CN102328952A - Preparation method for spherical lithium titanate material - Google Patents
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Abstract
The invention discloses a preparation method for a spherical lithium titanate material. The preparation method comprises the following steps of: mixing spherical titanium dioxide and aqueous solution of a lithium compound; performing hydrothermal reaction at the temperature of between 90 and 110 DEG C for 15 to 25 hours; drying and grinding the obtained intermediate; and sintering the intermediate at the high temperature of between 700 and 900 DEG C for 1 to 5 hours to obtain the spherical lithium titanate material. The spherical lithium titanate material prepared by the method has uniform granularity, tap density of 1.0 to 1.2 g/cm<3> and high electrochemical properties, and is an ideal negative electrode material for a high-power lithium ion power cell. The preparation method is simple and practical, low in cost and suitable for industrialized large-scale production.
Description
Technical field
The invention belongs to the lithium-ion secondary cell field of materials, be specifically related to a kind of preparation method who can be used as lithium-ion-power cell with spherical lithium titanate anode material.
Background technology
Automobile industry is the important mainstay industry of national economy, also is the significant industry that embodies national competitiveness.China has become the first in the world automobile production and marketing state; Also will keep quick growth than length China's automobile volume of production and marketing in one period from now on; Expecting the year two thousand twenty automobile pollution will be above 200,000,000; By current automobile fuel ecomomy horizontal estimated, fuel oil for vehicles year consumption will break through 400,000,000 tons, energy security that brings thus and environmental problem will be more outstanding.Therefore, greatly developing energy-conservation and new-energy automobile, accelerate to advance industrialization process energy-conservation and new-energy automobile, is to successfully manage the energy and environment challenge, realizes the inevitable choice of Chinese automobile industry Sustainable development.So need that research and development is high-power, high-energy, long lifetime, high security, low cost and eco-friendly power cell.Lithium-ion secondary cell has advantages such as good cycle, energy density height, voltage platform height, is considered to most possibly be used as the power cell of electromobile.The research and development of lithium-ion-power cell be Eleventh Five-Year Plan, " 863 Program " energy-conservation with the new-energy automobile major project in most important parts; Become state key and support and encourage the project of development; Simultaneously also be the focus of whole world research and development, so it is very necessary to research and develop high-performance, highly secure lithium ion dynamic battery.At present, the negative material of business-like lithium ion battery mainly is a carbon negative pole material, but its first charge-discharge irreversible capacity is higher, security is low, the characteristic of cycle performance difference, is not suitable for the equipment that electromobile etc. needs high current charge-discharge.Lithium titanate has long service life, and overcharging resisting is crossed and put the characteristics good with safety performance, satisfies the high-power demand that discharges and recharges.
At present, the preparation method of lithium titanate mainly is solid phase method and liquid phase method.Wherein, solid phase method is simple and practical, is fit to scale operation.But solid phase method often is difficult to guarantee that batch mixing is even, thereby makes the finished product performance be a greater impact; And mostly the lithium titanate crystal that general solid phase method synthesizes is irregularly shaped, and the big and skewness of material granule size causes by the battery performance of this material not good; And adopt solid phase method under comparatively high temps, (greater than 800 ℃) to carry out the long period thermal treatment of (greater than 15 hours), need the labor energy and time like this.Liquid phase synthesizing methods such as sol-gel method can the controlled small particle size material of preparation size, but its preparation process is loaded down with trivial details, the cycle is long and used organic raw material toxicity is big, cost is high, environment is had pollution, is not suitable for suitability for industrialized production.
Summary of the invention
The present invention mainly be inhomogeneous to batch mixing in the solid-phase synthesis process, thermal treatment temp is high, the time is long and liquid phase method in above-mentioned shortcomings such as complex steps, cost height, provide a kind of pattern to be the high-power lithium ion power cell of regular sphere, excellent performance and suitable commercial scale prodn preparation method with spherical lithium titanate anode material.
For realizing above-mentioned technical purpose, the technical scheme that the present invention adopts is:
A kind of preparation method of spherical lithium titanate material comprises the steps:
1) the preparation lithium concentration is the lithium compound aqueous solution of 0.5～5 mol;
2) spherical tio2 and lithium compound aqueous solution is even, in 90～110 ℃ of hydro-thermal reactions 15～25 hours, obtain midbody particle;
3) the gained midbody is dry and ground 5～30 minutes, 700～900 ℃ of high temperature sinterings are 1～5 hour then, obtain spherical lithium titanate material.
Further, behind the high temperature sintering products obtained therefrom is cooled off, pulverizes, sieves, obtain the spherical lithium titanate material of finished product.
Among the above-mentioned preparation method; The said lithium compound of step 1) can be the inorganic lithium compound, also can be organic lithium salt, from the being easy to get property and the cost consideration of material; Preferred inorganic lithium compound, for example one or more in the lithium compounds such as Lithium Hydroxide MonoHydrate, lithium chloride, lithium nitrate, Lithium Sulphate.
Above-mentioned steps 2) preferably take by weighing spherical tio2 and lithium compound aqueous solution by stoichiometric ratio, the molecular formula of lithium titanate is Li
4Ti
5O
12, in the mixture of the spherical tio2 and the lithium compound aqueous solution ratio of the amount of substance of Ti and Li be 5: 4 better, consider the volatility of lithium compound under the hot conditions, can suitably increase the consumption of lithium compound.
Above-mentioned steps 3) atmosphere of high temperature sintering not being had special qualification, can be air atmosphere or inert atmosphere, and directly sintering has been simplified processing condition greatly in air.
The temperature and time of spherical tio2 particulate size, high temperature sintering has determined the particle size of prepared spherical lithium titanate material, and wherein the particle diameter of spherical tio2 is preferably 0.1～5 μ m.Can prepare spherical tio2 through following method:
A) compound concentration is the titanium sulfate aqueous solution of 0.02～0.5 mol;
B) with titanium sulfate aqueous solution and alcoholic solvent equal-volume mixing, add the pyrrolidinone compounds polymeric surfactant then, it is fully dissolved;
C) with step b) gained mixing solutions 80～90 ℃ of hydrolysis, produce the spherical tio2 hydrate solids;
D) solid-liquid separation obtains the spherical tio2 hydrate, and it is used the pH value of deionized water wash to washing water is till 6～7, drying then, and, obtain spherical tio2 in 600～800 ℃ of thermal treatments 1～5 hour.
The size of product spherical tio2 depends mainly on the concentration of titanium sulfate aqueous solution, and the titanium sulfate aqueous solution concentration that preferred steps a) is prepared is 0.1～0.2 mol, and the size of prepared spherical tio2 is about 1 μ m.
The used alcoholic solvent organic solvent of hydroxyls such as ethanol, n-propyl alcohol, Virahol and propyl carbinol for example in the step b); Said tensio-active agent is Vinylpyrrolidone polymer K30 for example, and its addition is advisable with 4～6 grams per liter mixing solutionss.
The step c) hydrolysis time thoroughly is hydrolyzed to the spherical tio2 hydrate with reactant and is advisable.
The present invention has the following advantages:
1. utilize common raw material, the step through less need not long-time pyroprocessing and can synthesize spherical lithium titanate material.
2. the tap density of prepared spherical lithium titanate material reaches 1.0～1.2g/cm
3This material detects to pure spinel lithium titanate material through X-ray powder diffraction appearance (XRD), does not have other non-spinel impurity to exist mutually; Detect through sem (SEM), this lithium titanate material particle is spherical in shape, the size uniformity; Detect through laser particle size distribution instrument (PSD), the centralized particle diameter of this lithium titanate is about 1 μ m.
3. prepared spherical lithium titanate material has excellent electrochemical properties, comprises cycle performance and high-multiplying power discharge characteristic, is that ideal high-power lithium ion power cell is used negative material.Under the 0.2C current discharge, specific discharge capacity surpasses 160mAh/g, and average every circulation primary capacity attenuation rate is less than 0.04%; Still have 125mAh/g with 4C multiplying power discharging specific storage.
4. it is simple and practical that the present invention prepares the method for spherical lithium titanate material, and cost is low, is fit to commercial scale prodn.
Description of drawings
Fig. 1 is the X-ray powder diffraction pattern of the spherical lithium titanate material of embodiment 1 synthetic.
Fig. 2 is the scanning electron microscope diagram of the spherical lithium titanate material of embodiment 1 synthetic.
Fig. 3 is the particle size distribution figure of the spherical lithium titanate material of embodiment 1 synthetic.
Fig. 4 is the specific discharge capacity cycle diagram of embodiment 1 (800 ℃ of sintering temperatures) and the spherical lithium titanate of embodiment 3 (900 ℃ of sintering temperatures) synthetic.
Embodiment
Through embodiment, technical scheme of the present invention is further specified below.
1. spherical tio2 is synthetic
Compound concentration is the titanium sulfate aqueous solution of 0.2 mol.Measure 1 liter of titanium sulfate aqueous solution for preparing and 1 liter of n-propyl alcohol respectively in 2 liters reaction vessel, mix the back and add 10 gram Vinylpyrrolidone polymer K30, it is fully dissolved.Reaction vessel placed 80 ℃ temperature; Make the mixing solutions hydrolysis obtain the spherical tio2 hydrate in 100 minutes; Afterwards the gained material is changed over to and carry out solid-liquid separation in the solid-liquid separator, and the pH value of solid product to the washing water of use deionized water wash solid-liquid separation gained is 6.Place moisture eliminator dry the solid product of gained, afterwards it is transferred in the alumina crucible, in retort furnace, be warming up to and place 700 ℃ stove with 300 ℃/hour speed; Constant temperature 2 hours; Stop heating, in stove, naturally cool to room temperature, obtain spherical tio2.
2. spherical lithium titanate is synthetic
Compound concentration is the lithium hydroxide aqueous solution of 5 mol.Take by weighing the above-mentioned spherical tio2 that makes of 499.4 grams in hydrothermal reaction kettle, the lithium hydroxide aqueous solution of measuring 1 liter of preparation afterwards mixes in the baking oven that is placed on 100 ℃ and reacted 20 hours in hydrothermal reaction kettle.The hydro-thermal reaction products therefrom is taken out, and drying was also ground 5 minutes, transferred in the alumina crucible.Crucible is placed retort furnace, be warming up to 800 ℃ with 300 ℃/hour speed, constant temperature 2 hours stops heating, in stove, naturally cools to room temperature, obtains spherical lithium titanate product.Through the XRD test, show that material is the lithium titanate of single spinel structure, as shown in Figure 1; Observe through SEM, product particle is even, and is spherical in shape, as shown in Figure 2; The tap density of material is 1.0g/cm
3, through sreen analysis, particle D
50Be about 1 μ m, see Fig. 3.
3. the chemical property of spherical lithium titanate material
Spherical lithium titanate, acetylene black and the electrically conductive graphite that will synthesize, sticker PVDF PVDF by mass ratio 90: 4: 6 (wherein acetylene black and electrically conductive graphite with account for total proportion 4%) mix, be coated on the aluminium foil, be cut into pole piece after the drying.With ionogen LiPF
6It is that to form concentration in 1: 1 the mixing solutions of NSC 11801 (EC)/methylcarbonate (DMC) be the electrolytic solution of 1 mol that salt is dissolved in volume ratio; With the metallic lithium is counter electrode; In being full of the vacuum glove box of argon gas, be assembled into the R2032 button cell, carry out electrochemical property test.Charging/discharging voltage is 1.0～2.5V, and under the 0.2C current discharge, specific discharge capacity surpasses 160mAh/g, and average every circulation primary capacity attenuation rate is less than 0.04%; Still have 125mAh/g with 4C multiplying power discharging specific storage, see that the sintering temperature shown in Fig. 4 is 800 ℃ a curve.
1. spherical tio2 is synthetic
Prepare spherical tio2 according to embodiment 1 identical condition.
2. spherical lithium titanate is synthetic
Substitute 800 ℃ thermal treatment temp with 850 ℃ thermal treatment temps, other condition is identical with embodiment 1.Through the XRD test, show that material is the lithium titanate of single spinel structure; Observe through SEM, product particle is even, and is spherical in shape; The tap density of material is 1.2g/cm
3, through sreen analysis particle D
50Be about 1.3 μ m.
3. the chemical property of spherical lithium titanate material
According to the identical condition assembled battery of embodiment 1.Charging/discharging voltage is 1.0～2.5V, and under the 0.2C current discharge, specific discharge capacity is about 160mAh/g, and average every circulation primary capacity attenuation rate is about 110mAh/g less than 0.04% with 4C multiplying power discharging specific storage.
1. spherical tio2 is synthetic
Prepare spherical tio2 according to embodiment 1 identical condition.
2. spherical lithium titanate is synthetic
Substitute 800 ℃ thermal treatment temp with 900 ℃ thermal treatment temps, other condition is identical with embodiment 1.Through the XRD test, show that material is the lithium titanate of single spinel structure; Observe through sem (SEM), product particle is even, and is spherical in shape; The tap density of material is 1.2g/cm
3, through sreen analysis particle D
50Be about 1.8 μ m.
3. the chemical property of spherical lithium titanate material
According to the identical condition assembled battery of embodiment 1.Charging/discharging voltage is 1.0～2.5V, and under the 0.2C current discharge, specific discharge capacity is about 155mAh/g, and average every circulation primary capacity attenuation rate sees that less than 0.05% the sintering temperature shown in Fig. 4 is 900 ℃ a curve.
1. spherical tio2 is synthetic
Prepare spherical tio2 according to embodiment 1 identical condition.
2. spherical lithium titanate is synthetic
3. the chemical property of spherical lithium titanate material
According to the identical condition assembled battery of embodiment 1.Charging/discharging voltage is 1.0～2.5V, and under the 0.2C current discharge, specific discharge capacity is about 160mAh/g, and average every circulation primary capacity attenuation rate is about 130mAh/g less than 0.04% with 4C multiplying power discharging specific storage.
1. spherical tio2 is synthetic
Prepare spherical tio2 according to embodiment 1 identical condition.
2. spherical lithium titanate is synthetic
3. the chemical property of spherical lithium titanate material
According to the identical condition assembled battery of embodiment 1.Charging/discharging voltage is 1.0～2.5V, and under the 0.2C current discharge, specific discharge capacity is about 140mAh/g, and average every circulation primary capacity attenuation rate is less than 0.04%.
1. spherical tio2 is synthetic
Prepare spherical tio2 according to embodiment 1 identical condition.
2. spherical lithium titanate is synthetic
3. the chemical property of spherical lithium titanate material
According to the identical condition assembled battery of embodiment 1.Charging/discharging voltage is 1.0～2.5V, and under the 0.2C current discharge, specific discharge capacity is about 140mAh/g, and average every circulation primary capacity attenuation rate is less than 0.05%.
1. spherical tio2 is synthetic
Prepare spherical tio2 according to embodiment 1 identical condition.
2. spherical lithium titanate is synthetic
With 15 minutes alternative 5 minutes midbody milling time, other condition was identical with embodiment 1.Through the XRD test, show that material is the lithium titanate of single spinel structure; Observe through SEM, product particle is even, and is spherical in shape; The tap density of material is 1.0g/cm
3, through sreen analysis, particle D
50Be about 1 μ m.
3. the chemical property of spherical lithium titanate material
According to the identical condition assembled battery of embodiment 1.Charging/discharging voltage is 1.0～2.5V, and under the 0.2C current discharge, specific discharge capacity surpasses about 160mAh/g, and average every circulation primary capacity attenuation rate is less than 0.05%; Still have 120mAh/g with 4C multiplying power discharging capacity.
1. spherical tio2 is synthetic
2. spherical lithium titanate is synthetic
Prepare spherical lithium titanate according to embodiment 1 identical condition.Through the XRD test, show that material is the lithium titanate of single spinel structure; Observe through SEM, product particle is even, and is spherical in shape; The tap density of material is 1.0g/cm
3, through sreen analysis, particle D
50Be about 1 μ m.
3. the chemical property of spherical lithium titanate material
According to the identical condition assembled battery of embodiment 1.Charging/discharging voltage is 1.0～2.5V, and under the 0.2C current discharge, specific discharge capacity is about 160mAh/g, and average every circulation primary capacity attenuation rate is less than 0.05%; Still have 120mAh/g with 4C multiplying power discharging capacity.
Can find out that from above embodiment the product of employing gained of the present invention is the lithium titanate of single phase spinel structure, the shape particle diameter is even, consistent, and is spherical in shape.Under optimal conditions, promptly titanium oxide and lithium hydroxide aqueous solution were 100 ℃ of reactions 20 hours, and in 800 ℃, the chemical property of 2 hours spherical lithium titanates of gained of thermal treatment is best, the most suitable equally commercial scale prodn of this optimal conditions after the drying and grinding.
Claims (9)
1. the preparation method of a spherical lithium titanate material may further comprise the steps:
1) the preparation lithium concentration is the lithium compound aqueous solution of 0.5～5 mol;
2) spherical tio2 and lithium compound aqueous solution is even, in 90～110 ℃ of hydro-thermal reactions 15～25 hours, obtain midbody particle;
3) the gained midbody is dry and ground 5～30 minutes, 700～900 ℃ of high temperature sinterings are 1～5 hour then, obtain spherical lithium titanate material.
2. preparation method as claimed in claim 1 is characterized in that, the said lithium compound of step 1) is the inorganic lithium compound, is selected from Lithium Hydroxide MonoHydrate, lithium chloride, lithium nitrate, the Lithium Sulphate one or more.
3. preparation method as claimed in claim 1 is characterized in that step 2) particle diameter of used spherical tio2 is 0.1～5 μ m.
4. preparation method as claimed in claim 1 is characterized in that step 3) is high temperature sintering in air.
5. preparation method as claimed in claim 1 is characterized in that, prepares said spherical tio2 through following step:
A) compound concentration is the titanium sulfate aqueous solution of 0.02～0.5 mol;
B) with titanium sulfate aqueous solution and alcoholic solvent equal-volume mixing, add the pyrrolidinone compounds polymeric surfactant then, it is fully dissolved;
C) with step b) gained mixing solutions 80～90 ℃ of hydrolysis, produce the spherical tio2 hydrate solids;
D) solid-liquid separation obtains the spherical tio2 hydrate, and it is used the pH value of deionized water wash to washing water is till 6～7, drying then, and, obtain spherical tio2 in 600～800 ℃ of thermal treatments 1～5 hour.
6. preparation method as claimed in claim 5 is characterized in that, the titanium sulfate aqueous solution concentration that step a) is prepared is 0.1～0.2 mol.
7. preparation method as claimed in claim 5 is characterized in that, the said organic solvent of step b) is selected from one or more in ethanol, n-propyl alcohol, Virahol and the propyl carbinol.
8. preparation method as claimed in claim 5 is characterized in that, the said tensio-active agent of step b) is selected from Vinylpyrrolidone polymer K30.
9. preparation method as claimed in claim 8 is characterized in that, the addition of Vinylpyrrolidone polymer K30 is 4～6 grams per liter mixing solutionss in the step b).
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Cited By (10)
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| CN103346309A (en) * | 2013-06-24 | 2013-10-09 | 中国科学院长春应用化学研究所 | Preparation method of negative material lithium titanate for lithium-ion power battery |
| CN104282906A (en) * | 2014-09-19 | 2015-01-14 | 清华大学深圳研究生院 | Lithium titanate material of micro-nano structure and preparation method of lithium titanate material |
| CN104944465A (en) * | 2015-06-15 | 2015-09-30 | 山东玉皇新能源科技有限公司 | Preparation method and application of lithium titanate anode material |
| CN105958018A (en) * | 2016-05-10 | 2016-09-21 | 内蒙古科技大学 | Preparation method for vanadium-doped lithium titanate negative electrode material |
| CN109148858A (en) * | 2018-08-29 | 2019-01-04 | 西安交通大学苏州研究院 | A kind of lithium titanate-composite titania material and the preparation method and application thereof |
| CN109860541A (en) * | 2018-12-21 | 2019-06-07 | 上海纳米技术及应用国家工程研究中心有限公司 | The preparation of tubulose lithium titanate/composite titania material and product and application with rule defect |
| CN112072080A (en) * | 2019-06-11 | 2020-12-11 | 中国科学院过程工程研究所 | Preparation method of lithium titanate-titanium dioxide composite porous microsphere negative electrode material |
| CN112103494A (en) * | 2020-08-07 | 2020-12-18 | 华北电力大学 | Preparation method of high-purity lithium titanate material with controllable nano structure |
| CN113178552A (en) * | 2021-03-26 | 2021-07-27 | 四川大学 | High-tap-density porous silicon-carbon composite material, preparation method thereof and application of negative electrode of lithium ion battery |
| CN115799486A (en) * | 2023-02-03 | 2023-03-14 | 中国华能集团清洁能源技术研究院有限公司 | Micron-sized lithium titanate and multi-walled carbon nanotube composite material and preparation method and application thereof |
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| CN103346309A (en) * | 2013-06-24 | 2013-10-09 | 中国科学院长春应用化学研究所 | Preparation method of negative material lithium titanate for lithium-ion power battery |
| CN104282906A (en) * | 2014-09-19 | 2015-01-14 | 清华大学深圳研究生院 | Lithium titanate material of micro-nano structure and preparation method of lithium titanate material |
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| CN109148858A (en) * | 2018-08-29 | 2019-01-04 | 西安交通大学苏州研究院 | A kind of lithium titanate-composite titania material and the preparation method and application thereof |
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| CN109860541A (en) * | 2018-12-21 | 2019-06-07 | 上海纳米技术及应用国家工程研究中心有限公司 | The preparation of tubulose lithium titanate/composite titania material and product and application with rule defect |
| CN109860541B (en) * | 2018-12-21 | 2022-07-05 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation of tubular lithium titanate/titanium dioxide composite material with regular defects, product and application |
| CN112072080A (en) * | 2019-06-11 | 2020-12-11 | 中国科学院过程工程研究所 | Preparation method of lithium titanate-titanium dioxide composite porous microsphere negative electrode material |
| CN112103494A (en) * | 2020-08-07 | 2020-12-18 | 华北电力大学 | Preparation method of high-purity lithium titanate material with controllable nano structure |
| CN113178552A (en) * | 2021-03-26 | 2021-07-27 | 四川大学 | High-tap-density porous silicon-carbon composite material, preparation method thereof and application of negative electrode of lithium ion battery |
| CN115799486A (en) * | 2023-02-03 | 2023-03-14 | 中国华能集团清洁能源技术研究院有限公司 | Micron-sized lithium titanate and multi-walled carbon nanotube composite material and preparation method and application thereof |
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