CN110880593B - Solid electrolyte modified lithium titanate negative electrode material and preparation method thereof - Google Patents
Solid electrolyte modified lithium titanate negative electrode material and preparation method thereof Download PDFInfo
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Abstract
本发明涉及电极材料领域，公开了一种固态电解质改性钛酸锂负极材料及其制备方法，该钛酸锂负极材料的微观形貌为：二次颗粒呈现球状，粒径为5‑20μm，该二次颗粒由晶粒大小为20‑200 nm的一次颗粒组成；该钛酸锂负极材料中的钛酸锂颗粒表面附着含氟氧化物和氟化物组成的锂离子固态电解质，锂离子固态电解质的质量分数为0.1‑3%；其制备方法为：将一种或多种含氟的锂电池电解液、二氧化钛和锂盐经两次砂磨、两次喷雾造粒和两次固相煅烧制得。制得的钛酸锂负极材料振实密度达到1.3 g/cm3以上，pH值8‑10，并具有较好的倍率性能，5C放电容量达到135 mAh g‑1以上。
The invention relates to the field of electrode materials, and discloses a solid electrolyte modified lithium titanate negative electrode material and a preparation method thereof. The microscopic morphology of the lithium titanate negative electrode material is as follows: secondary particles are spherical, with a particle size of 5-20 μm, The secondary particles are composed of primary particles with a grain size of 20-200 nm; the surface of the lithium titanate particles in the lithium titanate negative electrode material is attached to the surface of the lithium ion solid state electrolyte composed of fluoride-containing oxide and fluoride, and the lithium ion solid state electrolyte The mass fraction is 0.1-3%; the preparation method is as follows: one or more fluorine-containing lithium battery electrolytes, titanium dioxide and lithium salt are subjected to two times of sand grinding, two times of spray granulation and two times of solid-phase calcination. have to. The prepared lithium titanate negative electrode material has a tap density of more than 1.3 g/cm 3 , a pH value of 8-10, good rate performance, and a 5C discharge capacity of more than 135 mAh g -1 .
Description
Technical Field
The invention relates to the field of electrode materials, in particular to a solid electrolyte modified lithium titanate negative electrode material and a preparation method thereof.
Background
Along with the rapid development of China in the fields of photovoltaic energy storage, aviation, aerospace, petroleum and natural gas drilling and military industry, the research and development of novel energy storage devices becomes increasingly urgent in stable long-term operation under extreme environments, and the developed energy storage devices have wider working temperature range than lead-acid batteries and common lithium batteries and become the most possible candidates. Lithium titanate batteries are increasingly popular in the market due to the congenital advantages of wide service temperature range, capability of being charged and discharged at a low temperature of-40 ℃, long cycle life, high safety performance and the like. The most core material in the lithium titanate battery is the lithium titanate cathode material, and the electrochemical performance of the device is directly determined. However, the lithium titanate material encounters many problems in the industrial production process, such as difficult calcination to pure phase and more impure phase, resulting in poor cycle and rate capability of the material; the surface alkalinity is too strong, which causes the slurry to be jelly-like, the processability is poor, the subsequent coating process is unstable, and the appearance and the quality of the pole piece are poor. How to further improve the performance of lithium titanate materials produced in an industrialized way, a new production process with low development cost and strong controllability is one of the key problems to be solved urgently in the research and development of lithium titanate batteries and the development of industries.
Disclosure of Invention
The purpose of the invention is as follows: aiming at the problems in the prior art, the invention provides a solid electrolyte modified lithium titanate negative electrode material and a preparation method thereof, wherein the tap density of the lithium titanate negative electrode material reaches 1.3 g/cm3Above, the pH value is 8-10, the discharge capacity of 5C reaches 135mAh g-1Above, 95% of the capacity at 0.1C; the raw materials in the production and preparation process are wide in source, the waste utilization can be realized, the preparation method is simple, the cost is low, the engineering amplification can be realized, and the continuous production can be realized.
The technical scheme is as follows: the invention provides a solid electrolyte modified lithium titanate negative electrode material, which has the following microscopic morphology: the secondary particles are spherical, the particle size is 5-20 μm, and the secondary particles are composed of primary particles with the grain size of 20-200 nm; the lithium ion solid electrolyte composed of fluorine-containing oxide and fluoride is attached to the surface of lithium titanate particles in the lithium titanate negative electrode material, and the mass fraction of the lithium ion solid electrolyte is 0.1-3%
The invention also provides a preparation method of the solid electrolyte modified lithium titanate negative electrode material, which comprises the following steps: s1: mixing titanium dioxide powder, lithium salt and deionized water, and performing primary sanding on the mixture to prepare a suspension A; s2: preparing the suspension A into a precursor B; s3: carrying out primary calcination on the precursor B to prepare primary calcined powder C; s4: uniformly mixing and stirring the primary calcined powder C and deionized water, and dropwise adding fluorine-containing lithium battery electrolyte into the mixture, wherein the temperature is not more than 25 ℃ in the dropwise adding process; then, carrying out secondary sanding to prepare a suspension D; s5: preparing the suspension D into a precursor E; s6: and carrying out secondary calcination on the precursor E to prepare secondary calcined powder F, wherein the secondary calcined powder F is the solid electrolyte modified lithium titanate negative electrode material.
Preferably, the fluorine-containing lithium battery electrolyte is expired or waste lithium battery electrolyte, electrolyte in a recycled lithium battery, defective lithium battery electrolyte or invalid lithium battery electrolyte with high water content.
Preferably, the solid content in the suspension A is 5% -25%; and/or the solid content of the suspension D is 5-25%.
Preferably, in S2, the suspension a is prepared into the precursor B by a spray granulation method; and/or preparing the suspension D into the precursor E by adopting a spray granulation method in the S5.
Preferably, in the S3, the environment of the primary calcination is: calcining in flowing air at 500-800 deg.c for 8-15 hr; and/or, in the S6, the environment of the secondary calcination is: calcining in flowing air at 500-800 deg.c for 8-15 hr.
Preferably, in S4, the lithium content in the dropwise added lithium battery electrolyte containing fluorine is 0.1-3% of the lithium content in the lithium salt, calculated according to the lithium content.
Preferably, the lithium salt is lithium carbonate, lithium hydroxide or lithium oxalate.
Preferably, the micro-morphology of the lithium titanate negative electrode material is as follows: the secondary particles are spherical and have a particle diameter of 5 to 20 μm, and the secondary particles are composed of primary particles having a crystal grain size of 20 to 200 nm.
Preferably, the titanium dioxide powder is anatase type industrial grade titanium dioxide.
Has the advantages that: the solid electrolyte modified lithium titanate negative electrode material and the preparation method thereof have the following advantages:
(1) the tap density of the solid electrolyte modified lithium titanate negative electrode material reaches 1.3 g/cm3The method has the advantages of good rate capability; the pH value of slurry prepared by using the solid electrolyte modified lithium titanate negative electrode material powder is 8-10, and the slurry is low in alkalinity; the 5C discharge capacity reaches 135mAh g-1The above content was 95% of the capacity at 0.1C.
(2) In the method for preparing the solid electrolyte modified lithium titanate cathode material, the fluorine-containing lithium battery electrolyte is dropwise added into the mixed solution of the primary calcined powder C and the deionized water, so that the fluorine-containing lithium battery electrolyte is hydrolyzed to generate fluoride products (such as LiF and PF)5、HPO2F2，H2PO3F、LiBF(OH)3、LiBF2(OH)2HF and the like), the surface alkalinity of the primary calcined powder C can be reduced in the hydrolysis process, heat can be generated in the hydrolysis process, and in order to ensure the normal operation of the reaction and ensure the uniformity of the finally formed suspension D, the mixed solution needs to be cooled and protected, so that the temperature of the mixed solution is not higher than 25 ℃; after forming a suspension D, preparing the suspension D into a precursor E by adopting a spray granulation method, then carrying out secondary calcination on the precursor E to prepare a secondary calcined powder F, and modifying the surface of fluorine-containing oxide and fluoride formed by calcining the hydrolysate of the electrolyte on the secondary calcined powder F, namely modifying the surface of the secondary calcined powder F modified with the fluorine-containing oxide and the fluoride to obtain the solid electrolyte modified lithium titanate negative electrode material; due to the fact that the surface of the material is modified by the fluorine-containing oxide and the fluoride, the solid electrolyte modified lithium titanate negative electrode material has the excellent performance of the point (1).
(3) The method adopts the technology of twice sanding and twice calcining to ensure that the lithium titanate generates a spinel pure phase, and ensures that the grain size and the secondary particle size of the lithium titanate are more controllable, thereby ensuring excellent electrochemical performance and excellent processing performance.
(4) The invention adopts the fluorine-containing lithium battery electrolyte, which can timely supplement lithium for lithium loss during calcination, and the hydrolysis product of the fluorine-containing lithium battery electrolyte can neutralize the surface alkalinity of the precursor so as to reduce the surface alkalinity of the product, and the pH value of the powder is 8-10; meanwhile, fluoride and phosphide generated by hydrolysis can form a solid electrolyte after calcination, and the solid electrolyte is similar to an artificial SEI film structure, so that the cycle and rate performance of the lithium titanate material are further improved.
(5) The fluorine-containing lithium battery electrolyte adopted by the invention is overdue or waste lithium battery electrolyte, electrolyte in recycled lithium batteries, defective lithium battery electrolyte or invalid lithium battery electrolyte with higher water content, and has wide raw material sources and low cost.
(6) The solid electrolyte is obtained by calcining a hydrolysate of fluorine-containing lithium battery electrolyte, is uniformly coated on the surface of lithium titanate particles, contains fluorine-containing oxide and fluoride, has high lithium ion conductivity, and improves the rate capability of the material.
(7) The lithium titanate material prepared by the invention has the advantages of high crystalline phase purity, small surface alkalinity, optimized sizes of crystal grains and powder, good processability, and good multiplying power and cycle performance.
(8) The lithium titanate material has the advantages of wide raw material source in the preparation process, simple preparation method, low cost, capability of realizing waste utilization, engineered amplification and capability of realizing continuous industrial production.
Drawings
FIG. 1 is a production flow chart of a solid electrolyte modified lithium titanate negative electrode material in the invention;
fig. 2 is a rate diagram of the lithium titanate material in embodiment 1 in a button half cell;
fig. 3 is a cycle diagram of the lithium titanate material in embodiment 1 in a half-cell button cell.
Detailed Description
The technical scheme of the invention is further explained by combining the specific embodiment as follows:
embodiment 1:
the embodiment provides a solid electrolyte modified lithium titanate negative electrode material, which has the following microscopic morphology: the secondary particles are spherical, the particle size is 5-20 μm, and the secondary particles are composed of primary particles with the grain size of 20-200 nm; the lithium ion solid electrolyte composed of fluorine-containing oxide and fluoride is attached to the surface of lithium titanate particles in the lithium titanate negative electrode material, and the mass fraction of the lithium ion solid electrolyte is 1%.
The preparation method of the solid electrolyte modified lithium titanate negative electrode material comprises the following steps (the process flow is shown in figure 1):
mixing industrial anatase titanium dioxide with lithium carbonate and deionized water, grinding and fully mixing in a sand mill to prepare suspension A with the solid content of 10%. And preparing the suspension A into a precursor B by adopting a spray granulation method. Calcining the precursor B in flowing air at 800 ℃ for 12 hours to prepare primary calcined powder C, mixing and stirring the primary calcined powder C and deionized water uniformly, and dropwise adding and recovering LiPF in the lithium battery under the protection of cooling6And (3) electrolyte, wherein the temperature of the mixed solution is not higher than 25 ℃ in the dropwise adding process, and the content of lithium in the electrolyte is 1% of that in the lithium carbonate. And (5) performing secondary sanding to prepare suspension D with the solid content of 10%. And preparing the suspension D into a precursor E by adopting a spray granulation method, calcining the precursor E in flowing air at 800 ℃ for 12 hours to prepare secondary calcined powder F, and obtaining the final product, namely the solid electrolyte modified lithium titanate negative electrode material. The tap density of the lithium titanate negative electrode material reaches 1.45 g/cm3The pH value is 8.5, the button half cell taking the metallic lithium as the counter electrode is manufactured, and the 1C discharge capacity reaches 156 mAh g-1And 5C discharge capacity reaches 138 mAh g-1As shown in fig. 2; the capacity retention rate was 87.5% at 5C for 500 cycles, as shown in fig. 3.
Embodiment 2:
the embodiment provides a solid electrolyte modified lithium titanate negative electrode material, which has the following microscopic morphology: the secondary particles are spherical, the particle size is 5-20 μm, and the secondary particles are composed of primary particles with the grain size of 20-200 nm; the lithium ion solid electrolyte composed of fluorine-containing oxide and fluoride is attached to the surface of lithium titanate particles in the lithium titanate negative electrode material, and the mass fraction of the lithium ion solid electrolyte is 2%.
The preparation method of the solid electrolyte modified lithium titanate negative electrode material comprises the following steps (the process flow is shown in figure 1):
mixing industrial anatase titanium dioxide with lithium hydroxide and deionized water, grinding in a sand mill, and fully mixing to prepare suspension A with the solid content of 12%. And preparing the suspension A into a precursor B by adopting a spray granulation method. Calcining the precursor B in flowing air at 800 ℃ for 10 hours to prepare primary calcined powder C, mixing and stirring the primary calcined powder C and deionized water uniformly, and dropwise adding LiBF of a lithium battery electrolyte manufacturer under the protection of cooling4And (3) adding the defective electrolyte, wherein the temperature of the mixed solution is not higher than 25 ℃ in the dropwise adding process, and the lithium content in the electrolyte is 2% of the lithium content in the lithium carbonate. And D, performing secondary sanding to prepare a suspension with the solid content of 12%. And preparing the suspension D into a precursor E by adopting a spray granulation method, calcining the precursor E in flowing air at 800 ℃ for 10 hours to prepare secondary calcined powder F, and obtaining the final product, namely the solid electrolyte modified lithium titanate negative electrode material. The tap density of the lithium titanate negative electrode material reaches 1.35 g/cm3pH value is 9.5, the button half cell taking metallic lithium as a counter electrode is manufactured, and 1C discharge capacity reaches 152 mAh g-1And 5C discharge capacity reaches 135mAh g-1And the capacity retention rate of 500 cycles at 5 ℃ is 94.2%.
Embodiment 3:
the embodiment provides a solid electrolyte modified lithium titanate negative electrode material, which has the following microscopic morphology: the secondary particles are spherical, the particle size is 5-20 μm, and the secondary particles are composed of primary particles with the grain size of 20-200 nm; the lithium ion solid electrolyte composed of fluorine-containing oxide and fluoride is attached to the surface of lithium titanate particles in the lithium titanate negative electrode material, and the mass fraction of the lithium ion solid electrolyte is 1.5%.
The preparation method of the solid electrolyte modified lithium titanate negative electrode material comprises the following steps (the process flow is shown in figure 1):
mixing industrial anatase titanium dioxide with oxalic acidLithium and deionized water were mixed, milled in a sand mill and mixed thoroughly to prepare suspension a with 8% solids. And preparing the suspension A into a precursor B by adopting a spray granulation method. Calcining the precursor B in flowing air at 750 ℃ for 14 hours to prepare primary calcined powder C, mixing and stirring the primary calcined powder C and deionized water uniformly, and dropwise adding LiPF of a lithium battery electrolyte manufacturer under cooling protection6And (3) adding the defective electrolyte, wherein the temperature of the mixed solution is not higher than 25 ℃ in the dropwise adding process, and the lithium content in the electrolyte is 1.5% of the lithium content in the lithium carbonate. And (5) performing secondary sanding to prepare suspension D with the solid content of 8%. And preparing the suspension D into a precursor E by adopting a spray granulation method, calcining the precursor E in flowing air at 750 ℃ for 14 hours to prepare secondary calcined powder F, and obtaining the final product, namely the solid electrolyte modified lithium titanate negative electrode material. The tap density of the lithium titanate negative electrode material reaches 1.3 g/cm3The pH value is 8, the button half cell taking the metallic lithium as the counter electrode is manufactured, and the 1C discharge capacity reaches 158 mAh g-1And 5C discharge capacity of 137mAh g-1The capacity retention rate of 500 cycles at 5C is 85.2 percent, and the capacity retention rate of 500 cycles at 5C is 500 percent.
The above embodiments are merely illustrative of the technical concepts and features of the present invention, and the purpose of the embodiments is to enable those skilled in the art to understand the contents of the present invention and implement the present invention, and not to limit the protection scope of the present invention. All equivalent changes and modifications made according to the spirit of the present invention should be covered within the protection scope of the present invention.
Claims (8)
1. A preparation method of a solid electrolyte modified lithium titanate negative electrode material is disclosed, wherein the micro-morphology of the lithium titanate negative electrode material is as follows: the secondary particles are spherical, the particle size is 5-20 μm, and the secondary particles are composed of primary particles with the grain size of 20-200 nm; the lithium ion solid electrolyte composed of fluorine-containing oxide and fluoride is attached to the surface of lithium titanate particles in the lithium titanate negative electrode material, and the mass fraction of the lithium ion solid electrolyte is 0.1-3%; the method is characterized by comprising the following steps:
s1: mixing titanium dioxide powder, lithium salt and deionized water, and performing primary sanding on the mixture to prepare a suspension A;
s2: preparing the suspension A into a precursor B by adopting a spray granulation method;
s3: carrying out primary calcination on the precursor B to prepare primary calcined powder C;
s4: uniformly mixing and stirring the primary calcined powder C and deionized water, and dropwise adding fluorine-containing lithium battery electrolyte into the mixture, wherein the temperature is not more than 25 ℃ in the dropwise adding process; then, carrying out secondary sanding to prepare a suspension D;
s5: preparing the suspension D into a precursor E by adopting a spray granulation method;
s6: and carrying out secondary calcination on the precursor E to prepare secondary calcined powder F, wherein the secondary calcined powder F is the solid electrolyte modified lithium titanate negative electrode material.
2. The method for preparing a solid electrolyte modified lithium titanate negative electrode material as claimed in claim 1, wherein the fluorine-containing lithium battery electrolyte is expired or waste lithium battery electrolyte, electrolyte in recycled lithium batteries, defective lithium battery electrolyte or failed lithium battery electrolyte with high water content.
3. The preparation method of the solid electrolyte modified lithium titanate negative electrode material according to claim 1, wherein the solid content of the suspension A is 5% -25%; and/or the solid content of the suspension D is 5-25%.
4. The method for preparing a solid electrolyte modified lithium titanate negative electrode material according to claim 1, wherein in the step S3, the environment of the primary calcination is: calcining in flowing air at 500-800 deg.c for 8-15 hr; and/or, in the S6, the environment of the secondary calcination is: calcining in flowing air at 500-800 deg.c for 8-15 hr.
5. The method for preparing a solid electrolyte modified lithium titanate negative electrode material as claimed in claim 1, wherein in the step S4, the lithium content of the fluorine-containing lithium battery electrolyte added dropwise is 0.1-3% of the lithium content of the lithium salt, calculated according to the lithium content.
6. The method for preparing a solid electrolyte modified lithium titanate negative electrode material according to claim 5, wherein the lithium salt is lithium carbonate, lithium hydroxide or lithium oxalate.
7. The method for preparing a solid electrolyte modified lithium titanate negative electrode material according to any one of claims 1 to 6, characterized in that: the micro-morphology of the lithium titanate negative electrode material is as follows: the secondary particles are spherical and have a particle diameter of 5 to 20 μm, and the secondary particles are composed of primary particles having a crystal grain size of 20 to 200 nm.
8. The method for preparing a solid electrolyte modified lithium titanate negative electrode material according to any one of claims 1 to 6, characterized in that: the titanium dioxide powder is anatase type industrial grade titanium dioxide.
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| CN111370752A (en) * | 2020-04-08 | 2020-07-03 | 隆能科技(南通)有限公司 | Fast charging and safe low temperature lithium ion battery and method of manufacturing the same |
| CN111276733A (en) * | 2020-04-21 | 2020-06-12 | 隆能科技(南通)有限公司 | Safe low-temperature lithium ion battery capable of being charged and discharged quickly and preparation method thereof |
| US20240186499A1 (en) * | 2021-03-31 | 2024-06-06 | Ube Corporation | Titanium-containing oxide powder, negative electrode active material composition using same, and all-solid-state secondary battery |
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| CN109411706B (en) * | 2018-09-13 | 2021-10-19 | 天津大学 | A modified working electrode and preparation method thereof |
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