CN104701499A - Preparation method of lithium iron phosphate/C composite material with high specific surface area - Google Patents
Preparation method of lithium iron phosphate/C composite material with high specific surface area Download PDFInfo
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- CN104701499A CN104701499A CN201310647936.9A CN201310647936A CN104701499A CN 104701499 A CN104701499 A CN 104701499A CN 201310647936 A CN201310647936 A CN 201310647936A CN 104701499 A CN104701499 A CN 104701499A
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Abstract
The invention relates to a preparation method of a lithium iron phosphate/C composite material with high specific surface area, which comprises the following steps: 1)taking battery grade nano ferric phosphate and battery grade lithium carbonate for mixing according to mol ratio of Fe: Li being at 0.99:1, grinding and adding butanone, regrinding, uniformly dispersing, adding 3% of polyvinyl alcohol aqueous solution, stirring to obtain uniform slurry, then slowly adding active carbon with high specific surface area, stirring to obtain the uniform slurry; 2)drying the slurry at 1-5 DEG C for 3-5 hours through air blast to become block solid; 3)under nitrogen protection, heating the block solid to 600 DEG C with speed of 2 DEG C/minute and sintering, keeping for 2 hours, heating to 720 DEG C with speed of 2 DEG C/minute and sintering, keeping for 4 hours, then stopping heating, naturally cooling to room temperature; and 4)grinding the sintered products, passing through a sieve with 325 meshes to obtain the lithium iron phosphate/C composite material with 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/, 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, active carbon is imported in ferrousphosphate lithium material preparation process, thus active carbon and LiFePO 4 are combined more, be conducive to the performance improving capacitor batteries.
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) get LITHIUM BATTERY nano ferric phosphate to mix according to mol ratio Fe:Li=0.99:1 ratio with battery-level lithium carbonate, put into mortar to grind, add according to 10% of mixture quality and analyze pure butanone, grind 30 minutes again, mixture is poured into small-sized dispersion pan mixer, add 3% polyvinyl alcohol water solution with ferric phosphate homogenous quantities again, stir with the rotating speed of 300 revs/min and become uniform slurry in 2 hours, then slowly add the active carbon with high specific surface area of ferric phosphate quality 10%, then stir with the rotating speed of 800 revs/min and become uniform slurry in 2 hours;
(2) slurry 105 DEG C of forced air dryings 3 ~ 5 hours, blocks of solid is become;
(3) blocks of solid under nitrogen protection, with the heating rate of 2 DEG C/min to 600 DEG C of sintering, keep 2 hours, with the heating rate of 2 DEG C/min to 720 DEG C of sintering, keep 4 hours, then stop heating, naturally cool to room temperature;
(4) sintered product is ground, cross 325 mesh sieves, obtain high-specific surface area LiFePO 4/C composite
;
(5) feature of the polyvinyl alcohol described in step (1) is that molecular weight is 5000 ~ 10000; Described nano ferric phosphate contains 2 crystallizations water;
(6) specific area of the active carbon with high specific surface area described in step (1) is at 1000 ~ 1500m
2/ g.
Advantage of the present invention is that process is simple, and the high-specific surface area LiFePO 4/C composite gram volume of preparation is at more than 110mAh/g, and specific area can reach 400m
2/ g, and can 40C charging, 60C electric discharge.
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 18.6g(99% purity is got, molecular formula FePO
42H
2o) with LITHIUM BATTERY micro mist lithium carbonate 3.79g(Shanghai China Lithium Industrial Co., Ltd., purity 99.9%) mixing, put into mortar to grind, add and analyze pure butanone 2.24g, then grind 30 minutes, mixture is poured into small-sized dispersion pan mixer, add 18.6g 3% polyvinyl alcohol (molecular weight the is 5000) aqueous solution again, stir with the rotating speed of 300 revs/min and become uniform slurry in 2 hours, (Korea S produces, specific area 1000 m then slowly to add 1.86g active carbon with high specific surface area while stirring
2/ g), then stir with the rotating speed of 800 turns minutes and become uniform slurry in 2 hours;
(2) slurry 105 DEG C of forced air dryings 5 hours, blocks of solid is become;
(3) blocks of solid under purity is 99.99% nitrogen protection, with the heating rate of 2 DEG C/min to 600 DEG C of sintering, keep 2 hours, with the heating rate of 2 DEG C/min to 720 DEG C of sintering, keep 4 hours, then stop heating, naturally cool to room temperature;
(4) sintered product is ground, cross 325 mesh sieves, obtain high-specific surface area LiFePO 4/C composite
;
Advantage of the present invention is that process is simple, and the high-specific surface area LiFePO 4/C composite gram volume of preparation is at more than 111mAh/g, and specific area can reach 405m
2/ g, and can 40C charging, 60C electric discharge.
Embodiment 2
(1) LITHIUM BATTERY nano ferric phosphate 18.6g(99% purity is got, molecular formula FePO
42H
2o) with LITHIUM BATTERY micro mist lithium carbonate 3.79g(Shanghai China Lithium Industrial Co., Ltd., purity 99.9%) mixing, put into mortar to grind, add and analyze pure butanone 2.24g, grind 30 minutes again, mixture is poured into small-sized dispersion pan mixer, add 18.6g 3% polyvinyl alcohol (molecular weight the is 10000) aqueous solution again, stir with the rotating speed of 300 revs/min and become uniform slurry in 2 hours, then (Korea S produces, specific area 1500 m slowly to add 1.86g active carbon with high specific surface area while stirring
2/ g), then stir with the rotating speed of 800 turns minutes and become uniform slurry in 2 hours;
(2) slurry 105 DEG C of forced air dryings 3 hours, blocks of solid is become;
(3) blocks of solid under purity is 99.99% nitrogen protection, with the heating rate of 2 DEG C/min to 600 DEG C of sintering, keep 2 hours, with the heating rate of 2 DEG C/min to 720 DEG C of sintering, keep 4 hours, then stop heating, naturally cool to room temperature;
(4) sintered product is ground, cross 325 mesh sieves, obtain high-specific surface area LiFePO 4/C composite
;
Advantage of the present invention is that process is simple, and the high-specific surface area LiFePO 4/C composite gram volume of preparation is at more than 111mAh/g, and specific area can reach 410m
2/ g, and can 43C charging, 66C electric discharge.
Embodiment 3
(1) LITHIUM BATTERY nano ferric phosphate 18.6g(99% purity is got, molecular formula FePO
42H
2o) with LITHIUM BATTERY micro mist lithium carbonate 3.79g(Shanghai China Lithium Industrial Co., Ltd., purity 99.9%) mixing, put into mortar to grind, add and analyze pure butanone 2.24g, then grind 30 minutes, mixture is poured into small-sized dispersion pan mixer, add 18.6g 3% polyvinyl alcohol (molecular weight the is 8000) aqueous solution again, stir with the rotating speed of 300 revs/min and become uniform slurry in 2 hours, (Korea S produces, specific area 1200 m then slowly to add 1.86g active carbon with high specific surface area while stirring
2/ g), then stir with the rotating speed of 800 turns minutes and become uniform slurry in 2 hours;
(2) slurry 105 DEG C of forced air dryings 4 hours, blocks of solid is become;
(3) blocks of solid under purity is 99.99% nitrogen protection, with the heating rate of 2 DEG C/min to 600 DEG C of sintering, keep 2 hours, with the heating rate of 2 DEG C/min to 720 DEG C of sintering, keep 4 hours, then stop heating, naturally cool to room temperature;
(4) sintered product is ground, cross 325 mesh sieves, obtain high-specific surface area LiFePO 4/C composite
;
Advantage of the present invention is that process is simple, and the high-specific surface area LiFePO 4/C composite gram volume of preparation is at more than 112mAh/g, and specific area can reach 410m
2/ g, and can 41C charging, 60C electric discharge.
Claims (4)
1. a preparation method for high-specific surface area LiFePO 4/C composite, is characterized in that: the step of preparation method is:
(1) get LITHIUM BATTERY nano ferric phosphate to mix according to mol ratio Fe:Li=0.99:1 ratio with battery-level lithium carbonate, put into mortar to grind, add according to 10% of mixture quality and analyze pure butanone, grind 30 minutes again, mixture is poured into small-sized dispersion pan mixer, add 3% polyvinyl alcohol water solution with ferric phosphate homogenous quantities again, stir with the rotating speed of 300 revs/min and become uniform slurry in 2 hours, then slowly add the active carbon with high specific surface area of ferric phosphate quality 10%, then stir with the rotating speed of 800 turns minutes and become uniform slurry in 2 hours;
(2) slurry 105 DEG C of forced air dryings 3 ~ 5 hours, blocks of solid is become;
(3) blocks of solid under nitrogen protection, with the heating rate of 2 DEG C/min to 600 DEG C of sintering, keep 2 hours, with the heating rate of 2 DEG C/min to 720 DEG C of sintering, keep 4 hours, then stop heating, naturally cool to room temperature;
(4) 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: the feature of described polyvinyl alcohol is that molecular weight is 5000 ~ 10000.
3. 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.
4. the preparation method of a kind of high-specific surface area LiFePO 4/C composite according to claim 1, is characterized in that: the specific area of described active carbon with high specific surface area is at 1000 ~ 1500m
2/ g.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110970608A (en) * | 2019-12-19 | 2020-04-07 | 湖南裕能新能源电池材料有限公司 | Lithium iron battery material and preparation method thereof |
Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1964106A (en) * | 2006-11-23 | 2007-05-16 | 武汉大学 | A method to manufacture anode material of LiFePO4/C for lithium ion cell |
| CN101159329A (en) * | 2007-11-12 | 2008-04-09 | 成都中科来方能源科技有限公司 | Composite positive pole material, battery-super electric capacity energy storage means and preparation method |
| CN101330141A (en) * | 2008-07-18 | 2008-12-24 | 清华大学 | Method for preparing lithium ionic battery anode material spherical LiFePO4 /C |
| WO2009117871A1 (en) * | 2008-03-28 | 2009-10-01 | Byd Company Limited | A method of preparing a lithium iron phosphate cathode material for lithium secondary batteries |
| CN101714627A (en) * | 2008-10-08 | 2010-05-26 | 中国科学院金属研究所 | Carbon nanotube/lithium iron phosphate composite positive electrode material and in situ 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 |
| CN102299319A (en) * | 2011-07-20 | 2011-12-28 | 彩虹集团公司 | Preparation method of lithium ion battery anode material LiFePO4 |
| CN102306783A (en) * | 2011-09-14 | 2012-01-04 | 哈尔滨工业大学 | Multi-layer graphene/lithium iron phosphate intercalated composite material, preparation method thereof, and lithium ion battery adopting multi-layer grapheme/lithium iron phosphate intercalated composite material as anode material |
| CN102610819A (en) * | 2012-04-05 | 2012-07-25 | 宁波力邦新能源科技有限公司 | Preparing method of high-activity material |
| CN103258995A (en) * | 2013-06-06 | 2013-08-21 | 郑州瑞普生物工程有限公司 | Preparation method of lithium iron phosphate material |
-
2013
- 2013-12-06 CN CN201310647936.9A patent/CN104701499B/en active Active
Patent Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1964106A (en) * | 2006-11-23 | 2007-05-16 | 武汉大学 | A method to manufacture anode material of LiFePO4/C for lithium ion cell |
| CN101159329A (en) * | 2007-11-12 | 2008-04-09 | 成都中科来方能源科技有限公司 | Composite positive pole material, battery-super electric capacity energy storage means and preparation method |
| WO2009117871A1 (en) * | 2008-03-28 | 2009-10-01 | Byd Company Limited | A method of preparing a lithium iron phosphate cathode material for lithium secondary batteries |
| KR20100139085A (en) * | 2008-03-28 | 2010-12-31 | 비와이디 컴퍼니 리미티드 | Method for producing lithium iron phosphate cathode material for lithium secondary battery |
| CN101330141A (en) * | 2008-07-18 | 2008-12-24 | 清华大学 | Method for preparing lithium ionic battery anode material spherical LiFePO4 /C |
| CN101714627A (en) * | 2008-10-08 | 2010-05-26 | 中国科学院金属研究所 | Carbon nanotube/lithium iron phosphate composite positive electrode material and in situ 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 |
| CN102299319A (en) * | 2011-07-20 | 2011-12-28 | 彩虹集团公司 | Preparation method of lithium ion battery anode material LiFePO4 |
| CN102306783A (en) * | 2011-09-14 | 2012-01-04 | 哈尔滨工业大学 | Multi-layer graphene/lithium iron phosphate intercalated composite material, preparation method thereof, and lithium ion battery adopting multi-layer grapheme/lithium iron phosphate intercalated composite material as anode material |
| CN102610819A (en) * | 2012-04-05 | 2012-07-25 | 宁波力邦新能源科技有限公司 | Preparing method of high-activity material |
| CN103258995A (en) * | 2013-06-06 | 2013-08-21 | 郑州瑞普生物工程有限公司 | Preparation method of lithium iron phosphate material |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110970608A (en) * | 2019-12-19 | 2020-04-07 | 湖南裕能新能源电池材料有限公司 | Lithium iron battery material and preparation method thereof |
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Effective date of registration: 20220608 Address after: 550400 Weng'an Economic Development Zone, Yinzhan Town, Weng'an county, Qiannan Buyei and Miao Autonomous Prefecture, Guizhou Province Patentee after: Guizhou batian new energy materials Co.,Ltd. Address before: 300402 7th Street, Gaoxin Avenue, yixingbu Industrial Zone, Beichen Science Park, Beichen District, Tianjin Patentee before: TIANJIN HEWEI TECHNOLOGY Co.,Ltd. |