CN106887573A - A kind of preparation method of rice-shaped pattern lithium ion battery negative material - Google Patents

A kind of preparation method of rice-shaped pattern lithium ion battery negative material Download PDF

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Publication number
CN106887573A
CN106887573A CN201710140156.3A CN201710140156A CN106887573A CN 106887573 A CN106887573 A CN 106887573A CN 201710140156 A CN201710140156 A CN 201710140156A CN 106887573 A CN106887573 A CN 106887573A
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preparation
lithium ion
ion battery
rice
negative material
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葛昊
王登虎
聂胜楠
崔潞霞
宋溪明
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Liaoning University
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Liaoning University
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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
    • 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
    • H01M4/362—Composites
    • H01M4/364—Composites as mixtures
    • 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

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Composite Materials (AREA)
  • Inorganic Chemistry (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)
  • Battery Electrode And Active Subsutance (AREA)

Abstract

The present invention discloses a kind of rice-shaped pattern lithium ion battery negative material Li4Ti5O12/rutile‑TiO2Preparation method, including：1) by LiOHH2O is placed in dimethylformamide, after stirring mixing, adds butyl titanate, and under drying condition, reaction obtains reaction solution；2) to adding deionized water in reaction solution, stir, obtain milky white solution, during milky white solution moved into reactor, precipitation is collected in 180 200 DEG C of 36 40h of reaction, centrifugation, and ethanol washing, 70 80 DEG C of 6 8h of vacuum drying obtain product presoma；3) product presoma is placed in air atmosphere, 490 700 DEG C of 6 7h of calcining naturally cool to room temperature, grind, and obtain target product.Not only solve the security hidden trouble of embedding lithium carbon material, and improve the chemical property of material, be advantageously implemented the commercialization of LTO electrode materials, promote the lithium ion battery negative material New Times.

Description

A kind of preparation method of rice-shaped pattern lithium ion battery negative material
Technical field
The present invention relates to technical field of lithium ion, a kind of lithium ion battery negative of rice-shaped pattern is specifically provided Material Li4Ti5O12/rutile-TiO2And preparation method thereof.
Background technology
The lithium-ion-power cell studied at present is generally using carbon material as negative material, but battery is in abuse state Lower electrolyte can occur violent chemical reaction with embedding cathode of lithium, release substantial amounts of heat, cause the blast of battery out of control.Therefore, Cannot effectively be solved always with the safety problem of the large-capacity high-power lithium ion battery of Carbon anode, govern industrialization Development.Lithium ion is less than normal in carbon-based inside battery diffusion coefficient simultaneously, and its intercalation potential is relatively low, and lithium is easy in electrode surface Deposition, forms lithium dendrite arm, causes battery irreversible capacity and potential safety hazard to increase, therefore carbon-based material is the lithium-ion electric of negative pole Pond rapid charge characteristic is poor.
Lithium titanate Li with spinel structure4Ti5O12(LTO) due to it, lattice parameter is almost during embedding de- lithium Do not change, be referred to as " zero strain material ", its theoretical intercalation potential (1.55V, VS Li/Li+) is high with security performance, Charge-discharge performance is good, cycle performance is excellent, charging/discharging voltage platform stable the advantages of, as lithium ion power cell cathode material Material, be expected to solve lithium ion battery rapid charge characteristic and security performance, but lithium titanate itself electron conduction and ion The characteristics of electric conductivity is poor constrains the large-scale production of lithium ion battery.
At present, successively have been reported that the method for various improvement LTO performances, such as, and the side such as high conductivity cladding, bulk phase-doped Method, it, in one layer of conductive layer of LTO Surface coatings, is most widely that carbon coating improves lithium ion on LTO surfaces that most effective of which is The chemical property of battery.But there is security sex chromosome mosaicism in carbon coating, therefore, many researchs are devoted to developing one kind of LTO Both have excellent chemical property, and safety and stability without carbon composite turn into new focus.
rutitle-TiO2Have the advantages that Lithium-ion embeding-deintercalation speed is fast, capacity is big, good cycling stability etc. is excellent Point, wherein rutitle-TiO2Insertion-deintercalation speed can well make up the deficiency of LTO ionic conductivities difference, therefore, Hen Duoyan Study carefully and be devoted to LTO and rutitle-TiO2Mesh is combined.It is reported that Li4Ti5O12/rutile-TiO2Composite material exhibits Excellent chemical property is gone out, with series of advantages such as Large Copacity, high rate capability, high power capacity conservation rate, stable circulations. But Li4Ti5O12/rutile-TiO2The common pattern of composite has had a strong impact on its electrochemistry for rambling sheet Performance.Therefore more researchs are wished by changing Li4Ti5O12/rutile-TiO2The pattern of composite so lifted its electricity Chemical property.
The content of the invention
In view of pattern is to Li4Ti5O12/rutile-TiO2The electrochemical properties of composite have important influence, this hair Improving eyesight is to provide a kind of lithium ion battery negative material Li of high-specific surface area rice-shaped pattern4Ti5O12/rutile-TiO2 Preparation method, by large specific surface area increase be used as negative pole Li4Ti5O12/rutile-TiO2Composite and electrolyte Contact area, further to improve Li4Ti5O12/rutile-TiO2The chemical property of composite.
The technical solution adopted by the present invention is：
A kind of rice-shaped pattern lithium ion battery negative material Li4Ti5O12/rutile-TiO2Preparation method, including such as Lower step：
1) at room temperature, by LiOHH2O is placed in dimethylformamide DMF, after being thoroughly mixed, adds the fourth of metatitanic acid four Ester, under drying condition, reacts 10-12h, obtains reaction solution；
2) to deionized water is added in the reaction solution, 1-2min is stirred, milky white solution is obtained, by the milky white solution Move in reactor, precipitation, ethanol washing, 70-80 DEG C of vacuum drying 6- are collected in 180-200 DEG C of reaction 36-40h, centrifugation 8h, obtains product presoma；
3) the product presoma is placed in air atmosphere, 490-700 DEG C of calcining 6-7h naturally cools to room temperature, grinds Mill, obtains target product.
Described preparation method, step 1) in LiOHH2O and butyl titanate are 4 according to Li/Ti mol ratios:5~5.5 Ratio carry out dispensing.
Described preparation method, step 1) in butyl titanate feed postition to be added dropwise over.
Described preparation method, step 1) in stirring be magnetic agitation.
Described preparation method, step 1) in LiOHH2O and dimethylformamide are 0.169- by matter liquid g/ml ratios 0.175：The ratio of 25-28 carries out dispensing.
Described preparation method, step 3) in calcining temperature be 590-600 DEG C.
The invention has the advantages that：
The lithium ion battery negative material Li that the present invention is provided4Ti5O12/rutile-TiO2Preparation method, is to use hydro-thermal Synthetic method, with butyl titanate and LiOHH2O is raw material, with dimethylformamide (DMF) as solvent, under room temperature condition, Reaction is obtained presoma；By presoma in air atmosphere, high temperature sintering obtains target product, the lithium being prepared from by the method Ion battery cathode material is rice-shaped Li4Ti5O12/rutile-TiO2Composite, is keeping the premise of LTO good characteristics Under, not only realize solving the security hidden trouble of embedding lithium carbon material, and particular, it is important that its shape structure further increases The specific surface area of material, and then the chemical property of material is improve, and it uses extremely simple hydro-thermal method one-step synthesis, It is particularly conducive to realize the commercialization of LTO electrode materials, promotes the lithium ion battery negative material New Times.
Brief description of the drawings
Fig. 1 is that embodiment 1-3 different temperatures calcines gained cell negative electrode material Li4Ti5O12/rutile-TiO2XRD； Wherein, a, 490-500 DEG C；b、590-600℃；c、690-700℃.
Fig. 2 is that embodiment 1-3 different temperatures calcines gained cell negative electrode material Li4Ti5O12/rutile-TiO2SEM figure； Wherein, a, 490-500 DEG C；b、590-600℃；c、690-700℃.
Specific embodiment
The present invention is further expalined with reference to specific embodiment, but be not intended to limit the invention Protection domain.In order to solve the influence of the pattern to its electrochemical properties of conventional lithium ion battery negative material, the present embodiment There is rice-shaped pattern lithium ion battery negative material Li there is provided one kind4Ti5O12/rutile-TiO2Preparation method, including Following steps：
1) at room temperature, by LiOHH2O is placed in dimethylformamide (DMF), after being thoroughly mixed, adds metatitanic acid four Butyl ester, under drying condition, reacts 10-12h, obtains reaction solution；
2) to deionized water is added in the reaction solution, 1-2min is stirred, milky white solution is obtained, by the milky white solution Move in reactor, precipitation, ethanol washing, 70-80 DEG C of vacuum drying 6- are collected in 180-200 DEG C of reaction 36-40h, centrifugation 8h, obtains product presoma；
3) the product presoma is placed in air atmosphere, 490-700 DEG C of calcining 6-7h naturally cools to room temperature, grinds Mill, obtains target product.
Wherein, in order to really enable the negative material being prepared from that rice-shaped is presented, in step 1) it is middle from as Li sources With two kinds of raw materials in Ti sources, it is necessary for liquid, so that dissolving LiOHH using dimethylformamide (DMF)2O, in order to Dimethylformamide (DMF) is set fully to dissolve LiOHH2O, the LiOHH of usual 0.169-0.175g2O needs 25- 28ml dimethylformamides (DMF)；Step 2) middle addition deionized water, stirring, is in order that butyl titanate is further abundant Hydrolysis.Gained milky white solution is then moved into reactor, 180-200 DEG C of reaction 36-40h, it is therefore an objective to before hydro-thermal reaction is formed Drive body；Step 3) purpose calcined in air atmosphere is that presoma is converted into Li under the high temperature conditions4Ti5O12/ rutile-TiO2Negative material, so as to obtain preferable negative material.In order to ensure obtained negative material can be the grain of rice Shape Li4Ti5O12/rutile-TiO2Composite, so as to increase the specific surface area of material, improves the chemical property of material, excellent Choosing, using as the raw material Li OHH in Li sources and Ti sources2O and butyl titanate are according to Li/Ti=4:5~5.5 are matched somebody with somebody Material, above-mentioned Li/Ti refers to mol ratio, is Li with ensure to be formed4Ti5O12/rutile-TiO2Negative material.In order to really make raw material LiOH·H2O and butyl titanate can fully react, as the improvement of technical scheme, by butyl titanate being added dropwise over Mode added.
Wherein, step 1) in by LiOHH2The stirring that O is placed in dimethylformamide (DMF), preferably magnetic agitation, To control mixing speed, uniformity coefficient is improved.Step 3) in calcining temperature be preferably 590-600 DEG C.
Beneficial effects of the present invention are further illustrated with reference to specific embodiment.
A kind of rice-shaped pattern lithium ion battery negative material Li of embodiment 14Ti5O12/rutile-TiO2
Follow the steps below preparation：
1) at room temperature, by the LiOHH of 0.173g2O is placed in the dimethylformamide of 27ml (DMF), and magnetic agitation is filled After dividing mixing, butyl titanate (TBT) is added dropwise over, under drying condition, reacts 10-12h, obtain reaction solution, and LiOHH2O and Butyl titanate is Li/Ti=4 according to mol ratio:5~5.5 ratio carries out dispensing；
2) to 25-30ml deionized waters are added in reaction solution, strong stirring 1-2min obtains milky white solution, by milky Solution is moved in reactor, 180-200 DEG C of reaction 36-40h, and reactor bottom powder precipitation, ethanol washing are collected in centrifugation 4-6 times, 70-80 DEG C of vacuum drying 6-8h obtains product presoma；
3) product presoma is placed in air atmosphere, 490-500 DEG C of calcining 6-7h of Muffle furnace high temperature naturally cools to room Temperature, grinding, obtains target product.
A kind of rice-shaped pattern lithium ion battery negative material Li of embodiment 24Ti5O12/rutile-TiO2
Follow the steps below preparation：
1) with embodiment 1.
2) with embodiment 1.
3) product presoma is placed in air atmosphere, 590-600 DEG C of calcining 6-7h of Muffle furnace high temperature naturally cools to room Temperature, grinding, obtains target product.
A kind of rice-shaped pattern lithium ion battery negative material Li of embodiment 34Ti5O12/rutile-TiO2
Follow the steps below preparation：
1) with embodiment 1.
2) with embodiment 1.
3) product presoma is placed in air atmosphere, 690-700 DEG C of calcining 6-7h of Muffle furnace high temperature naturally cools to room Temperature, grinding, obtains target product.
Embodiment 4
The lithium ion battery negative material Li that embodiment 1,2 and 3 is obtained4Ti5O12/rutile-TiO2Carry out XRD and SEM Detection, as a result as shown in Figure 1 and Figure 2.As seen from Figure 1, the target product that embodiment 1-3 is obtained, is the LTO of rice-shaped pattern With rutile-TiO2Composite, have no other impurities appearance, and with calcining heat improve, material crystalline degree enhancing.By Fig. 2 is visible, the target product that embodiment 1-3 is obtained, and is rice-shaped structure, and as calcining heat is improved, its rice-shaped knot Structure increasing proportion.Complex chart 1, Fig. 2 can be obtained, and embodiment 1-3 resulting materials are rice-shaped spinel-type Li4Ti5O12/ rutile-TiO2Composite, has no the material doped appearance of other impurities, and with the raising of calcining heat, its crystallinity, rice Kernel structure size all increases.
Embodiment 5
LTO materials are bought for embodiment 1-3 resulting materials and common market, using it as cell negative electrode material, Lithium piece is assembled into button cell as to electrode, and electrochemical property test is carried out to it, the results are shown in Table 1.
The different negative material chemical properties of table 1 compare (charge-discharge magnification 1C)
Research shows more than, and compared to common LTO negative materials, the rice-shaped point of method of the present invention synthesis is brilliant Stone-type Li4Ti5O12/rutile-TiO2The chemical property of composite is improved significantly, and can be seen that 590~600 DEG C Material obtained by temperature lower calcination, its chemical property substantially significantly larger than has 490~500 DEG C of good chemical property With 690~700 DEG C under the conditions of calcine resulting material, this just on the premise of LTO good characteristics are kept, not only realizes solution The security hidden trouble of embedding lithium carbon material, and due to its rice-shaped structure, the specific surface area of material is further increased, enter And the chemical property of material is improve, and it uses extremely simple hydro-thermal method one-step synthesis, is particularly conducive to realize LTO electricity The commercialization of pole material, promotes the lithium ion battery negative material New Times.
The preferred embodiments of the present invention are the foregoing is only, is not intended to limit the invention, for the skill of this area For art personnel, the present invention can have various modifications and variations.It is all within the spirit and principles in the present invention, made any repair Change, equivalent, improvement etc., should be included within the scope of the present invention.

Claims (6)

1. a kind of preparation method of rice-shaped pattern lithium ion battery negative material, it is characterised in that comprise the following steps：
1) at room temperature, by LiOHH2O is placed in dimethylformamide DMF, after being thoroughly mixed, adds butyl titanate, is done Under the conditions of dry, 10-12h is reacted, obtain reaction solution；
2) to deionized water is added in the reaction solution, 1-2min is stirred, obtains milky white solution, the milky white solution is moved to In reactor, precipitation is collected in 180-200 DEG C of reaction 36-40h, centrifugation, and ethanol is washed, 70-80 DEG C of vacuum drying 6-8h, Obtain product presoma；
3) the product presoma is placed in air atmosphere, 490-700 DEG C of calcining 6-7h naturally cools to room temperature, grinds, and obtains Target product-rice-shaped pattern lithium ion battery negative material Li4Ti5O12/rutile-TiO2。
2. according to the preparation method described in claim 1, it is characterised in that：Step 1) in LiOHH2O and butyl titanate according to Li/Ti mol ratios are 4:5~5.5 ratio carries out dispensing.
3. according to the preparation method described in claim 1, it is characterised in that：Step 1) in butyl titanate feed postition be by It is added dropwise to.
4. according to the preparation method described in claim 1, it is characterised in that：Step 1) in stirring be magnetic agitation.
5. according to the preparation method described in claim 1, it is characterised in that：Step 1) in LiOHH2O and dimethylformamide are pressed Matter liquid g/ml ratios are 0.169-0.175：The ratio of 25-28 carries out dispensing.
6. according to the preparation method described in claim 1, it is characterised in that：Step 3) in calcining temperature be 590-600 DEG C.
CN201710140156.3A 2017-03-10 2017-03-10 A kind of preparation method of rice-shaped pattern lithium ion battery negative material Pending CN106887573A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108417824A (en) * 2018-03-06 2018-08-17 辽宁大学 A kind of preparation method of high-performance lithium battery negative material carbon cladding lithium titanate
CN109437331A (en) * 2018-09-20 2019-03-08 广东佳纳能源科技有限公司 A kind of method of precursor of lithium ionic cell positive material impurity removal
CN109546095A (en) * 2017-09-22 2019-03-29 银隆新能源股份有限公司 A kind of preparation method of lithium ion battery negative material

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Publication number Priority date Publication date Assignee Title
CN104157833A (en) * 2014-08-25 2014-11-19 厦门大学 Graphene/titanium dioxide composite porous material, preparation method and application thereof
CN106374086A (en) * 2016-09-27 2017-02-01 彭成信 Nano lithium titanate-graphene composite material and preparation method therefor

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104157833A (en) * 2014-08-25 2014-11-19 厦门大学 Graphene/titanium dioxide composite porous material, preparation method and application thereof
CN106374086A (en) * 2016-09-27 2017-02-01 彭成信 Nano lithium titanate-graphene composite material and preparation method therefor

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
XI-PING LI ET AL: ""Sol-hydrothermal synthesis of Li4Ti5O12/rutile-TiO2 composite as high rate anode material for lithium ion batteries"", 《CERAMICS INTERNATIONAL》 *

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109546095A (en) * 2017-09-22 2019-03-29 银隆新能源股份有限公司 A kind of preparation method of lithium ion battery negative material
CN109546095B (en) * 2017-09-22 2022-03-15 银隆新能源股份有限公司 Preparation method of lithium ion battery negative electrode material
CN108417824A (en) * 2018-03-06 2018-08-17 辽宁大学 A kind of preparation method of high-performance lithium battery negative material carbon cladding lithium titanate
CN108417824B (en) * 2018-03-06 2020-10-09 辽宁大学 Preparation method of high-performance lithium battery cathode material carbon-coated lithium titanate
CN109437331A (en) * 2018-09-20 2019-03-08 广东佳纳能源科技有限公司 A kind of method of precursor of lithium ionic cell positive material impurity removal

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