CN101901892A - Lithium-ion secondary battery anode and lithium-ion secondary battery - Google Patents
Lithium-ion secondary battery anode and lithium-ion secondary battery Download PDFInfo
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- CN101901892A CN101901892A CN2009101420625A CN200910142062A CN101901892A CN 101901892 A CN101901892 A CN 101901892A CN 2009101420625 A CN2009101420625 A CN 2009101420625A CN 200910142062 A CN200910142062 A CN 200910142062A CN 101901892 A CN101901892 A CN 101901892A
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Abstract
The invention belongs to the lithium-ion secondary battery field, and provides a lithium-ion secondary battery anode. The lithium-ion secondary battery anode comprises an anode current collector and an anode material coated and/or filled on the anode current collector; the anode material comprises at least two anode active substances with different crystal structures, and the following two anode active substances are necessary: the first anode active substance is LiFeMxPO4 with a peridot structure, wherein M is selected from at least one of Co, Ni, Mn, Al, Mg, Ti, V, Zn, B, Nb, Cu, Ca, Mo, W and Zr, and x is more than or equal to 0 and less than or equal to 1; the second anode active substance is LiNi1-(y+z)CoyMzO2 with a spinelle structure, wherein y is more than or equal to 0.1 and less than or equal to 0.2, and z is more than or equal to 0 and less than or equal to 0.1; and the first anode active substance accounts for 10 to 70 percent of the total mass of the first active substance and the second active substance. The electrolyte of the anode has good wetting property, so the lithium-ion secondary battery of the anode has good normal-temperature circulating performance.
Description
Technical field
The present invention relates to a kind of lithium ion secondary battery positive electrode, and the lithium rechargeable battery that uses this positive pole.
Background technology
At present, the trend that lithium ion secondary battery positive electrode is made is to improve the dressing density of positive active material as far as possible, thereby improves the capacity of battery.A problem that may cause thus is that electrolyte can not well soak into positive plate owing to dressing on the positive plate is too closely knit, and the capacity performance of battery is not come out, and cycle performance also descends to some extent.But if reduce the dressing amount, reduce dressing density and increase the wettability of electrolyte, then because the reduction of dressing amount on the pole piece (being that positive active material content reduces on the pole piece) can make battery capacity also decrease to pole piece.
Summary of the invention
In order to solve the technical problem that electrolyte can not well soak into the big lithium ion secondary battery positive electrode of dressing density in the prior art, the present invention at first provides a kind of lithium ion secondary battery positive electrode, comprise plus plate current-collecting body and coating and/or be filled in positive electrode on the plus plate current-collecting body, described positive electrode comprises at least 2 kinds of positive active materials that crystalline texture is different, and 2 kinds of positive active materials as described below are essential:
First positive active material is the LiFeM with olivine structural
xPO
4, wherein, M is selected from least a among Co, Ni, Mn, Al, Mg, Ti, V, Zn, B, Nb, Cu, Ca, Mo, W, the Zr, 0≤x≤1;
Second positive active material comprises the LiNi with spinel structure
1-(y+z)Co
yM
zO
2, wherein, 0.1≤y≤0.2,0≤z≤0.1;
And the percentage that the quality of described first positive active material accounts for first active material and the second active material gross mass is 10～70wt%.
Electrolyte can not well soak into the big lithium ion secondary battery positive electrode of dressing density in the prior art in order to solve, thereby influence the technical problem of cycle performance of battery, the present invention and then a kind of lithium rechargeable battery is provided, comprise battery container, electrode group and electrolyte, electrode group and electrolyte are sealed in the battery container, the electrode group comprises reels or stacked positive pole, barrier film and negative pole successively, described just very according to lithium ion secondary battery positive electrode of the present invention.
Beneficial effect of the present invention:
The present invention has adopted following technical scheme: the positive electrode on the lithium ion secondary battery positive electrode collector comprises at least 2 kinds of positive active materials that crystalline texture is different, and 2 kinds of positive active materials as described below are essential:
First positive active material is the LiFeM with olivine structural
xPO
4, wherein, M is selected from least a among Co, Ni, Mn, Al, Mg, Ti, V, Zn, B, Nb, Cu, Ca, Mo, W, the Zr, 0≤x≤1;
Second positive active material comprises the LiNi with spinel structure
1-(y+z)Co
yM
zO
2, wherein, 0.1≤y≤0.2,0≤z≤0.1;
And the percentage that the quality of described first positive active material accounts for first active material and the second active material gross mass is 10～70wt%.
Adopt technique scheme to solve for the big lithium-ion secondary battery positive plate of dressing density, be used alone the positive active material of crystalline texture, though or the positive active material of at least 2 kinds of different crystalline textures of use, but do not comprise 2 kinds of positive active materials of the present invention, though or comprise 2 kinds of positive active materials of the present invention, but when the content of first positive active material does not satisfy above-mentioned scope, when the dressing density on the positive plate is big, electrolyte is bad to the wettability of positive plate, thereby influence the technical problem of battery performance, make battery at normal temperatures the capability retention after 290 charge and discharge cycles compared with prior art improved 5% at least more than 85%.
Description of drawings
Fig. 1 electrolyte is to the wettability test result of the positive plate of the embodiment of the invention and Comparative Examples
Discharge capacitance test result under the battery normal temperature of Fig. 2 embodiment of the invention and Comparative Examples
Embodiment
Describe the present invention below in detail.
The specific embodiment of the invention at first provides a kind of anode of secondary battery, comprise plus plate current-collecting body and coating and/or be filled in positive electrode on the plus plate current-collecting body, described positive electrode comprises at least 2 kinds of positive active materials that crystalline texture is different, and 2 kinds of positive active materials as described below are essential:
First positive active material is the LiFeM with olivine structural
xPO
4, wherein, M is selected from least a among Co, Ni, Mn, Al, Mg, Ti, V, Zn, B, Nb, Cu, Ca, Mo, W, the Zr, 0≤x≤1;
Second positive active material comprises the LiNi with spinel structure
1-(y+z)Co
yM
zO
2, wherein, 0.1≤y≤0.2,0≤z≤0.1;
And the percentage that the quality of described first positive active material accounts for first active material and the second active material gross mass is 10～70wt%.
The inventor finds: after the positive electrode that comprises above-mentioned first positive active material and second positive active material is coated on the positive plate, because the crystalline texture difference of two kinds of positive active materials, there is boundary after the mixing, electrolyte helps improving the wettability of electrolyte to positive plate the meeting enrichment of boundary place (being that concentration increases).Simultaneously, the percentage that the quality of first positive active material accounts for first active material and the second active material gross mass is that 10～70wt% can make the porosity on the positive plate increase, and then electrolyte is to the wettability raising of pole piece.Though if positive electrode comprises above-mentioned 2 kinds of positive active materials, the content of the two does not satisfy above-mentioned scope, and is then not obvious to the infiltrating improvement of the electrolyte of pole piece.
The first active material LiFeM
xPO
4Preferred LiFeMn
0.5PO
4, LiFeCoPO
4, LiFePO
4In at least a.
The preferred LiNi of second positive active material
0.8Co
0.15Al
0.05O
2, LiNi
0.8Co
0.15Mn
0.05O
2, LiNi
0.8Co
0.2O
2In at least a.At least a and first positive active material LiFeM in this 3 kind of second positive active material
xPO
4When being used in combination, the circulation volume conservation rate of battery is better under the normal temperature.
The average grain diameter of the positive active material of the specific embodiment of the invention does not have specific (special) requirements, can select according to state of the art.That is, select to use which kind of positive active material, the average grain diameter of its particle is selected in the average particle size range that this positive active material is used always with regard to corresponding.
The median particle diameter D of first positive active material
50 1Preferred satisfied 1 μ m≤D
50 1≤ 5 μ m.Use median particle diameter D
50 1Satisfy 1 μ m≤D
50 1Above-mentioned first positive active material of≤5 μ m, the circulation volume conservation rate of battery in the charge and discharge cycles process is better under the normal temperature.
The median particle diameter D of second positive active material
50 2Preferred satisfied 5 μ m≤D
50 2≤ 10 μ m.Use median particle diameter D
50 2Satisfy 5 μ m≤D
50 2Above-mentioned second positive active material of≤10 μ m, the circulation volume conservation rate of battery in the charge and discharge cycles process is better under the normal temperature.
A kind of lithium rechargeable battery, comprise battery container, electrode group and electrolyte, electrode group and electrolyte are sealed in the battery container, the electrode group comprises reels or stacked positive pole, barrier film and negative pole successively, described just very according to the described lithium ion secondary battery positive electrode of the specific embodiment of the invention.
The material of the battery container of lithium rechargeable battery, the prescription of electrolyte, anodal binding agent, negative material, barrier film and cell production process etc. all can be selected according to the state of the art.Wherein, the prescription of electrolyte is preferably: electrolytic salt comprises LiPF
6, its concentration is 0.5～1.5mol/L, solvent is ethylene carbonate (EC) and diethyl carbonate (DEC) by quality than ethylene carbonate: the mixed solvent that diethyl carbonate=1.5～2.5 are formed.
1. the preparation of positive plate
With LiFeMn
0.5PO
4, cobalt acid lithium (LiCoO
2), conductive agent acetylene black, binding agent Kynoar (PVDF), organic solvent N-dimethyl pyrrolidone (NMP) is according to mass ratio LiFeMn
0.5PO
4: LiCoO
2: acetylene black: PVDF: NMP=50: 50: 4: 1.5: 40 mixing and stirring, make anode sizing agent.Wherein, the first positive active material LiFeMn
0.5PO
4Median particle diameter D
50 1=4 μ m, the second positive active material LiCoO
2Median particle diameter D
50 2=8 μ m.The first positive active material LiFeMn
0.5PO
4Account for the first active material LiFeMn
0.5PO
4With the second active material LiCoO
2The 50wt% of gross mass.
Above-mentioned anode sizing agent is coated on coating machine on the aluminium foil of long 763mm, wide 55.5mm, thick 12 μ m, and 110 ℃ of oven dry, calendering are cut then, obtain the positive plate of length * wide * height=763mm * 55.5mm * 145 μ m.Contain 15.2 gram positive active materials (total amount of first active material and second active material) on the every positive plate.
2. the preparation of negative plate
With 100g negative electrode active material native graphite, 2g adhesive butadiene-styrene rubber (SBR) and 1.5g thickener sodium carboxymethylcellulose (CMC, number-average molecular weight about 400,000), 2g conductive agent carbon black joins in the 120g deionized water, in de-airing mixer, stir then and make cathode size.Cathode size is coated on the negative current collector Copper Foil with coating machine, 110 ℃ of dry 15min, compressing tablet, section then obtains the negative plate of length * wide * height=790mm * 57.5mm * 135 μ m.The content of negative electrode active material native graphite is 7.05g on every negative plate.
The positive and negative plate that obtains is above overlayed the both sides (being that barrier film is kept apart positive and negative plate) of barrier film (polypropylene, polyethylene of thick 16 μ m/polypropylene trilamellar membrane), reel then and make pole piece.Pole piece is put into steel cylinder type lithium ion secondary battery housing, inject 5ml electrolyte then, seal and make battery.The high 65mm of battery, diameter 18mm.The composition of electrolyte: LiPF
61mol/L, quality is than ethylene carbonate (EC): diethyl carbonate (DEC)=1.8.
Embodiment 2
Method according to embodiment 1 obtains battery Y, and different is: first positive active material is median particle diameter D
50 1The LiFeCoPO of=5 μ m
4, second positive active material is median particle diameter D
50 2The LiNi of=15 μ m
0.8Co
0.15Al
0.05O
2, both mass ratioes are 3: 7.The first positive active material LiFeCoPO
4Account for the first active material LiFeCoPO
4With the second active material LiNi
0.8Co
0.15Al
0.05O
2The 30wt% of gross mass.The composition of electrolyte: LiPF
61mol/L, quality is than ethylene carbonate (EC): diethyl carbonate (DEC)=2: 1.
Embodiment 3
Method according to embodiment 1 obtains battery Z, and different is: first positive active material is median particle diameter D
50 1The LiFePO of=4 μ m
4, second positive active material is median particle diameter D
50 2The LiNi of=11 μ m
0.8Co
0.15Mn
0.05O
2, both mass ratioes are 2: 3, the first positive active material LiFePO
4Account for the first active material LiFePO
4With the second active material LiNi
0.8Co
0.15Mn
0.05O
2The 40wt% of gross mass.The composition of electrolyte: LiPF
61mol/L, quality is than ethylene carbonate (EC): diethyl carbonate (DEC)=2: 1.
Comparative Examples 1
Method according to embodiment 1 obtains battery G, and different is: only use a kind of positive active material LiFeCoPO
4, its median particle diameter D
50=4 μ m.
The raw material of using in the embodiment of the invention are commercial.
The positive plate of embodiment and Comparative Examples is done the test of electrolyte wettability, obtain test result as shown in Figure 1.The battery of embodiment and Comparative Examples is done normal-temperature circulating performance test (BK6016 tests cabinet, blue strange production the in Guangzhou), and the result as shown in Figure 2.
Electrolyte is to the wettability method of testing of anode: the electrolyte of getting 10 microlitres, drip on certain position of positive plate, the moment of dripping electrolyte on positive plate is designated as tests the zero hour, the moment that the electrolyte that range estimation drips is just absorbed fully by positive plate is designated as EOT constantly, and the time difference between the two is the time of positive plate Electolyte-absorptive.Repeat aforesaid operations 10 times, each electrolyte that drips on the diverse location of positive plate obtains 10 test values like this.Utilize DOE software (experimental design software, design ofexperiment), the rectangle with a minimum in coordinate system shown in Figure 1 encloses above-mentioned 10 test values, forms box figure shown in Figure 1.The long limit of each box figure (promptly corresponding with embodiment 1,2,3 and Comparative Examples 1 respectively than large rectangle), or claim the horizontal edge that is parallel to transverse axis not have physical significance; Minor face, or claim the longitudinal edge that is parallel to the longitudinal axis to represent the length of electrolyte to the positive plate infiltrating time.Calculate the arithmetic mean of these 10 test values, be marked on the central authorities of box figure, promptly the pairing Y value of blockage in the middle of each box figure among Fig. 1 is the infiltrating time of electrolyte to this positive plate.
Electrolyte was respectively 112 seconds, 94 seconds, 102.5 seconds, 122 seconds the infiltrating time of the positive plate of embodiment 1～3 and Comparative Examples 1.From these data as can be seen, electrolyte is best to the wettability of the positive plate of embodiment 2.
The projection that 2 antenna-like are all arranged with the blockage corresponding position of box figure central authorities on each box figure among Fig. 1, the end value of these 2 projections is represented maximum and the minimum value in above-mentioned 10 measured values respectively, be maximum and the minimum value of electrolyte to the infiltrating time of the diverse location of anode, the difference of these two values is more little, the distribution of pores that positive plate is described is even more, and the infiltrating consistency of electrolyte is good more.Among Fig. 1, the infiltrating greatest measurement of the electrolyte of the positive plate of embodiment 1, minimum measured value were respectively 115 seconds, 109 seconds, and the difference of the two is 8 seconds; Above-mentioned three values of the positive plate of embodiment 2, embodiment 3, Comparative Examples 1 are respectively: 97 seconds, 92 seconds, 5 seconds, and 104 seconds, 100 seconds, 4 seconds, 125 seconds, 118.5 seconds, 6.5 seconds.From these numerical value as can be seen, the electrolyte wettability of embodiment 2 and 3 positive plate is better.
The method of testing of battery normal-temperature circulating performance shown in Figure 2 is as follows: the 0.7C constant current charge, and cut-ff voltage 3.65V shelves 5min, and 0.5C discharges into 2.5V then.
Test result by Fig. 1 and Fig. 2 is as can be seen:
1. electrolyte was lacked 10～30 seconds the infiltrating time of the anode of the infiltrating time comparison Comparative Examples of the anode of embodiment 1～3.Wherein, electrolyte was lacked about 30 seconds the infiltrating time of the anode of Comparative Examples 1 than electrolyte the infiltrating time of the anode of embodiment 2, illustrated that electrolyte is best to the wettability of the anode of embodiment 2.Electrolyte was lacked about 20 seconds the infiltrating time of the battery/anode of the infiltrating time comparison Comparative Examples 1 of the anode of embodiment 3, illustrated that electrolyte is also fine to the wettability of battery/anode of embodiment 3.
2. from the cycle performance of battery test result of Fig. 2 as can be seen: 15% (embodiment 1) that descend at most of the capability retention under the normal temperature after 290 charge and discharge cycles of battery of embodiment 1～3, all less than 20% of Comparative Examples.And that discharge capacity reduces after 290 charge and discharge cycles of the battery of embodiment 2 is minimum, only is declined by less than 1%, so the normal temperature circulation volume conservation rate of the battery of embodiment 2 is best.Discharge capacity reduces less than 5%, so the normal temperature circulation volume conservation rate of the battery of embodiment 3 is also fine after 290 charge and discharge cycles of the battery of embodiment 3.
Therefore, be better than the electrolyte wettability of the positive pole of the positive active material that only uses a kind of crystalline texture in the prior art according to the electrolyte wettability of the lithium-ion secondary battery positive plate of the specific embodiment of the invention.Accordingly, the normal temperature circulation volume conservation rate of the lithium rechargeable battery of the specific embodiment of the invention also is better than positive pole, and to include only a kind of battery normal temperature circulation volume conservation rate of normal temperature circulation volume conservation rate, especially embodiment 2 of lithium rechargeable battery of positive active material of crystalline texture best.
Claims (7)
1. lithium ion secondary battery positive electrode, comprise plus plate current-collecting body and coating and/or be filled in positive electrode on the plus plate current-collecting body, it is characterized in that described positive electrode comprises at least 2 kinds of positive active materials that crystalline texture is different, and 2 kinds of positive active materials as described below are essential:
First positive active material is the LiFeM with olivine structural
xPO
4, wherein, M is selected from least a among Co, Ni, Mn, Al, Mg, Ti, V, Zn, B, Nb, Cu, Ca, Mo, W, the Zr, 0≤x≤1;
Second positive active material comprises the LiNi with spinel structure
1-(y+z)Co
yM
zO
2, wherein, 0.1≤y≤0.2,0≤z≤0.1;
And the percentage that the quality of described first positive active material accounts for first active material and the second active material gross mass is 10～70wt%.
2. according to the lithium rechargeable battery pole piece of claim 1, it is characterized in that the first active material LiFeM
xPO
4Be selected from LiFeMn
0.5PO
4, LiFeCoPO
4, LiFePO
4In at least a.
3. according to the lithium rechargeable battery pole piece of claim 1, it is characterized in that LiNi
1-(y+z)Co
yM
zO
2Be selected from LiNi
0.8Co
0.15Al
0.05O
2, LiNi
0.8Co
0.15Mn
0.05O
2, LiNi
0.8Co
0.2O
2In at least a.
4. according to the lithium ion secondary battery positive electrode of claim 1, it is characterized in that the median particle diameter D of first positive active material
50 1Satisfy 1 μ m≤D
50 1≤ 5 μ m.
5. according to the lithium ion secondary battery positive electrode of claim 1, it is characterized in that the median particle diameter D of second positive active material
50 2Satisfy 5 μ m≤D
50 2≤ 10 μ m.
6. lithium rechargeable battery, comprise battery container, electrode group and electrolyte, electrode group and electrolyte are sealed in the battery container, the electrode group comprises reels or stacked positive pole, barrier film and negative pole successively, it is characterized in that described lithium ion secondary battery positive electrode just very according to claim 1.
7. according to the lithium rechargeable battery of claim 6, it is characterized in that bath composition is as follows: electrolytic salt comprises LiPF
6, its concentration is 0.5～1.5mol/L, solvent is ethylene carbonate and diethyl carbonate by quality than ethylene carbonate: the mixed solvent that diethyl carbonate=1.5～2.5 are formed.
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| CN112736227A (en) * | 2020-12-29 | 2021-04-30 | 天津国安盟固利新材料科技股份有限公司 | Composite cathode and secondary battery using the same |
| WO2023159385A1 (en) * | 2022-02-23 | 2023-08-31 | 宁德时代新能源科技股份有限公司 | Positive electrode sheet, secondary battery, battery module, battery pack, electric device, and method for balancing internal voltage difference of battery |
| CN114597382A (en) * | 2022-03-29 | 2022-06-07 | 烟台大学 | Zn3V4-xMx(PO4)6Application of positive active material as zinc ion battery |
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