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CN101916848A - LiFePO4 coating LiMn2O4 composite electrode material and preparation method thereof - Google Patents

LiFePO4 coating LiMn2O4 composite electrode material and preparation method thereof Download PDF

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CN101916848A
CN101916848A CN2010102488543A CN201010248854A CN101916848A CN 101916848 A CN101916848 A CN 101916848A CN 2010102488543 A CN2010102488543 A CN 2010102488543A CN 201010248854 A CN201010248854 A CN 201010248854A CN 101916848 A CN101916848 A CN 101916848A
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lifepo
limn
electrode material
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lifepo4
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王宏栋
方振华
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SHANDONG JIULI ELECTRONIC TECHNOLOGY Co Ltd
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SHANDONG JIULI ELECTRONIC TECHNOLOGY Co Ltd
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Abstract

The invention relates to a LiFePO4 coating LiMn2O4 composite electrode material and a preparation method thereof, belonging to the technical field of lithium ion battery electrode materials and preparation thereof. In the invention, LiMn2O4 is used as a base body, the nanometer level of the LiFePO4 is coated on the surface thereof, and the amount of the LiFePO4 accounts for 5-25% of LiFePO4 and LiMn2O4 by weight percent. Combined with different advantages of LiMn2O4 materials and LiFePO4 materials, the LiMn2O4 is coated by the LiFePO4 so that the LiMn2O4 electrode material of the inner layer is separated from electrolytes, the reaction of the electrode and an electrolyte solution can be inhibited, the manganic solution loss is reduced, and the electrochemistry performance and the high temperature performance thereof are enhanced. Furthermore, because a LiFePO4 discharging platform is lower than the LiMn2O4, a ferromanganese iron battery can still discharge stably at the lower voltage and is not damaged, thereby improving the service performance of the battery and prolonging the service life of the battery. The invention has the advantages of simple preparation process, favorable coating effect, convenient operation and easy implementation of mass industrial production; and the obtained composite electrode material has excellent electrochemistry temperature performance and anti-overcharge performance.

Description

A kind of LiFePO 4 coating LiMn 2 O 4 composite electrode material and preparation method thereof
Technical field
The invention belongs to lithium ion battery electrode material and preparing technical field thereof, a kind of LiFePO4 (LiFePO is provided especially 4) coating LiMn 2 O (LiMn 2O 4) combination electrode material and preparation method thereof.
Background technology
Along with the fast development of lithium-ion-power cell, more and more higher to the requirement of battery material.Current business-like power battery anode material is mainly LiMn 2O 4With LiFePO 4
Lithium manganate having spinel structure (LiMn 2O 4) as anode material for lithium-ion batteries, have the operating voltage height, security performance is good, cheap and the advantage such as nontoxic pollution-free, is considered to one of the most promising anode material for lithium-ion batteries.But this material capacity attenuation in the charge and discharge cycles process is very fast, and especially more than 55 ℃ the time, its circulation and storge quality sharply worsen, and this has limited development and the application of this material.
LiFePO4 (LiFePO 4)As anode material for lithium-ion batteries, have advantages such as good cycle, security performance are good, nontoxic pollution-free, be considered to one of the most promising anode material for lithium-ion batteries.But its operating voltage is than LiMn 2O 4Low, preparation cost is higher, and discharge capacity is low at low temperatures, has limited equally the application and development of this material.
Summary of the invention
The objective of the invention is in conjunction with LiMn 2O 4With LiFePO 4The advantage of material provides a kind of LiFePO 4Coat LiMn 2O 4Combination electrode material and preparation method thereof.
For achieving the above object, the technical solution used in the present invention is:
A kind of LiFePO 4 coating LiMn 2 O 4 composite electrode material comprises: LiFePO4 (LiFePO 4) and lithium manganate having spinel structure (LiMn 2O 4), it is characterized in that: LiFePO 4Evenly be coated on spinel-type LiMn 2O 4The surface; LiFePO 4Quality account for LiFePO 4And LiMn 2O 4The percentage of summation quality is 5%～25%.
According to described LiFePO 4 coating LiMn 2 O 4 composite electrode material, it is characterized in that: described LiFePO 4Be nanoscale.
According to described LiFePO 4 coating LiMn 2 O 4 composite electrode material, it is characterized in that: described LiFePO 4Quality account for LiFePO 4And LiMn 2O 4The percentage of summation quality is 15%.
According to described LiFePO 4 coating LiMn 2 O 4 composite electrode material, it is characterized in that: described LiFePO 4Quality account for LiFePO 4And LiMn 2O 4The percentage of summation quality is 20%.
According to described LiFePO 4 coating LiMn 2 O 4 composite electrode material, it is characterized in that: described LiFePO 4Quality account for LiFePO 4And LiMn 2O 4The percentage of summation quality is 25%.
A kind of method for preparing described LiFePO 4 coating LiMn 2 O 4 composite electrode material is characterized in that may further comprise the steps:
A, with nanoscale LiFePO 4Join in the glucose solution, be made into LiFePO 4Concentration is the suspension of 0.01～0.2mol/L, is 20～60 ℃ in temperature, and power is to stir 20～60 minutes under the condition of 1000～2000W/L; Then with LiFePO 4 Measure 4～9 times LiMn 2O 4Add in the suspension, mechanical agitation 60～120 minutes is filtered the suspension that obtains, and filter cake grinds at 100～150 ℃ of lower dry 6～12h.
B, steps A gained material is warming up to 600～1800 ℃ with 2～10 ℃/min speed, and constant temperature 5～15h, naturally cool to then room temperature, obtain LiFePO 4The LiMn that coats 2O 4Combination electrode material.
According to the described method for preparing LiFePO 4 coating LiMn 2 O 4 composite electrode material, it is characterized in that: take by weighing 5g with nanoscale LiFePO 4Joining in the 100mL D/W, be made into the suspension that LiFePO4 concentration is 0.03mol/L, is 20 ℃ in temperature, and power is to stir 30 minutes under the condition of 1000W/L; Then with 95g LiMn 2O 4Add in the suspension, mechanical agitation 90 minutes is filtered the suspension that obtains, and filter cake grinds at 120 ℃ of lower dry 12h; The powder body material that grinding is obtained is warming up to 600 ℃ with 10 ℃/min speed, and constant temperature 10h, naturally cools to then room temperature, obtains LiFePO 4The LiMn that coats 2O 4Combination electrode material.
According to the described method for preparing LiFePO 4 coating LiMn 2 O 4 composite electrode material, it is characterized in that: take by weighing 10g with nanoscale LiFePO 4Join in the 100mL D/W, be made into LiFePO 4Concentration is the suspension of 0.06mol/L, is 30 ℃ in temperature, and power is to stir 45 minutes under the condition of 1200W/L; Then with 90g LiMn 2O 4Add in the suspension, mechanical agitation 90 minutes is filtered the suspension that obtains, and filter cake grinds at 120 ℃ of lower dry 12h; The powder body material that grinding is obtained is warming up to 800 ℃ with 10 ℃/min speed, and constant temperature 10h, naturally cools to then room temperature, obtains LiFePO 4The LiMn that coats 2O 4Combination electrode material.
According to the described method for preparing LiFePO 4 coating LiMn 2 O 4 composite electrode material, it is characterized in that: take by weighing 15g with nanoscale LiFePO 4Join in the 100mL D/W, be made into LiFePO 4Concentration is the suspension of 0.09mol/L, is 40 ℃ in temperature, and power is to stir 45 minutes under the condition of 1400W/L; Then with 85g LiMn 2O 4Add in the suspension, mechanical agitation 90 minutes is filtered the suspension that obtains, and filter cake grinds at 120 ℃ of lower dry 12h; The powder body material that grinding is obtained is warming up to 1000 ℃ with 10 ℃/min speed, and constant temperature 10h, naturally cools to then room temperature, obtains LiFePO 4The LiMn that coats 2O 4Combination electrode material.
According to the described method for preparing LiFePO 4 coating LiMn 2 O 4 composite electrode material, it is characterized in that: take by weighing 25g with nanoscale LiFePO 4Join in the 100mL D/W, be made into LiFePO 4Concentration is the suspension of 0.16mol/L, is 60 ℃ in temperature, and power is to stir 60 minutes under the condition of 1800W/L; Then with 75g LiMn 2O 4Add in the suspension, mechanical agitation 90 minutes is filtered the suspension that obtains, and filter cake grinds at 120 ℃ of lower dry 12h; The powder body material that grinding is obtained is warming up to 1400 ℃ with 10 ℃/min speed, and constant temperature 10h, naturally cools to then room temperature, obtains LiFePO 4The LiMn that coats 2O 4Combination electrode material.
Beneficial effect of the present invention: preparation LiFePO provided by the invention 4Coat LiMn 2O 4Combination electrode material and preparation method thereof technology is simple, with low cost, and clad is even, suitability for scale production.Adopt LiFePO 4To LiMn 2O 4Coat modification, so that the LiMn of internal layer 2O 4Electrode material and electrolyte separate, and can suppress the reaction of electrode and electrolyte, reduce the molten damage of manganese, improve its chemical property and high-temperature behavior.In addition, because LiFePO 4Discharge platform is than LiMn 2O 4Low, so, LiFePO 4Coat LiMn 2O 4Combination electrode material still can steadily discharge under lower voltage, and can not cause damage to material, has improved the serviceability of battery, has prolonged the service life of battery.
Description of drawings
Fig. 1 is anodal Experimental cell charging and discharging curve for the LiMn2O4 composite that coats take LiFePO4.Its charging/discharging voltage scope is 3.0～4.2V; Abscissa is the time of discharging and recharging, and unit is minute (min); Ordinate is a voltage, and unit is a volt (V).
Fig. 2 is that the LiMn2O4 material of uncoated processing is anodal Experimental cell charging and discharging curve.Its charging/discharging voltage scope is 3.0～4.2V; Abscissa is the time of discharging and recharging, and unit is minute (min); Ordinate is a voltage, and unit is a volt (V).
Fig. 3 is the cycle performance curve of the Experimental cell of positive pole for the LiMn2O4 composite material that coats with LiFePO4.Its charging/discharging voltage scope is 3.0～4.2V; Abscissa is a cycle-index, and unit is inferior; Ordinate is a capability retention.
Fig. 4 is the cycle performance curve of the LiMn2O4 material of uncoated processing.Its charging/discharging voltage scope is 3.0～4.2V; Abscissa is a cycle-index, and unit is inferior; Ordinate is a capability retention.
Embodiment
The invention will be further described below in conjunction with specific embodiment:
A kind of LiFePO of the present invention 4Coat LiMn 2O 4Positive electrode and preparation method thereof belongs to lithium ion battery electrode material and preparing technical field thereof.With LiMn 2O 4Be matrix, at its surperficial clad nano level LiFePO 4, LiFePO 4Amount account for LiFePO 4+ LiMn 2O 4Mass percent 5%～25%.The present invention is in conjunction with LiMn 2O 4Material and LiFePO 4The advantage that material is different is to LiMn 2O 4Carry out LiFePO 4Coat, so that the LiMn of internal layer 2O 4Electrode material and electrolyte separate, and can suppress the reaction of electrode and electrolyte, reduce the molten damage of manganese, improve its chemical property and high-temperature behavior.In addition, because LiFePO 4Discharge platform is than LiMn 2O 4Low, the ferromanganese battery still can steadily discharge under lower voltage, and can not cause damage to battery, has improved the serviceability of battery, has prolonged the service life of battery.Preparation technology of the present invention is simple, and covered effect is good, and the combination electrode material that is obtained has good electrochemistry temperature and anti-over-charging electrical property.Easy to operate, be easy to realize large-scale industrial production.
Preparation method of the present invention is with business-like nanoscale LiFePO 4And LiMn 2O 4Be raw material, earlier with LiFePO 4Join in the glucose solution, mechanical agitation adds LiMn again after a period of time 2O 4Stir a period of time, after filtration, obtain LiFePO after the washing, heat treatment 4Coat LiMn 2O 4Combination electrode material, the concrete technology step is as follows:
A, with nanoscale LiFePO 4Join in the D/W, be made into LiFePO 4Concentration is the suspension of 0.01～0.2mol/L, is 20～60 ℃ in temperature, and power is to stir 20～60 minutes under the condition of 1000～2000W/L; Then with LiFePO 4 Measure 4～9 times LiMn 2O 4Add in the suspension, mechanical agitation 60～120 minutes is filtered the suspension that obtains, and filter cake grinds at 100～150 ℃ of lower dry 6～12h.
B, steps A gained material is warming up to 600～1800 ℃ with 2～10 ℃/min speed, and constant temperature 5～15h, naturally cool to then room temperature, obtain LiFePO 4The LiMn that coats 2O 4Combination electrode material.
The synthetic LiFePO of the inventive method will be adopted 4Coat LiMn 2O 4Composite positive pole mixes by the mass ratio by 91: 5: 4 with super carbon black conductive agent and Kynoar (PVDF) binding agent, and the thickness of compressing tablet to 100～150 μ m, in 115 ℃ of vacuum (＜0.085MPa) dry 12h, with Delanium as negative pole, adopt the Celgard barrier film, the LiPF of 1mol/L 6+ EC+DMC+DEC is electrolyte, is made into 165870A 4Ah battery, adopts road China cell tester to carry out electrochemical property test.LiFePO by embodiment of the invention acquisition 4Coat LiMn 2O 4The chemical composition of sample, electro-chemical test condition, the reversible specific discharge capacity when reversible specific discharge capacity, circulation 50 times, 100 times, 200 times is shown in Table 1 first.Also listed in the table 1 not through coating the LiMn that processes 2O 4The Electrochemical results of sample.
Embodiment 1:
Take by weighing 5g with nanoscale LiFePO 4Joining in the 100mL D/W, be made into the suspension that LiFePO4 concentration is 0.03mol/L, is 20 ℃ in temperature, and power is to stir 30 minutes under the condition of 1000W/L; Then with 95g LiMn 2O 4Add in the suspension, mechanical agitation 90 minutes is filtered the suspension that obtains, and filter cake grinds at 120 ℃ of lower dry 12h.
The powder body material that grinding is obtained is warming up to 600 ℃ with 10 ℃/min speed, and constant temperature 10h, naturally cools to then room temperature, obtains LiFePO 4The LiMn that coats 2O 4Combination electrode material.Electrochemical results sees Table 1.
Embodiment 2:
Take by weighing 10g with nanoscale LiFePO 4Join in the 100mL D/W, be made into LiFePO 4Concentration is the suspension of 0.06mol/L, is 30 ℃ in temperature, and power is to stir 45 minutes under the condition of 1200W/L; Then with 90g LiMn 2O 4Add in the suspension, mechanical agitation 90 minutes is filtered the suspension that obtains, and filter cake grinds at 120 ℃ of lower dry 12h.The powder body material that grinding is obtained is warming up to 800 ℃ with 10 ℃/min speed, and constant temperature 10h, naturally cools to then room temperature, obtains LiFePO 4The LiMn that coats 2O 4Combination electrode material.Electrochemical results sees Table 1.
Embodiment 3:
Take by weighing 15g with nanoscale LiFePO 4Join in the 100mL D/W, be made into LiFePO 4Concentration is the suspension of 0.09mol/L, is 40 ℃ in temperature, and power is to stir 45 minutes under the condition of 1400W/L; Then with 85g LiMn 2O 4Add in the suspension, mechanical agitation 90 minutes is filtered the suspension that obtains, and filter cake grinds at 120 ℃ of lower dry 12h.The powder body material that grinding is obtained is warming up to 1000 ℃ with 10 ℃/min speed, and constant temperature 10h, naturally cools to then room temperature, obtains LiFePO 4The LiMn that coats 2O 4Combination electrode material.Electrochemical results sees Table 1.
Embodiment 4:
Take by weighing 20g with nanoscale LiFePO 4Join in the 100mL D/W, be made into LiFePO 4Concentration is the suspension of 0.13mol/L, is 50 ℃ in temperature, and power is to stir 50 minutes under the condition of 1600W/L; Then with 80g LiMn 2O 4Add in the suspension, mechanical agitation 90 minutes is filtered the suspension that obtains, and filter cake grinds at 120 ℃ of lower dry 12h.
The powder body material that grinding is obtained is warming up to 1200 ℃ with 10 ℃/min speed, and constant temperature 10h, naturally cools to then room temperature, obtains LiFePO 4The LiMn that coats 2O 4Combination electrode material.Electrochemical results sees Table 1.
Embodiment 5:
Take by weighing 25g with nanoscale LiFePO 4Join in the 100mL D/W, be made into LiFePO 4Concentration is the suspension of 0.16mol/L, is 60 ℃ in temperature, and power is to stir 60 minutes under the condition of 1800W/L; Then with 75g LiMn 2O 4Add in the suspension, mechanical agitation 90 minutes is filtered the suspension that obtains, and filter cake grinds at 120 ℃ of lower dry 12h.
The powder body material that grinding is obtained is warming up to 1400 ℃ with 10 ℃/min speed, and constant temperature 10h, naturally cools to then room temperature, obtains LiFePO 4The LiMn that coats 2O 4Combination electrode material.Electrochemical results sees Table 1.
The composition of table 1 electrode material and electrochemistry cycle performance
Embodiment recited above is described preferred implementation of the present invention; be not that design of the present invention and protection range are limited; under the prerequisite that does not break away from design concept of the present invention; common engineers and technicians make technical scheme of the present invention in this area various modification and improvement all should fall into protection scope of the present invention.

Claims (10)

1. a LiFePO 4 coating LiMn 2 O 4 composite electrode material comprises: LiFePO4 (LiFePO 4) and lithium manganate having spinel structure (LiMn 2O 4), it is characterized in that: LiFePO 4Evenly be coated on spinel-type LiMn 2O 4The surface; LiFePO 4Quality account for LiFePO 4And LiMn 2O 4The percentage of summation quality is 5%～25%.
2. LiFePO 4 coating LiMn 2 O 4 composite electrode material according to claim 1 is characterized in that: described LiFePO 4Be nanoscale.
3. LiFePO 4 coating LiMn 2 O 4 composite electrode material according to claim 1 is characterized in that: described LiFePO 4Quality account for LiFePO 4And LiMn 2O 4The percentage of summation quality is 15%.
4. LiFePO 4 coating LiMn 2 O 4 composite electrode material according to claim 1 is characterized in that: described LiFePO 4Quality account for LiFePO 4And LiMn 2O 4The percentage of summation quality is 20%.
5. LiFePO 4 coating LiMn 2 O 4 composite electrode material according to claim 1 is characterized in that: described LiFePO 4Quality account for LiFePO 4And LiMn 2O 4The percentage of summation quality is 25%.
6. method for preparing the described LiFePO 4 coating LiMn 2 O 4 composite electrode material of claim 1 is characterized in that may further comprise the steps:
A, with nanoscale LiFePO 4Join in the glucose solution, be made into LiFePO 4Concentration is the suspension of 0.01～0.2mol/L, is 20～60 ℃ in temperature, and power is to stir 20～60 minutes under the condition of 1000～2000W/L; Then with LiFePO 4Measure 4～9 times LiMn 2O 4Add in the suspension, mechanical agitation 60～120 minutes is filtered the suspension that obtains, and filter cake grinds at 100～150 ℃ of lower dry 6～12h.
B, steps A gained material is warming up to 600～1800 ℃ with 2～10 ℃/min speed, and constant temperature 5～15h, naturally cool to then room temperature, obtain LiFePO 4The LiMn that coats 2O 4Combination electrode material.
7. the method for preparing LiFePO 4 coating LiMn 2 O 4 composite electrode material according to claim 6 is characterized in that: take by weighing 5g with nanoscale LiFePO 4Joining in the 100mL D/W, be made into the suspension that LiFePO4 concentration is 0.03mol/L, is 20 ℃ in temperature, and power is to stir 30 minutes under the condition of 1000W/L; Then with 95g LiMn 2O 4Add in the suspension, mechanical agitation 90 minutes is filtered the suspension that obtains, and filter cake grinds at 120 ℃ of lower dry 12h; The powder body material that grinding is obtained is warming up to 600 ℃ with 10 ℃/min speed, and constant temperature 10h, naturally cools to then room temperature, obtains LiFePO 4The LiMn that coats 2O 4Combination electrode material.
8. the method for preparing LiFePO 4 coating LiMn 2 O 4 composite electrode material according to claim 6 is characterized in that: take by weighing 10g with nanoscale LiFePO 4Join in the 100mL D/W, be made into LiFePO 4Concentration is the suspension of 0.06mol/L, is 30 ℃ in temperature, and power is to stir 45 minutes under the condition of 1200W/L; Then with 90g LiMn 2O 4Add in the suspension, mechanical agitation 90 minutes is filtered the suspension that obtains, and filter cake grinds at 120 ℃ of lower dry 12h; The powder body material that grinding is obtained is warming up to 800 ℃ with 10 ℃/min speed, and constant temperature 10h, naturally cools to then room temperature, obtains LiFePO 4The LiMn that coats 2O 4Combination electrode material.
9. the method for preparing LiFePO 4 coating LiMn 2 O 4 composite electrode material according to claim 6 is characterized in that: take by weighing 15g with nanoscale LiFePO 4Join in the 100mL D/W, be made into LiFePO 4Concentration is the suspension of 0.09mol/L, is 40 ℃ in temperature, and power is to stir 45 minutes under the condition of 1400W/L; Then with 85g LiMn 2O 4Add in the suspension, mechanical agitation 90 minutes is filtered the suspension that obtains, and filter cake grinds at 120 ℃ of lower dry 12h; The powder body material that grinding is obtained is warming up to 1000 ℃ with 10 ℃/min speed, and constant temperature 10h, naturally cools to then room temperature, obtains LiFePO 4The LiMn that coats 2O 4Combination electrode material.
10. the method for preparing LiFePO 4 coating LiMn 2 O 4 composite electrode material according to claim 6 is characterized in that: take by weighing 25g with nanoscale LiFePO 4Join in the 100mL D/W, be made into LiFePO 4Concentration is the suspension of 0.16mol/L, is 60 ℃ in temperature, and power is to stir 60 minutes under the condition of 1800W/L; Then with 75g LiMn 2O 4Add in the suspension, mechanical agitation 90 minutes is filtered the suspension that obtains, and filter cake grinds at 120 ℃ of lower dry 12h; The powder body material that grinding is obtained is warming up to 1400 ℃ with 10 ℃/min speed, and constant temperature 10h, naturally cools to then room temperature, obtains LiFePO 4The LiMn that coats 2O 4Combination electrode material.
CN2010102488543A 2010-08-06 2010-08-06 LiFePO4 coating LiMn2O4 composite electrode material and preparation method thereof Pending CN101916848A (en)

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CN103078102A (en) * 2013-01-05 2013-05-01 宁波大学 A kind of defect structure LiFePO4 surface modification layer-spinel composite lithium-rich positive electrode material and preparation method
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CN103078102A (en) * 2013-01-05 2013-05-01 宁波大学 A kind of defect structure LiFePO4 surface modification layer-spinel composite lithium-rich positive electrode material and preparation method
CN103117385A (en) * 2013-01-05 2013-05-22 宁波大学 A kind of defect structure LiFePO4 surface modified lithium-rich layer-layer positive electrode material and preparation method
CN103117385B (en) * 2013-01-05 2016-05-18 宁波大学 A kind of defect sturcture LiFePO4The rich lithium layer-layer positive electrode of surface modification and preparation method
CN103474625A (en) * 2013-08-05 2013-12-25 合肥国轩高科动力能源股份公司 Coating method for core-shell novel positive electrode material for lithium ion battery
CN103474625B (en) * 2013-08-05 2016-01-13 合肥国轩高科动力能源有限公司 Novel lithium ion battery anode material coating method with core-shell structure
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CN106935808B (en) * 2015-12-31 2020-02-07 比亚迪股份有限公司 Positive active material, preparation method thereof, battery slurry, positive electrode and lithium battery
CN110690426A (en) * 2019-10-12 2020-01-14 洛阳超特电源科技有限公司 Composite lithium iron phosphate material for low-temperature rate discharge, positive plate and lithium ion battery
CN111416111A (en) * 2020-04-17 2020-07-14 中国科学院物理研究所 A kind of modified lithium manganate material and preparation method thereof and lithium battery
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Application publication date: 20101215