CN109860587A - Positive electrode of lithium ion battery and preparation method thereof, lithium ion battery - Google Patents
Positive electrode of lithium ion battery and preparation method thereof, lithium ion battery Download PDFInfo
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Abstract
The invention proposes positive electrodes of lithium ion battery and preparation method thereof, lithium ion battery, and the anode positive electrode is by Li2‑x‑yNaxMyO2It is formed, wherein at least one of M Ni, Co, Mn, Fe, Cu, Al, V, Mg, Te, Ti, Cr and Zr, 0.001≤x≤0.2 and 0.5≤y < 1.The positive electrode of lithium ion battery proposed by the invention, part lithium ion in its layer structure is replaced by sodium ion, the interlamellar spacing of Li can be expanded, to effectively improve diffusion velocity of the lithium ion in lattice, and then help to significantly improve the chemical property of stratiform lithium-rich anode material.
Description
Technical field
The present invention relates to technical field of lithium ion, specifically, the present invention relates to the positive electrode of lithium ion battery and
Preparation method, lithium ion battery.
Background technique
With chemical structure xLi2MnO3·(1-x)LiMO2Stratified material, as electric vehicle (EV) and plug-in mixing
The candidate positive electrode of the lithium ion battery of power car (PHEV), more by more concern that arrives.This positive electrode can provide
High capacity (> 250mAh/g) and good cyclical stability, this is the energy density of twice existing available intercalation material.So
And, it may have the major defects such as voltage attenuation, poor lithium ion diffusion.And some other positive electrodes, it is specific for example,
LiMn2O4With olivine-type LiFePO4Though it is more stable than lithium-rich anode material in structure, they are practical to be only capable of providing
The lower voltage of 3V and the capacity of 100~120mAh/g, these may be unable to satisfy using the material energy densities in terms of EV
It is required that.
Getting up early studies have shown that surface covering (such as Al2O3、AlPO4、AlF3Deng) above-mentioned lack can be solved to a certain extent
It falls into.Because surface covering can inhibit the formation of solid electrolyte interface film layer and surface phase of de- lithium initial stage, both of which is considered
It is the main reason for lithium ion diffusion is poor.But surface covering is only capable of the lithium ion diffusion of enhancing surface region, and can not increase
Lithium ion diffusion in strong positive electrode body phase.
In addition, utilizing other ions (such as Mg2+、Al3+、Ti3+And Cr3+) doping method, can slow down under cyclical voltage
Drop shows metal-doped, especially containing transition metal but without conclusive evidence, can be enhanced in positive electrode body phase
Lithium ion diffusion.
Summary of the invention
The present invention is the following discovery based on inventor and completes:
The present inventor has found in the course of the research, can improve expansion of the lithium ion in lattice by expanding the interlamellar spacing of Li
Speed is dissipated, to help to significantly improve the chemical property of stratiform lithium-rich anode material.Specifically, it is big that ionic radius may be selected
In Li+(r=0.076nm) Na+(r=0.102nm), K+Or Se+Deng for example, by by the part Na in lithium-rich anode material+
Replace Li+, the chemical property of positive electrode can be effectively improved.In this way, adulterating one using into stratiform lithium-rich anode material
The sodium of certainty ratio can be used as the specific strategy for promoting the multiplying power property of lithium-rich anode material.
In view of this, a kind of an object of the present invention is to provide multiplying power properties higher, high magnification discharge capacity is more
High anode material for lithium-ion batteries.
In the first aspect of the present invention, the invention proposes a kind of positive electrodes of lithium ion battery.
According to an embodiment of the invention, the positive electrode is by Li2-x-yNaxMyO2Formed, wherein M Ni, Co, Mn, Fe,
At least one of Cu, Al, V, Mg, Te, Ti, Cr and Zr, 0.001≤x≤0.2 and 0.5≤y < 1.
Inventor has found that the positive electrode of the lithium ion battery of the embodiment of the present invention, in layer structure
Part lithium ion is replaced by sodium ion, can expand the interlamellar spacing of Li, so that diffusion velocity of the lithium ion in lattice is effectively improved,
And then help to significantly improve the chemical property of stratiform lithium-rich anode material.
In addition, positive electrode according to the above embodiment of the present invention, can also have the following additional technical features:
According to an embodiment of the invention, 0.001≤x≤0.02 and 0.5≤y≤0.8.
According to an embodiment of the invention, M is NiaCobMnc, wherein 0.05≤a≤0.2,0.05≤b≤0.2,0.3≤c
≤0.8。
According to an embodiment of the invention, the positive electrode is by Li (Li0.22Na0.01Ni0.1Co0.1Mn0.57)O2It is formed.
In the second aspect of the present invention, the invention proposes a kind of sides of positive electrode for preparing above-mentioned lithium ion battery
Method.
According to an embodiment of the invention, the described method includes: (1) carries out first time calcination processing to the presoma of metal M,
To obtain transition metal oxide；(2) transition metal oxide is mixed and is ground with lithium salts, sodium salt, to be mixed
Powder；(3) second of calcination processing is carried out to the mixed-powder, to obtain the positive electrode.
Inventor has found that the method for the positive electrode for preparing lithium ion battery using the embodiment of the present invention,
The better natrium doping stratiform lithium-rich anode material of chemical property can quickly and efficiently be synthesized.Those skilled in the art can manage
It solves, feature and advantage described in the positive electrode above for lithium ion battery are still applied to this and prepare lithium-ion electric
The method of the positive electrode in pond, details are not described herein.
In addition, preparation method according to the above embodiment of the present invention, can also have the following additional technical features:
According to an embodiment of the invention, the presoma of the metal M is Ni0.15Co0.15Mn0.7(OH)2。
According to an embodiment of the invention, the temperature of the first time calcination processing is 600 degrees Celsius, the time is 8 hours.
According to an embodiment of the invention, the temperature of second of calcination processing is 800 degrees Celsius, the time is 14~18 small
When.
In the third aspect of the present invention, the invention proposes a kind of lithium ion batteries.
According to an embodiment of the invention, the lithium ion battery includes anode, electrolyte layer and cathode, wherein it is described just
Active material in extremely includes above-mentioned positive electrode.
Inventor has found that the lithium ion battery of the embodiment of the present invention, specific capacity of the anode under high magnification
It is higher, to keep the energy density of the lithium ion battery higher.It will be appreciated to those of skill in the art that above for lithium from
Feature and advantage described in the positive electrode of sub- battery are still applied to the lithium ion battery, and details are not described herein.
Additional aspect and advantage of the invention will be set forth in part in the description, and will partially become from the following description
Obviously, or practice through the invention is recognized.
Detailed description of the invention
Above-mentioned aspect combination following accompanying drawings of the invention explains the description of embodiment, in which:
Fig. 1 is the Atomic Arrangement schematic diagram before and after the stratiform richness lithium cathode material sodium contaminated of one embodiment of the invention；
Fig. 2 is the method flow schematic diagram of the positive electrode for preparing lithium ion battery of one embodiment of the invention；
Fig. 3 is the sodium contaminated of one embodiment of the invention and the XRD diagram of undoped positive electrode；
Fig. 4 is the sodium contaminated of one embodiment of the invention and the XRD analysis table of undoped positive electrode；
Fig. 5 is the sodium contaminated of one embodiment of the invention and the multiplying power property analysis result of undoped positive electrode；
Fig. 6 is the sodium contaminated of one embodiment of the invention and the charging and discharging curve of undoped positive electrode.
Specific embodiment
The embodiment of the present invention is described below in detail, those skilled in the art is it will be appreciated that following example is intended for solving
The present invention is released, and is not construed as limitation of the present invention.Unless stated otherwise, it is not expressly recited in embodiment below specific
Technology or conditions, those skilled in the art can be according to common technology or conditions in the art or according to product description
It carries out.
In one aspect of the invention, the invention proposes a kind of positive electrodes of lithium ion battery.
According to an embodiment of the invention, positive electrode is by Li2-x-yNaxMyO2It is formed, wherein M is nickel (Ni), cobalt (Co), manganese
(Mn), at least one in iron (Fe), copper (Cu), aluminium (Al), vanadium (V), magnesium (Mg), antimony (Te), titanium (Ti), chromium (Cr) and zirconium (Zr)
Kind, 0.001≤x≤0.2 and 0.5≤y < 1.In this way, replacing the part lithium ion in layer structure by sodium ion, Li can be expanded
Interlamellar spacing, to improve diffusion velocity of the lithium ion in lattice, and then help to significantly improve stratiform lithium-rich anode material
Chemical property.
Inventor has found in the course of the research, with reference to (a) of Fig. 1, undoped layer structure xLi2MnO3·(1-x)
LiMO2Middle lithium ion and transition metal oxide are layer distributeds, so, Li is greater than by Doped ions radius+(r=
Na 0.076nm)+(r=0.102nm), K+Or Se+Deng with reference to (b) of Fig. 1, so that the interlamellar spacing of big lithium ion can be mentioned effectively
Diffusion velocity of the high-lithium ion in lattice, and then help to significantly improve the chemical property of stratiform lithium-rich anode material.
In some embodiments of the invention, 0.001≤x≤0.02 and 0.5≤y≤0.8, in this way, need to only adulterate a small amount of
Na, stratiform lithium-rich anode material yLi can be made2MnO3·(1-y)LiMO2Under high magnification (discharge-rate is not less than 1C)
Discharge capacity is obviously improved 20% or so.
In some embodiments of the invention, Li2-x-yNaxMyO2In M can be NiaCobMnc, wherein 0.05≤a≤
0.2,0.05≤b≤0.2,0.3≤c≤0.8, in this way, the stratiform lithium-rich anode material of high Mn content, low nickel content is few in doping
After measuring Na, discharge capacity of the positive electrode under high magnification can still be made to reach 200mAh/g or so.
In some specific examples, positive electrode can be by Li (Li0.22Na0.01Ni0.1Co0.1Mn0.57)O2It is formed, in this way, sodium
The doping of ion has not been changed the crystal structure of stratiform lithium-rich anode material, and only lattice parameter c increases, and the rich lithium after natrium doping
Discharge capacity of the capacitance of positive electrode under high magnification (discharge-rate is not less than 1C), than undoped lithium-rich anode material
It is high by 20% or so, thus the multiplying power property for being remarkably improved lithium-rich anode material by adulterating a small amount of sodium ion.
In conclusion according to an embodiment of the invention, the invention proposes a kind of positive electrode of lithium ion battery, layer
Part lithium ion in shape structure is replaced by sodium ion, can expand the interlamellar spacing of Li, to effectively improve lithium ion in lattice
Diffusion velocity, and then help to significantly improve the chemical property of stratiform lithium-rich anode material.
In another aspect of the invention, the invention proposes a kind of positive electrodes for preparing above-mentioned lithium ion battery
Method.According to an embodiment of the invention, with reference to Fig. 2, which includes:
S100: first time calcination processing is carried out to the presoma of metal M, to obtain transition metal oxide.
In this step, first time calcination processing carried out to the presoma of metal M, M Ni, Co, Mn, Fe, Cu, Al, V,
At least one of Mg, Te, Ti, Cr and Zr, in this way, can get transition metal oxide.In some specific examples, metal M
Presoma can be Ni0.15Co0.15Mn0.7(OH)2, in this way, passing through first time calcination processing, mixing lithium salts and sodium salt and second
After calcination processing, the stratiform lithium-rich anode material Li of the higher natrium doping of discharge capacity under high magnification can be finally prepared
(Li0.22Na0.01Ni0.1Co0.1Mn0.57)O2。
In some embodiments of the invention, the temperature of first time calcination processing can for 600 degrees Celsius, the time can be 8 small
When.In this way, using the first time calcination processing of above-mentioned condition, it can be by Ni0.15Co0.15Mn0.7(OH)2Equal presomas be sintered into containing
The transition metal oxide of Ni, Co or Mn etc.；Also, if the temperature of first time calcination processing is lower than 600 degrees Celsius, it is unfavorable for
Improve the lattice of stratiform transition metal oxide；If the time of first time calcination processing is less than 8 hours, the transition metal of acquisition
The crystallinity of oxide is not high enough, to be easy to cause the positive electrode defect finally prepared more and reduce its service life.
S200: transition metal oxide is mixed and is ground with lithium salts, sodium salt, to obtain mixed-powder.
In this step, by the transition metal oxide after step S100 first time calcination processing, continue and lithium salts, sodium salt
It is sufficiently mixed simultaneously grind into powder, in this way, being used for subsequent second of calcination processing, the stratiform that can finally prepare natrium doping is rich
Lithium anode material.In some embodiments of the invention, it can be ground by the method for ball milling, in this way, the mixed powder obtained
End is more evenly and partial size is other in the micron-scale.
S300: second of calcination processing is carried out to mixed-powder, to obtain positive electrode.
In this step, the mixed-powder after step S200 being mixed and ground carries out second of calcination processing, can get
The stratiform lithium-rich anode material of natrium doping.In some specific examples, for Ni0.15Co0.15Mn0.7(OH)2Presoma, second
It can get the stratiform lithium-rich anode material Li of the higher natrium doping of discharge capacity under high magnification after calcination processing
(Li0.22Na0.01Ni0.1Co0.1Mn0.57)O2。
In some embodiments of the invention, the temperature of second of calcination processing can for 800 degrees Celsius, the time can be 14~
18 hours, specifically such as 16 hours.Using second of calcination processing of above-mentioned condition, can by transition metal oxide, lithium salts and
Sodium salt is sintered into Li (Li0.22Na0.01Ni0.1Co0.1Mn0.57)O2The stratiform lithium-rich anode material of equal natrium dopings；Also, if
The temperature of secondary clacining processing is lower than 800 degrees Celsius, is unfavorable for the lithium ion of sodium ion replacement part；If at second of calcining
The time of reason is less than 14 hours, and the crystallinity of the stratiform lithium-rich anode material of the natrium doping of acquisition is not high enough, to be easy to cause
Its defect is more, service life reduction.
In conclusion according to an embodiment of the invention, the invention proposes a kind of positive electrodes for preparing lithium ion battery
Method, can quickly and efficiently synthesize the better natrium doping stratiform lithium-rich anode material of chemical property.Those skilled in the art
Member is still applied to the preparation, it is understood that feature and advantage described in positive electrode above for lithium ion battery
The method of the positive electrode of lithium ion battery, details are not described herein.
In another aspect of the invention, the invention proposes a kind of lithium ion batteries.
According to an embodiment of the invention, lithium ion battery includes anode, electrolyte layer and cathode, wherein the work in anode
Property substance includes above-mentioned positive electrode.
It should be noted that the lithium ion battery is other than including anode, cathode and electrolyte layer, it further include that other must
The Nomenclature Composition and Structure of Complexes wanted, specifically such as positive collector, negative collector, circuit trace or shell, those skilled in the art can root
It is correspondingly supplemented according to the specifically used requirement of the lithium ion battery, details are not described herein.
In conclusion according to an embodiment of the invention, anode is in high magnification the invention proposes a kind of lithium ion battery
Under specific capacity it is higher, to keep the energy density of the lithium ion battery higher.It will be appreciated to those of skill in the art that preceding
Feature and advantage described in positive electrode of the face for lithium ion battery, are still applied to the lithium ion battery, no longer superfluous herein
It states.
Below with reference to specific embodiment, present invention is described, it should be noted that these embodiments are only descriptive
, without limiting the invention in any way.
Embodiment 1
In this embodiment, the stratiform lithium-rich anode material Li (Li of natrium doping is prepared0.22Na0.01Ni0.1Co0.1Mn0.57)
O2.The specific method is as follows: (1) to presoma Ni0.15Co0.15Mn0.7(OH)2First time calcination processing is carried out, the temperature of calcining is
600 degrees Celsius, the time be 8 hours；(2) lithium salts, sodium salt are added to the product after first time calcination processing, ball again after being sufficiently mixed
Mill obtains mixed-powder；(3) second of calcination processing is carried out to mixed-powder, the temperature of calcining is 800 degrees Celsius, the time 16
Hour, and calcined product is ground up, sieved, it can be obtained the positive electrode of natrium doping.
Comparative example 1
In the comparative example, undoped stratiform lithium-rich anode material Li (Li is prepared0.22Ni0.1Co0.1Mn0.58)O2.Specifically
Method is as follows: (1) to presoma Ni0.15Co0.15Mn0.7(OH)2First time calcination processing is carried out, the temperature of calcining is 600 Celsius
Degree, time are 8 hours；(2) lithium salts is added to the product after first time calcination processing, ball milling obtains mixed powder again after being sufficiently mixed
End；(3) second of calcination processing is carried out to mixed-powder, the temperature of calcining is 800 degrees Celsius, the time is 16 hours, and will forge
Product after burning is ground up, sieved, and can be obtained undoped positive electrode.
Embodiment 2
In this embodiment, the undoped positive electrode of the positive electrode to the natrium doping of embodiment 1 and comparative example 1,
XRD test is carried out respectively.Wherein, the positive electrode (Li (Li of natrium doping0.22Na0.01Ni0.1Co0.1Mn0.57)O2) and it is undoped
Positive electrode (Li (Li0.22Ni0.1Co0.1Mn0.58)O2) XRD diagram as shown in figure 3, also, specific XRD analysis table such as Fig. 4 institute
Show.
From figure 3, it can be seen that the sample of sodium contaminated and undoped sample diffraction maximum having the same, and all diffraction maximum categories
In the a-NaFeO of space group R_3m and C3m2Stratiform hexagonal structure.And it as can be seen from Figure 4, can due to the insertion of sodium ion
Observe the increase of lattice parameter c, this also indicates that the sodium ion in lithium ion layer there are larger size.
Embodiment 3
In this embodiment, the undoped positive electrode of the positive electrode to the natrium doping of embodiment 1 and comparative example 1,
Multiplying power property test is carried out under different multiplying respectively.Specifically, in the glove box of argon gas filling just by positive electrode and lithium
Pole piece is assembled into CR2025 button cell, then carries out electrochemical property test.It wherein, can be by ready powder and 4wt% carbon
Material, 4wt% polyvinyl dichloride (PVDF) prepare positive plate by adhesive mixing；And with the EC/DEC of 1mol/L LiPF6
(volume ratio 3:7) mixed solution uses more empty glass fibre separators will anode and lithium-rich anode material as electrolyte
Anode separates.
And at room temperature, electrochemical property test is carried out between 2.5~4.8V relative to Li+/Li electrode；Initial fills
Discharge curve test is to carry out under 0.1C multiplying power, and current density 1C is set as 300mAh/g, and subsequent multiplying power is changed to respectively
0.2C, 0.5C, 1.0C and 2.0C are tested again.And positive electrode (Li (the Li of natrium doping0.22Na0.01Ni0.1Co0.1Mn0.57)O2)
With undoped positive electrode (Li (Li0.22Ni0.1Co0.1Mn0.58)O2) high rate performance analysis as a result, as shown in Figure 5.
As can be seen from Figure 5, the capacitance of the lithium-rich anode material after natrium doping is in high magnification (discharge-rate is not less than 1C)
Under, discharge capacity is high than undoped lithium-rich anode material by 20% or so.
Embodiment 4
In this embodiment, the undoped positive electrode of the positive electrode to the natrium doping of embodiment 1 and comparative example 1,
Charge and discharge cycles test is carried out under 0.1C and 1C multiplying power respectively.Wherein, the positive electrode (Li of natrium doping
(Li0.22Na0.01Ni0.1Co0.1Mn0.57)O2) and undoped positive electrode (Li (Li0.22Ni0.1Co0.1Mn0.58)O2) charge and discharge
Electric curve is as shown in Figure 6.
As can be seen from Figure 6, discharge capacity of the capacitance of the lithium-rich anode material after natrium doping under high magnification is more preferable.
In the description of the present invention, it is to be understood that, in addition, term " first ", " second " are used for description purposes only, and
It cannot be understood as indicating or implying relative importance or implicitly indicate the quantity of indicated technical characteristic.It defines as a result,
The feature of " first ", " second " can explicitly or implicitly include at least one of the features.In the description of the present invention, " more
It is a " it is meant that at least two, such as two, three etc., unless otherwise specifically defined.
In the description of this specification, reference term " one embodiment ", " some embodiments ", " example ", " specifically show
The description of example " or " some examples " etc. means specific features, structure, material or spy described in conjunction with this embodiment or example
Point is included at least one embodiment or example of the invention.In the present specification, schematic expression of the above terms are not
It must be directed to identical embodiment or example.Moreover, particular features, structures, materials, or characteristics described can be in office
It can be combined in any suitable manner in one or more embodiment or examples.In addition, without conflicting with each other, the skill of this field
Art personnel can tie the feature of different embodiments or examples described in this specification and different embodiments or examples
It closes and combines.
Although the embodiments of the present invention has been shown and described above, it is to be understood that above-described embodiment is example
Property, it is not considered as limiting the invention, those skilled in the art within the scope of the invention can be to above-mentioned
Embodiment is changed, modifies, replacement and variant.
Claims (9)
1. a kind of positive electrode of lithium ion battery, which is characterized in that the positive electrode is by Li2-x-yNaxMyO2It is formed, wherein
M is at least one of Ni, Co, Mn, Fe, Cu, Al, V, Mg, Te, Ti, Cr and Zr, 0.001≤x≤0.2 and 0.5≤y < 1.
2. positive electrode according to claim 1, which is characterized in that 0.001≤x≤0.02 and 0.5≤y≤0.8.
3. positive electrode according to claim 1, which is characterized in that M NiaCobMnc, wherein 0.05≤a≤0.2,
0.05≤b≤0.2、0.3≤c≤0.8。
4. positive electrode according to claim 3, which is characterized in that the positive electrode is by Li
(Li0.22Na0.01Ni0.1Co0.1Mn0.57)O2It is formed.
5. a kind of method for the positive electrode for preparing lithium ion battery according to any one of claims 1 to 4, feature exist
In, comprising:
(1) first time calcination processing is carried out to the presoma of metal M, to obtain transition metal oxide；
(2) transition metal oxide is mixed and is ground with lithium salts, sodium salt, to obtain mixed-powder；
(3) second of calcination processing is carried out to the mixed-powder, to obtain the positive electrode.
6. according to the method described in claim 5, it is characterized in that, the presoma of the metal M is Ni0.15Co0.15Mn0.7
(OH)2。
7. according to the method described in claim 5, it is characterized in that, the temperature of the first time calcination processing be 600 degrees Celsius,
Time is 8 hours.
8. according to the method described in claim 5, it is characterized in that, the temperature of second of calcination processing be 800 degrees Celsius,
Time is 14~18 hours.
9. a kind of lithium ion battery, which is characterized in that including anode, electrolyte layer and cathode, wherein the activity in the anode
Substance includes positive electrode according to any one of claims 1 to 4.
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| CN114144919A (en) * | 2021-03-26 | 2022-03-04 | 宁德新能源科技有限公司 | Positive pole piece, electrochemical device comprising positive pole piece and electronic device |
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