CN104868111A - Preparation method of Ce doped Li4Ti5O12 lithium ion battery cathode material - Google Patents

Preparation method of Ce doped Li4Ti5O12 lithium ion battery cathode material Download PDF

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CN104868111A
CN104868111A CN201510141708.3A CN201510141708A CN104868111A CN 104868111 A CN104868111 A CN 104868111A CN 201510141708 A CN201510141708 A CN 201510141708A CN 104868111 A CN104868111 A CN 104868111A
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solution
lithium ion
preparation
ion battery
doped
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曹丽云
柴思敏
殷立雄
乔晓宁
王鑫
程娅伊
欧阳海波
黄剑锋
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Shaanxi University of Science and Technology
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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
    • 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
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • H01M4/624—Electric conductive fillers
    • H01M4/626—Metals
    • 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 provides a preparation method of a Ce doped Li4Ti5O12 lithium ion battery nano cathode material. The method comprises the steps of preparing a lithium ion aqueous solution, a Ce(NO3)4 aqueous solution and a TiCl4 aqueous solution, adjusting pH (potential of hydrogen) of the TiCl4 aqueous solution, mixing the three aqueous solutions, and preparing a target product by a hydrothermal electrodeposition method. According to the method, arc discharge heating is adopted in the hydrothermal electrodeposition method, so that the temperature can instantly reach the reaction temperature, and the reaction time is shortened; and in addition, hydrothermal heating is adopted in the hydrothermal electrodeposition method, so that the heating is uniform, the shape of the final product can be controlled, and an electrochemical property is improved. The preparation method has the advantages of low cost, simplicity in operation and short preparation cycle. The material prepared by the method is ball-flower powder in a nano sheet structure, is high in purity, high in crystallinity and uniform in shape, and has excellent charging and discharging properties.

Description

A kind of Ce Li doped 4ti 5o 12the preparation method of lithium ion battery negative material
Technical field
The present invention relates to a kind of preparation method of lithium ion battery negative material, be specifically related to a kind of Ce Li doped 4ti 5o 12the preparation method of nanometer negative materials for Li-ion batteries.
Background technology
Lithium titanate is the negative material just starting the lithium ion battery risen a kind of recent years, it has the crystal structure of spinel-type, when as electrode material, along with the crystal structure carrying out lithium titanate of charge and discharge process does not change substantially, deformation ratio is less than 1%, be called as " zero strain " material, therefore it can have good cycle performance.But it also also exists certain defect, such as the electronic conductivity of material itself is very low, is approximately 10 -9s/cm, close to insulating material, and its intercalation potential is relatively high, is about 1.5V, and this makes the output voltage of battery on the low side.If carry out its conductance of modification raising of certain method to lithium titanate, the content of adding titanium resource is very abundant and very little to the adverse effect of environment, and it probably replaces now widely used carbon negative pole material and becomes the lithium ion battery negative material of a new generation.
Ion doping improves Li 4ti 5o 12conductivity mainly to have come by charge compensation.In doping process, by adding the cation of high price as Mg 2+, Zn 2+, Al 3+deng the Li replacing low price +, cause charge excess, now in order to keep the electric neutrality of crystal, Ti 4+will occur to Ti 3+transformation, Ti 3+content is more, Li 4ti 5o 12conductivity better.
Because granule-morphology also may affect to the chemical property of sample, particle is less, specific area is larger, then the contact of material and electrolyte is better, Li +migration distance also can shorten, be so more conducive to the lifting of lithium ion battery negative material high rate performance.In addition, monodimension nanometer material such as these special structures such as nanometer rods, nanotube, nano wire can produce the feature of some novelties in chemical property etc.
Transition metal is owing to having the valency layer d track of underfill, and based on eighteen-electron rule, character and other yuan have significant difference, therefore preparation Ce Li doped 4ti 5o 12lithium ion cell nano material has very large research using value.
That reports at present is mainly high temperature solid-state method [F.X.Wu, Z.X.Wang, X.H.Li by the method preparing lithium ion battery negative material of adulterating, L.Wu, X.J.Wang, X.P.Zhang, et al.Preparationand characterization of spinel Li 4ti 5o 12anode material from industrial titanyl sulfatesolution [J] .J.Alloys Compd., 2011,509:596-601.], sol-gal process [Y.K.Sun, D.J.Jung, Y.S.Lee, K.S.Nahm, Synthesis and electrochemical characterization of spinelLi [Li (1-x)/ 3cr xti (5-2x)/3] O 4anode materials [J] .J.Power Sources 2004,125 (2): 242-245.], wherein high temperature solid-state method calcination is of long duration, energy consumption is large, efficiency is low, the uniformity of target material is poor, the target product chemical property of preparation is poor, uniform recipe design is difficult; Sol-gel method for preparing is simple, and reaction condition is gentle, but easily occurs precipitation, can not get gel, thus is difficult to obtain product.
Summary of the invention
For overcoming the problems of the prior art, the object of this invention is to provide a kind of Ce Li doped 4ti 5o 12the preparation method of lithium ion battery negative material, the method has the advantages that preparation cost is low, simple to operate, manufacturing cycle is short, prepared Ce Li doped 4ti 5o 12nanometer negative materials for Li-ion batteries purity is high, crystallinity is strong, pattern is even.
For achieving the above object, the present invention adopts following technical scheme:
1) lithium source is dissolved in deionized water, is mixed with the solution A that lithium concentration is 0.5 ~ 0.9mol/L, by Ce (NO 3) 4be dissolved in deionized water, be mixed with the solution B that concentration is 0.1 ~ 0.2mol/L, by TiCl 4be dissolved in deionized water, being mixed with concentration is 0.2 ~ 0.5mol/L solution C, and regulates the pH value of solution C to be 1 ~ 3;
2) by the solution C after solution A, solution B, adjust ph according to Li, Ce, Ti elemental mole ratios n li: n ce: n ti=(4 ~ 6): (0.05 ~ 0.1): the ratio of (5 ~ 7.5) mixes, obtain mixed solution D;
3) filter after mixed solution D being adopted hydrothermal electrodeposition method reaction, obtain filter cake, filtration cakes torrefaction is obtained Ce Li doped 4ti 5o 12lithium ion battery negative material; Wherein, the actual conditions of hydrothermal electrodeposition method reaction is: reaction temperature is 80 ~ 120 DEG C, and positive and negative polarities voltage is 800 ~ 1000V, and pulse duty factor is 50% ~ 60%.
Described step 1) in lithium source be LiOHH 2o, Li 2cO 3, LiNO 3or LiOH.
Described step 1) in the pH value of solution C be adopt the hydrochloric acid of 0.5-2mol/L to carry out regulating.
Described step 2) in the actual conditions that mixes be stir 1 ~ 3h at 40 ~ 60 DEG C.
Described step 3) in mixed solution D is transferred in hydrothermal electrodeposition reactor, then carry out hydrothermal electrodeposition method reaction, wherein, the volume packing ratio of reactor is 50% ~ 60%.
Described step 3) in by before filtration cakes torrefaction, first adopt deionized water by Washing of Filter Cake 2 ~ 3 times, then adopt absolute ethanol washing 2 ~ 3 times.
Described step 3) in dry temperature be 80 ~ 100 DEG C, the dry time is 1 ~ 3h.
Described step 3) in the reaction time be 1 ~ 3 hour.
Compared with prior art, the useful effect that has of the present invention: the present invention by first preparation containing lithium ion aqueous solution, Ce (NO 3) 4the aqueous solution and TiCl 4the aqueous solution, then, regulates TiCl 4by three kinds of aqueous solution after pH value of water solution, obtain Ce Li doped by the mode of hydrothermal electrodeposition method 4ti 5o 12lithium ion battery negative material, the mass transfer velocity in solution can be accelerated due to the specific physical chemical environment under hydrothermal condition in the present invention, so preparation temperature is low and nano material that is preparation does not need the crystallization and thermal treatment in later stage, the defects such as curling, the grain coarsening can avoiding to a certain extent may causing in Post isothermal treatment process; The present invention adopts electro-deposition method to prepare nano material, simple to operate, and raw-material utilance is high, and can obtain the nano and micro materials had compared with bigger serface, and this is conducive to the lifting of cell negative electrode material chemical property.Hydro thermal method is combined with electro-deposition method by the present invention, utilizes hydrothermal electrodeposition technology to synthesize Ce Li doped at a lower temperature 4ti 5o 12nanometer negative materials for Li-ion batteries, purity is high, crystallinity is strong, pattern is even, and the method preparation cost is low, simple to operate simultaneously, manufacturing cycle is short.
Owing to adopting arc discharge to heat in hydrothermal electrodeposition method of the present invention, so can make that temperature is instantaneous reaches reaction temperature, thus shorten the reaction time, in addition owing to adopting hydro-thermal to heat in hydrothermal electrodeposition method, so have homogeneous heating, the pattern of final products can be controlled, and then improve chemical property.Preparation method provided by the invention has the advantage that cost is low, simple to operate, manufacturing cycle is short.Ce Li doped prepared by the present invention 4ti 5o 12the flower ball-shaped powder that lithium ion battery negative material forms for flaky nanometer structure, purity is high, crystallinity is strong, pattern is even, there is excellent charge-discharge performance, under 0.1C low range, its first discharge capacity can reach 300mAh/g, under the high magnification of 10C, its first discharge capacity can reach 180mAh/g.
Accompanying drawing explanation
Fig. 1 is Ce Li doped prepared by the embodiment of the present invention 1 4ti 5o 12the SEM figure of lithium ion cell nano material.
Specific embodiment
Below in conjunction with accompanying drawing, by specific embodiment, the present invention is described in detail.
Embodiment 1
1) by LiOHH 2o is dissolved in deionized water, is mixed with the solution A that lithium concentration is 0.5mol/L, by Ce (NO 3) 4be dissolved in deionized water, be mixed with the solution B that concentration is 0.1mol/L, by TiCl 4be dissolved in deionized water, being mixed with concentration is 0.2mol/L solution C, is then 1 by the pH value of 1mol/L hydrochloric acid conditioning solution C.
2) by the three kinds of solution of the solution C after solution A, solution B, adjust ph according to Li, Ce, Ti elemental mole ratios n li: n ce: n tiafter the ratio mixing of=4:0.05:5, stir 1h at 40 DEG C of lower magnetic forces, form uniform and stable mixed solution D.
3) mixed solution D is put into hydrothermal electrodeposition reactor, sealed reactor, controlling volume packing ratio is 50%, and reaction temperature controls at 80 DEG C, and positive and negative polarities voltage is 800V, and pulse duty factor is 50%, adopts arc discharge hydro-thermal reaction 1h.
4) after question response still cools straight room temperature naturally, obtain filter cake after filtration, first adopted by filter cake deionized water to wash 2 times, then obtain powder 2 times with absolute ethanol washing, then with 1h dry at 80 DEG C, obtain Ce Li doped 4ti 5o 12lithium ion battery negative material.
Fig. 1 is the Ce Li doped that embodiment 1 obtains 4ti 5o 12the SEM figure of lithium ion battery negative material, the sample surfaces as can be seen from Figure 1 after doping is by nanometer sheet from the flower-like structure formed, and the thickness of nanometer sheet is approximately several nanometer.
Embodiment 2
1) by Li 2cO 3be dissolved in deionized water, be mixed with the solution A that lithium concentration is 0.7mol/L, by Ce (NO 3) 4be dissolved in deionized water, be mixed with the solution B that concentration is 0.15mol/L, by TiCl 4be dissolved in deionized water, being mixed with concentration is 0.35mol/L solution C, is 2 by the pH value of 0.5mol/L hydrochloric acid conditioning solution C simultaneously.
2) by the three kinds of solution of the solution C after solution A, solution B, adjust ph according to Li, Ce, Ti element mole n li: n ce: n tiafter the ratio mixing of=5:0.1:6, stir 3h at 50 DEG C of lower magnetic forces, form uniform and stable mixed solution D.
3) mixed solution D is put into hydrothermal electrodeposition reactor, sealed reactor, controlling volume packing ratio is 55%, and reaction temperature controls at 100 DEG C, and positive and negative polarities voltage is 900V, and pulse duty factor is 55%, adopts arc discharge hydro-thermal reaction 2h.
4) after question response still naturally cools to room temperature, obtain filter cake after filtration, first adopted by filter cake deionized water to wash 3 times, then obtain powder 3 times with absolute ethanol washing, then dry 2h at 90 DEG C, obtains Ce Li doped 4ti 5o 12lithium ion battery negative material.
Embodiment 3
1) by LiNO 3be dissolved in deionized water, be mixed with the solution A that lithium concentration is 0.9mol/L, by Ce (NO 3) 4be dissolved in deionized water, be mixed with the solution B that concentration is 0.2mol/L, by TiCl 4be dissolved in deionized water, being mixed with concentration is 0.5mol/L solution C, is 3 by the pH value of 2mol/L hydrochloric acid conditioning solution C simultaneously.
2) by the three kinds of solution of the solution C after solution A, solution B, adjust ph according to Li, Ce, Ti element mole n li: n ce: n tiafter the ratio mixing of=6:0.05:7.5, stir 3h at 60 DEG C of lower magnetic forces, form uniform and stable mixed solution D.
3) mixed solution D is put into hydrothermal electrodeposition reactor, sealed reactor, controlling volume packing ratio is 60%, and reaction temperature controls at 120 DEG C, and positive and negative polarities voltage is 1000V, and pulse duty factor is 60%, adopts arc discharge hydro-thermal reaction 3h.
4) after question response still naturally cools to room temperature, obtain filter cake after filtration, first adopted by filter cake deionized water to wash 3 times, then obtain powder 3 times with absolute ethanol washing, then dry 3h at 100 DEG C, obtains Ce Li doped 4ti 5o 12lithium ion battery negative material.
Embodiment 4
1) LiOH is dissolved in deionized water, is mixed with the solution A that lithium concentration is 0.6mol/L, by Ce (NO 3) 4be dissolved in deionized water, be mixed with the solution B that concentration is 0.2mol/L, by TiCl 4be dissolved in deionized water, being mixed with concentration is 0.4mol/L solution C, and adopts the pH value of the hydrochloric acid conditioning solution C of 1.5mol/L to be 2.5;
2) by the solution C after solution A, solution B, adjust ph according to Li, Ce, Ti elemental mole ratios n li: n ce: n tithe ratio mixing of=4.5:0.06:6.5, and 1h is stirred at 55 DEG C, obtain mixed solution D;
3) mixed solution D is transferred in hydrothermal electrodeposition reactor, and the volume packing ratio of reactor is 52%, then filter after adopting hydrothermal electrodeposition method reaction 3h, obtain filter cake, first adopted by filter cake deionized water by Washing of Filter Cake 2 times, adopt absolute ethanol washing again 3 times, then dry 3h at 85 DEG C, obtains Ce Li doped 4ti 5o 12lithium ion battery negative material; Wherein, the actual conditions of hydrothermal electrodeposition method reaction is: reaction temperature is 90 DEG C, and positive and negative polarities voltage is 960V, and pulse duty factor is 53%.
Embodiment 5
1) by LiOHH 2o is dissolved in deionized water, is mixed with the solution A that lithium concentration is 0.8mol/L, by Ce (NO 3) 4be dissolved in deionized water, be mixed with the solution B that concentration is 0.1mol/L, by TiCl 4be dissolved in deionized water, being mixed with concentration is 0.3mol/L solution C, and adopts the pH value of the hydrochloric acid conditioning solution C of 2mol/L to be 1.5;
2) by the solution C after solution A, solution B, adjust ph according to Li, Ce, Ti elemental mole ratios n li: n ce: n tithe ratio mixing of=5.5:0.08:5.5, and 2h is stirred at 45 DEG C, obtain mixed solution D;
3) mixed solution D is transferred in hydrothermal electrodeposition reactor, and the volume packing ratio of reactor is 58%, then filter after adopting hydrothermal electrodeposition method reaction 1.5h, obtain filter cake, first adopted by filter cake deionized water by Washing of Filter Cake 3 times, adopt absolute ethanol washing again 2 times, then dry 1h at 95 DEG C, obtains Ce Li doped 4ti 5o 12lithium ion battery negative material; Wherein, the actual conditions of hydrothermal electrodeposition method reaction is: reaction temperature is 105 DEG C, and positive and negative polarities voltage is 850V, and pulse duty factor is 56%.
The present invention prepares Ce doping bouquet sheet Li 4ti 5o 12the method of nanometer negative materials for Li-ion batteries, has the advantages that preparation cost is low, simple to operate, manufacturing cycle is short, prepared Ce doping bouquet sheet Li 4ti 5o 12nanometer negative materials for Li-ion batteries purity is high, crystallinity is strong, pattern is even.
Ce Li doped prepared by the present invention 4ti 5o 12the flower ball-shaped powder that lithium ion battery negative material forms for flaky nanometer structure, its charge-discharge performance is excellent, under 0.1C low range, its first discharge capacity can reach 300mAh/g, under the high magnification of 10C, its first discharge capacity can reach 180mAh/g.

Claims (8)

1. a Ce Li doped 4ti 5o 12the preparation method of lithium ion battery negative material, is characterized in that, comprises the following steps:
1) lithium source is dissolved in deionized water, is mixed with the solution A that lithium concentration is 0.5 ~ 0.9mol/L, by Ce (NO 3) 4be dissolved in deionized water, be mixed with the solution B that concentration is 0.1 ~ 0.2mol/L, by TiCl 4be dissolved in deionized water, being mixed with concentration is 0.2 ~ 0.5mol/L solution C, and regulates the pH value of solution C to be 1 ~ 3;
2) by the solution C after solution A, solution B, adjust ph according to Li, Ce, Ti elemental mole ratios n li: n ce: n ti=(4 ~ 6): (0.05 ~ 0.1): the ratio of (5 ~ 7.5) mixes, obtain mixed solution D;
3) filter after mixed solution D being adopted hydrothermal electrodeposition method reaction, obtain filter cake, filtration cakes torrefaction is obtained Ce Li doped 4ti 5o 12lithium ion battery negative material; Wherein, the actual conditions of hydrothermal electrodeposition method reaction is: reaction temperature is 80 ~ 120 DEG C, and positive and negative polarities voltage is 800 ~ 1000V, and pulse duty factor is 50% ~ 60%.
2. Ce Li doped according to claim 1 4ti 5o 12the preparation method of lithium ion battery negative material, is characterized in that, described step 1) in lithium source be LiOHH 2o, Li 2cO 3, LiNO 3or LiOH.
3. Ce Li doped according to claim 1 4ti 5o 12the preparation method of lithium ion battery negative material, is characterized in that, described step 1) in the pH value of solution C be adopt the hydrochloric acid of 0.5-2mol/L to carry out regulating.
4. Ce Li doped according to claim 1 4ti 5o 12the preparation method of lithium ion battery negative material, is characterized in that, described step 2) in the actual conditions that mixes be stir 1 ~ 3h at 40 ~ 60 DEG C.
5. Ce Li doped according to claim 1 4ti 5o 12the preparation method of lithium ion battery negative material, is characterized in that, described step 3) in mixed solution D is transferred in hydrothermal electrodeposition reactor, then carry out hydrothermal electrodeposition method reaction, wherein, the volume packing ratio of reactor is 50% ~ 60%.
6. Ce Li doped according to claim 1 4ti 5o 12the preparation method of lithium ion battery negative material, is characterized in that, described step 3) in by before filtration cakes torrefaction, first adopt deionized water by Washing of Filter Cake 2 ~ 3 times, then adopt absolute ethanol washing 2 ~ 3 times.
7. Ce Li doped according to claim 1 4ti 5o 12the preparation method of lithium ion battery negative material, is characterized in that, described step 3) in dry temperature be 80 ~ 100 DEG C, the dry time is 1 ~ 3h.
8. Ce Li doped according to claim 1 4ti 5o 12the preparation method of lithium ion battery negative material, is characterized in that, described step 3) in the reaction time be 1 ~ 3 hour.
CN201510141708.3A 2015-03-27 2015-03-27 Preparation method of Ce doped Li4Ti5O12 lithium ion battery cathode material Pending CN104868111A (en)

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Application publication date: 20150826