CN101609880A - A kind of ferrousphosphate lithium material of carbon coated and preparation technology thereof - Google Patents
A kind of ferrousphosphate lithium material of carbon coated and preparation technology thereof Download PDFInfo
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Abstract
The invention discloses a kind of ferrousphosphate lithium material and preparation technology thereof of carbon coated, ferrous oxalate, lithium carbonate and ammonium dihydrogen phosphate are carried out ball milling to mix, anoxybiotic presintering once, get powder A after the cooling, powder A and carbon source are carried out the ball milling carbon coated, coat back gained slurry drying and get powder material B, powder material B is passed through the anoxybiotic sintering again, cool off, promptly get the ferrousphosphate lithium material of carbon coated; Wherein, the used carbon source of carbon coated is mainly super conductive carbon black and polytetrafluoroethylene.Excellent material performance of the present invention can satisfy the above discharge of 30C; Long-term cycle performance is better, 1500 circulations, and capability retention is more than 85%, and technology is simple, and cost is low, is convenient to large-scale production.
Description
Technical field:
The invention belongs to the lithium ion battery field, be specifically related to a kind of ferrousphosphate lithium material and preparation technology thereof of carbon coated.
Background technology:
" ferrousphosphate lithium material " and " ferrous phosphate lithium battery " is the most popular keyword in the current battery industry.Have than much longer useful life of similar battery as the lithium ion battery of positive electrode and have safer characteristic with ferrousphosphate lithium material, and wherein contain heavy metal and noble metal hardly, therefore in the long run this series products manufacturing cost will inevitably be reduced to masses can generally accepted level, its cost performance of product will surpass at present institute widely lead-acid battery, nickel-cadmium cell, Ni-MH battery and the present lithium manganate battery and the cobalt acid lithium battery of use.
Ferrousphosphate lithium material has olivine crystal structure, is one of popular anode material for lithium-ion batteries of Recent study.Its theoretical capacity is 170mAh/g, and its actual capacity is not up to 110mAh/g when having doping vario-property.By to LiFePO
4Carry out finishing, its actual capacity can be up to 165mAh/g, very near theoretical capacity.Operating voltage range is about 2.5～4.0V.LiFePO
4Major defect be that theoretical capacity has only 170mAh/g, under low temperature and the room temperature conductivity have only ten thousand of cobalt acid lithium material/, the material tap density also has only 1.0g/cm
3About, cause the battery volumetric specific energy made little.Based on above reason, LiFePO
4Extraordinary application prospect is being arranged aspect the large-scale lithium ion battery.But to demonstrate the powerful market competitiveness, LiFePO in the entire lithium ion battery field
4But face following unfavorable factor: (1) is from LiMn
2O
4, LiMnO
2, LiNiMO
2The low-cost competition of positive electrode; (2) may preferentially select the particular battery material that is more suitable for different application people; (3) LiFePO
4Gram volume not high; What (4) more pay close attention to the high-tech sector people may not be cost but performance, as is applied to mobile phone and notebook computer, and people may be more prone to select for use cobalt acid lithium (5) LiFePO
4Be badly in need of to improve its conductive capability during deep discharge under 1C speed, improve its specific capacity with this.(6) aspect fail safe, LiCoO
2Representing the safety standard of industrial quarters at present, and LiNiO
2Fail safe also have increased significantly, have only LiFePO
4Show higher security performance,, could guarantee its sufficient competition advantage at secure context especially in the application of aspects such as electric automobile.
Pure ferrousphosphate lithium material conductivity is bad, has limited its capacity performance in battery.In order to improve the performance of ferrousphosphate lithium material, around the particle of ferrousphosphate lithium material, coat one deck carbon, strengthen its conductive capability, can reduce the size of LiFePO 4 particle simultaneously.The invention provides a kind of ferrousphosphate lithium material and preparation technology thereof of carbon coated, this technology is simple and easy to implement, and gained material conductive capability is strong, and effect is obvious, is worthy to be popularized.
Summary of the invention:
The objective of the invention is to overcome ferrousphosphate lithium material and the preparation technology thereof that above-mentioned weak point provides a kind of carbon coated.
The present invention seeks to realize in the following manner:
A kind of ferrousphosphate lithium material of carbon coated, this material is prepared by following method: with ferrous oxalate, lithium carbonate, the ammonium dihydrogen phosphate molar ratio 0.95-1.1 according to Li, Fe, P element: 0.97-1.05: the 0.97-1.05 ball milling mixes, anoxybiotic presintering once, get powder A after the cooling, powder A and carbon source are carried out the ball milling carbon coated, coat back gained slurry drying and get powder material B, powder material B is passed through the anoxybiotic sintering again, cool off, promptly get the ferrousphosphate lithium material of carbon coated; Wherein, the used carbon source of carbon coated is mainly super conductive carbon black (super-p) and polytetrafluoroethylene.
Above-mentioned ferrous oxalate, lithium carbonate, ammonium dihydrogen phosphate are that 1.05: 1: 1 ball millings mix according to the amount of substance ratio of Li, Fe, P preferably.
Above-mentioned carbon source is the super conductive carbon black (2-2.5% of preferred powder A weight) of powder A weight 0.5-5.5%, the deionized water of the polytetrafluoroethylene of powder A weight 0.5-2.5% and powder A weight 35-55% (40-55% of preferred powder A weight).
The preparation technology of the ferrousphosphate lithium material of above-mentioned carbon coated, it is characterized in that ferrous oxalate, lithium carbonate, the ammonium dihydrogen phosphate molar ratio 0.95-1.1 according to Li, Fe, P element: 0.97-1.05: the 0.97-1.05 ball milling mixes, anoxybiotic presintering once, get powder A after the cooling, powder A and carbon source are carried out the ball milling carbon coated, coat back gained slurry drying and get powder material B, powder material B is passed through the anoxybiotic sintering again, cool off, promptly get the ferrousphosphate lithium material of carbon coated; Wherein, the used carbon source of carbon coated is mainly super conductive carbon black (super-p) and polytetrafluoroethylene.
The technology of the ferrousphosphate lithium material of above-mentioned carbon coated specifically can may further comprise the steps:
A, ferrous oxalate, lithium carbonate, ammonium dihydrogen phosphate are carried out the solid phase ball milling mix, ball milling time 8-24h, ball milling finish pellet is separated;
B, the above-mentioned raw material that mix are carried out anoxybiotic presintering 2-4h, sintering temperature is selected 150-350 ℃ (preferred 200-300 ℃), and take out the cooling back, powder A;
C, above-mentioned powder A is poured in the agitating ball mill, add super conductive carbon black, polytetrafluoroethyl-ne aqueous solution and deionized water, stirring ball-milling 0.5-3h, slurry is extracted out;
D, with above-mentioned slurry via spray drying, baking temperature is selected 120-175 ℃ for use, powder material B;
E, with above-mentioned powder material B anoxybiotic sintering 2-18h (preferred sintering 10-18h), sintering temperature is selected 550-725 ℃ (preferred sintering temperature 650-700 ℃), takes out behind the cool to room temperature, pulverizes, and obtains the ferrousphosphate lithium material of finished product carbon coated.All commercially available the getting of material that the present invention is used.
Beneficial effect of the present invention compared with prior art: 1. it is low to select for use super conductive carbon black and aqueous binders PTFE to wrap up cost, and effect is obvious.Agitating ball mill is as parcel equipment, the efficient height, and energy consumption is low, can high volume applications, present large-scale agitating ball mill once can be handled about 5000kg powder.2. the method for synthesizing lithium ferrous phosphate is simple, is convenient to large-scale production.Dry ball milling is adopted in the precursor preparation, can effectively control manufacturing cost; Carry out the secondary wet process stirring ball-milling during carbon coated, can strengthen the uniformity coefficient of the batch mixing in the raw material, the performance of final products is better.3. according to the LiFePO 4 of this method production, carbon and tight by combination between the LiFePO 4 that coats finally can be owing to disintegrating process changes carbon content.The final products excellent performance can satisfy the above discharge of 30C; Long-term cycle performance is better, 1500 circulations, and capability retention is more than 85%.
Embodiment
Embodiment 1.
1. take by weighing 189g ferrous oxalate, 37g lithium carbonate, 115g ammonium dihydrogen phosphate, place planetary ball mill high speed ball milling 9h after, mixture, take out standby.
2. said mixture is placed the stainless steel saggar, put into chamber type electric resistance furnace anoxybiotic presintering 2h, temperature is 250 ℃, gets powder A after the cooling.
3. take by weighing 300g powder A; add the super conductive carbon black SP-Li of 6g (Shanghai converge general industrial chemical Co., Ltd); 2.5g concentration is 60% PTFE (polytetrafluoroethylene) aqueous solution (polytetrafluoroethylene be powder A weight 0.5%); the deionized water of 120g; above-mentioned raw materials places 0.5L agitating ball mill stirring ball-milling 0.5h, and the slurry that mixes is released.
4. above-mentioned slurry is inserted drying on the mini spray dryer, baking temperature is selected 120 ℃, obtains powder material B.
5. powder material B is placed the stainless steel saggar, place 675 ℃ resistance furnace anoxybiotic sintering 10h, cooling is taken out, and pulverizes, and obtains the ferrousphosphate lithium material of finished product carbon coated.
Final carbon content analytical test is 2.76% in the finished product LiFePO 4, and theoretical value is 2.97%, and material is almost not loss of carbon in building-up process, and visible carbon and LiFePO 4 combination are closely.
The ferrousphosphate lithium material half-cell test of finished product carbon coated, gram volume reaches 163mAh/g; Test after making model 063048 actual battery, capacity is up to 550mAh, the 1C charge-discharge test, and 1500 circulations, capability retention is more than 88%.
Embodiment 2.
1. take by weighing 198g ferrous oxalate, 38.48g lithium carbonate, 120.75g ammonium dihydrogen phosphate, place planetary ball mill high speed ball milling 9h, get mixture, take out standby.
2. said mixture is placed the stainless steel saggar, put into chamber type electric resistance furnace anoxybiotic pre-burning 2.5h, temperature is selected 285 ℃, gets powder A after the cooling.
3. take by weighing 300g powder A, add the super conductive carbon black of 6.6g, 5g concentration is 60% PTFE (polytetrafluoroethylene) aqueous solution (polytetrafluoroethylene be powder A weight 1%), the deionized water of 135g, above-mentioned raw materials places 0.5L agitating ball mill stirring ball-milling 0.5h, and the slurry that mixes is released.
4. above-mentioned slurry is inserted drying on the mini spray dryer, baking temperature is selected 145 ℃, obtains powder material B.
5. powder material B is placed the stainless steel saggar, place 685 ℃ resistance furnace anoxybiotic sintering 12h, cooling is taken out, and pulverizes, and obtains the ferrousphosphate lithium material of finished product carbon coated.
Final carbon content analytical test is 3.16% in the finished product LiFePO 4, and theoretical value is 3.21%, and material is almost not loss of carbon in building-up process, and visible carbon and LiFePO 4 combination are closely.
The ferrousphosphate lithium material half-cell test of finished product carbon coated, gram volume reaches 157mAh/g; Test after making model 063048 actual battery, capacity is up to 535mAh, the 1C charge-discharge test, and 1500 circulations, capability retention is more than 89%.
Embodiment 3.
1. take by weighing 171g ferrous oxalate, 37g lithium carbonate, 111.55g ammonium dihydrogen phosphate, place planetary ball mill high speed ball milling 18h, get mixture, take out standby.
2. said mixture is placed the stainless steel saggar, put into chamber type electric resistance furnace anoxybiotic pre-burning 3.5h, temperature is selected 200 ℃, gets powder A after the cooling.
3. take by weighing 300g powder A, add the super conductive carbon black of 6.6g, 5g concentration is 60% PTFE (polytetrafluoroethylene) aqueous solution (polytetrafluoroethylene be powder A weight 1%), and the deionized water of 165g, above-mentioned raw materials place 0.5L agitating ball mill stirring ball-milling 0.75h.The slurry that mixes is released.
4. above-mentioned slurry is inserted drying on the mini spray dryer, baking temperature is selected 175 ℃, obtains powder material B.
5. powder material B is placed the stainless steel saggar, place 700 ℃ resistance furnace anoxybiotic sintering 18h, cooling is taken out, and pulverizes, and obtains the ferrousphosphate lithium material of finished product carbon coated.
Final carbon content analytical test is 3.16% in the finished product LiFePO 4, and theoretical value is 3.21%, and material is almost not loss of carbon in building-up process, and visible carbon and LiFePO 4 combination are closely.
The ferrousphosphate lithium material half-cell test of finished product carbon coated, gram volume reaches 159mAh/g; Test after making model 063048 actual battery, capacity is up to 545mAh, the 1C charge-discharge test, and 1500 circulations, capability retention is more than 85.3%.
Embodiment 4
1. take by weighing 180g ferrous oxalate, 35.9g lithium carbonate, 115g ammonium dihydrogen phosphate, place planetary ball mill high speed ball milling 8h, get mixture, take out standby.
2. said mixture is placed the stainless steel saggar, put into chamber type electric resistance furnace anoxybiotic pre-burning 2h, temperature is selected 150 ℃, gets powder A after the cooling.
3. take by weighing 300g powder A, add the super conductive carbon black of 1.5g, 10g concentration is 60% PTFE (polytetrafluoroethylene) aqueous solution (polytetrafluoroethylene be powder A weight 2%), and the deionized water of 105g, above-mentioned raw materials place 0.5L agitating ball mill stirring ball-milling 3h.The slurry that mixes is released.
4. above-mentioned slurry is inserted drying on the mini spray dryer, baking temperature is selected 120 ℃, obtains powder material B.
5. powder material B is placed the stainless steel saggar, place 700 ℃ resistance furnace anoxybiotic sintering 2h, cooling is taken out, and pulverizes, and obtains the ferrousphosphate lithium material of finished product carbon coated.
Final carbon content analytical test is 0.722% in the finished product LiFePO 4, and theoretical value is 0.731%, and material is almost not loss of carbon in building-up process, and visible carbon and LiFePO 4 combination are closely.
The ferrousphosphate lithium material half-cell test of finished product carbon coated, gram volume reaches 161mAh/g; Test after making model 063048 actual battery, capacity is up to 549mAh, the 1C charge-discharge test, and 1500 circulations, capability retention is 85.21%.
Embodiment 5
1. take by weighing 180g ferrous oxalate, 37g lithium carbonate, 115g ammonium dihydrogen phosphate, place planetary ball mill high speed ball milling 18h, get mixture, take out standby.
2. said mixture is placed the stainless steel saggar, put into chamber type electric resistance furnace anoxybiotic pre-burning 3.5h, temperature is selected 200 ℃, gets powder A after the cooling.
3. take by weighing 300g powder A, add the super conductive carbon black of 16.5g, 12.5g concentration is 60% PTFE (polytetrafluoroethylene) aqueous solution (polytetrafluoroethylene be powder A weight 2.5%), the deionized water of 165g, above-mentioned raw materials place 0.5L agitating ball mill stirring ball-milling 0.75h.The slurry that mixes is released.
4. above-mentioned slurry is inserted drying on the mini spray dryer, baking temperature is selected 150 ℃, obtains powder material B.
5. powder material B is placed the stainless steel saggar, place 700 ℃ resistance furnace anoxybiotic sintering 8h, cooling is taken out, and pulverizes, and obtains the ferrousphosphate lithium material of finished product carbon coated.
Final carbon content analytical test is 9.01% in the finished product LiFePO 4, and theoretical value is 9.26%, and material is almost not loss of carbon in building-up process, and visible carbon and LiFePO 4 combination are closely.
The ferrousphosphate lithium material half-cell test of finished product carbon coated, gram volume reaches 149mAh/g; Test after making model 063048 actual battery, capacity is up to 533mAh, the 1C charge-discharge test, and 1500 circulations, capability retention is 92.7%.
Comparative Examples 1.
1. take by weighing 180g ferrous oxalate, 37g lithium carbonate, 115g ammonium dihydrogen phosphate, add the super conductive carbon black of 3g, the deionized water of 165g (dry powder quality about 50%).Above-mentioned raw materials places 0.5L agitating ball mill stirring ball-milling 0.75h.The slurry that mixes is released.
2. above-mentioned slurry is inserted drying on the mini spray dryer, baking temperature is selected 175 ℃.The powder that obtains is waited until down the step and is used.
3. above-mentioned powder is placed the stainless steel saggar, place 700 ℃ resistance furnace anoxybiotic sintering 18h, cooling is taken out, and pulverizes, and obtains the ferrousphosphate lithium material of finished product carbon coated.
Final carbon content analytical test is 1.17% in the finished product LiFePO 4, and theoretical value is 1.97%, and material carbon loss in building-up process is bigger, and visible carbon and LiFePO 4 be not in conjunction with tight.
The ferrousphosphate lithium material half-cell test of finished product carbon coated, gram volume only is 145mAh/g; Test after making model 063048 actual battery, capacity is up to 490mAh, the 1C charge-discharge test, and 1500 circulations, capability retention is more than 79%.
Embodiment and Comparative Examples experimental result contrast table
| The test carbon content | Theoretical carbon content | Gram volume | |
| Embodiment 1 | ??2.76％ | ??2.97％ | ??163mAh/g |
| Embodiment 2 | ??3.16％ | ??3.21％ | ??157mAh/g |
| Embodiment 3 | ??3.16％ | ??3.21％ | ??159mAh/g |
| Embodiment 4 | ??0.722％ | ??0.731％ | ??161mAh/g |
| Embodiment 5 | ??9.01％ | ??9.26％ | ??149mAh/g |
| Comparative Examples 1 | ??1.17％ | ??1.97％ | ??145mAh/g |
Claims (5)
1, a kind of ferrousphosphate lithium material of carbon coated, it is characterized in that this material is prepared by following method: with ferrous oxalate, lithium carbonate, the ammonium dihydrogen phosphate molar ratio 0.95-1.1 according to Li, Fe, P element: 0.97-1.05: the 0.97-1.05 ball milling mixes, anoxybiotic presintering once, get powder A after the cooling, powder A and carbon source are carried out the ball milling carbon coated, coat back gained slurry drying and get powder material B, powder material B is passed through the anoxybiotic sintering again, cool off, promptly get the ferrousphosphate lithium material of carbon coated; Wherein, the used carbon source of carbon coated is mainly super conductive carbon black and polytetrafluoroethylene.
2, the ferrousphosphate lithium material of carbon coated according to claim 1 is characterized in that described ferrous oxalate, lithium carbonate, ammonium dihydrogen phosphate carry out ball milling according to the mol ratio of Li, Fe, P element and mix at 1.05: 1: 1.
3, the ferrousphosphate lithium material of carbon coated according to claim 1, it is characterized in that described carbon source is the super conductive carbon black of powder A weight 0.5-5.5%, the deionized water of the polytetrafluoroethylene of powder A weight 0.5-2.5% and powder A weight 35-55%.
4, the preparation technology of the ferrousphosphate lithium material of the described carbon coated of a kind of claim 1, it is characterized in that this technology may further comprise the steps: with ferrous oxalate, lithium carbonate and the ammonium dihydrogen phosphate mol ratio 0.95-1.1 according to Li, Fe, P element: 0.97-1.05: the 0.97-1.05 ball milling mixes, anoxybiotic presintering once, get powder A after the cooling, powder A and carbon source are carried out the ball milling carbon coated, coat back gained slurry drying and get powder material B, powder material B is passed through the anoxybiotic sintering again, cool off, promptly get the ferrousphosphate lithium material of carbon coated; Wherein, the used carbon source of carbon coated is mainly super conductive carbon black and polytetrafluoroethylene.
5, the preparation technology of the ferrousphosphate lithium material of carbon coated according to claim 4 is characterized in that this technology specifically may further comprise the steps:
A, ferrous oxalate, lithium carbonate, ammonium dihydrogen phosphate are carried out the solid phase ball milling mix, ball milling time 8-24h, ball milling finish pellet is separated;
B, the above-mentioned raw material that mix are carried out anoxybiotic presintering 2-4h, sintering temperature is selected 150-350 ℃, and take out the cooling back, powder A;
C, above-mentioned powder A is poured in the agitating ball mill, add super conductive carbon black, polytetrafluoroethyl-ne aqueous solution and deionized water, stirring ball-milling 0.5-3h, slurry is extracted out;
D, with above-mentioned slurry spray drying, baking temperature is selected 120-175 ℃ for use, powder material B;
E, with above-mentioned powder material B anoxybiotic sintering 2-18h, sintering temperature is selected 550-725 ℃, takes out behind the cool to room temperature, pulverizes, and obtains the ferrousphosphate lithium material of finished product carbon coated.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102148367A (en) * | 2010-02-08 | 2011-08-10 | 江西省金锂科技有限公司 | Method for preparing lithium-ion battery anode material of lithium iron phosphate |
| CN102237520A (en) * | 2010-04-23 | 2011-11-09 | 刘国奇 | Method for preparing high capacity lithium iron phosphate cathode material by double sintering |
| CN105513820A (en) * | 2016-01-12 | 2016-04-20 | 浙江大学 | Preparation method of carbon-coated LiMnPO4 material, and product and application of carbon-coated LiMnPO4 material |
| CN108134074A (en) * | 2017-12-26 | 2018-06-08 | 宁波职业技术学院 | The preparation method of anode of magnesium ion battery material |
| CN109755489A (en) * | 2017-11-08 | 2019-05-14 | 中国科学院大连化学物理研究所 | A kind of fluorophosphoric acid vanadium sodium/preparation of carbon complex and the application of compound |
| CN109920989A (en) * | 2019-03-01 | 2019-06-21 | 沈阳国科金能科技有限公司 | A kind of preparation method of three layers of carbon coating composite lithium iron phosphate cathode material |
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2009
- 2009-07-16 CN CNA200910181435XA patent/CN101609880A/en active Pending
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102148367A (en) * | 2010-02-08 | 2011-08-10 | 江西省金锂科技有限公司 | Method for preparing lithium-ion battery anode material of lithium iron phosphate |
| CN102237520A (en) * | 2010-04-23 | 2011-11-09 | 刘国奇 | Method for preparing high capacity lithium iron phosphate cathode material by double sintering |
| CN105513820A (en) * | 2016-01-12 | 2016-04-20 | 浙江大学 | Preparation method of carbon-coated LiMnPO4 material, and product and application of carbon-coated LiMnPO4 material |
| CN105513820B (en) * | 2016-01-12 | 2018-03-16 | 浙江大学 | A kind of preparation method of lithium manganese phosphate material of carbon coating and products thereof and application |
| CN109755489A (en) * | 2017-11-08 | 2019-05-14 | 中国科学院大连化学物理研究所 | A kind of fluorophosphoric acid vanadium sodium/preparation of carbon complex and the application of compound |
| CN108134074A (en) * | 2017-12-26 | 2018-06-08 | 宁波职业技术学院 | The preparation method of anode of magnesium ion battery material |
| CN109920989A (en) * | 2019-03-01 | 2019-06-21 | 沈阳国科金能科技有限公司 | A kind of preparation method of three layers of carbon coating composite lithium iron phosphate cathode material |
| CN109920989B (en) * | 2019-03-01 | 2022-01-14 | 沈阳国科金能科技有限公司 | Preparation method of three-layer carbon-coated composite lithium iron phosphate cathode material |
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Application publication date: 20091223 |