CN104370303A - Preparing method of lithium titanate with good rate performance - Google Patents
Preparing method of lithium titanate with good rate performance Download PDFInfo
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- CN104370303A CN104370303A CN201410707344.6A CN201410707344A CN104370303A CN 104370303 A CN104370303 A CN 104370303A CN 201410707344 A CN201410707344 A CN 201410707344A CN 104370303 A CN104370303 A CN 104370303A
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- lithium titanate
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/003—Titanates
- C01G23/005—Alkali titanates
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/485—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/01—Crystal-structural characteristics depicted by a TEM-image
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a preparing method of lithium titanate with good rate performance and belongs to the technical field of electrode material for batteries. The preparing method includes the steps of 1, preparing a lithium source into 1.0-2.5mol/L lithium-containing solution, adding a titanium source, performing mixing to obtain mixed solution, and mixing well the mixed solution to obtain reaction precursor liquid; 2, after microwave hydrothermal reaction, cooling the reaction precursor, performing centrifuging to obtain sediment, and washing and drying the sediment to obtain lithium titanate precursor; 3, heating the lithium titanate precursor at 200-500 DEG C for 2-15h to obtain the lithium titanate with good rate performance. The lithium titanate electrode material is prepared by means of microwave hydrothermal reaction; the advantages of the hydrothermal process and those of the microwave technique are effectively combined, and lithium titanate powder good in product purity and crystallinity is prepared in a short time; meanwhile, the microwave hydrothermal process is simple in flow, conditions are moderate, no special equipment is required, and industrial production is easy.
Description
Technical field
The invention belongs to the electrode materials technical field of battery, be specifically related to the preparation method of the good lithium titanate of a kind of high rate performance.
Background technology
Lithium ion battery has that specific storage is high, quality is light, the life-span is long and the significant advantage such as without memory due to it, and obtains in fields such as aerospace, hybrid-electric car and portable electric appts and apply widely.At present, the lithium ion battery negative material commercially produced is mainly embedding lithium carbon material.But carbon material also exist easily separate out Li dendrite, first charge-discharge efficiency low, easily and electrolytic solution have an effect and there is the shortcomings such as obvious voltage delay.As the equivalent material of lithium ion batteries anodes, spinel type lithium titanate (Li
4ti
5o
12) be the focus that lithium ion battery negative material is studied all the time.Lithium titanate has significant advantage as a kind of zero strain material: good cycle, has good charge and discharge platform, and do not react with electrolytic solution, low price, easily prepares.
The preparation method of current lithium titanate mainly contains: solid phase method, sol-gel method, solvent-thermal method and hydrothermal method.There is intrinsic shortcoming in solid phase method, as reacted incomplete, needs high temperature long heat treatment, the more difficult control of product morphology waits [high civilization. preparation and modification research [D] of lithium titanate. Tianjin: University Of Tianjin, 2006.].Sol-gel method prepares Li
4ti
5o
12the melting of easy generation particle and reunion [
skin, Barbara Kos ' cielska, Wojciech Sadowski.The study of structure and surfacemorphology of lithium titanate sol-gel derived thin films [J] .Journal of Physics andChemistry of Solids 74 (2013) 575-578.].Solvent-thermal method needs strict condition [Yu-Sheng Lin, Jenq-Gong Duh, Min-Chiao Tsai, the Chi-Young Lee.Self-assembledsynthesis of monodispersed mesoporous Li controlling solvent thermal
4ti
5o
12beads and their applications insecondary lithium-ion batteries [J] .Electrochimica Acta 83 (2012) 47-52.].There is shortcoming [Wenli Zhang, Jinfeng Li, YibiaoGuan, Yi Jin, Wentao Zhu, Xun Guo, the Xinping Qiu.Nano-Li such as the high and poor safety performance of long reaction time, cost in hydrothermal method
4ti
5o
12with high rateperformance synthesized by a glycerol assisted hydrothermal method [J] .Journal ofPower Sources 243 (2013) 661-667.].And microwave hydrothermal technology prepares the more common Moist chemical synthesis method of electrode materials, but for the synthesis of Li
4ti
5o
12research less.Microwave hydrothermal technology by molecular polarization and ionic conduction two effects to material direct heating, which eliminate the calorific loss of traditional heating mode, thus the thermo-efficiency of microwave heating is high especially, has that rate of heating is fast, homogeneous heating is without thermograde, without features such as lag-effects.
Summary of the invention
The object of the present invention is to provide the preparation method of the lithium titanate that a kind of high rate performance is good, the method rate of heating is fast, and production efficiency is high, and preparation process is simple, is applicable to suitability for industrialized production.
The present invention is achieved through the following technical solutions:
A preparation method for the lithium titanate that high rate performance is good, comprises the following steps:
1) choose lithium source, this lithium source is mixed with the lithium-containing solution that concentration is 1.0 ~ 2.5mol/L, adds titanium source in lithium-containing solution, mixing obtains mixing solutions, by mixing solutions at 20 ~ 100 DEG C, stirs, obtains reaction precursor liquid; Wherein, in mixing solutions, the mol ratio of lithium atom and titanium atom is 2 ~ 15:1;
2) by reaction precursor liquid at 120 ~ 220 DEG C, microwave hydrothermal reaction 20 ~ 150min, cooling, is then centrifugally precipitated, and carries out drying, obtain lithium titanate precursor by after precipitation cleaning;
3) by lithium titanate precursor at 200 ~ 500 DEG C, thermal treatment 2 ~ 15h, obtains the lithium titanate that high rate performance is good.
Described lithium source is Quilonum Retard, lithium oxalate, lithium nitrate, Lithium Acetate or lithium hydroxide.
Described titanium source is one or more in tetrabutyl titanate, isopropyl titanate, titanium sulfate, titanium dioxide or metatitanic acid.
Step 1) described in stir be by mixing solutions magnetic agitation 20 ~ 120min.
Step 2) described in microwave hydrothermal reaction microwave power be 400 ~ 1200 watts.
Step 2) described in microwave hydrothermal reaction be that the microwave hydrothermal reaction kettle be placed in using tetrafluoroethylene as liner is carried out by reaction precursor liquid, the packing ratio of described microwave hydrothermal reaction kettle is 30% ~ 70%.
Step 2) described in cleaning be successively through deionized water and washes of absolute alcohol by the centrifugal precipitation obtained.
Step 2) described in drying be by cleaning after be deposited in 50 ~ 100 DEG C at dry 1 ~ 8h.
Compared with prior art, the present invention has following useful technique effect:
The present invention adopts microwave-hydrothermal method to prepare lithium titanate electrode material, the method combines the advantage of hydrothermal method and microwave technology effectively, the lithium titanate powdery that product purity is high, crystallinity is good can be prepared within the short time, simultaneously, this microwave-hydrothermal method preparation technology flow process is simple, condition is moderate, does not need special processing unit, is easy to suitability for industrialized production.
The lithium titanate material prepared through the inventive method can reach nano level, this material shortens the evolving path of lithium ion effectively, improve its high rate performance, this material has larger specific surface area simultaneously, effectively increase the contact area with electrolytic solution, improve its electroconductibility, there is good chemical property.
Accompanying drawing explanation
Fig. 1 is lithium titanate X-ray diffractogram prepared by the present invention;
Fig. 2 is lithium titanate Flied emission shape appearance figure prepared by the present invention;
Fig. 3 is lithium titanate transmission electron microscope picture prepared by the present invention;
Fig. 4 is the high rate performance test pattern of lithium titanate electrode material prepared by the present invention;
Fig. 5 is that the lithium titanate electrode material prepared of the present invention is at 0.1C first charge-discharge graphic representation.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in further detail, and the explanation of the invention is not limited.
Embodiment 1
A preparation method for the lithium titanate that high rate performance is good, comprises the following steps:
(1) compound concentration is the Lithium carbonate solution 40mL of 2.5mol/L, adds titanium dioxide, and mixing obtains mixing solutions, and make lithium and titanium mol ratio be 3:1, by this mixing solutions at 20 DEG C, magnetic agitation 80min, obtains reaction precursor liquid;
(2) reaction precursor liquid is transferred in teflon-lined microwave hydrothermal reaction kettle, at 150 DEG C, under 600 watts, microwave hydrothermal reaction 80min, the packing ratio of microwave hydrothermal reaction kettle is 50%; Room temperature is cooled to after reaction, centrifugal afterwards, isolate throw out, clean with deionized water and dehydrated alcohol respectively.By throw out dry 1h at 150 DEG C, obtain lithium titanate precursor;
(3) by this lithium titanate precursor at 300 DEG C of thermal treatment 8h, finally obtain the lithium titanate that product high rate performance is good.
As can be seen from Figure 1, prepared lithium titanate is pure phase lithium titanate, its each diffraction peak all with standard card Li
4ti
5o
12all corresponding fine of the base peak of (JCPDS No.49-0207), do not have obvious impurity to occur, product purity is higher, and product crystallinity is better.As can be seen from Figures 2 and 3, prepared lithium titanate is nano-scale particle.Fig. 4 is the first charge-discharge graphic representation of this lithium titanate electrode material under 0.1C multiplying power, can find out that it has obvious charge and discharge platform, and specific discharge capacity is higher, has exceeded its theoretical value 175.4mAh/g.As can be seen from the high rate performance test pattern of this lithium titanate electrode material of Fig. 5, under the multiplying power of 0.1C, its specific discharge capacity remains on 175mAh/g, under the multiplying power of 20C, its specific discharge capacity remains on 135mAh/g, is about 77% of 0.1C multiplying power, demonstrates it and has good high rate performance; The loading capacity of getting back to after large multiplying power discharging under little multiplying power is still very high, substantially can return to original level, and tend to be steady, indicate it and have good chemical property.
Embodiment 2
A preparation method for the lithium titanate that high rate performance is good, comprises the following steps:
(1) by compound concentration be the lithium oxalate solution 50mL of 1.5mol/L, add titanium dioxide, mixing obtains mixing solutions, and make lithium and titanium mol ratio be 5:1, by this mixing solutions at 60 DEG C, magnetic agitation 100min, obtains reaction precursor liquid;
(2) reaction precursor liquid is transferred in teflon-lined microwave hydrothermal reaction kettle, at 180 DEG C, under 800 watts, microwave hydrothermal reaction 100min, the packing ratio of microwave hydrothermal reaction kettle is 30%; Room temperature is cooled to after reaction, centrifugal afterwards, isolate throw out, clean with deionized water and dehydrated alcohol respectively, by throw out dry 3h at 70 DEG C, obtain lithium titanate precursor;
(3) by lithium titanate precursor at 500 DEG C of thermal treatment 6h, finally obtain the lithium titanate that product high rate performance is good.
Embodiment 3
A preparation method for the lithium titanate that high rate performance is good, comprises the following steps:
(1) compound concentration is the Lithium Acetate solution 40mL of 1.8mol/L, adds titanium sulfate, and mixing obtains mixing solutions, and make lithium and titanium mol ratio be 8:1, by this mixing solutions at 800 DEG C, magnetic agitation 80min, obtains reaction precursor liquid;
(2) reaction precursor liquid is transferred in teflon-lined microwave hydrothermal reaction kettle, at 200 DEG C, under 1200 watts, microwave hydrothermal reaction 120min, the packing ratio of microwave hydrothermal reaction kettle is 70%; Room temperature is cooled to after reaction, centrifugal afterwards, isolate throw out, clean with deionized water and dehydrated alcohol respectively, by throw out dry 2h at 60 DEG C, obtain lithium titanate precursor;
(3) by lithium titanate precursor at 300 DEG C of thermal treatment 10h, finally obtain the lithium titanate that product high rate performance is good.
Embodiment 4
A preparation method for the lithium titanate that high rate performance is good, comprises the following steps:
(1) compound concentration is the lithium hydroxide solution 60mL of 2.0mol/L, adds metatitanic acid and tetrabutyl titanate, and mixing obtains mixing solutions, and make lithium and titanium mol ratio be 15:1, by this mixing solutions at 70 DEG C, magnetic agitation 100min, obtains reaction precursor liquid;
(2) reaction precursor liquid is transferred in teflon-lined microwave hydrothermal reaction kettle, at 150 DEG C, 400 watts of lower microwave hydrothermal reaction 80min, the packing ratio of microwave hydrothermal reaction kettle is 50%; Room temperature is cooled to after reaction, centrifugal afterwards, isolate throw out, clean with deionized water and dehydrated alcohol respectively, by throw out dry 5h at 100 DEG C, obtain lithium titanate precursor;
(3) by lithium titanate precursor at 400 DEG C of thermal treatment 2h, finally obtain the lithium titanate that product high rate performance is good.
Embodiment 5
A preparation method for the lithium titanate that high rate performance is good, comprises the following steps:
(1) compound concentration is the lithium nitrate solution 50mL of 1.2mol/L, adds isopropyl titanate, metatitanic acid and titanium sulfate, and mixing obtains mixing solutions, lithium and titanium mol ratio is made to be 2:1, by this mixing solutions at 80 DEG C, magnetic agitation 40min, obtains reaction precursor liquid;
(2) reaction precursor liquid is transferred in teflon-lined microwave hydrothermal reaction kettle, at 130 DEG C, under 1000 watts, microwave hydrothermal reaction 40min, the packing ratio of microwave hydrothermal reaction kettle is 60%; Room temperature is cooled to after reaction, centrifugal afterwards, isolate throw out, clean with deionized water and dehydrated alcohol respectively, by throw out dry 4h at 90 DEG C, obtain lithium titanate precursor;
(3) by lithium titanate precursor at 200 DEG C of thermal treatment 12h, finally obtain the lithium titanate that product high rate performance is good.
Claims (9)
1. a preparation method for the lithium titanate that high rate performance is good, is characterized in that, comprises the following steps:
1) choose lithium source, this lithium source is mixed with the lithium-containing solution that concentration is 1.0 ~ 2.5mol/L, adds titanium source in lithium-containing solution, mixing obtains mixing solutions, by mixing solutions at 20 ~ 100 DEG C, stirs, obtains reaction precursor liquid; Wherein, in mixing solutions, the mol ratio of lithium atom and titanium atom is 2 ~ 15:1;
2) by reaction precursor liquid at 120 ~ 220 DEG C, microwave hydrothermal reaction 20 ~ 150min, cooling, is then centrifugally precipitated, and carries out drying, obtain lithium titanate precursor by after precipitation cleaning;
3) by lithium titanate precursor at 200 ~ 500 DEG C, thermal treatment 2 ~ 15h, obtains the lithium titanate that high rate performance is good.
2. the preparation method of the lithium titanate that a kind of high rate performance according to claim 1 is good, is characterized in that, described lithium source is Quilonum Retard, lithium oxalate, lithium nitrate, Lithium Acetate or lithium hydroxide.
3. the preparation method of the lithium titanate that a kind of high rate performance according to claim 1 is good, is characterized in that, described titanium source is one or more in tetrabutyl titanate, isopropyl titanate, titanium sulfate, titanium dioxide or metatitanic acid.
4. the preparation method of the lithium titanate that a kind of high rate performance according to claim 1 is good, is characterized in that, step 1) described in stir be by mixing solutions magnetic agitation 20 ~ 120min.
5. the preparation method of the lithium titanate that a kind of high rate performance according to claim 1 is good, is characterized in that, step 2) described in microwave hydrothermal reaction microwave power be 400 ~ 1200 watts.
6. the preparation method of the lithium titanate that a kind of high rate performance according to claim 1 is good, is characterized in that, step 2) described in microwave hydrothermal reaction be that the microwave hydrothermal reaction kettle be placed in using tetrafluoroethylene as liner is carried out by reaction precursor liquid.
7. the preparation method of the lithium titanate that a kind of high rate performance according to claim 6 is good, is characterized in that, the packing ratio of described microwave hydrothermal reaction kettle is 30% ~ 70%.
8. the preparation method of the lithium titanate that a kind of high rate performance according to claim 1 is good, is characterized in that, step 2) described in cleaning be successively through deionized water and washes of absolute alcohol by the centrifugal precipitation obtained.
9. the preparation method of the lithium titanate that a kind of high rate performance according to claim 1 is good, is characterized in that, step 2) described in drying be by cleaning after be deposited in 50 ~ 100 DEG C at dry 1 ~ 8h.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104868111A (en) * | 2015-03-27 | 2015-08-26 | 陕西科技大学 | Preparation method of Ce doped Li4Ti5O12 lithium ion battery cathode material |
| CN110165151A (en) * | 2018-02-05 | 2019-08-23 | 北京欧美中科学技术研究院 | A kind of graphene aerogel negative electrode material of high capacity and preparation method thereof |
| CN110380053A (en) * | 2019-08-01 | 2019-10-25 | 银隆新能源股份有限公司 | A kind of lithium titanate composite material and preparation method thereof, button cell and preparation method thereof |
| CN111710854A (en) * | 2020-06-18 | 2020-09-25 | 电子科技大学 | Lithium titanate electrode material with oxygen defect and preparation method and application thereof |
| CN112038625A (en) * | 2020-08-14 | 2020-12-04 | 合肥国轩高科动力能源有限公司 | Lithium titanate negative electrode material and preparation method thereof |
| CN114634200A (en) * | 2022-02-24 | 2022-06-17 | 四川国创成电池材料有限公司 | Preparation method of lithium titanate negative electrode material |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104868111A (en) * | 2015-03-27 | 2015-08-26 | 陕西科技大学 | Preparation method of Ce doped Li4Ti5O12 lithium ion battery cathode material |
| CN110165151A (en) * | 2018-02-05 | 2019-08-23 | 北京欧美中科学技术研究院 | A kind of graphene aerogel negative electrode material of high capacity and preparation method thereof |
| CN110380053A (en) * | 2019-08-01 | 2019-10-25 | 银隆新能源股份有限公司 | A kind of lithium titanate composite material and preparation method thereof, button cell and preparation method thereof |
| CN111710854A (en) * | 2020-06-18 | 2020-09-25 | 电子科技大学 | Lithium titanate electrode material with oxygen defect and preparation method and application thereof |
| CN112038625A (en) * | 2020-08-14 | 2020-12-04 | 合肥国轩高科动力能源有限公司 | Lithium titanate negative electrode material and preparation method thereof |
| CN114634200A (en) * | 2022-02-24 | 2022-06-17 | 四川国创成电池材料有限公司 | Preparation method of lithium titanate negative electrode material |
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