CN104701497A - Preparation method of ferrous phosphate Li/C composite material with high specific surface area - Google Patents
Preparation method of ferrous phosphate Li/C composite material with high specific surface area Download PDFInfo
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Abstract
The invention relates to a preparation method of a ferrous phosphate Li/C composite material with a high specific surface area. The preparation method comprises the steps: (1) mixing battery-level nano ferric phosphate and thermosetting phenol-formaldehyde resin liquid according to the mass ratio of 2: 1, and stirring so as to prepare uniform slurry; (2) heating the slurry at the temperature of 60-80 DEG C so as to solidify the slurry, and then, heating to the temperature of 180-200 DEG C so as to coke; (3) heating the coked material to the temperature of 400 DEG C, and maintaining for 2 hours so as to char; (4) mixing the charred material and a 10% lithium hydroxide solution, uniformly stirring, heating to the temperature of 700 DEG C at the rate of 10 DEG C per minute under the protection of high-purity nitrogen, maintaining for 6 hours, then, stopping heating, and naturally cooling to room temperature; (5) grinding a sintered product, and sieving the ground sintered product with a sieve with the pore size of 325 meshes, thereby obtaining the ferrous phosphate Li/C composite material with a high specific surface area.
Description
Technical field
The invention belongs to new chemical energy storage field, particularly a kind of preparation method of high-specific surface area LiFePO 4/C composite.
Background technology
Ferrousphosphate lithium material is a kind of positive electrode of lithium ion battery, there is cheap, abundant raw materials, nontoxic, Heat stability is good, specific energy are high, have extended cycle life, service time is of a specified duration, security performance is given prominence to and the feature of environmentally safe, its theoretical specific capacity is 170mAh/g, theoretical work voltage is about 3.45V, is the potential Olivine-type Cathode Material in Li-ion Batteries of a kind of most.The part but lithium iron phosphate positive material still comes with some shortcomings, as low in conductivity, the shortcoming such as ionic diffusion coefficient is low, poor performance at low temperatures, multiplying power discharging ability, causes its application aspect to receive many restrictions.Ultracapacitor is a kind of novel chemical device, its capacitance is higher than the traditional capacitance of same volume 100,000 times, there is high power charging-discharging ability good, have extended cycle life and the good advantage of low temperature aspect performance, but its specific energy is low, the energy that unit mass stores is well below the level of lithium ion battery.In recent years, domestic-developed has gone out the product that lithium ion battery and ultracapacitor are combined, and become capacitor batteries, its specific energy is 3 ~ 5 times of ultracapacitor, and discharge-rate is 10 ~ 20 times of conventional lithium-ion battery, has good application prospect.Capacitor batteries selects LiFePO 4 to mix as positive electrode with active carbon with high specific surface area usually, and both mixing uniformity with there is some problems in conjunction with tightness degree, the invention discloses the preparation method of a kind of high-specific surface area LiFePO 4/C composite, phenolic resins is introduced as carbon source in ferrousphosphate lithium material preparation process, the active carbon of high-specific surface area has been prepared while preparing LiFePO4, thus make active carbon and LiFePO 4 micro Distribution evenly, be conducive to the performance improving LiFePO 4/C composite.
Summary of the invention
The object of the present invention is to provide the preparation method of the composite material of a kind of LiFePO 4/C of high-specific surface area, the existing high-specific surface area of material of preparation, have again higher gram volume, and charge-discharge magnification is strong.
The technical scheme that the present invention realizes object is:
A kind of preparation method of high-specific surface area LiFePO 4/C composite, the step of preparation method is:
(1) LITHIUM BATTERY nano ferric phosphate mixes according to mass ratio 2:1 with thermosetting phenolic resin liquid, and mixture is poured into dispersion pan mixer, then stirs with the rotating speed of 800 revs/min and become uniform slurry in 1 hour;
(2) slurry is poured out within 2 hours, make it solidify 60 ~ 80 DEG C of heating, be then warmed up to 180 ~ 200 DEG C of maintenances with the speed of 1 DEG C/min and carry out coking in 4 hours;
(3) coked material grind into powder, be heated to 400 DEG C, keep 2 hours, obtain carbonated material, be reduced to room temperature;
(4) carbonated material is mixed with 10% lithium hydroxide solution, stir, and under high pure nitrogen protection, with the heating rate of 10 DEG C/min to 700 DEG C of sintering, keep 6 hours, then stop heating, naturally cool to room temperature;
(5) sintered product is ground, cross 325 mesh sieves, obtain high-specific surface area LiFePO 4/C composite
;
(6) nano ferric phosphate described in step (1) contains 2 crystallizations water;
(7) feature of the lithium hydroxide described in step (4) is that the molal quantity of lithium hydroxide used is identical with the molal quantity of nano ferric phosphate.
Advantage of the present invention is that process is simple, phenolic resins is utilized to produce active carbon, simultaneously as the ferric iron in reducing agent reduction ferric phosphate, lithium hydroxide has activated active carbon on the one hand, react with ferric phosphate on the other hand and prepared ferrousphosphate lithium material, thus form uniform high-specific surface area LiFePO 4/C composite.
embodiment
Below in conjunction with embodiment, the present invention is further described, and following embodiment is illustrative, is not determinate, can not limit protection scope of the present invention with following embodiment.
Embodiment 1
(1) LITHIUM BATTERY nano ferric phosphate 186g(99% purity is got, molecular formula FePO
42H
2o) mix with 93g thermosetting phenolic resin liquid (solid content 75%), mixture is poured into small-sized dispersion pan mixer, then stir with the rotating speed of 800 revs/min and become uniform slurry in 1 hour;
(2) slurry is poured out within 2 hours, make it solidify 80 DEG C of heating, be then warmed up to 200 DEG C of maintenances with the speed of 1 DEG C/min and carry out coking in 4 hours;
(3) coked material grind into powder, be heated to 400 DEG C, keep 2 hours, obtain carbonated material, be reduced to room temperature;
(4) carbonated material is mixed with 237.6g 10% lithium hydroxide solution, stir, and under high pure nitrogen protection, with the heating rate of 10 DEG C/min to 700 DEG C of sintering, keep 6 hours, then stop heating, naturally cool to room temperature;
(5) sintered product is ground, cross 325 mesh sieves, obtain high-specific surface area LiFePO 4/C composite
;
Test the material of preparation, specific area is 615m
2/ g, specific capacity is 80mAh/g.
Embodiment 2
(1) LITHIUM BATTERY nano ferric phosphate 186g(99% purity is got, molecular formula FePO
42H
2o) mix with 93g thermosetting phenolic resin liquid (solid content 75%), mixture is poured into small-sized dispersion pan mixer, then stir with the rotating speed of 800 revs/min and become uniform slurry in 1 hour;
(2) slurry is poured out within 2 hours, make it solidify 60 DEG C of heating, be then warmed up to 180 DEG C of maintenances with the speed of 1 DEG C/min and carry out coking in 4 hours;
(3) coked material grind into powder, be heated to 400 DEG C, keep 2 hours, obtain carbonated material, be reduced to room temperature;
(4) carbonated material is mixed with 237.6g 10% lithium hydroxide solution, stir, and under high pure nitrogen protection, with the heating rate of 10 DEG C/min to 700 DEG C of sintering, keep 6 hours, then stop heating, naturally cool to room temperature;
(5) sintered product is ground, cross 325 mesh sieves, obtain high-specific surface area LiFePO 4/C composite
;
Test the material of preparation, specific area is 585m
2/ g, specific capacity is 82mAh/g.
Claims (3)
1. a preparation method for high-specific surface area LiFePO 4/C composite, is characterized in that: the step of preparation method is:
(1) LITHIUM BATTERY nano ferric phosphate mixes according to mass ratio 2:1 with thermosetting phenolic resin liquid, and mixture is poured into dispersion pan mixer, then stirs with the rotating speed of 800 revs/min and become uniform slurry in 1 hour;
(2) slurry is poured out within 2 hours, make it solidify 60 ~ 80 DEG C of heating, be then warmed up to 180 ~ 200 DEG C of maintenances with the speed of 1 DEG C/min and carry out coking in 4 hours;
(3) coked material grind into powder, be heated to 400 DEG C, keep 2 hours, obtain carbonated material, be reduced to room temperature;
(4) carbonated material is mixed with 10% lithium hydroxide solution, stir, and under high pure nitrogen protection, with the heating rate of 10 DEG C/min to 700 DEG C of sintering, keep 6 hours, then stop heating, naturally cool to room temperature;
(5) sintered product is ground, cross 325 mesh sieves, obtain high-specific surface area LiFePO 4/C composite.
2. the preparation method of a kind of high-specific surface area LiFePO 4/C composite according to claim 1, is characterized in that: described nano ferric phosphate contains 2 crystallizations water.
3. the preparation method of a kind of high-specific surface area LiFePO 4/C composite according to claim 1, is characterized in that: the feature of described lithium hydroxide is, the molal quantity of lithium hydroxide is identical with the molal quantity of nano ferric phosphate.
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Citations (9)
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| CN101373667A (en) * | 2008-09-17 | 2009-02-25 | 四川大学 | High potential super capacitor electrode material and preparing method thereof |
| CN101944588A (en) * | 2010-09-14 | 2011-01-12 | 哈尔滨工业大学 | Capacitor carbon/lithium iron phosphate composite material, preparation method thereof and lithium-ion capacitor battery using same as cathode material |
| CN101527356B (en) * | 2009-04-17 | 2011-04-20 | 湖南工业大学 | LiFePO4/C composite anode material of carbon core structure and preparation method thereof |
| CN102110811A (en) * | 2011-01-14 | 2011-06-29 | 浙江大学 | Method for preparing nanoscale lithium ion battery LiFePo4/C anodal material |
| US20120099246A1 (en) * | 2010-10-21 | 2012-04-26 | Samsung Electro-Mechanics Co., Ltd. | Lithium ion capacitor |
| CN102769134A (en) * | 2012-08-15 | 2012-11-07 | 吉林大学 | Preparation method of lithium ion battery anode composite material LiFePO4/C |
| CN103682341A (en) * | 2013-12-26 | 2014-03-26 | 山东精工电子科技有限公司 | Method for synthesizing high-tap-density lithium iron phosphate material |
-
2013
- 2013-12-07 CN CN201310668111.5A patent/CN104701497A/en active Pending
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101237043A (en) * | 2008-01-31 | 2008-08-06 | 东北师范大学 | Method for making ferrous lithium phosphate/carbon compound material of high active disorderly ferric phosphate |
| CN101279726A (en) * | 2008-04-11 | 2008-10-08 | 赵兵 | Preparation for lithium iron phosphate |
| CN101373667A (en) * | 2008-09-17 | 2009-02-25 | 四川大学 | High potential super capacitor electrode material and preparing method thereof |
| CN101527356B (en) * | 2009-04-17 | 2011-04-20 | 湖南工业大学 | LiFePO4/C composite anode material of carbon core structure and preparation method thereof |
| CN101944588A (en) * | 2010-09-14 | 2011-01-12 | 哈尔滨工业大学 | Capacitor carbon/lithium iron phosphate composite material, preparation method thereof and lithium-ion capacitor battery using same as cathode material |
| US20120099246A1 (en) * | 2010-10-21 | 2012-04-26 | Samsung Electro-Mechanics Co., Ltd. | Lithium ion capacitor |
| CN102110811A (en) * | 2011-01-14 | 2011-06-29 | 浙江大学 | Method for preparing nanoscale lithium ion battery LiFePo4/C anodal material |
| CN102769134A (en) * | 2012-08-15 | 2012-11-07 | 吉林大学 | Preparation method of lithium ion battery anode composite material LiFePO4/C |
| CN103682341A (en) * | 2013-12-26 | 2014-03-26 | 山东精工电子科技有限公司 | Method for synthesizing high-tap-density lithium iron phosphate material |
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