CN104037414A - Modified lithium-titanate material for lithium ion battery and preparation method of modified lithium-titanate material - Google Patents
Modified lithium-titanate material for lithium ion battery and preparation method of modified lithium-titanate material Download PDFInfo
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- CN104037414A CN104037414A CN201410277886.4A CN201410277886A CN104037414A CN 104037414 A CN104037414 A CN 104037414A CN 201410277886 A CN201410277886 A CN 201410277886A CN 104037414 A CN104037414 A CN 104037414A
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- lithium
- lithium titanate
- ion battery
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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
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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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/628—Inhibitors, e.g. gassing inhibitors, corrosion inhibitors
-
- 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 modified lithium-titanate material for a lithium ion battery and a preparation method of the modified lithium-titanate material. The method comprises the following steps: (1) adopting polyacrylamide as a carbon source, adding the polyacrylamide into distilled water or deionized water, and stirring into uniform emulsion; (2) weighing nano titanium dioxide and lithium hydroxide according to the molar ratio of Li to Ti of (4-4.3); firstly adding the nano titanium dioxide into the emulsion prepared in the step (1), uniformly stirring, slowly adding the lithium hydroxide in a stirring state so as to obtain mixed liquid, then carrying out drying treatment on the mixed liquid to obtain a precursor, wherein the used amount of the carbon source accounts for 10-50% of the total mass of three materials; and (3) putting the precursor into an atmosphere furnace filled with inert gas for baking, wherein the baking temperature is 550-850 DEG C and the baking time is 2-24 hours, and cooling, so as to obtain carbon-coated lithium titanate. The method provided by the invention has the advantages that the process is simple, the large-scale production is easy, the material is low in price and easy to obtain and the yield is high; the prepared modified lithium-titanate material is good in electrical conductivity and excellent in charging-discharging performances and rate performance.
Description
Technical field
The invention belongs to lithium ion battery field, relate to a kind of electrode material for lithium ion cell and preparation method thereof, particularly a kind of modified lithium titanate material and preparation method thereof.
Background technology
Lithium-ions battery, as one of most popular green battery, relies on the advantages such as its specific energy is high, the life-span is long, open circuit voltage is high, self-discharge rate is low, environmentally friendly, cheap, becomes the Xin Li army of Battery Market.Along with lithium-ions battery civil area (as, mobile phone, notebook, video camera, electronic toy etc.) obtained being widely used, its fail safe and practicality all obtain industry favorable comment.At present, lithium-ions battery is towards high-power, high-energy-density, and high cycle life direction develops rapidly, and the electric automobile that the lithium ion battery of take is power source will progressively replace part fuel-engined vehicle; Large-scale lithium ion pile more enters in energy-accumulating power station, smart electric grid system as energy storage device.
The negative material of lithium ion battery adopts various embedding lithium material with carbon elements mostly at present.But the current potential of the current potential of carbon electrode and lithium metal is very approaching, when battery overcharge, the easy precipitating metal lithium of carbon electrodes, can form Li dendrite and cause short circuit; During excess Temperature, easily cause thermal runaway etc.; Meanwhile, lithium ion, repeatedly taking off in embedding process, can make material with carbon element structure be damaged, thereby cause the decay of capacity.Therefore, find than embedding lithium under the slightly positive current potential of carbon negative pole current potential, new negative material cheap and easy to get, safe and reliable and height ratio capacity is highly significant.
Titanyl compounds is a class negative material of studying now often, comprises TiO
2, LiTi
2o
4, Li
4ti
5o
12, Li
2ti
3o
7, K
xti
8o
16, and their doping vario-property material.From structure angle, Li
4ti
5o
12be desirable embedded type electrode, the growth of its cell volume parameter in charge and discharge process can be ignored, and electrode structure can hold a large amount of lithiums.The degree of depth discharging and recharging by restriction, can maintain the integrality of electrode structure, and can obtain larger cycle life.Li
4ti
5o
12although theoretical capacity only has 175mAhg
-1, but irreversible capacity loss is very little, thereby to lithium ion battery Li
4ti
5o
12the research of material is significant.
Lithium titanate has good chemical property and security performance, in the lithium-ion-power cell requiring at high security, high magnification and energy-storage battery field, have broad application prospects, but, the conductivity of lithium titanate is low, when high power charging-discharging, capacitance can not be brought into play well, therefore, need to improve its conductivity to its modification.
Summary of the invention
The object of this invention is to provide a kind of modified lithium titanate material and method thereof for lithium ion battery, the method technique is simple, is easy to large-scale production, and raw material is cheap and easy to get, wide material sources, and productive rate is high; Prepared modified lithium titanate material conductivity is good, and charge-discharge performance and high rate performance are excellent.
For achieving the above object, the invention provides the preparation method of modified lithium titanate material for a kind of lithium ion battery, the method comprises following concrete steps:
Step 1, the polyacrylamide of usining adds in distilled water or deionized water as carbon source, stirs and becomes uniform emulsion;
Step 2, by Li: Ti=(4 ~ 4.3): 5 molar ratio weighs nano titanium oxide and lithium hydroxide; In the emulsion that first nano titanium oxide is added step 1 to prepare, stir, more slowly add lithium hydroxide under stirring, prepare mixed liquor, then to mixed liquor be dried processing (as, be placed in convection oven or vacuum drying chamber), with except anhydrating, obtain presoma; Wherein, the consumption of described carbon source accounts for the 10-50% of the gross mass of three kinds of raw materials;
Step 3, by above-mentioned presoma be full of the atmosphere of inert gas (as, put into the atmosphere furnace that is full of inert gas) cure, stoving temperature is 550 ℃ to 850 ℃, the time of curing is 2 to 24 hours, cooling rear acquisition carbon is coated lithium titanate.
The preparation method of modified lithium titanate material for above-mentioned lithium ion battery, wherein, described nano titanium oxide is selected any one in amorphous nano titanium oxide, anatase-type nanometer titanium dioxide and rutile type nano titanic oxide.
The preparation method of modified lithium titanate material for above-mentioned lithium ion battery, wherein, described lithium hydroxide is anhydrous lithium hydroxide or hydronium(ion) oxidation lithium.
The preparation method of modified lithium titanate material for above-mentioned lithium ion battery, wherein, any one in the combination of combination, argon gas and the hydrogen of described inert gas selection argon gas and nitrogen, nitrogen, argon gas.
The preparation method of modified lithium titanate material for above-mentioned lithium ion battery, wherein, the quality of described carbon source accounts for the 20-35% of described precursor gross mass.
The present invention also provides a kind of lithium ion battery modified lithium titanate material prepared by said method that adopts, and this material is the coated lithium titanate of carbon, and its molecular formula is Li
4ti
5o
12/ C, Li prepared by the method
4ti
5o
12/ C particle diameter is evenly distributed, and particle size range is 0.1 ~ 1 μ m, and purity is high, and electric conductivity is good, and high rate charge-discharge performance is good, and 0.5C specific discharge capacity reaches 152mAh/g, more than under 3C multiplying power discharging, specific capacity still can keep 100mAh/g.
The present invention adopts the polyacrylamide with thickener and drag reducer effect as carbon source, during reaction, first nano titanium oxide is added in the solution of polyacrylamide formation, nano titanium oxide is disperseed equably and be adsorbed in organic high molecular compound polyacrylamide, effectively guaranteed that the coated lithium titanate material of product carbon has the primary particle size of nanoscale, the formation uniformity that is conducive to carbon coating layer in the coated lithium titanate material of product carbon, realized the even mixing of reaction raw materials molecular level level under semi-liquid phase condition, particle contact is more abundant, react more abundant, significantly improved the purity of reaction efficiency and product, polyacrylamide also has the effect that particle size were is grown up that suppresses, can guarantee the homogeneity of particle size were.
The present invention has the following advantages:
1, raw material sources of the present invention are extensive, preparation technology is simple and practical, safe, with low cost.
2, the lithium titanate anode material that prepared by the present invention has uniform carbon coating layer, and particle diameter is even, and conductivity is good, and charge-discharge performance and high rate performance are excellent.
Accompanying drawing explanation
Fig. 1 is X-ray diffraction (XRD) figure of the coated lithium titanate material of the prepared carbon of embodiments of the invention 1.
Fig. 2 is transmission electron microscope (TEM) figure of the coated lithium titanate material of the prepared carbon of embodiments of the invention 1.
Fig. 3 a, 3b are that the coated lithium titanate material of the prepared carbon of embodiments of the invention 1 and pure lithium titanate material are respectively at Open Circuit Potential (~ 3.0V vs. Li
+/ Li, (~ 1.55V vs. Li under Fig. 3 a) He half charged state
+/ Li, Fig. 3 b) AC impedance spectrogram during two kinds of different Charging states.
Fig. 4 is the cycle performance curve chart of the coated lithium titanate material of the prepared carbon of embodiments of the invention 1 and pure lithium titanate material.
Embodiment
Below in conjunction with drawings and Examples, describe the specific embodiment of the present invention in detail.
Embodiment 1
Step 1, takes polyacrylamide 6.80g and adds in 200mL distilled water, stirs and becomes homogeneous latex emulsion.
Step 2, takes 0.150mol anatase type nano TiO by the molar ratio of Li:Ti=4.1:5
2and 0.123molLiOHH
2o, by TiO
2add in emulsion and stir, more slowly add LiOHH under stirring
2o, prepares mixed liquor, then mixed liquor is placed in to baking oven and is dried processing, obtains presoma.
Step 3, puts into by above-mentioned presoma the atmosphere furnace that is full of argon gas and cures, and stoving temperature is 800 ℃, and the time of curing is 5 hours, and cooling rear acquisition carbon is coated lithium titanate (Li
4ti
5o
12/ C), material particle size is evenly distributed, and particle size were distribution is 0.2 ~ 1 μ m.
Be illustrated in figure 1 the coated lithium titanate material (Li of this carbon
4ti
5o
12/ C) X-ray diffraction (XRD) figure, calculates product granularity, Li by X-ray live width method according to Scherrer formula
4ti
5o
12the particle mean size of/C material is about 59nm.Calculate a=8.3556, basic identical with the numerical value of pure lithium titanate, show that this material is face-centred cubic structure, belongs to Fd3m space group.
Be illustrated in figure 2 the coated lithium titanate material (Li of this carbon
4ti
5o
12/ C) transmission electron microscope (TEM) is schemed, and is coated on as we can clearly see from the figure the even C layer of material surface, and thickness is about 8nm.
As Fig. 3 a, 3b are depicted as the coated lithium titanate (Li of this carbon
4ti
5o
12/ C) material and pure lithium titanate (Li
4ti
5o
12) the AC impedance spectrogram of material.As can be seen from the figure, bi-material is at Open Circuit Potential (~ 3.0V vs. Li
+/ Li, is shown in (~ 1.55V vs. Li under Fig. 3 a) He half charged state
+/ Li, is shown in Fig. 3 b) during two kinds of different Charging states, AC impedance spectrogram, by the rectilinear(-al) of a semicircle and an inclination, it has been generally acknowledged that high frequency semicircle mainly represents charge transfer resistance (R
ct), that low frequency straight line portion is described is Li
+weber impedance (the Z spreading in solid phase active material
w).With the reduction of voltage, whole electrode impedance obviously reduces, and reason is the carrying out along with charging, Li
+continuous embedding, electrode wettability improves, ionic conductivity improves.With Li
4ti
5o
12compare Li
4ti
5o
12the high frequency semi arch that/C electrode pair is answered obviously reduces, and shows the coated surface electronic conductivity that can obviously improve material of carbon.
Be illustrated in figure 4 the coated lithium titanate (Li of this carbon
4ti
5o
12/ C) material and pure lithium titanate (Li
4ti
5o
12) the cycle performance curve chart of material.As can be seen from the figure, Li
4ti
5o
12/ C electric conductivity is good, and high rate charge-discharge performance is good, and 0.5C specific discharge capacity is 152mAh/g, and under 3C multiplying power discharging, capacity still can reach the more than 70% of 0.5C discharge capacity.In addition, with the increase of charge-discharge magnification, the discharge capacity of bi-material all decreases, Li
4ti
5o
12the discharge capacity of/C material increases with multiplying power the ratio reducing will be lower than Li
4ti
5o
12material, this absolutely proves that being introduced in of carbon formed good conductive network between lithium titanate particle and connected, and can play reduction sheet resistance, thereby improve the chemical property of material.
Embodiment 2
Step 1, takes polyacrylamide 8.04g and adds in 200mL distilled water, stirs and becomes homogeneous latex emulsion.
Step 2, takes 0.150mol anatase type nano TiO by the molar ratio of Li:Ti=4.1:5
2and 0.123molLiOHH
2o, by TiO
2add in emulsion and stir, more slowly add LiOHH under stirring
2o, prepares mixed liquor, then mixed liquor is placed in to baking oven and is dried processing, obtains presoma.
Step 3, puts into above-mentioned presoma to be full of the argon-mixed atmosphere furnace of nitrogen and to cure, and stoving temperature is 750 ℃, and the time of curing is 8 hours, and cooling rear acquisition carbon is coated lithium titanate (Li
4ti
5o
12/ C).
Through check, the coated lithium titanate material particle diameter of this carbon is evenly distributed, and distribution is 0.1 ~ 1 μ m, and electric conductivity is good, and high rate charge-discharge performance is good, and 0.5C specific discharge capacity is 155mAh/g, more than under 3C multiplying power discharging, capacity still can keep 100mAh/g.
Embodiment 3
Step 1, takes polyacrylamide 3.71g and adds in 200mL distilled water, stirs and becomes homogeneous latex emulsion.
Step 2, takes 0.150mol anatase type nano TiO by the molar ratio of Li:Ti=4:5
2and 0.120molLiOHH
2o, by TiO
2add in emulsion and stir, more slowly add LiOHH under stirring
2o, prepares mixed liquor, then mixed liquor is placed in to baking oven and is dried processing, obtains presoma.
Step 3, puts into above-mentioned presoma to be full of the argon-mixed atmosphere furnace of nitrogen and to cure, and stoving temperature is 700 ℃, and the time of curing is 10 hours, and cooling rear acquisition carbon is coated lithium titanate (Li
4ti
5o
12/ C).
Through check, the coated lithium titanate material particle diameter of this carbon is evenly distributed, and distribution is 0.1 ~ 1 μ m, and electric conductivity is good, and high rate charge-discharge performance is good, and 0.5C specific discharge capacity is 160mAh/g, more than under 3C multiplying power discharging, capacity still can keep 100mAh/g.
Embodiment 4
Step 1, takes polyacrylamide 1.65g and adds in 200mL distilled water, stirs and becomes homogeneous latex emulsion.
Step 2, takes 0.150mol rutile type nano TiO by the molar ratio of Li:Ti=4:5
2and 0.120molLiOHH
2o, by TiO
2add in emulsion and stir, more slowly add LiOHH under stirring
2o, prepares mixed liquor, then mixed liquor is placed in to baking oven and is dried processing, obtains presoma.
Step 3, puts into above-mentioned presoma to be full of hydrogen-argon-mixed atmosphere furnace and to cure, and stoving temperature is 850 ℃, and the time of curing is 2 hours, and cooling rear acquisition carbon is coated lithium titanate (Li
4ti
5o
12/ C).
Through check, the coated lithium titanate material particle diameter of this carbon is evenly distributed, and distribution is 0.1 ~ 1 μ m, and electric conductivity is good, and high rate charge-discharge performance is good, and 0.5C specific discharge capacity is 163mAh/g, more than under 3C multiplying power discharging, capacity still can keep 100mAh/g.
Embodiment 5
Step 1, takes polyacrylamide 15.1g and adds in 200mL distilled water, stirs and becomes homogeneous latex emulsion.
Step 2, takes the amorphous nano-TiO of 0.150mol by the molar ratio of Li:Ti=4.3:5
2and 0.129molLiOHH
2o, by TiO
2add in emulsion and stir, more slowly add LiOHH under stirring
2o, prepares mixed liquor, then mixed liquor is placed in to baking oven and is dried processing, obtains presoma.
Step 3, puts into by above-mentioned presoma the atmosphere furnace that is full of nitrogen and cures, and stoving temperature is 550 ℃, and the time of curing is 24 hours, and cooling rear acquisition carbon is coated lithium titanate (Li
4ti
5o
12/ C).
Through check, the coated lithium titanate material particle diameter of this carbon is evenly distributed, and distribution is 0.2 ~ 1 μ m, and electric conductivity is good, and high rate charge-discharge performance is good, and 0.5C specific discharge capacity is 153mAh/g, more than under 5C multiplying power discharging, capacity still can keep 100mAh/g.
Although content of the present invention has been done detailed introduction by above preferred embodiment, will be appreciated that above-mentioned description should not be considered to limitation of the present invention.Those skilled in the art, read after foregoing, for multiple modification of the present invention with to substitute will be all apparent.Therefore, protection scope of the present invention should be limited to the appended claims.
Claims (6)
1. a preparation method for modified lithium titanate material for lithium ion battery, is characterized in that, the method comprises following concrete steps:
Step 1, the polyacrylamide of usining adds in distilled water or deionized water as carbon source, stirs and becomes uniform emulsion;
Step 2, by Li: Ti=(4 ~ 4.3): 5 molar ratio weighs nano titanium oxide and lithium hydroxide; In the emulsion that first nano titanium oxide is added step 1 to prepare, stir, more slowly add lithium hydroxide under stirring, prepare mixed liquor, then mixed liquor is dried to processing, obtain presoma; Wherein, the consumption of described carbon source accounts for the 10-50% of three kinds of raw material gross masses;
Step 3, above-mentioned presoma cures in being full of the atmosphere of inert gas, and stoving temperature is 550 ℃ to 850 ℃, and the time of curing is 2 to 24 hours, and cooling rear acquisition carbon is coated lithium titanate.
2. the preparation method of modified lithium titanate material for lithium ion battery as claimed in claim 1, it is characterized in that, described nano titanium oxide is selected any one in amorphous nano titanium oxide, anatase-type nanometer titanium dioxide and rutile type nano titanic oxide.
3. the preparation method of modified lithium titanate material for lithium ion battery as claimed in claim 1, is characterized in that, described lithium hydroxide is anhydrous lithium hydroxide or hydronium(ion) oxidation lithium.
4. the preparation method of modified lithium titanate material for lithium ion battery as claimed in claim 1, is characterized in that, any one in the combination of combination, argon gas and the hydrogen of described inert gas selection argon gas and nitrogen, nitrogen, argon gas.
5. the preparation method of modified lithium titanate material for lithium ion battery as claimed in claim 1, is characterized in that, the quality of described carbon source accounts for the 20-35% of described precursor gross mass.
6. adopt the lithium ion battery modified lithium titanate material that prepared by method described in claim 1, it is characterized in that, this material is the coated lithium titanate of carbon, and its molecular formula is Li
4ti
5o
12/ C, this material particle size is evenly distributed, and particle size range is 0.1 ~ 1 μ m, and 0.5C specific discharge capacity reaches 152mAh/g, more than under 3C multiplying power discharging, specific capacity still can keep 100mAh/g.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105977466A (en) * | 2016-06-30 | 2016-09-28 | 湖南桑顿新能源有限公司 | Conductive oxide coated lithium ion battery tri-element anode material and preparation method thereof |
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Application publication date: 20140910 |