CN106410264B - The molten salt preparation method of lithium ion battery negative material zinc titanate - Google Patents

The molten salt preparation method of lithium ion battery negative material zinc titanate Download PDF

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CN106410264B
CN106410264B CN201610470483.0A CN201610470483A CN106410264B CN 106410264 B CN106410264 B CN 106410264B CN 201610470483 A CN201610470483 A CN 201610470483A CN 106410264 B CN106410264 B CN 106410264B
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zinc
fused salt
nanotubed
titanic acid
lithium ion
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CN106410264A (en
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张纪伟
张春丽
王金凤
郭建辉
张玉
张经纬
张治军
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Henan University
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Henan 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
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/052—Li-accumulators
    • H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • 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
    • H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
    • H01M4/139—Processes of manufacture
    • H01M4/1391—Processes of manufacture of electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
    • 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
    • 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
    • H01M4/483—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides for non-aqueous cells
    • 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 belongs to the preparation fields of lithium ion battery negative material zinc titanate, specifically disclose a kind of molten salt preparation method of lithium ion battery negative material zinc titanate.The zinc titanate is face-centered cubic phase Zn2Ti3O8, preparation process is：Ball milling is carried out after nanotubed titanic acid, zinc acetylacetonate and fused salt are mixed, 0.5 8 h are calcined in drying under protective atmosphere in 500 650 DEG C after grinding, product is by washing removal fused salt, drying to get product；Wherein, zinc acetylacetonate, nanotubed titanic acid An Xin ︰ titaniums molar ratio be 1 ︰ 0.9 1.5；The fused salt is one or more kinds of mixtures in LiCl, KCl and NaCl.The present invention prepares that metatitanic acid Zinc material required temperature is low, reaction is uniform, and products obtained therefrom has the advantages that capacity height without dephasign, even particle distribution, for lithium ion battery negative material, good rate capability, has extended cycle life.

Description

The molten salt preparation method of lithium ion battery negative material zinc titanate
Technical field
The invention belongs to the preparation fields of lithium ion battery negative material zinc titanate, and in particular to a kind of lithium ion battery is negative The molten salt preparation method of pole material zinc titanate.
Background technology
Lithium ion battery has many advantages, such as that high operating voltage, higher energy density, memory-less effect, safety are good, It is used widely in small-sized electronic product such as mobile phone, laptop and other portable electronic devices.Electrode Material is the core of lithium ion battery, and determines the key factor of performance of lithium ion battery.Currently, lithium ion battery material Material is usually used graphitic carbon and does negative material, and graphite rich reserves have good kinetics, but filled in high magnification Chemical property is poor when electric discharge, and the intercalation potential of graphite close to 0V cause to form Li dendrite in charge and discharge process, Jin Eryin Safety problem is sent out, these problems are more prominent especially in motive-power battery.Therefore, under exploitation non-carbon negative material is applied to Generation power-type lithium ion battery is particularly important.
Lithium titanate is considered as one of preferred material of power battery by its security performance outstanding and cycle performance, so And its theoretical capacity only has 175 mAh/g, embedding lithium platform to be up to 1.55 V, this further decreases the energy density of material.Moreover, It is to use high temperature solid-state method that tradition, which prepares lithium titanate material all, this needs prolonged high-temperature calcination processing, and on the one hand consume energy ratio It is larger, it is often more important that high-temperature process be easy to cause granular grows it is excessive and reunite, be unfavorable for preparing high performance electrode material. It is still researchers to find new have higher theoretical capacity, the excellent negative material of cycle performance and simple preparation process Striving direction.
Zinc titanate has the advantages that theoretical capacity is high, voltage platform is low as lithium ion battery negative material, is one non- Normal potential lithium ion battery negative material.However the poor performance for limiting high-power performance of its electric conductivity, it needs to it It is modified to meet the requirement of high power density.
It is, thus, sought for a kind of preparation process route and its modification simple, that be easy to industrialized metatitanic acid Zinc material Method.
Invention content
The purpose of the present invention is to provide a kind of molten salt preparation methods of lithium ion battery negative material zinc titanate.
To achieve the above object, the technical solution adopted by the present invention is as follows：
The molten salt preparation method of lithium ion battery negative material zinc titanate：The zinc titanate is face-centered cubic phase Zn2Ti3O8, Preparation process is：Ball milling is carried out after nanotubed titanic acid, zinc acetylacetonate and fused salt are mixed, is dried, in protective atmosphere after grinding Under calcine 0.5-8 h in 500-650 DEG C, product is by washing removal fused salt, dry to get product；Wherein, zinc acetylacetonate, The molar ratio of nanotubed titanic acid An Xin ︰ titaniums is 1 ︰ 0.9-1.5；The fused salt is one kind or two in LiCl, KCl and NaCl Kind or more mixture, the total addition level of fused salt is the quality sum of nanotubed titanic acid and zinc acetylacetonate.
Most preferably, ball milling is carried out after nanotubed titanic acid, zinc acetylacetonate and fused salt being mixed, is dried, in argon gas after grinding 2h is calcined under atmosphere in 600 DEG C, product is by washing removal fused salt, drying to get product；Wherein, zinc acetylacetonate, nanotube The molar ratio of metatitanic acid An Xin ︰ titaniums is 1 ︰ 1.1；The fused salt is the mixture of LiCl and KCl, and the molar ratio of the two is 0.59 ︰ 0.41, the total addition level of fused salt is the quality sum of nanotubed titanic acid and zinc acetylacetonate.
Preferably, the ball milling is carried out at 200-400 r/min, and Ball-milling Time is 0.5-6 h.
In the present invention, select nanotubed titanic acid as titanium source, zinc acetylacetonate is zinc source, with substantive distinguishing features and significantly Progress, is in particular in：Using nanotubed titanic acid as titanium source, the spy of a large amount of body phase Lacking oxygens is generated using its thermal dehydration process Property, the body mutually metatitanic acid Zinc material containing Lacking oxygen defect is prepared, its body phase electronic conductivity is improved；Using zinc acetylacetonate as zinc Source, also serve as carbon source, and while nanotubed titanic acid reacts generation zinc titanate with zinc acetylacetonate, zinc acetylacetonate, which decomposes, to be generated Carbon in-stiu coating on the surface of zinc titanate, realize closer equably compound with zinc titanate, overcome traditional additional carbon and lead The shortcomings that carbon coated of cause is uneven, discontinuous state in disperse.Uniformly, continuous carbon coating layer reduce particle it Between contact resistance.So solving zinc titanate as negative electrode of lithium ion battery material using both special titanium sources and zinc source Electronics and ion assign material excellent chemical property in surface and interface and the problem of electrode interior transport property difference when material.
In addition, the present invention makees flux using fuse salt, zinc titanate is prepared using molte-salt synthesis, the salt that melts of low melting point is reaction Provide a liquid phase environment, make reactant come into full contact with and high ion diffusion rates and strong solvability and make reaction Accelerate, be effectively reduced reaction temperature and shorten the reaction time, and product purity, control product morphology, solution can be improved well The prolonged calcination processing of high temperature determined needed for solid sintering technology is reacted uneven and solion exchange process ion and is handed over The not high problem of product purity caused by changing not exclusively.
Compared with the prior art, beneficial effects of the present invention are：Prepare that metatitanic acid Zinc material required temperature is low, reaction is uniform, Products obtained therefrom has capacity height, good rate capability, cycle without dephasign, even particle distribution, for lithium ion battery negative material The advantages of long lifespan.
Description of the drawings
Fig. 1：The X-ray diffractogram of 1 products therefrom of embodiment.
Fig. 2：Transmission electron microscope picture under 1 products therefrom different amplification of embodiment.
Fig. 3：The electron paramagnetic resonance spectrum of 1 products therefrom of embodiment 1 and reference examples.
Fig. 4：The high rate performance figure (a) and cycle performance figure (b) of 1 products therefrom of embodiment；Wherein, in Fig. 4 b, upper curve Charging is represented, lower curve represents electric discharge.
Fig. 5：The high rate performance figure of 1 products therefrom of reference examples.
Fig. 6：The high rate performance figure of 2 products therefrom of reference examples.
Fig. 7：The high rate performance figure of 3 products therefrom of reference examples.
Fig. 8：The high rate performance figure of 4 products therefrom of reference examples.
Specific implementation mode
Many details are elaborated in the description of specific embodiment below to facilitate a thorough understanding of the present invention, still originally Invention can also be implemented using other different from other manner described here, therefore the present invention is not by following public specific The limitation of embodiment.
Embodiment 1
Nanotubed titanic acid is as titanium source, and for zinc acetylacetonate as zinc source, the molar ratio of zinc and titanium is 1:1.1, LiCl and KCl Mixture be fused salt, the molar ratio of the two is 0.59:0.41, the total addition level of fused salt is nanotubed titanic acid and zinc acetylacetonate Quality sum.Nanotubed titanic acid, zinc acetylacetonate, fused salt are put into ball grinder ball milling 3h, ball under the rotating speed of 300 r/min Grind, be transferred in porcelain boat after drying materials after mill, be put into tube furnace argon gas atmosphere protection calcining, from room temperature with 10 DEG C/ Min heating rates are warming up to 600 DEG C, keep 2 h, after naturally cooling to room temperature, fused salt are washed away with distilled water, until not having in supernatant There is Cl-, filter, 60 DEG C of dryings to product.
X-ray powder diffraction is carried out to products therefrom（XRD）Test, gained spectrogram are as shown in Figure 1.It will be seen from figure 1 that The product is single face-centered cubic phase Zn2Ti3O8, without other dephasigns.
The transmission electron microscope of products therefrom（TEM）Figure is shown in Fig. 2, the results showed that：The product particle size of gained is smaller, in 20- The specific surface area of 30 nm or so, distribution uniform, products obtained therefrom are 70 m2/g。
The electron paramagnetic resonance spectrum of products therefrom is shown in Fig. 3.Fig. 3 electron paramagnetic resonance spectrum (EPR)s are shown：Utilize nanotubed titanic acid The Zn prepared as titanium source2Ti3O8Sample contains Lacking oxygen defect and Ti3+, to improve the electric conductivity of sample, be conducive to ion With the transmission of electronics, and then be conducive to the raising of battery performance.
Simulated battery is formed, electrochemical property test is carried out：
S1：By Zn2Ti3O8（0.32g）, conductive agent（Acetylene black）, binder（PVDF）With 8:1:1 mass ratio is mixed in In mortar, 30 min are ground, 0.5 mL solvents are added（N-Methyl pyrrolidone）, it is sufficiently stirred mixing, is coated on copper foil, 120 DEG C of 12 h of vacuum drying are cut into the electrode slice of 15 mm of diameter as working electrode.
S2：Button cell assembles in the glove box full of argon gas, is anode with the electrode slice of above-mentioned preparation, lithium piece is negative Pole, microporous polypropylene membrane are diaphragm, the lithium hexafluoro phosphate of 1 mol/L（LiPF6）It is 1 to be dissolved in volume ratio:1:1 EC: DEC: In DMC solvents（EC is ethylene carbonate, and DEC is diethyl carbonate, and DMC is dimethyl carbonate）For electrolyte, it is assembled into simulation Battery.
S3：Carry out electrochemical property test：Battery first choice carries out under the current density of 0.1,0.2,0.5,1,2,5 A/g High rate performance is tested（As a result see Fig. 4 a）, battery first discharge specific capacity at 0.1 A/g is 470 mAh/g, is recycled by 5 times Stablize afterwards in 245 mAh/g, after then respectively being recycled using 5 times under the current density of 0.2,0.5,1,2,5 A/g, puts Electric specific capacity is respectively 216,180,154,126,88 mAh/g, shows preferable high rate performance；Complete times of electrode test is forthright After energy, loop test is then carried out under the current density of 0.1 A/g（As a result see Fig. 4 b）, after 500 charge and discharge cycles Capacity remains to keep 210 mAh/g, cycle performance very excellent.
Reference examples 1-- difference titanium sources
With P25-TiO2As titanium source, other technological parameters are same as Example 1.
The electron paramagnetic resonance spectrum of products therefrom is shown in Fig. 3.It can be seen that from Fig. 3 electron paramagnetic resonance spectrum figures：With P25- TiO2As titanium source, not oxygen-containing vacancy and Ti in the metatitanic acid Zinc material of preparation3+Defect.
High rate performance figure is shown in Fig. 5.As can be seen from Figure 5：Putting under the current density of 0.1,0.2,0.5,1,2,5 A/g Electric specific capacity is respectively 155,132,98,76,54,25 mAh/g.
Reference examples 2-- Different Zinc Sources
Zn(CH3COOH)2·H2For O as zinc source, other technological parameters are same as Example 1.
High rate performance figure is shown in Fig. 6.As can be seen from Figure 6：Putting under the current density of 0.1,0.2,0.5,1,2,5 A/g Electric specific capacity is respectively 216,190,163,107,65,23mAh/g.
Reference examples 3-- difference calcination atmospheres
Sample is calcined under tube furnace air atmosphere, and other technological parameters are same as Example 1.
It obtains containing only Lacking oxygen and Ti after calcining in air3+The zinc titanate of defect（There is no carbon coating）.High rate performance Figure is shown in Fig. 7.As can be seen from Figure 7：Specific discharge capacity under the current density of 0.1,0.2,0.5,1,2,5 A/g is respectively 246、194、146、105、74、32 mAh/g。
Reference examples 4-- difference calcination temperatures
Sample keeps 2h, other technological parameters same as Example 1 at being 700 DEG C in tube furnace calcination temperature condition.
High rate performance figure is shown in Fig. 8.As can be seen from Figure 8：Putting under the current density of 0.1,0.2,0.5,1,2,5 A/g Electric specific capacity distinguishes 72,65,59,51,41,24 mAh/g.
The high rate performance data of comparative example 1 and reference examples 1-4 products, it is known that：In the specific titanium source of the present invention（It receives Mitron metatitanic acid）With zinc source（Zinc acetylacetonate）Under, using molten-salt growth method, 2h, obtained titanium are calcined at 600 DEG C under protective atmosphere The significantly excellent zinc titanate obtained under the conditions of other of the performance of sour zinc.

Claims (3)

1. the molten salt preparation method of lithium ion battery negative material zinc titanate, it is characterised in that：The zinc titanate is face-centered cubic Phase Zn2Ti3O8, preparation process is：Ball milling is carried out after nanotubed titanic acid, zinc acetylacetonate and fused salt are mixed, is dried, after grinding 0.5-8 h are calcined in 500-650 DEG C under protective atmosphere, product is by washing removal fused salt, drying to get product；Wherein, second Acyl acetone zinc, nanotubed titanic acid An Xin ︰ titaniums molar ratio be 1 ︰ 0.9-1.5；The fused salt is in LiCl, KCl and NaCl One or more kinds of mixtures, the total addition level of fused salt are the quality sum of nanotubed titanic acid and zinc acetylacetonate.
2. molten salt preparation method as described in claim 1, it is characterised in that：By nanotubed titanic acid, zinc acetylacetonate and fused salt Ball milling is carried out after mixing, is dried, and calcines 2h after grinding in 600 DEG C under argon gas, product is by washing removal fused salt, drying, i.e., Obtain product；Wherein, zinc acetylacetonate, nanotubed titanic acid An Xin ︰ titaniums molar ratio be 1 ︰ 1.1；The fused salt is LiCl's and KCl Mixture, the molar ratio of the two are 0.59 ︰ 0.41, the total addition level of fused salt be nanotubed titanic acid and zinc acetylacetonate quality it With.
3. molten salt preparation method as claimed in claim 1 or 2, it is characterised in that：The ball milling is at 200-400 r/min It carries out, Ball-milling Time is 0.5-6 h.
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CN106848296A (en) * 2017-03-20 2017-06-13 华南师范大学 A kind of lithium ion battery manganese base lithium-rich anode material and preparation method thereof
CN109928422A (en) * 2018-08-14 2019-06-25 华北理工大学 A kind of method that fused salt prepares potassium titanate crystal

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