CN103682278B - The preparation method of the coated lithium titanate anode material of a kind of nanometer carbon - Google Patents
The preparation method of the coated lithium titanate anode material of a kind of nanometer carbon Download PDFInfo
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- CN103682278B CN103682278B CN201310727836.7A CN201310727836A CN103682278B CN 103682278 B CN103682278 B CN 103682278B CN 201310727836 A CN201310727836 A CN 201310727836A CN 103682278 B CN103682278 B CN 103682278B
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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
- H01M4/362—Composites
- H01M4/366—Composites as layered products
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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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
- 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
- H01M4/625—Carbon or graphite
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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
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- 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 preparation method of the coated lithium titanate anode material of a kind of nanometer carbon, comprise following step: (1) configuration strong base solution, take titanium dioxide, add autoclave, between 160-180 DEG C, 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 dry; (2) press titanium dioxide powder material after Li:Ti molar ratio weighing lithium source and pretreatment, be placed in ball grinder, and then take solubility carbon source and add a small amount of distilled water, under normal temperature or heating condition, dissolve, and be all transferred to agitator tank; (3) spray-dried slurry device is realized to rapid draing, then material is all transferred to corundum crucible or saggar, be placed in Muffle furnace at protective gas sintering; (4) gains abrasive lapping is sieved, obtain the coated lithium titanate anode material of carbon.
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 in 60-70 age the earliest. Through the exploration of nearly 20 years, taken the lead in developing taking material with carbon element as negative pole, with LiCoO by Japanese Sony energy company and gondola Moli energy company in nineteen ninety2For 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 DEG C-60 DEG C, 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 is mainly made up 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 is taking graphite, hard carbon as main, and lithium titanate anode material is emerging high cycle performance negative material of 21 century. Compared to the lithium rechargeable battery of carbon negative pole composition, 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, avoid the generation of lithium dendrite arm, ensure the safety of lithium ion battery. The another one important feature of lithium titanate battery is to form SEI film, has so just reduced the loss of lithium ion battery irreversible capacity, the therefore graphite cathode material the most frequently used with respect to lithium ion battery, and lithium titanate battery has better durability. Result shows by experiment, use lithium titanate as the lithium battery of negative pole compared with conventional graphite lithium battery, the life-span can extend to 4-6 doubly. This has just been avoided changing battery at vehicle service life phase internal cause deterioration of battery, more can not cause the use cost of user's vehicle to go up. Toshiba of Japan is just used the car lithium battery of lithium titanate at present in volume production. EnerSol energy resource system company of the U.S. finds that lithium titanate battery is adapted at applying in intelligent grid energy storage and electric automobile, at present also the affiliate who actively finds lithium titanate battery development& testing.
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, but that solid phase method is produced the lithium titanate material particle size obtaining 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 preparation method that can realize material particle nanometer and realize simultaneously the coated lithium titanate anode material of the coated a kind of nanometer carbon of the even carbon of material.
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 DEG C, 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 DEG C 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 pretreatment, 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 DEG C 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 DEG C of reactions 5 hours, reaction finishes, by hydrochloric acid cleaning number time for the sediment in autoclave polyethylene liner, wash and filter with distilled water again, be finally placed in 100 DEG C, drying equipment and be dried 5 hours; (2) be that 0.84:1 weighs titanium dioxide powder material after lithium carbonate and pretreatment by Li:Ti mol ratio, 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 DEG C 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 DEG C, react 3 hours, reaction finishes, by hydrochloric acid cleaning number time for the sediment in autoclave polyethylene liner, wash and filter with distilled water again, be finally placed in 100 DEG C, drying equipment and be dried 5 hours;
(2) be that 0.84:1 weighs titanium dioxide powder material after lithium carbonate and pretreatment by Li:Ti mol ratio, 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 spray-dried above-mentioned gained material equipment rapid draing, then material is all transferred to corundum crucible or saggar, is placed in Muffle furnace sintering 15 hours under 800 DEG C 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; obtain nano level titanium dioxide powder material; and by solubility carbon source, material is carried out to abundant infiltration; in the process of decomposing in carbon source, 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, save production cost, and strong base solution is to the TiO2 pretreatment 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 electrical conductivity, when having realized raising material property, reduced manufacturing cost.
Brief description of the drawings
Fig. 1 is the X ray diffracting spectrum of the lithium titanate material prepared of embodiment 1;
Fig. 2 is the scanning electron microscope image of embodiment 1 gained lithium titanate material;
Fig. 3 is that the coated lithium titanate material of carbon and nickel-cobalt lithium manganate material prepared by embodiment 1 is made into the cycle characteristics collection of illustrative plates of simulating button cell.
Detailed description of the invention
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 coated composite lithium titanate negative material of nanometer and carbon, 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 DEG C, reacts 5 hours. Reaction finishes, and by hydrochloric acid cleaning number time for the sediment in autoclave polyethylene liner, then wash and filters with distilled water, is finally placed in 100 DEG C, drying equipment and is dried 5 hours; (2) be that 0.84:1 weighs titanium dioxide powder material after lithium carbonate and pretreatment by Li:Ti mol ratio, 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 also dissolve with a small amount of distilled water, 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 DEG C of conditions of protective gas; (4) gains abrasive lapping is sieved, obtain lithium titanate anode material.
Then take lithium titanate material, conductive agent and binding agent by the mass ratio of 85:10:5, 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 DEG C 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 DEG C, reacts 3 hours. Reaction finishes, and by hydrochloric acid cleaning number time for the sediment in autoclave polyethylene liner, then wash and filters with distilled water, is finally placed in 100 DEG C, drying equipment and is dried 5 hours; (2) be that 0.84:1 weighs titanium dioxide powder material after lithium carbonate and pretreatment by Li:Ti mol ratio, 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 also dissolve with a small amount of distilled water, be more all transferred to ball grinder, put into agate ball ball milling 1 hour; (3) by spray-dried above-mentioned gained material equipment rapid draing, then material is all transferred to corundum crucible or saggar, is placed in Muffle furnace sintering 15 hours under 800 DEG C 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) be that 0.84:1 weighs titanium dioxide powder material after lithium carbonate and pretreatment by Li:Ti mol ratio, be placed in ball grinder; Then add a small amount of distilled water, then put into agate ball, ball milling 1 hour.
(2) by spray-dried above-mentioned gained material equipment rapid draing, then material is all transferred to corundum crucible or saggar, is placed in Muffle furnace sintering 15 hours under 800 DEG C 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. a preparation method for the coated lithium titanate anode material of nanometer carbon, is characterized in that: comprise following step:
(1) strong base solution of configuration 1-15mol/L, be that 10-50:1 takes titanium dioxide by the mass ratio of strong base solution and titanium dioxide, add autoclave, between 160-180 DEG C, 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 DEG C 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 pretreatment, be placed in ball grinder, and then to take molal weight be Ti salt molal weight 0.1-0.2 solubility carbon source doubly, add a small amount of distilled water, under normal temperature or heating condition, dissolve, and be all transferred to agitator tank, and continue to stir 0.5-1 hour, obtain slurry;
(3) spray-dried above-mentioned slurry device 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 DEG C condition, obtain material;
(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 DEG C of reactions 5 hours, reaction finishes, by hydrochloric acid cleaning number time for the sediment in autoclave polyethylene liner, wash and filter with distilled water again, be finally placed in 100 DEG C of vacuum drying of drying equipment 5 hours;
(2) be that 0.84:1 weighs titanium dioxide powder material after lithium carbonate and pretreatment by Li:Ti mol ratio, be placed in ball grinder; And then take the solubility carbon source that molal weight is 0.2 times of Ti salt molal weight, and add in beaker and also dissolve with a small amount of distilled water, be more all transferred to ball grinder, put into agate ball ball milling 1 hour, obtain slurry;
(3) the spray-dried equipment 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 15 hours under 800 DEG C of conditions of protective gas, obtain material;
(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 in 180 DEG C of reactions 3 hours, reaction finishes, by hydrochloric acid cleaning number time for the sediment in autoclave polyethylene liner, wash and filter with distilled water again, be finally placed in 100 DEG C of vacuum drying of drying equipment 5 hours;
(2) be that 0.84:1 weighs titanium dioxide powder material after lithium carbonate and pretreatment by Li:Ti mol ratio, be placed in ball grinder; And then take the solubility carbon source that molal weight is 0.2 times of Ti salt molal weight, and add in beaker and also dissolve with a small amount of distilled water, be more all transferred to ball grinder, put into agate ball ball milling 1 hour, obtain slurry;
(3) by spray-dried above-mentioned gained slurry equipment rapid draing, then material is all transferred to corundum crucible or saggar, is placed in Muffle furnace sintering 15 hours under 800 DEG C of conditions of protective gas, obtain material;
(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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| CN104393273A (en) * | 2014-10-27 | 2015-03-04 | 山东精工电子科技有限公司 | Preparation method of lithium titanate negative electrode material |
| CN104934589A (en) * | 2015-07-15 | 2015-09-23 | 田东 | Amorphous carbon deposit modified lithium titanate negative electrode material preparation method |
| CN107055595A (en) * | 2017-04-17 | 2017-08-18 | 黄正平 | A kind of preparation method of lithium cell cathode material |
| 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) |
| 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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