CN102328952B - 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 lithium-ion secondary cell Material Field, be specifically related to a kind of preparation method of spherical lithium titanate cathode material for lithium-ion-power cell that can be used as.
Background technology
Automobile industry is the important mainstay industry of national economy, is also the significant industry that embodies national competitiveness.China has become the first in the world automobile production and marketing state, in compare Chang Yiduan China in period automobile volume of production and marketing from now on, also will keep the rapid growth impetus, expecting the year two thousand twenty automobile pollution will be over 200,000,000, by current automobile fuel ecomomy horizontal estimated, fuel oil for vehicles Year's consumption will be broken through 400,000,000 tons, and the energy security bringing thus and environmental problem will be more outstanding.Therefore, greatly developing energy-conservation and new-energy automobile, accelerate the industrialization process of propulsion energy-saving and new-energy automobile, is to successfully manage the energy and environment challenge, realizes the inevitable choice of Chinese Auto Industry Sustainable development.So just need to research and develop high-power, high-energy, long lifetime, high security, low cost and eco-friendly power cell.Lithium-ion secondary cell has the advantages such as good cycle, energy density is high, voltage platform is high, is considered to most possibly be used as the power cell of electromobile.The research and development of lithium-ion-power cell is most important part in the energy-conservation and new-energy automobile major project of Eleventh Five-Year Plan, " 863 Program ", become state key and support and encourage the project of development, also simultaneously the focus of whole world research and development, so research and development high-performance, highly secure lithium ion dynamic battery are very necessary.At present, the negative material of business-like lithium ion battery is mainly carbon negative pole material, but its characteristic that first charge-discharge irreversible capacity is higher, security is low, cycle performance is poor 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 feature good with safety performance, meets the high-power demand discharging and recharging.
At present, the preparation method of lithium titanate is mainly solid phase method and liquid phase method.Wherein, solid phase method is simple and practical, is applicable to scale operation.But solid phase method is often difficult to guarantee that batch mixing is even, thereby the finished product performance is a greater impact; And the lithium titanate crystal that general solid phase method synthesizes mostly is irregularly shaped, the large and skewness of material granule size, causes the battery performance made by this material not good; And adopt solid phase method under comparatively high temps, (to be greater than 800 ℃) to carry out the long period thermal treatment of (being greater than 15 hours), need expend mass energy and time like this.The 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 compared with long and organic raw material toxicity used is large, cost is high, environment is had to pollution, is not suitable for suitability for industrialized production.
Summary of the invention
The present invention be mainly in solid-phase synthesis process, batch mixing is inhomogeneous, thermal treatment temp is high, the time is long and liquid phase method in complex steps, the above-mentioned shortcoming of high in cost of production, that a kind of pattern is provided is rule is spherical, the preparation method of spherical lithium titanate cathode material for the high-power lithium ion power cell of excellent performance and applicable commercial scale production.
For realizing above-mentioned technical purpose, the technical solution used in the present invention is:
A preparation method for spherical lithium titanate material, comprises the steps:
1) preparation lithium concentration is the lithium compound aqueous solution of 0.5～5 mol/L;
2) spherical tio2 and lithium compound aqueous solution is even, in 90～110 ℃ of hydro-thermal reactions 15～25 hours, obtain midbody particle;
3) gained intermediate is dried and is ground 5～30 minutes, then 700～900 ℃ of high temperature sinterings are 1～5 hour, obtain spherical lithium titanate material.
Further, after high temperature sintering, products obtained therefrom is cooling, pulverize, sieve, obtain finished product spherical lithium titanate material.
In above-mentioned preparation method, step 1) described lithium compound can be inorganic lithium compound, can be also organic lithium salt, from being easy to get property and the cost consideration of material, preferred inorganic lithium compound, one or more in lithium compounds such as lithium hydroxide, lithium chloride, lithium nitrate, Lithium Sulphate.
Above-mentioned steps 2) preferably by stoichiometric ratio, take spherical tio2 and lithium compound aqueous solution, the molecular formula of lithium titanate is Li
4ti
5o
12, in the mixture of 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 hot conditions, can suitably increase the consumption of lithium compound.
Above-mentioned steps 3) atmosphere of high temperature sintering being not particularly limited, can be air atmosphere or inert atmosphere, and directly in air, sintering has been simplified processing condition greatly.
The size of spherical tio2 particle, the temperature and time of high temperature sintering have determined the granular 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 by following method:
A) compound concentration is the titanium sulfate aqueous solution of 0.02～0.5 mol/L;
B) titanium sulfate aqueous solution and alcoholic solvent equal-volume are mixed, then add pyrrolidinone compounds polymeric surfactant, it is fully dissolved;
C) by step b) gained mixing solutions is 80～90 ℃ of hydrolysis, produces spherical tio2 hydrate solids;
D) solid-liquid separation obtains spherical tio2 hydrate, by it, by deionized water wash to the pH value of washing water, is till 6～7, is then dried, and in 600～800 ℃ of thermal treatments 1～5 hour, obtains spherical tio2.
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/L, and the size of prepared spherical tio2 is in 1 μ m left and right.
Step b) organic solvent of the hydroxyls such as alcoholic solvent such as ethanol, n-propyl alcohol, Virahol and propyl carbinol used in; Described tensio-active agent is PVP K30 for example, and its addition is advisable with 4～6 grams per liter mixing solutionss.
Step c) hydrolysis time is thoroughly hydrolyzed to spherical tio2 hydrate with reactant and is advisable.
The present invention has the following advantages:
1. utilize common raw material, through less step, without long-time pyroprocessing, can synthesize spherical lithium titanate material.
2. the tap density of prepared spherical lithium titanate material reaches 1.0～1.2g/cm
3.This material detects as pure spinel lithium titanate material through X-ray powder diffraction instrument (XRD), without other non-spinel impurity phases, exists; Through scanning electronic microscope (SEM), detect, this lithium titanate material particle is spherical in shape, size uniformity; Through laser fineness gage (PSD), detect, the centralized particle diameter of this lithium titanate is in 1 μ m left and right.
3. prepared spherical lithium titanate material has good chemical property, comprises cycle performance and high-multiplying-power discharge performance, is desirable high-power lithium ion power cell negative material.Under 0.2C current discharge, specific discharge capacity surpasses 160mAh/g, and average every circulation primary capacity attenuation rate is less than 0.04%; With 4C multiplying power discharging specific storage, still have 125mAh/g.
4. the present invention prepares the method simple practical of spherical lithium titanate material, and cost is low, is applicable to commercial scale production.
Accompanying drawing explanation
Fig. 1 is the X-ray powder diffraction pattern of the synthetic spherical lithium titanate material of embodiment 1.
Fig. 2 is the scanning electron microscope diagram of the synthetic spherical lithium titanate material of embodiment 1.
Fig. 3 is the particle size distribution figure of the synthetic spherical lithium titanate material of embodiment 1.
Fig. 4 is the specific discharge capacity cycle diagram of the synthetic spherical lithium titanate of embodiment 1 (800 ℃ of sintering temperatures) and embodiment 3 (900 ℃ of sintering temperatures).
Embodiment
Below by embodiment, technical scheme of the present invention is further described in detail.
1. spherical tio2 is synthetic
Compound concentration is the titanium sulfate aqueous solution of 0.2 mol/L.Measure respectively 1 liter of titanium sulfate aqueous solution preparing and 1 liter of n-propyl alcohol in the reaction vessel of 2 liters, after mixing, add 10 grams of PVP K30s, it is fully dissolved.Reaction vessel is placed in to the temperature of 80 ℃, make mixing solutions hydrolysis within 100 minutes, obtain spherical tio2 hydrate, afterwards gained material is proceeded to and in solid-liquid separator, carry out solid-liquid separation, and be 6 by the solid product of deionized water wash solid-liquid separation gained to the pH value of washing water.The solid product of gained is placed in to moisture eliminator dry, is transferred to afterwards in alumina crucible, the speed with 300 ℃/h in retort furnace is warming up to the stove that is placed in 700 ℃, 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/L.Take 499.4 grams of above-mentioned spherical tio2s that make in hydrothermal reaction kettle, measure afterwards the lithium hydroxide aqueous solution of 1 liter of preparation in hydrothermal reaction kettle, be uniformly mixed in the baking oven that is placed on 100 ℃ and react 20 hours.Hydro-thermal reaction products therefrom is taken out, be dried and grind 5 minutes, transfer in alumina crucible.Crucible is placed in to retort furnace, with the speed of 300 ℃/h, is warming up to 800 ℃, constant temperature 2 hours, stops heating, naturally cools to room temperature in stove, obtains spherical lithium titanate product.Through XRD test, show that material is the lithium titanate of single spinel structure, as shown in Figure 1; Through SEM, observe, product particle is even, spherical in shape, as shown in Figure 2; The tap density of material is 1.0g/cm
3, through sreen analysis, particle D
50be 1 μ m left and right, see Fig. 3.
3. the chemical property of spherical lithium titanate material
By the spherical lithium titanate, acetylene black and the electrically conductive graphite that synthesize, binding agent poly(vinylidene fluoride) PVDF 90: 4: 6 in mass ratio (wherein acetylene black and electrically conductive graphite and account for total proportion 4%) mix, be coated on aluminium foil, after being dried, be cut into pole piece.By ionogen LiPF
6it is to form the electrolytic solution that concentration is 1 mol/L in the mixing solutions of NSC 11801 (EC)/methylcarbonate (DMC) of 1: 1 that salt is dissolved in volume ratio, take metallic lithium as to electrode, in being full of the vacuum glove box of argon gas, be assembled into R2032 button cell, carry out electrochemical property test.Charging/discharging voltage is 1.0～2.5V, and under 0.2C current discharge, specific discharge capacity surpasses 160mAh/g, and average every circulation primary capacity attenuation rate is less than 0.04%; With 4C multiplying power discharging specific storage, still have 125mAh/g, see that the sintering temperature shown in Fig. 4 is the curve of 800 ℃.
1. spherical tio2 is synthetic
According to the condition that embodiment 1 is identical, prepare spherical tio2.
2. spherical lithium titanate is synthetic
With the thermal treatment temps of 850 ℃, substitute the thermal treatment temp of 800 ℃, other condition is identical with embodiment 1.Through XRD test, show that material is the lithium titanate of single spinel structure; Through SEM, observe, product particle is even, spherical in shape; The tap density of material is 1.2g/cm
3, through sreen analysis particle D
50be 1.3 μ m left and right.
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 0.2C current discharge, specific discharge capacity is in 160mAh/g left and right, and average every circulation primary capacity attenuation rate is less than 0.04%, take 4C multiplying power discharging specific storage as 110mAh/g left and right.
1. spherical tio2 is synthetic
According to the condition that embodiment 1 is identical, prepare spherical tio2.
2. spherical lithium titanate is synthetic
With the thermal treatment temps of 900 ℃, substitute the thermal treatment temp of 800 ℃, other condition is identical with embodiment 1.Through XRD test, show that material is the lithium titanate of single spinel structure; Through scanning electronic microscope (SEM), observe, product particle is even, spherical in shape; The tap density of material is 1.2g/cm
3, through sreen analysis particle D
50be 1.8 μ m left and right.
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 0.2C current discharge, specific discharge capacity is in 155mAh/g left and right, and average every circulation primary capacity attenuation rate is less than 0.05%, sees that the sintering temperature shown in Fig. 4 is the curve of 900 ℃.
1. spherical tio2 is synthetic
According to the condition that embodiment 1 is identical, prepare spherical tio2.
2. spherical lithium titanate is synthetic
With the hydrothermal temperatures of 25 hours, 90 ℃, substitute the hydrothermal temperature of 20 hours, 100 ℃, other condition is identical with embodiment 1.Through XRD test, show that material is the lithium titanate of single spinel structure; Through SEM, observe, product particle is even, spherical in shape; The tap density of material is 1.2g/cm
3, through sreen analysis particle D
50it is 1 μ m left and right.
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 0.2C current discharge, specific discharge capacity is in 160mAh/g left and right, and average every circulation primary capacity attenuation rate is less than 0.04%, take 4C multiplying power discharging specific storage as 130mAh/g left and right.
1. spherical tio2 is synthetic
According to the condition that embodiment 1 is identical, prepare spherical tio2.
2. spherical lithium titanate is synthetic
With the heat treatment time of 1 hour, substitute the heat treatment time of 2 hours, other condition is identical with embodiment 1.Through XRD test, show that material is the lithium titanate of single spinel structure; Through SEM, observe, product particle is even, spherical in shape; The tap density of material is 1.0g/cm
3.
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 0.2C current discharge, specific discharge capacity is in 140mAh/g left and right, and average every circulation primary capacity attenuation rate is less than 0.04%.
1. spherical tio2 is synthetic
According to the condition that embodiment 1 is identical, prepare spherical tio2.
2. spherical lithium titanate is synthetic
With the heat treatment times of 5 hours, substitute the heat treatment time of 2 hours, other condition is identical with embodiment 1.Through XRD test, show that material is the lithium titanate of single spinel structure; Through SEM, observe, product particle is even, spherical in shape; The tap density of material is 1.2g/cm
3.
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 0.2C current discharge, specific discharge capacity is in 140mAh/g left and right, and average every circulation primary capacity attenuation rate is less than 0.05%.
1. spherical tio2 is synthetic
According to the condition that embodiment 1 is identical, prepare spherical tio2.
2. spherical lithium titanate is synthetic
With the intermediate milling time of 15 minutes alternative 5 minutes, other condition was identical with embodiment 1.Through XRD test, show that material is the lithium titanate of single spinel structure; Through SEM, observe, product particle is even, spherical in shape; The tap density of material is 1.0g/cm
3, through sreen analysis, particle D
50it is 1 μ m left and right.
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 0.2C current discharge, specific discharge capacity surpasses 160mAh/g left and right, and average every circulation primary capacity attenuation rate is less than 0.05%; With 4C multiplying power discharging capacity, still have 120mAh/g.
1. spherical tio2 is synthetic
With the hydrolysis temperatures of 85 ℃, substitute the hydrolysis temperature of 80 ℃, other condition is identical with embodiment 1.
2. spherical lithium titanate is synthetic
According to the identical condition of embodiment 1, prepare spherical lithium titanate.Through XRD test, show that material is the lithium titanate of single spinel structure; Through SEM, observe, product particle is even, spherical in shape; The tap density of material is 1.0g/cm
3, through sreen analysis, particle D
50it is 1 μ m left and right.
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 0.2C current discharge, specific discharge capacity is in 160mAh/g left and right, and average every circulation primary capacity attenuation rate is less than 0.05%; With 4C multiplying power discharging capacity, still have 120mAh/g.
As can be seen from the above embodiments, the product of employing gained of the present invention is the lithium titanate of single-phase spinel structure, and shape particle diameter evenly, unanimously, spherical in shape.Under optimal conditions, titanium dioxide reacts 20 hours at 100 ℃ with lithium hydroxide aqueous solution, and after drying and grinding, in 800 ℃, the chemical property of 2 hours spherical lithium titanates of gained of thermal treatment is best, the most applicable equally commercial scale production of this optimal conditions.
Claims (7)
1. a preparation method for spherical lithium titanate material, comprises the following steps:
1) preparation lithium concentration is the lithium compound aqueous solution of 0.5～5 mol/L;
2) prepare spherical tio2, its step comprises:
A) compound concentration is the titanium sulfate aqueous solution of 0.02～0.5 mol/L;
B) titanium sulfate aqueous solution and alcoholic solvent equal-volume are mixed, then add pyrrolidinone compounds polymeric surfactant, it is fully dissolved;
C) by step b) gained mixing solutions 80～90 ℃ of hydrolysis, produce spherical tio2 hydrate solids;
D) solid-liquid separation obtains spherical tio2 hydrate, by it, by deionized water wash to the pH value of washing water, is till 6～7, is then dried, and in 600～800 ℃ of thermal treatments 1～5 hour, obtains spherical tio2;
3) by particle diameter, be that spherical tio2 and the lithium compound aqueous solution of 0.1～5 μ m is even, in 90～110 ℃ of hydro-thermal reactions 15～25 hours, obtain midbody particle;
4) gained intermediate is dried and is ground 5～30 minutes, then 700～900 ℃ of high temperature sinterings are 1～5 hour, obtain spherical lithium titanate material.
2. preparation method as claimed in claim 1, is characterized in that, lithium compound is inorganic lithium compound described in step 1), is selected from one or more in lithium hydroxide, lithium chloride, lithium nitrate, Lithium Sulphate.
3. preparation method as claimed in claim 1, is characterized in that, step 4) is high temperature sintering in air.
4. preparation method as claimed in claim 1, is characterized in that, the titanium sulfate aqueous solution concentration that step a) is prepared is 0.1～0.2 mol/L.
5. preparation method as claimed in claim 1, is characterized in that, organic solvent is selected from one or more in ethanol, n-propyl alcohol, Virahol and propyl carbinol described in step b).
6. preparation method as claimed in claim 1, is characterized in that, tensio-active agent is selected from PVP K30 described in step b).
7. preparation method as claimed in claim 6, is characterized in that, in step b), the addition of PVP K30 is 4～6 grams per liter mixing solutionss.
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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 |
| CN104282906B (en) * | 2014-09-19 | 2017-04-12 | 清华大学深圳研究生院 | Lithium titanate material of micro-nano structure and preparation method of lithium titanate material |
| CN104944465B (en) * | 2015-06-15 | 2017-07-11 | 山东玉皇新能源科技有限公司 | A kind of preparation method and applications 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 |
| CN109148858B (en) * | 2018-08-29 | 2021-12-07 | 西安交通大学苏州研究院 | Lithium titanate-titanium dioxide composite material and preparation method and application thereof |
| 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 |
| CN113178552B (en) * | 2021-03-26 | 2023-03-10 | 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 |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101279766A (en) * | 2008-04-25 | 2008-10-08 | 陕西科技大学 | Preparation of spherical nano-titanic oxide |
| CN101696109A (en) * | 2009-10-19 | 2010-04-21 | 青岛科技大学 | Method for preparing mesoporous titanium dioxide microspheres |
| JP2010228980A (en) * | 2009-03-27 | 2010-10-14 | Jgc Catalysts & Chemicals Ltd | Method for manufacturing crystalline lithium titanate, and crystalline lithium titanate |
| CN101967009A (en) * | 2010-11-09 | 2011-02-09 | 中国海洋石油总公司 | Method for preparing lithium titanate cathode material for lithium ion power batteries |
-
2011
- 2011-06-30 CN CN201110183575.8A patent/CN102328952B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101279766A (en) * | 2008-04-25 | 2008-10-08 | 陕西科技大学 | Preparation of spherical nano-titanic oxide |
| JP2010228980A (en) * | 2009-03-27 | 2010-10-14 | Jgc Catalysts & Chemicals Ltd | Method for manufacturing crystalline lithium titanate, and crystalline lithium titanate |
| CN101696109A (en) * | 2009-10-19 | 2010-04-21 | 青岛科技大学 | Method for preparing mesoporous titanium dioxide microspheres |
| CN101967009A (en) * | 2010-11-09 | 2011-02-09 | 中国海洋石油总公司 | Method for preparing lithium titanate cathode material for lithium ion power batteries |
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Effective date of registration: 20140123 Address after: 100871 Beijing the Summer Palace Road, Haidian District, No. 5 Applicant after: Peking University Applicant after: Hohhot Ruozi New Energy Co., Ltd. Applicant after: University of Science and Technology of Inner Mongolia Address before: 100871 Beijing the Summer Palace Road, Haidian District, No. 5 Applicant before: Peking University Applicant before: Hohhot Ruozi New Energy Co., Ltd. |
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