CN101391806A - Method for manufacturing spinelle lithium titanate for lithium ionic cell cathode material - Google Patents
Method for manufacturing spinelle lithium titanate for lithium ionic cell cathode material Download PDFInfo
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- CN101391806A CN101391806A CNA2007101220742A CN200710122074A CN101391806A CN 101391806 A CN101391806 A CN 101391806A CN A2007101220742 A CNA2007101220742 A CN A2007101220742A CN 200710122074 A CN200710122074 A CN 200710122074A CN 101391806 A CN101391806 A CN 101391806A
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Abstract
The invention provides a method for preparing spinel lithium titanate used for the negative electrode materials of lithium ion batteries, which comprises the following steps of: mixing compounds of metatitanic acid and lithium according to an atomic ratio of lithium to titanium between 0.8 and 0.88; adding into carbon or powder former body of the carbon; carrying out an even mixing for 5 to 72 hours in a medium and then drying the mixture; carrying out treatment for 2 to 20 hours under the temperature between 200 and 500 DEG C; then synthesizing for 2 to 72 hours under the temperature between 600 and 900 DEG C, to acquire spinel-structure lithium titanate for the negative electrode materials of the lithium ion batteries. Adopting the cheap metatitanic acid as the raw materials and adding into the carbon or powder former body of the carbons, the method for preparing spinel lithium titanate for the negative electrode materials of the lithium ion batteries realizes the synthesis of spinel-structure lithium titanate with grains diameter less than 500 nanometers under lower temperatures and greatly improves the rate capacity, while the traditional high-temperature solid state method, with a sintering temperature generally between 800 and 100 DEG centigrade, only produces larger lithium carbonate particles at micron levels. With simple technique and strong operability, the method for preparing spinel lithium titanate for the negative electrode materials of the lithium ion batteries is easy to realize large-scale production.
Description
Technical field
The present invention relates generally to a kind of lithium ionic cell cathode material spinelle lithium titanate (Li that is used for
4Ti
5O
12) the preparation method, belong to the lithium ion battery negative material preparing technical field.
Background technology
From nineteen ninety Sony corporation of Japan develop adopt refinery coke to be the lithium ion battery of negative pole since, carbon material just is subjected to people's attention, kind comprises synthetic graphite, natural graphite, carbonaceous mesophase spherules, petroleum coke, carbon fiber etc., is the main negative material of commercialization lithium ion battery.But there is following shortcoming in carbon material: 1 and electrolytic solution react, form SEI, cause first charge-discharge efficiency lower; 2, at the easy metal refining lithium of negative terminal surface, adding charging does not have tangible voltage indication latter stage, causes safety issue easily; 3, poor with the electrolytic solution consistency, as the electrolytic solution that contains PC produces insertion altogether etc. in the graphite-like carbon material; 4, volume change is bigger in the charge and discharge process, and cyclical stability is undesirable.Compare with carbon material, the structural changes of lithium titanate with spinel structure charge and discharge process is very little, a kind of zero strain material of being known as, thereby have good cyclical stability; With respect to metallic lithium, plateau potential is about 1.55V, and away from the metallic lithium sedimentation potential, charging in addition exists tangible voltage indication latter stage, so security is better; Good with the electrolytic solution consistency on the other hand, initial charge does not have the SEI film to form, and efficiency for charge-discharge is higher.In view of above-mentioned advantage, lithium titanate with spinel structure is considered to a kind of new type lithium ion battery negative material of excellence, also is a kind of promising asymmetric super capacitor anode material simultaneously.
Lithium titanate (Li
4Ti
5O
12) the preparation method conventional high-temperature solid phase method, sol-gel method etc. are generally arranged, the conventional high-temperature solid phase method is with TiO
2With Li
2CO
3Perhaps LiOH etc. is synthetic under 800 ℃～1000 ℃ high temperature, and in general 12～24 hours of reaction times, this method advantage is that technology is simple, scale operation easily, and shortcoming is that the product particle is thicker, generally all is micron order, lack of homogeneity; It is precursor that sol-gel method generally adopts organic alkoxide of titanium and lithium; prepare target product through hydrolysis and sol gel process; this method is compared with the conventional high-temperature solid phase method; product chemical purity height, good uniformity, particle are thinner etc.; but this method has adopted organic compound to cause cost to raise; complicated operation is not suitable for large-scale production in addition.
Summary of the invention
The metatitanic acid that the objective of the invention is to cheapness is a raw material, adds carbon or carbon precursor, reduces conventional high-temperature solid phase method sintering temperature, obtains the tiny lithium titanate of particle; A kind of strong operability is provided, and technology is simple, and product performance are better than the preparation method of conventional high-temperature solid phase method.
For achieving the above object, the present invention takes following technical scheme:
A kind of preparation method who is used for lithium ionic cell cathode material spinelle lithium titanate, the compound of metatitanic acid, lithium is prepared burden according to atomic ratio Li/Ti=0.8～0.88, the precursor that adds carbon or carbon again, uniform mixing is 5～72 hours in medium, dry then, under 200 ℃～500 ℃ conditions, handled 2～20 hours again, be then under 600 ℃～900 ℃ conditions Synthetic 2～72 hour to obtain lithium ion battery lithium titanate with spinel structure negative material.
The compound of said lithium is one or more mixtures in lithium hydroxide, Quilonum Retard, lithium chloride, lithium iodide, lithium nitrate, Trilithium phosphate, Lithium Acetate and the lithium oxalate.
Said carbon is graphite, acetylene black, and carbon matrix precursor is one or more in polyoxyethylene glycol, polyvinyl alcohol and the sugar, and add-on accounts for 2～30wt% of gross weight.Gross weight described here is the gross weight of raw material, i.e. the gross weight of the precursor of the compound of metatitanic acid, lithium and carbon or carbon.
Said medium is that water, ethanol, acetone, propyl carbinol, n-propyl alcohol, Virahol, second are fine, one or more mixtures in the ether, thanomin.
Said drying temperature is 70 ℃～200 ℃.The exsiccant purpose is that the liquid medium in the mixed material is vapored away, and therefore, the exsiccant time is as the criterion so that liquid medium is vapored away.
It is raw material that the present invention adopts cheap metatitanic acid, the precursor that in starting material, adds carbon or carbon, reduced synthesis temperature, the particle that the precursor of these carbon or carbon has suppressed lithium titanate in reaction process is grown up, and the high temperature solid-state method of comparing has obtained the less lithium titanate product of particle diameter.The principal element of decision lithium ion battery charge-discharge velocity is the rate of diffusion of lithium ion in electrode solid phase inside, if reduce the lithium titanate particle size, can effectively improve the material high rate during charging-discharging, improves the lithium ion battery power characteristic.The spinel lithium titanate of the present invention's preparation shows excellent chemical property as lithium ion battery negative, has broad application prospects.
Positive effect of the present invention is that the cheap metatitanic acid of employing is starting material, the method that adds carbon or carbon precursor, realized that synthetic particle diameter is less than the lithium titanate with spinel structure of 500 nanometers under the lesser temps, its high rate performance is greatly improved, and conventional high-temperature solid phase method sintering temperature is generally 800 ℃～1000 ℃, and the Quilonum Retard particle that obtains is thick, generally is micron-sized product.This method technology is simple, workable, easy realization of large-scale production.
Description of drawings
Fig. 1 embodiment 1 granule-morphology
Fig. 2 embodiment 2 granule-morphologies
Fig. 3 comparative example granule-morphology
Fig. 4 embodiment 3XRD spectrogram
Fig. 5 embodiment 3 charging and discharging curves
Fig. 6 embodiment 1 cyclic curve
Fig. 7 embodiment 1 high rate performance
Fig. 8 comparative example high rate performance
Embodiment
Method of the present invention is synthesized according to following steps:
(1), with the metatitanic acid is the titanium source, with Quilonum Retard or lithium hydroxide etc. is the lithium source, prepares burden according to the ratio of lithium titanium mol ratio 0.8～0.88, and adds the carbon of 5～30wt% of all raw material gross weights or the precursor of carbon, and in medium uniform mixing 5～72 hours, drying;
(2), the exsiccant solid mixture was put into 200 ℃～500 ℃ subzero treatment of retort furnace 2～20 hours, reaction 2-72 hour under 600～900 ℃ of high temperature then naturally cools to room temperature, obtains lithium ion battery lithium titanate with spinel structure negative material.
The lithium source that the present invention selects for use is one or more mixtures in lithium hydroxide, Quilonum Retard, lithium chloride, lithium iodide, lithium nitrate, Trilithium phosphate, Lithium Acetate, the lithium oxalate; Carbon of selecting for use or carbon precursor are selected from one or several in graphite, acetylene black, polyvinyl alcohol, polyoxyethylene glycol, the sugar.
In order to detect physics and the chemical property of lithium ion battery of the present invention, carry out structured testing with Dutch X ' Pert PRO MPD type XRD diffractometer with lithium titanate anode material; Adopt Japanese HITACHI S-4800 field emission scanning electron microscope instrument (5.0kv, 8.7mm * 1.00k) lithium titanate is carried out the SEM morphology analysis; The method of all knowing with the those of ordinary skill under this area, it is assembled into flat test cell carries out electrochemical property test, with lithium ion battery of the present invention lithium titanate material 83% (weight percentage), binding agent PVDF (polyvinylidene difluoride (PVDF)) 10%, acetylene black 7% is mixed the furnishing pulpous state, be coated on the two sides of Copper Foil,, make electrode at air drying.Counter electrode is formed test cell for the lithium tinsel.Electrolytic solution is 1M (mol/L) LiPF
6/ EC+DMC etc., EC are NSC 11801, and DMC is a methylcarbonate.Charging and discharging currents density 0.1C～1C, discharging and recharging upper and lower limit voltage is 2.5～1V, specific storage method of calculation C=mA * h/g, wherein C: specific storage, temperature is 25 ± 2 ℃, the continuous current tester that computerizeds control carries out electrochemistry capacitance and loop test.
Take by weighing the metatitanic acid 93.5g of purity 98% and the Lithium Acetate (CH of purity 99% according to lithium titanium mol ratio 0.88
3COOLi.2H
2O) 84.88g puts into mixing vessel, adds 19.82g acetylene black, and uniform mixing is 10 hours in ethanol medium, dry down at 80 ℃, put into alumina crucible then, handled 10 hours for 300 ℃ in the retort furnace, obtained lithium titanate with spinel structure down in synthetic 15 hours at 700 ℃ then.Electrochemical property test specific storage 156mAh/g, the ratio of 1C/0.1C specific storage is 91%.The granule-morphology of the lithium titanate with spinel structure that embodiment 1 obtains as shown in Figure 1, its particle grain size is less than 500 nanometers.The cyclic curve of the lithium titanate with spinel structure that embodiment 1 obtains as shown in Figure 6.The high rate performance of the lithium titanate with spinel structure that embodiment 1 obtains as shown in Figure 7, the lithium titanate with spinel structure that obtains with comparative example among Fig. 8 high rate performance compare, high rate performance of the present invention is greatly improved.
Take by weighing the metatitanic acid 93.5g of purity 98% and the lithium hydroxide (LiOH.H of purity 95% according to lithium titanium mol ratio 0.88
2O) 36.38g puts into mixing vessel, adds the 20g polyvinyl alcohol, and uniform mixing is 20 hours in the mixture medium of second alcohol and water, dry down at 120 ℃, put into alumina crucible then, handled 8 hours for 400 ℃ in the retort furnace, 600 ℃ of following Synthetic 2s obtained lithium titanate with spinel structure in 5 hours then.Electrochemical property test specific storage 152mAh/g, the ratio of 1C/0.1C specific storage is 93%.The granule-morphology of the lithium titanate with spinel structure that embodiment 2 obtains as shown in Figure 2, its particle grain size is less than 500 nanometers.
Embodiment 3
Take by weighing the metatitanic acid 93.5g of content purity 98% and the Quilonum Retard 31.05g of purity 98% puts into mixing vessel according to lithium titanium mol ratio 0.88, the graphite that adds 14g, uniform mixing is 30 hours in medium-acetone, dry down at 70 ℃, put into alumina crucible then, handled 5 hours for 500 ℃ in the retort furnace, 800 ℃ obtained lithium titanate with spinel structure down in synthetic 5 hours then.Electrochemical property test specific storage 153mAh/g, the ratio of 1C/0.1C specific storage is 88%.The XRD spectra of the lithium titanate with spinel structure that embodiment 3 obtains as shown in Figure 4.The charging and discharging curve of the lithium titanate with spinel structure that embodiment 3 obtains as shown in Figure 5.
Comparative Examples
Take by weighing the titanium dioxide 66.8g of purity 99.9% and the Quilonum Retard 27.72g of purity 98% puts into mixing vessel according to lithium titanium mol ratio 0.88, behind the uniform mixing, put into alumina crucible then, handled 10 hours for 400 ℃ in the retort furnace, obtained lithium titanate with spinel structure down in synthetic 10 hours at 800 ℃ then.Electrochemical property test specific storage 147mAh/g, the ratio of 1C/0.1C specific storage is 53%.The granule-morphology of the lithium titanate with spinel structure that comparative example obtains as shown in Figure 3, its particle is thick.The lithium titanate with spinel structure that comparative example obtains high rate performance as shown in Figure 8.
Claims (5)
1, a kind of preparation method who is used for lithium ionic cell cathode material spinelle lithium titanate, it is characterized in that: the compound of metatitanic acid, lithium is prepared burden according to atomic ratio Li/Ti=0.8～0.88, the precursor that adds carbon or carbon again, uniform mixing is 5～72 hours in medium, dry then, under 200 ℃～500 ℃ conditions, handled 2～20 hours again, be then under 600 ℃～900 ℃ conditions Synthetic 2～72 hour to obtain lithium ion battery lithium titanate with spinel structure negative material.
2, the preparation method who is used for lithium ionic cell cathode material spinelle lithium titanate according to claim 1 is characterized in that: the compound of said lithium is one or more mixtures in lithium hydroxide, Quilonum Retard, lithium chloride, lithium iodide, lithium nitrate, Trilithium phosphate, Lithium Acetate and the lithium oxalate.
3, the preparation method who is used for lithium ionic cell cathode material spinelle lithium titanate according to claim 1 and 2, it is characterized in that: said carbon is graphite, acetylene black, carbon matrix precursor is one or more in polyoxyethylene glycol, polyvinyl alcohol and the sugar, and add-on accounts for 2～30wt% of gross weight.
4, the preparation method who is used for lithium ionic cell cathode material spinelle lithium titanate according to claim 1 and 2 is characterized in that: said medium is that water, ethanol, acetone, propyl carbinol, n-propyl alcohol, Virahol, second are fine, one or more mixtures in the ether, thanomin.
5, the preparation method who is used for lithium ionic cell cathode material spinelle lithium titanate according to claim 1 and 2 is characterized in that: said drying temperature is 70 ℃～200 ℃.
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101794876A (en) * | 2010-03-19 | 2010-08-04 | 常州康维电子科技有限公司 | Cathode material of battery with high rate performance and preparation method thereof |
| CN101924201A (en) * | 2010-07-26 | 2010-12-22 | 郑州大学 | Method for preparing lithium ion battery negative material carbon-coated and metal-doped lithium titanate |
| CN101944591A (en) * | 2010-09-14 | 2011-01-12 | 耿世达 | Lithium titanate anode material for lithium ion batteries and preparation method thereof |
| CN101986445A (en) * | 2010-05-12 | 2011-03-16 | 罗劲松 | Method for producing lithium battery cathode material lithium titanate |
| CN102104142A (en) * | 2009-12-16 | 2011-06-22 | 清华大学 | Ion-doped spherical Li4Ti5O12/C lithium ion battery anode material and preparation method thereof |
| CN102130324A (en) * | 2011-01-05 | 2011-07-20 | 上海大学 | Preparation method of lithium titanate/carbon nano tube composite cathode material |
| CN102299313A (en) * | 2011-08-10 | 2011-12-28 | 东莞市迈科科技有限公司 | Preparation method of spinel-type lithium titanate |
| CN101630732B (en) * | 2009-07-27 | 2011-12-28 | 深圳市德方纳米科技有限公司 | Nanoscale lithium titanate compound and preparation method thereof |
| CN102557121A (en) * | 2010-12-29 | 2012-07-11 | 河南师范大学 | Method for synthesizing porous spherical lithium titanate |
| CN102945952A (en) * | 2012-12-05 | 2013-02-27 | 吉林大学 | Method for preparing anode material carbon coated lithium titanate for lithium ion power batteries |
| CN105895895A (en) * | 2016-04-28 | 2016-08-24 | 深圳市力为锂能科技有限公司 | Lithium titanate negative electrode material and preparation method therefor |
| CN106486662A (en) * | 2016-12-09 | 2017-03-08 | 江南大学 | The preparation method of carbon-coated lithium ion battery negative material |
| CN110021750A (en) * | 2019-04-17 | 2019-07-16 | 东北大学 | A kind of method of mechanical force assisted Solid-state synthesis lithium titanate anode material |
| CN112624183A (en) * | 2020-12-21 | 2021-04-09 | 四川大学 | Lithium titanate for preparing lithium battery negative electrode material, preparation method and application |
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2007
- 2007-09-20 CN CNA2007101220742A patent/CN101391806A/en active Pending
Cited By (17)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101630732B (en) * | 2009-07-27 | 2011-12-28 | 深圳市德方纳米科技有限公司 | Nanoscale lithium titanate compound and preparation method thereof |
| CN102104142A (en) * | 2009-12-16 | 2011-06-22 | 清华大学 | Ion-doped spherical Li4Ti5O12/C lithium ion battery anode material and preparation method thereof |
| CN101794876A (en) * | 2010-03-19 | 2010-08-04 | 常州康维电子科技有限公司 | Cathode material of battery with high rate performance and preparation method thereof |
| CN101794876B (en) * | 2010-03-19 | 2012-10-03 | 苏州能斯特新能源有限公司 | Cathode material of battery with high rate performance and preparation method thereof |
| CN101986445A (en) * | 2010-05-12 | 2011-03-16 | 罗劲松 | Method for producing lithium battery cathode material lithium titanate |
| CN101924201A (en) * | 2010-07-26 | 2010-12-22 | 郑州大学 | Method for preparing lithium ion battery negative material carbon-coated and metal-doped lithium titanate |
| CN101944591A (en) * | 2010-09-14 | 2011-01-12 | 耿世达 | Lithium titanate anode material for lithium ion batteries and preparation method thereof |
| CN101944591B (en) * | 2010-09-14 | 2012-11-28 | 耿世达 | Lithium titanate anode material for lithium ion batteries and preparation method thereof |
| CN102557121A (en) * | 2010-12-29 | 2012-07-11 | 河南师范大学 | Method for synthesizing porous spherical lithium titanate |
| CN102557121B (en) * | 2010-12-29 | 2013-08-14 | 河南师范大学 | Method for synthesizing porous spherical lithium titanate |
| CN102130324A (en) * | 2011-01-05 | 2011-07-20 | 上海大学 | Preparation method of lithium titanate/carbon nano tube composite cathode material |
| CN102299313A (en) * | 2011-08-10 | 2011-12-28 | 东莞市迈科科技有限公司 | Preparation method of spinel-type lithium titanate |
| CN102945952A (en) * | 2012-12-05 | 2013-02-27 | 吉林大学 | Method for preparing anode material carbon coated lithium titanate for lithium ion power batteries |
| CN105895895A (en) * | 2016-04-28 | 2016-08-24 | 深圳市力为锂能科技有限公司 | Lithium titanate negative electrode material and preparation method therefor |
| CN106486662A (en) * | 2016-12-09 | 2017-03-08 | 江南大学 | The preparation method of carbon-coated lithium ion battery negative material |
| CN110021750A (en) * | 2019-04-17 | 2019-07-16 | 东北大学 | A kind of method of mechanical force assisted Solid-state synthesis lithium titanate anode material |
| CN112624183A (en) * | 2020-12-21 | 2021-04-09 | 四川大学 | Lithium titanate for preparing lithium battery negative electrode material, preparation method and application |
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Application publication date: 20090325 |