CN103682278A - Preparation method of nanocarbon coated lithium titanate cathode material - Google Patents
Preparation method of nanocarbon coated lithium titanate cathode material Download PDFInfo
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- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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- B82—NANOTECHNOLOGY
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- H—ELECTRICITY
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- 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
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- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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- H—ELECTRICITY
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- 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
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Abstract
A preparation method of a nanocarbon coated lithium titanate cathode material comprises the following steps of: (1) preparing a strongly alkaline solution, weighing titanium dioxide, adding into an autoclave for reaction for 3-5h at 160-180 DEG C, cleaning a precipitate in a polyethene lining of the autoclave with hydrochloric acid for several times, performing filtration washing with distilled water, then putting in vacuum drying equipment for drying, (2) weighing a lithium source and pretreated titanium dioxide powder material according to an Li:Ti mole ratio, putting in a ball milling tank, then weighing a soluble carbon source, adding a little distilled water, dissolving at room temperature or under a heating condition, transferring all into a mixing tank, (3) quickly drying slurry with a spray dryer, transferring all materials into a corundum crucible or a saggar, putting in a muffle furnace for sintering in shielding gas, and (4) grinding and sieving an obtained material, and obtaining the carbon coated lithium titanate cathode material.
Description
Technical field
The present invention relates to a kind of preparation method of lithium ion secondary battery cathode material lithium titanate, relate in particular to the preparation method of the coated lithium titanate anode material of a kind of nanometer carbon.
Background technology
Lithium ion battery is to have another name called " lithium-ions battery ", is the day by day exhausted important new energy technology constantly worsening with environment of the 21 century reply energy.Its development starts from the world oil crisis period of 60-seventies the earliest.Through the exploration of nearly 20 years, in nineteen ninety, by Japanese Sony energy company and gondola Moli energy company, taken the lead in developing and take material with carbon element as negative pole, with LiCoO
2for anodal lithium ion battery.Henceforth, lithium ion battery has obtained develop rapidly.Meanwhile, lithium ion battery energy density is large, and average output voltage is high, and self discharge is little, does not have memory effect, operating temperature range to be-20 ℃-60 ℃, cycle performance is superior, can fast charging and discharging, charge efficiency is up to 100%.And its power output is large, long service life, containing poisonous and harmful substance, thereby be called as green battery.
Lithium ion battery mainly consists of positive electrode, negative material, barrier film and electrolyte.The positive electrode of lithium ion battery has cobalt acid lithium, LiMn2O4, nickel cobalt manganese lithium and LiFePO4 etc.; Negative material be take graphite, hard carbon as main, and lithium titanate anode material is emerging high cycle performance negative material of 21 century.The lithium rechargeable battery forming compared to carbon negative pole, lithium titanate battery has the advantages such as high security, high stability, long-life, fast charging and discharging and cryogenic property are good, and the current potential of lithium titanate itself is higher, avoided the generation of lithium dendrite arm, ensured the safety of lithium ion battery.The another one important feature of lithium titanate battery is can not form SEI film, has so just reduced the loss of lithium ion battery irreversible capacity, so the graphite cathode material the most frequently used with respect to lithium ion battery, and lithium titanate battery has better durability.Result shows by experiment, uses lithium titanate to compare with conventional graphite lithium battery as the lithium battery of negative pole, and the life-span can extend to 4-6 doubly.This changes battery with regard to having been avoided at vehicle service life phase internal cause deterioration of battery, more can not cause the use cost of user's vehicle to go up.Japan Toshiba is just used the car lithium battery of lithium titanate at present in volume production.U.S. EnerSol energy resource system company finds that lithium titanate battery is adapted at applying in intelligent grid energy storage and electric automobile, is also actively finding the affiliate of lithium titanate battery development& testing at present.
The most frequently used preparation method of lithium titanate anode material is that synthetic method is decomposed in solid phase method and organic titanium source, yet the lithium titanate material particle size that solid phase method production obtains is large, and agglomeration is obvious, and capacity attenuation speed is fast, and cycle performance is bad; Although utilizing organic titanium source to prepare lithium titanate material for raw material can refinement scantling, it is expensive, and production cost is larger, is not suitable for mass industrial production, and lithium titanate intrinsic conductivity is low simultaneously, is unfavorable for the large multiplying power discharging of positive electrode.
Summary of the invention
The object of this invention is to provide a kind of material particle nanometer that can realize and realize the preparation method that the coated a kind of nanometer carbon of the even carbon of material is coated lithium titanate anode material simultaneously.
For achieving the above object, the technical solution used in the present invention is: the preparation method of the coated lithium titanate anode material of a kind of nanometer carbon, it is characterized in that: comprise following step: the strong base solution of (1) configuration 1-15mol/L, take the titanium dioxide that mass ratio is 10-50:1, add autoclave, between 160-180 ℃, react 3-5 hour, by hydrochloric acid cleaning number time for sediment in autoclave polyethylene liner, and use distilled water filtration washing, be then placed in vacuum dryer 80-100 ℃ of dry 2-5 hour; (2) press Li:Ti mol ratio for (0.8-0.88): titanium dioxide powder material after 1 weighing lithium source and preliminary treatment, be placed in ball grinder, and then the solubility carbon source that takes 0.1-0.2 times of molal weight adds a small amount of distilled water, under normal temperature or heating condition, dissolve, and be all transferred to agitator tank, continue to stir 0.5-1 hour; (3) the spray-dried device of above-mentioned gained slurry is realized to rapid draing, then material is all transferred to corundum crucible or saggar, be placed in Muffle furnace sintering 8-15 hour under protective gas 750-900 ℃ condition; (4) gains abrasive lapping is sieved, obtain the coated lithium titanate anode material of carbon.
In the method, comprise following step: the strong base solution of (1) configuration 8mol/L, measuring 80ml adds in the autoclave polytetrafluoroethyllining lining of 100ml, taking 2g titanium dioxide adds wherein again, then be placed in baking oven in 160 ℃ of reactions 5 hours, reaction finishes, by hydrochloric acid cleaning number time for the sediment in autoclave polyethylene liner, with distilled water, wash and filter again, be finally placed in 100 ℃, drying equipment and be dried 5 hours; (2) by Li:Ti mol ratio, be that 0.84:1 weighs titanium dioxide powder material after lithium carbonate and preliminary treatment, be placed in ball grinder; And then take the solubility carbon source of 0.2 times of molal weight, and add in beaker and with a small amount of distilled water dissolving, be more all transferred to ball grinder, put into agate ball ball milling 1 hour; (3) the spray-dried equipment of above-mentioned gained material is realized to rapid draing, then material is all transferred to corundum crucible or saggar, be placed in Muffle furnace sintering 15 hours under 800 ℃ of conditions of protective gas; (4) gains abrasive lapping is sieved, obtain the coated lithium titanate anode material of carbon.
In the method, comprise following step: the strong base solution of (1) configuration 6mol/L, measuring 80ml adds in the autoclave polytetrafluoroethyllining lining of 100ml, taking 2g titanium dioxide adds wherein again, then be placed in baking oven and between 180 ℃, react 3 hours, reaction finishes, by hydrochloric acid cleaning number time for the sediment in autoclave polyethylene liner, with distilled water, wash and filter again, be finally placed in 100 ℃, drying equipment and be dried 5 hours;
(2) by Li:Ti mol ratio, be that 0.84:1 weighs titanium dioxide powder material after lithium carbonate and preliminary treatment, be placed in ball grinder; And then take the solubility carbon source of 0.2 times of molal weight, and add in beaker and with a small amount of distilled water dissolving, be more all transferred to ball grinder, put into agate ball ball milling 1 hour; (3) by the spray-dried equipment rapid draing of above-mentioned gained material, then material is all transferred to corundum crucible or saggar, is placed in Muffle furnace sintering 15 hours under 800 ℃ of conditions of protective gas; (4) gains abrasive lapping is sieved, obtain the coated lithium titanate anode material of carbon.
In the method, described lithium source is lithium carbonate, lithium hydroxide, a kind of in lithium nitrate or their mixture.
In the method, described titanium dioxide is a kind of in anatase titanium dioxide, unformed titanium dioxide or their mixture.
In the method, described solubility carbon source is a kind of in glucose, citric acid, polyethylene glycol, starch or their mixture.
Advantageous effect of the present invention is: because the present invention has used this method; utilize hydrothermal technique to carry out forerunner's processing to titanium dioxide; obtained nano level titanium dioxide powder material; and by solubility carbon source, material has been carried out to abundant infiltration; in the process that carbon source is decomposed, realized to material evenly be coated and provide growth epipole, so effective refinement lithium titanate material and protected lithium titanate material in course of reaction with the interaction of electrolyte.In strong base solution recycling largely after hydro-thermal, saved production cost, and strong base solution is to the TiO2 preliminary treatment material particle size that effectively improved the active and refinement of material particle, overcome that organic titanium source is expensive, commercialization TiO2 structure and stable in properties and difficult hydroxylated shortcoming, the even carbon that the even decomposition of solubility carbon source has realized lithium titanate material is coated, effectively improve lithium titanate conductivity, when having realized raising material property, reduced manufacturing cost.
Accompanying drawing explanation
Fig. 1 is the X ray diffracting spectrum of the lithium titanate material of embodiment 1 preparation;
Fig. 2 is the scanning electron microscope image of embodiment 1 gained lithium titanate material;
Fig. 3 is the cycle characteristics collection of illustrative plates that the coated lithium titanate material of the carbon of embodiment 1 preparation and nickel-cobalt lithium manganate material are made into simulation button cell.
Embodiment
Below in conjunction with the drawings and specific embodiments, the invention will be further described:
The present invention as shown in Figure 1, 2, 3,
The present invention adopts the particle size nanometer that realizes lithium titanate raw material of hydro-thermal technology of preparing, then utilizes solubility carbon source to mix with lithium titanate raw material, and spraying is dry, finally carries out high temperature sintering, obtains the coated lithium titanate anode material of carbon,
Embodiment 1:
A preparation method for the composite lithium titanate negative material that nanometer and carbon are coated, comprises the following steps:
(1) strong base solution of configuration 8mol/L, measures 80ml and adds in the autoclave polytetrafluoroethyllining lining of 100ml, then take 2g titanium dioxide and add wherein, is then placed in baking oven and between 160 ℃, reacts 5 hours.Reaction finishes, and by hydrochloric acid cleaning number time for the sediment in autoclave polyethylene liner, then washs and filters with distilled water, is finally placed in 100 ℃, drying equipment and is dried 5 hours; (2) by Li:Ti mol ratio, be that 0.84:1 weighs titanium dioxide powder material after lithium carbonate and preliminary treatment, be placed in ball grinder; Then take the solubility carbon source (with respect to Ti salt) that takes again 0.2 times of molal weight, add in beaker and with a small amount of distilled water and dissolve, be more all transferred to ball grinder, put into agate ball ball milling 1 hour; (3) the spray-dried equipment of above-mentioned gained material is realized to rapid draing, then material is all transferred to corundum crucible or saggar, be placed in Muffle furnace sintering 15 hours under 800 ℃ of conditions of protective gas; (4) gains abrasive lapping is sieved, obtain lithium titanate anode material.
Then by the mass ratio of 85:10:5, take lithium titanate material, conductive agent and binding agent, add 7ml ethanolic solution to stir into bulk, utilize film laminator to be pressed into the pole piece of 0.1mm left and right, under 100 ℃ of conditions, dry 1h, then utilize 15mm blunderbuss that its blunderbuss is made to uniform diaphragm, take its quality, put into glove box and be made into simulation button cell, and utilize blue electric system to test its electrochemical properties.Charging and discharging currents is 0.2C, 0.5C, 1C; Voltage range is 0.7-2.5V, and table 1 is embodiment 1 and makes carbon clad composite material chemical property.
Embodiment 2:
(1) strong base solution of configuration 6mol/L, measures 80ml and adds in the autoclave polytetrafluoroethyllining lining of 100ml, then take 2g titanium dioxide and add wherein, is then placed in baking oven and between 180 ℃, reacts 3 hours.Reaction finishes, and by hydrochloric acid cleaning number time for the sediment in autoclave polyethylene liner, then washs and filters with distilled water, is finally placed in 100 ℃, drying equipment and is dried 5 hours; (2) by Li:Ti mol ratio, be that 0.84:1 weighs titanium dioxide powder material after lithium carbonate and preliminary treatment, be placed in ball grinder; Then take the solubility carbon source (with respect to Ti salt) that takes again 0.2 times of molal weight, add in beaker and with a small amount of distilled water and dissolve, be more all transferred to ball grinder, put into agate ball ball milling 1 hour; (3) by the spray-dried equipment rapid draing of above-mentioned gained material, then material is all transferred to corundum crucible or saggar, is placed in Muffle furnace sintering 15 hours under 800 ℃ of conditions of protective gas; (4) gains abrasive lapping is sieved, obtain lithium titanate anode material.
Lithium titanate material is made into cathode pole piece by embodiment 1 mode and mates with 811 type nickle cobalt lithium manganates and make button half-cell and test its cycle performance, as shown in Figure 3.
Comparative example 1
(1) by Li:Ti mol ratio, be that 0.84:1 weighs titanium dioxide powder material after lithium carbonate and preliminary treatment, be placed in ball grinder; Then add a small amount of distilled water, then put into agate ball, ball milling 1 hour.
(2) by the spray-dried equipment rapid draing of above-mentioned gained material, then material is all transferred to corundum crucible or saggar, is placed in Muffle furnace sintering 15 hours under 800 ℃ of conditions of protective gas.
(3) gains abrasive lapping is sieved, obtain lithium titanate anode material.
Table 1. embodiment 1 makes the coated composite lithium titanate material electrochemical performance of carbon.
Claims (6)
1. nanometer carbon is coated a preparation method for lithium titanate anode material, it is characterized in that: comprise following step:
(1) strong base solution of configuration 1-15mol/L, take the titanium dioxide that mass ratio is 10-50:1, add autoclave, between 160-180 ℃, react 3-5 hour, by hydrochloric acid cleaning number time for sediment in autoclave polyethylene liner, and use distilled water filtration washing, be then placed in vacuum dryer 80-100 ℃ of dry 2-5 hour;
(2) press Li:Ti mol ratio for (0.8-0.88): titanium dioxide powder material after 1 weighing lithium source and preliminary treatment, be placed in ball grinder, and then the solubility carbon source that takes 0.1-0.2 times of molal weight adds a small amount of distilled water, under normal temperature or heating condition, dissolve, and be all transferred to agitator tank, continue to stir 0.5-1 hour;
(3) the spray-dried device of above-mentioned gained slurry is realized to rapid draing, then material is all transferred to corundum crucible or saggar, be placed in Muffle furnace sintering 8-15 hour under protective gas 750-900 ℃ condition;
(4) gains abrasive lapping is sieved, obtain the coated lithium titanate anode material of carbon.
2. according to the preparation method of the coated lithium titanate anode material of a kind of nanometer carbon described in claims 1, it is characterized in that: comprise following step: the strong base solution of (1) configuration 8mol/L, measuring 80ml adds in the autoclave polytetrafluoroethyllining lining of 100ml, taking 2g titanium dioxide adds wherein again, then be placed in baking oven in 160 ℃ of reactions 5 hours, reaction finishes, by hydrochloric acid cleaning number time for the sediment in autoclave polyethylene liner, with distilled water, wash and filter again, be finally placed in 100 ℃, drying equipment and be dried 5 hours;
(2) by Li:Ti mol ratio, be that 0.84:1 weighs titanium dioxide powder material after lithium carbonate and preliminary treatment, be placed in ball grinder; And then take the solubility carbon source of 0.2 times of molal weight, and add in beaker and with a small amount of distilled water dissolving, be more all transferred to ball grinder, put into agate ball ball milling 1 hour;
(3) the spray-dried equipment of above-mentioned gained material is realized to rapid draing, then material is all transferred to corundum crucible or saggar, be placed in Muffle furnace sintering 15 hours under 800 ℃ of conditions of protective gas;
(4) gains abrasive lapping is sieved, obtain the coated lithium titanate anode material of carbon.
3. according to the preparation method of the coated lithium titanate anode material of a kind of nanometer carbon described in claims 1, it is characterized in that: comprise following step: the strong base solution of (1) configuration 6mol/L, measuring 80ml adds in the autoclave polytetrafluoroethyllining lining of 100ml, taking 2g titanium dioxide adds wherein again, then be placed in baking oven reacts 3 hours between 180 ℃, reaction finishes, by hydrochloric acid cleaning number time for the sediment in autoclave polyethylene liner, with distilled water, wash and filter again, be finally placed in 100 ℃, drying equipment and be dried 5 hours;
(2) by Li:Ti mol ratio, be that 0.84:1 weighs titanium dioxide powder material after lithium carbonate and preliminary treatment, be placed in ball grinder; And then take the solubility carbon source of 0.2 times of molal weight, and add in beaker and with a small amount of distilled water dissolving, be more all transferred to ball grinder, put into agate ball ball milling 1 hour;
(3) by the spray-dried equipment rapid draing of above-mentioned gained material, then material is all transferred to corundum crucible or saggar, is placed in Muffle furnace sintering 15 hours under 800 ℃ of conditions of protective gas;
(4) gains abrasive lapping is sieved, obtain the coated lithium titanate anode material of carbon.
4. according to the preparation method of the coated lithium titanate anode material of a kind of nanometer carbon described in claims 1, it is characterized in that: described lithium source is lithium carbonate lithium hydroxide, a kind of in lithium nitrate or their mixture.
5. according to the preparation method of the coated lithium titanate anode material of a kind of nanometer carbon described in claims 4, it is characterized in that: described titanium dioxide is a kind of in anatase titanium dioxide, unformed titanium dioxide or their mixture.
6. according to the preparation method of the coated lithium titanate anode material of a kind of nanometer carbon described in claims 5, it is characterized in that: described solubility carbon source is a kind of in glucose, citric acid, polyethylene glycol, starch or their mixture.
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WO2017008614A1 (en) * | 2015-07-15 | 2017-01-19 | 田东 | Method for fabricating modified lithium titanate negative-electrode material by amorphous carbon deposition |
CN107055595A (en) * | 2017-04-17 | 2017-08-18 | 黄正平 | A kind of preparation method of lithium cell cathode material |
CN108682795A (en) * | 2018-03-28 | 2018-10-19 | 合肥国轩高科动力能源有限公司 | A kind of ternary cathode material of lithium ion battery surface acid-washing cladding TiO2Method |
CN108682795B (en) * | 2018-03-28 | 2021-01-08 | 合肥国轩高科动力能源有限公司 | Surface pickling coating TiO of ternary anode material of lithium ion battery2Method (2) |
CN113346057A (en) * | 2021-05-18 | 2021-09-03 | 贵州理工学院 | Lithium battery electrical property improvement and test method based on material modification technology |
CN113346057B (en) * | 2021-05-18 | 2023-03-14 | 贵州理工学院 | Lithium battery electrical property improvement and test method based on material modification technology |
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