method of claim 1, wherein the temperature of the calcination is 450 to 950 ℃; the time is 8 to 100 hours.
9. The carbon-coated lithium-rich lithium ferrite prepared by any one of the methods of claims 1 to 8, characterized in that the particle size of the carbon-coated lithium-rich lithium ferrite is 3 to 20 μm, and the first-turn specific charge capacity at 0.05C is above 650 mAh/g.
10. Use of the carbon-coated lithium-rich lithium iron oxide of claim 9 in a lithium ion battery positive electrode lithium supplement agent.
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| CN117317415A (en) * | 2023-11-15 | 2023-12-29 | 银贮(宁波)科技有限公司 | Carbon-coated lithium ferrate lithium supplementing additive and preparation method thereof |
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| CN117317415A (en) * | 2023-11-15 | 2023-12-29 | 银贮(宁波)科技有限公司 | Carbon-coated lithium ferrate lithium supplementing additive and preparation method thereof |
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