CN109037660A - A kind of preparation method of composite lithium iron phosphate material - Google Patents
A kind of preparation method of composite lithium iron phosphate material Download PDFInfo
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- CN109037660A CN109037660A CN201811025474.6A CN201811025474A CN109037660A CN 109037660 A CN109037660 A CN 109037660A CN 201811025474 A CN201811025474 A CN 201811025474A CN 109037660 A CN109037660 A CN 109037660A
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- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
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Abstract
The present invention provides a kind of preparation methods of composite lithium iron phosphate material, include the following steps, (1) lithium source, source of iron, phosphorus source are mixed, and after mixing, the molar ratio of elemental lithium, ferro element and P elements is 0.95~1.05:0.95~1.05:0.95~1.05, and accessory positive material is added in mixed process, obtain mixed material A；(2) material A is ground, carbon source is added during the grinding process, control grinding partial size D50 is 0.05~1.0 μm, obtains material B；(3) material B is heated up under an inert atmosphere with the rate of heat addition of 2~20 DEG C/min, in 700~900 DEG C constant temperature calcining 4~12 hours, obtain sintered composite lithium iron phosphate cathode material C；(4) sintered positive electrode C will be obtained to crush, obtain final composite lithium iron phosphate material.The composite lithium iron phosphate material 1C that preparation method obtains through the invention discharges in 143mAh/g or more, and compacted density has good operability and lower cost advantage between 2.4~2.53.
Description
Technical field
The invention belongs to lithium iron phosphate positive material synthesis technical field more particularly to a kind of composite lithium iron phosphate materials
Preparation method.
Background technique
Currently, with advances in technology and expanding economy, lithium ion battery applications are more and more extensive.Wherein with ferric phosphate
Lithium material is the lithium ion battery of anode because having high safety, cyclical stability and reliability, gradually becomes China's vapour
The mainstream of vehicle power battery.But the compacted density of general LiFePO 4 material is lower, and manufactured lithium ion battery is caused to compare energy
Measure it is relatively low, although ternary battery energy density be much higher than phosphoric acid lithium battery, its price is more expensive, cycle performance and security performance
It is poor.If the compacted density of LiFePO 4 material can be increased substantially, the specific energy of ferric phosphate lithium cell can be significantly
It improves, so developing low-cost high-energy density ferric phosphate lithium cell accords with the demands of the market.
It is needed in the preparation method of iron phosphate compound anode material of lithium in the prior art using cosolvent NaPO3F and/or
LiPO3F, secondary granulation processing carry out under 100~900 DEG C of protective atmosphere, and secondary granulation handles the time as 12h~48h.It should
Method, time-consuming and fluxing agent need to be added for required secondary treatment, and fluxing agent is conducive to that lithium iron phosphate particles are secondary to grow up, but fluxing
Agent can also make to adulterate the impurity such as P in positive electrode simultaneously, influence the performance of positive electrode.If not using cosolvent, and can mention
The compacted density of high LiFePO 4 material, becomes urgent problem to be solved.
Summary of the invention
In view of this, the present invention is directed to propose a kind of preparation method of composite lithium iron phosphate material, to overcome the prior art
In deficiency, the present invention is added the accessory positive material of high-pressure solid, high capacity in LiFePO4 synthesis process, and with it is additional just
Pole material is kernel, and reaction is generated using LiFePO4 as inner casing, using conductive carbon layer as the core-shell type composite lithium iron phosphate material of shell
Material；This method will can effectively reduce the contact gap of each material after the processing of various raw material nanoizations, significant increase material is being burnt
Heat conduction efficiency, shortening firing time during knot, while the LiFePO4 for being also beneficial to reaction generation can be coated uniformly
In accessory positive material peripheral.
In order to achieve the above objectives, the technical scheme of the present invention is realized as follows:
A kind of preparation method of composite lithium iron phosphate material, includes the following steps,
(1) lithium source, source of iron, phosphorus source are mixed, and after mixing, the molar ratio of elemental lithium, ferro element and P elements
For 0.95~1.05:0.95~1.05:0.95~1.05, and accessory positive material is added in mixed process, obtains mixture
Expect A；
(2) material A being ground, carbon source is added during the grinding process, control grinding partial size D50 is 0.05~1.0 μm,
Obtain material B；
(3) material B is heated up under an inert atmosphere with the rate of heat addition of 2~20 DEG C/min, in 700~900 DEG C of perseverances
Temperature roasting 4~12 hours, obtains sintered composite lithium iron phosphate cathode material C；
(4) sintered positive electrode C will be obtained to crush, obtain final composite lithium iron phosphate material.
Preferably, in the step 1), accessory positive material is in cobalt acid lithium, LiMn2O4, lithium nickelate or nickle cobalt lithium manganate
One or more；The quality of accessory positive material accounts for lithium source, source of iron and phosphorus source material gross mass 5%~25%.
Preferably, in the step (1), lithium source be lithium hydroxide, lithium dihydrogen phosphate, lithium nitrate, lithium oxalate, lithium acetate,
One or more of lithium carbonate；The source of iron is ferric phosphate, in ferrous oxalate, ferric acetate, di-iron trioxide, ferric nitrate
One or more；Phosphorus source is phosphoric acid, ammonium dihydrogen phosphate, diammonium hydrogen phosphate, ammonium phosphate, ferric phosphate, biphosphate
One or more of lithium.
Preferably, in the step (2), carbon source is glucose, sucrose, citric acid, polyethylene glycol, polyvinyl alcohol, carbon are received
One or more of mitron, conductive black；Material A is added according to the 1%~20% of material A mass ratio in the carbon source
In.
Preferably, in the step (2), the method for the grinding is dry grinding and/or air-flow crushing.
Preferably, in the step (3), inert gas is one or more of nitrogen, argon gas, carbon dioxide.
Preferably, in the step (4), positive electrode C is crushed, and smashed partial size D50 is 0.5~3.0 μm.
The present invention also provides the composite lithium iron phosphate materials that the preparation method of composite lithium iron phosphate material as described above obtains
Material.
Present invention simultaneously provides a kind of anode, the composite lithium iron phosphate material obtained including preparation method as described above.
The present invention also provides a kind of lithium ion battery, the composite lithium iron phosphate material obtained including preparation method as described above
Material.
Compared with the existing technology, the preparation method of composite lithium iron phosphate material of the present invention, has the advantage that
The composite lithium iron phosphate material 1C that preparation method obtains through the invention discharges in 140mAh/g or more, compacted density
Between 2.4~2.53, and have good operability and lower cost advantage.
Detailed description of the invention
Fig. 1 is the SEM figure of composite lithium iron phosphate material prepared by the embodiment of the present invention 1；
Fig. 2 is the SEM figure of composite lithium iron phosphate material prepared by the embodiment of the present invention 1；
Fig. 3 is the SEM figure of positive electrode active materials prepared by comparative example 1 of the present invention.
Specific embodiment
In addition to being defined, technical term used in following embodiment has universal with those skilled in the art of the invention
The identical meanings of understanding.Test reagent used in following embodiment is unless otherwise specified conventional biochemical reagent；It is described
Experimental method is unless otherwise specified conventional method.
Below with reference to embodiment, the present invention will be described in detail.
Embodiment 1
Lithium carbonate, ferric phosphate are mixed according to molar ratio 1.05:1, and according to lithium carbonate and phosphoric acid weight of iron
10% addition cobalt acid lithium, after according to gross mass 15% be added sucrose, grind 3h after test D50=0.8 μm of mixed powder, will
Material is heated up in a nitrogen atmosphere with the rate of heat addition of 2 DEG C/min after grinding, is burnt within constant temperature calcining 6 hours in 750 DEG C
Lithium iron phosphate positive material after knot crushes sintered LiFePO4, D50=1.5 μm of Control granularity, is compacted
Density 2.45g/cm3Powdered composite lithium iron phosphate cathode material.
Embodiment 2
Lithium carbonate, ferric phosphate are mixed according to molar ratio 1.02:0.95, and according to lithium carbonate and phosphoric acid weight of iron
15% addition LiMn2O4, after according to gross mass 10% be added conductive black, grind 4h after test mixed powder D50=0.68
μm, material after grinding is heated up in a nitrogen atmosphere with the rate of heat addition of 10 DEG C/min, in 730 DEG C constant temperature calcining 8 hours
Sintered lithium iron phosphate positive material is obtained, sintered LiFePO4 is crushed, D50=1.5 μm of Control granularity, is obtained
To compacted density 2.48g/cm3Powdered composite lithium iron phosphate cathode material.
Embodiment 3
Lithium carbonate, ferric phosphate are mixed according to molar ratio 1.05:1, and according to lithium carbonate and phosphoric acid weight of iron
20% addition NCM622 (LiNi0.6Co0.2Mn0.2O2), glucose is added according to the 20% of gross mass after, is tested after grinding 5h
D50=0.55 μm of mixed powder, material after grinding is heated up in a nitrogen atmosphere with the rate of heat addition of 15 DEG C/min, in
800 DEG C obtain sintered lithium iron phosphate positive material in constant temperature calcining 6 hours, and sintered LiFePO4 is crushed, control
D50=1.5 μm of granulation degree obtains compacted density 2.43g/cm3Powdered composite lithium iron phosphate cathode material.
Embodiment 4
It is according to the molar ratio of elemental lithium, ferro element and P elements by lithium hydroxide, ferrous oxalate, phosphoric acid hydrogen ammonia
1.05:0.95:1.0 is mixed, and according to 17% addition lithium nickelate of gross mass, after according to the 18% of gross mass lemon is added
Lemon acid tests D50=0.45 μm of mixed powder after grinding 5h, by material after grinding in a nitrogen atmosphere with the heating of 10 DEG C/min
Rate heats up, and sintered lithium iron phosphate positive material is obtained within constant temperature calcining 7 hours in 850 DEG C, by sintered phosphoric acid
Iron lithium is crushed, and D50=1.3 μm of Control granularity, obtains compacted density 2.52g/cm3Powdered composite lithium iron phosphate anode material
Material.
Embodiment 5
By lithium hydroxide, lithium carbonate, ferrous oxalate, ferric phosphate, phosphoric acid hydrogen ammonia according to elemental lithium, ferro element and P elements
Molar ratio be that 1.03:1.02:0.98 is mixed, and according to 15% addition LiNi of gross mass0.5Co0.2Mn0.3O2, after
Dextrose and saccharose (mixture quality ratio is 1:1) is added according to the 15% of gross mass, tests mixed powder D50=after grinding 6h
0.32 μm, material after grinding is heated up in a nitrogen atmosphere with the rate of heat addition of 10 DEG C/min, in 750 DEG C of constant temperature calcinings 10
Hour obtains sintered lithium iron phosphate positive material, sintered LiFePO4 is crushed, Control granularity D50=1.3 μ
M obtains compacted density 2.49g/cm3Powdered composite lithium iron phosphate cathode material.
Comparative example 1
Lithium carbonate, ferric phosphate are mixed according to molar ratio 1.05:1, and according to lithium carbonate and phosphoric acid weight of iron
15% is added sucrose, D50=0.7 μm of mixed powder is tested after grinding 3h, by material after grinding in a nitrogen atmosphere with 2 DEG C/min
The rate of heat addition heat up, sintered lithium iron phosphate positive material is obtained within constant temperature calcining 6 hours in 750 DEG C, after sintering
LiFePO4 crushed, D50=1.5 μm of Control granularity, obtain compacted density 2.28g/cm3Powdered composite lithium iron phosphate
Positive electrode.
Performance test
(1) preparation of battery
The preparation of anode
The compound LiFePO of positive active material as made from embodiment 1-3 and comparative example 1 by 93 grams respectively4, 3 grams of binders
Kynoar (PVDF) and 4 grams of conductive agent acetylene blacks are added in 100 grams of N-Methyl pyrrolidones, then in de-airing mixer
Middle stirring forms uniform anode sizing agent.The anode sizing agent is uniformly coated to a thickness of the two sides of 16 microns of aluminium foil, so
Afterwards drying, roll-in (and the maximum of test material can use compacted density) at 120 DEG C, cut and be made having a size of 540 × 43.5 millimeters
Anode, wherein contain about 6 grams of compound LiFePO of active constituent4。
The preparation of cathode
95 grams of negative electrode active ingredient natural graphites, 1.2 grams of CMC, 2 grams of conductive agent carbon blacks are added to 120 grams of deionized waters
In, then stirring is formed uniformly in de-airing mixer, is eventually adding 1.8 grams of SBR and formed after mixing slowly 30 minutes
Even negative electrode slurry.The negative electrode slurry is uniformly coated to then dry at 90 DEG C with a thickness of the two sides of 8 microns of copper foil
Dry, roll-in cuts the cathode having a size of 500 × 44 millimeters is made, wherein containing about 3.5 grams of active constituent natural graphites.
The assembly of battery
Above-mentioned positive and negative electrode and polypropylene screen are wound into the pole piece of a square lithium ion battery respectively, then will
LiPF6Nonaqueous electrolytic solution is formed by the in the mixed solvent that the concentration of 1 mol/L is dissolved in EC/EMC/DEC=1:1:1, by the electricity
Liquid is solved so that in the amount injection battery aluminum shell of 3.2g/Ah, lithium ion secondary battery is respectively prepared in sealing.
(2) battery performance test
Lithium ion secondary battery obtained above is individually placed in test cabinet, is first carried out in 25 degree of insulating boxs with 0.2C
Constant-current constant-voltage charging, charging upper limit 3.65V；It shelves after twenty minutes, 2.0V is discharged to from 3.65V with the electric current of 0.2C, record
The discharge capacity for the first time of battery, and the specific discharge capacity of battery is calculated according to the following equation；
Specific discharge capacity=battery discharge capacity (milliampere hour)/positive electrode weight (gram) for the first time
Lithium ion secondary battery obtained above is individually placed in test cabinet in 25 degree of insulating boxs to carry out charge and discharge with 1C
Electrical testing, voltage range 2.0V~3.65V record the circulating cycle when circulation volume is lower than 80% than the average value of first three weeks capacity
Number.
1 finished battery performance of table
By the test result of experimental example it is found that compared with the prior art, the purer phosphorus of composite lithium iron phosphate material of the invention
Sour iron lithium material capacity improves 2.8~6.4%, and limit percent consolidation improves 6.5~10.5%, and circulation cycle is not substantially reduced,
It is high using the lithium ion battery energy density of composite lithium iron phosphate of the invention, have extended cycle life, security performance it is excellent.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Within mind and principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (10)
1. a kind of preparation method of composite lithium iron phosphate material, it is characterised in that: include the following steps,
(1) lithium source, source of iron, phosphorus source are mixed, and after mixing, the molar ratio of elemental lithium, ferro element and P elements is
0.95~1.05:0.95~1.05:0.95~1.05, and accessory positive material is added in mixed process, obtain mixed material
A；
(2) material A is ground, carbon source is added during the grinding process, control grinding partial size D50 is 0.05~1.0 μm, is obtained
Material B；
(3) material B is heated up under an inert atmosphere with the rate of heat addition of 2~20 DEG C/min, is roasted in 700~900 DEG C of constant temperature
It burns 4~12 hours and obtains sintered composite lithium iron phosphate cathode material C；
(4) sintered positive electrode C will be obtained to crush, obtain final composite lithium iron phosphate material.
2. the preparation method of composite lithium iron phosphate material according to claim 1, it is characterised in that: in the step 1),
Accessory positive material is one or more of cobalt acid lithium, LiMn2O4, lithium nickelate or nickle cobalt lithium manganate；Accessory positive material
Quality account for lithium source, source of iron and phosphorus source material gross mass 5%~25%.
3. the preparation method of composite lithium iron phosphate material according to claim 1, it is characterised in that: in the step (1),
Lithium source is one or more of lithium hydroxide, lithium dihydrogen phosphate, lithium nitrate, lithium oxalate, lithium acetate, lithium carbonate；It is described
Source of iron is one or more of ferric phosphate, ferrous oxalate, ferric acetate, di-iron trioxide, ferric nitrate；Phosphorus source is phosphorus
One or more of acid, ammonium dihydrogen phosphate, diammonium hydrogen phosphate, ammonium phosphate, ferric phosphate, lithium dihydrogen phosphate.
4. the preparation method of composite lithium iron phosphate material according to claim 1, it is characterised in that: in the step (2),
Carbon source be one or both of glucose, sucrose, citric acid, polyethylene glycol, polyvinyl alcohol, carbon nanotube, conductive black with
On；The carbon source is added in material A according to the 1%~20% of material A mass ratio.
5. the preparation method of composite lithium iron phosphate material according to claim 1, it is characterised in that: in the step (2),
The method of the grinding is dry grinding and/or air-flow crushing.
6. the preparation method of composite lithium iron phosphate material according to claim 1, it is characterised in that: in the step (3),
Inert gas is one or more of nitrogen, argon gas, carbon dioxide.
7. the preparation method of composite lithium iron phosphate material according to claim 1, it is characterised in that: in the step (4),
Positive electrode C is crushed, and smashed partial size D50 is 0.5~3.0 μm.
8. the composite lithium iron phosphate that the preparation method of composite lithium iron phosphate material as described in any one of claims 1 to 7 obtains
Material.
9. a kind of anode, it is characterised in that: the compound phosphoric acid obtained including the described in any item preparation methods of claim 1~7
Iron lithium material.
10. a kind of lithium ion battery, it is characterised in that: answered including what the described in any item preparation methods of claim 1~7 obtained
Close LiFePO 4 material.
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Cited By (4)
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| CN109867268A (en) * | 2019-01-31 | 2019-06-11 | 鲍君杰 | A kind of preparation method of high-pressure solid high capacity LiFePO4 |
| CN111740101A (en) * | 2020-06-17 | 2020-10-02 | 东莞东阳光科研发有限公司 | Lithium iron phosphate material and preparation method thereof |
| CN115557482A (en) * | 2021-07-01 | 2023-01-03 | 惠州比亚迪电池有限公司 | Preparation method of lithium iron phosphate cathode material and lithium ion battery |
| WO2023174130A1 (en) * | 2022-03-14 | 2023-09-21 | 湖北万润新能源科技股份有限公司 | Iron-based composite phosphate positive electrode material and preparation method therefor, positive plate and sodium ion battery |
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| CN111740101A (en) * | 2020-06-17 | 2020-10-02 | 东莞东阳光科研发有限公司 | Lithium iron phosphate material and preparation method thereof |
| CN111740101B (en) * | 2020-06-17 | 2022-07-08 | 东莞东阳光科研发有限公司 | Lithium iron phosphate material and preparation method thereof |
| CN115557482A (en) * | 2021-07-01 | 2023-01-03 | 惠州比亚迪电池有限公司 | Preparation method of lithium iron phosphate cathode material and lithium ion battery |
| WO2023174130A1 (en) * | 2022-03-14 | 2023-09-21 | 湖北万润新能源科技股份有限公司 | Iron-based composite phosphate positive electrode material and preparation method therefor, positive plate and sodium ion battery |
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