CN108417783A - The nickel-cobalt lithium manganate cathode material and preparation method of the modified oxidized tin cladding of niobium manganese - Google Patents
The nickel-cobalt lithium manganate cathode material and preparation method of the modified oxidized tin cladding of niobium manganese Download PDFInfo
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- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
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- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/485—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
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- H01M4/505—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy
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- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
- H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
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Abstract
The present invention is suitable for technical field of lithium batteries, provides a kind of nickel-cobalt lithium manganate cathode material and preparation method of the modified oxidized tin cladding of niobium manganese, the method includes：Rapid S1, the oxide for weighing tin oxide and niobium manganese, low-temperature treatment after mixing obtain niobium manganese oxidation tin mixture；Step S2, nickel-cobalt-manganese ternary material is weighed in proportion, and with niobium manganese oxidation tin mixture be sufficiently mixed uniformly, obtains mixture；Step S3, the obtained mixtures of step S2 are encased in saggar, are sintered, obtain the nickel-cobalt lithium manganate cathode material of the modified oxidized tin cladding of niobium manganese.The present invention can be effectively protected the surface texture of material using the tin oxide that niobium manganese is modified to coat tertiary cathode material, reduce Ni2+Generation, effectively inhibit Lattice Oxygen abjection, improve the cycle and high rate performance of material, while can also effectively reduce side effect caused by tin oxide own material defect, keep material property better.
Description
Technical field
The invention belongs to the nickle cobalt lithium manganates of technical field of lithium batteries more particularly to a kind of modified oxidized tin cladding of niobium manganese just
Pole material and preparation method.
Background technology
Nickel-cobalt-manganese ternary anode material for lithium-ion batteries due to higher energy density and relatively low cost and
It is widely used in new energy battery industry.The structural stability of the especially nickelic product of nickle cobalt lithium manganate (LNCM) is not good enough, is filling
It is easy to the deintercalation due to Li ions and the variation of Ni, Co, Mn ionic valence condition in discharge process, causes the effusion of Lattice Oxygen,
Collapsing for material structure is caused, the cycle life and safety of material are caused great harm；Simultaneously surface texture be easy with
Electrolyte reacts, Ni3+Easily it is reduced into Ni2+Inertia valence state, surface Ni2+Content accounts for Ni in entire crystal structure2+'s
2/3rds, so as to cause Li+、Ni2+Mixing influences the first effect and cycle performance of product.
Invention content
In view of the above problems, the purpose of the present invention is to provide a kind of nickle cobalt lithium manganates of the modified oxidized tin cladding of niobium manganese just
Pole material and preparation method, it is intended to solve the poor technical problem of existing nickle cobalt lithium manganate cycle performance of battery.
The preparation method of the nickel-cobalt lithium manganate cathode material of the modified oxidized tin cladding of niobium manganese includes the following steps：
Step S1, the oxide of tin oxide and niobium manganese is weighed, low-temperature treatment after mixing obtains niobium manganese oxidation tin mixture；
Step S2, nickel-cobalt-manganese ternary material is weighed in proportion, and is sufficiently mixed with niobium manganese oxidation tin mixture
Uniformly, mixture is obtained；
Step S3, the obtained mixtures of step S2 are encased in saggar, are sintered, obtain the modified oxidized Xi Bao of niobium manganese
The nickel-cobalt lithium manganate cathode material covered.
Further, in the oxide of step S1 is weighed tin oxide and niobium manganese, the molar ratio Sn of tin niobium manganese：Nb：Mn=
1:(0.1~0.3)：(0.2~0.5), ranging from 200-500 DEG C of low-temperature treatment..
Further, in step S2, niobium manganese oxidation tin mixture accounts for the 0.05- of nickel-cobalt-manganese ternary material in mass ratio
0.4% weighs nickel-cobalt-manganese ternary material.
Further, in step S3, the sintering temperature of sintering process is 600-1000 DEG C, sintering time 4-12h.
On the other hand, the nickel-cobalt lithium manganate cathode material is prepared using the above method, and material matrix is nickel cobalt manganese
Ternary material, material shell are the compound coating layer of tin oxide-manganese-niobium.
The beneficial effects of the invention are as follows：The present invention forms tin oxide-manganese-niobium by the modified oxidized tin of manganese, in material surface
Compound coating layer, barrier material surface texture and electrolyte are in direct contact, simultaneously because the electric conductivity of tin oxide is effective
Internal resistance is reduced, the electronics residual in charge and discharge process is reduced；In addition the tin oxide being modified through niobium-manganese so that tin oxide is in charge and discharge
Since the addition of niobium makes its volume expansion temperature be promoted in electric process, the volume expansion of material is made to be effectively suppressed and slow down,
And due to the addition of manganese so that the structure of niobium-manganese-tin oxide clad, which tends to layer structure and matrix, better matching
Property, Lacking oxygen is reduced, the generation for inhibiting oxygen defect is contributed to.
Description of the drawings
Fig. 1 is the charge and discharge cycles number and capacity relationship figure of test example 1 and comparative example 1 of the present invention；
Fig. 2 is the charge and discharge cycles number and capacity relationship figure of test example 2 and comparative example 2 of the present invention.
Specific implementation mode
In order to make the purpose , technical scheme and advantage of the present invention be clearer, with reference to the accompanying drawings and embodiments, right
The present invention is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, and
It is not used in the restriction present invention.
In order to illustrate technical solutions according to the invention, illustrated below by specific embodiment.
The preparation method of the nickel-cobalt lithium manganate cathode material of the modified oxidized tin cladding of niobium manganese provided by the invention includes subordinate
Step：
Step S1, the oxide of tin oxide and niobium manganese is weighed, low-temperature treatment after mixing obtains niobium manganese oxidation tin mixture.
In the oxide of tin oxide and niobium manganese that this step weighs, the molar ratio Sn of tin niobium manganese：Nb：Mn=1:(0.1~
0.3)：(0.2~0.5), ranging from 200-500 DEG C of low-temperature treatment.The tin oxide is tin monoxide or stannic oxide.It is described
The oxide of niobium manganese is total appellation of niobium element and the various oxides of manganese element, and there are many selections, for example niobium oxide can be with
For columbium monoxide, columbium dioxide, columbium sesquioxide, niobium pentaoxide etc., manganese oxide can be manganese monoxide, manganese dioxide etc..
Step S2, nickel-cobalt-manganese ternary material is weighed in proportion, and is sufficiently mixed with niobium manganese oxidation tin mixture
Uniformly, mixture is obtained.
The 0.05-0.4% that this step niobium manganese oxidation tin mixture in mass ratio accounts for nickel-cobalt-manganese ternary material weighs nickel cobalt manganese
Ternary material.
Step S3, the obtained mixtures of step S2 are encased in saggar, are sintered, sintering temperature 600-1000
DEG C, sintering time 4-12h obtains the nickel-cobalt lithium manganate cathode material of the modified oxidized tin cladding of niobium manganese.
The present invention coats nickel-cobalt-manganese ternary material using the modified oxidized tin of niobium manganese, and internal layer is nickel-cobalt-manganese ternary material
Material, shell are the compound coating layer of tin oxide-manganese-niobium.The structural stability of the especially nickelic product of nickle cobalt lithium manganate is not good enough,
It is easy to the deintercalation due to Li ions and the variation of Ni, Co, Mn ionic valence condition in charge and discharge process, causes the ease of Lattice Oxygen
Go out, cause collapsing for material structure, the cycle life and safety of material are caused great harm；If directly using oxidation
Tin coats, but is that will produce volume expansion in charge and discharge process the shortcomings that tin oxide, adds the object phase of matrix and tin oxide
Structure is not exactly the same, and through cycle after a period of time, clad can fall off from matrix, just lose the effect of cladding.The present invention
Tin oxide is modified through niobium-manganese so that tin oxide, since the addition of niobium makes its volume expansion temperature be promoted, makes in charge and discharge process
The volume expansion of material is effectively suppressed and slows down, and due to the addition of manganese so that the structure of niobium-manganese-tin oxide clad
Tending to layer structure and matrix has better matching, reduces Lacking oxygen, contributes to the generation for inhibiting oxygen defect.
This material result is verified below by test example and comparative example.
Test example 1：
Weigh stannic oxide, niobium pentaoxide, manganese monoxide, wherein the molar ratio Sn of tin niobium manganese：Nb：Mn=1:0.1：
0.2,200 DEG C of low-temperature treatments after mixing obtain niobium manganese oxidation tin mixture, and niobium manganese oxidation tin mixture in mass ratio accounts for 0.1%
NCM811 ternary materials are weighed, and with niobium manganese oxidation tin mixture be sufficiently mixed uniformly, obtain mixture；Mixture is filled
Enter into saggar, it is 650 DEG C, sintering time 6h to be sintered sintering temperature, finally obtains the modified oxidized tin cladding of niobium manganese
Nickel-cobalt lithium manganate cathode material.
Test example 2：
Weigh stannic oxide, niobium pentaoxide, manganese monoxide, wherein the molar ratio Sn of tin niobium manganese：Nb：Mn=1:0.3：
350 DEG C of low-temperature treatments after 0.5 mixing obtain niobium manganese oxidation tin mixture, and niobium manganese oxidation tin mixture in mass ratio accounts for 0.25%
NCM523 ternary materials are weighed, and with niobium manganese oxidation tin mixture be sufficiently mixed uniformly, obtain mixture；Mixture is filled
Enter into saggar, it is 890 DEG C, sintering time 7.5h to be sintered sintering temperature, finally obtains the modified oxidized tin cladding of niobium manganese
Nickel-cobalt lithium manganate cathode material.
Comparative example 1：
Stannic oxide is weighed, tin oxide in mass ratio accounts for ternary material 0.08% and weighs NCM811 ternary materials, and and oxygen
Change tin be sufficiently mixed uniformly, obtains mixture；Mixture is encased in saggar, it is 650 DEG C to be sintered sintering temperature,
Sintering time is 6h, finally obtains the nickel-cobalt lithium manganate cathode material of tin oxide cladding.
Comparative example 2：
Stannic oxide is weighed, tin oxide in mass ratio accounts for ternary material 0.14% and weighs NCM523 ternary materials, and and oxygen
Change tin be sufficiently mixed uniformly, obtains mixture；Mixture is encased in saggar, it is 890 DEG C to be sintered sintering temperature,
Sintering time is 7.5h, finally obtains the nickel-cobalt lithium manganate cathode material of tin oxide cladding.
For the positive electrode being prepared respectively using test example 1,2 and comparative example 1,2 as positive active material, lithium piece is negative
Pole is assembled into button cell.The group of positive plate becomes m (active material)：M (acetylene black)：M (PVDF)=80:12:8, using indigo plant
Electrical measurement test system is tested, and charging/discharging voltage is 2.75~4.3V, and cycle performance test is carried out under normal temperature environment.Charge and discharge
Cycle-index and the relationship of capacity are as shown in Figure 1, 2.
As can be known from Fig. 1, the lithium battery that prepared by the positive electrode of 1 tin oxide of comparative example cladding is rapid in 70 circle left and right capacity
Decline, and lithium battery prepared by the NCM811 positive electrodes of the modified oxidized tin cladding of niobium manganese, it is still steady being recycled to 100 circles
Downward trend.
As can be known from Fig. 2, the lithium battery that prepared by the positive electrode of 2 tin oxide of comparative example cladding is kept in 80 circle left and right capacity
Rate is 98% or so, and 100 circles decay to 95.7%, and the NCM523 positive electrodes of the modified oxidized tin cladding of niobium manganese is used to prepare
Lithium battery, material 80 enclose capacity retention ratio in 99.3%, 100 circle conservation rate 97.7%.
It can be seen that nickel-cobalt lithium manganate cathode material of the present invention by the modified oxidized tin cladding of niobium manganese is compared to common oxygen
Change the nickel-cobalt lithium manganate cathode material of tin cladding, cycle performance of battery is obviously improved.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
All any modification, equivalent and improvement etc., should all be included in the protection scope of the present invention made by within refreshing and principle.
Claims (5)
1. a kind of preparation method of the nickel-cobalt lithium manganate cathode material of the modified oxidized tin cladding of niobium manganese, which is characterized in that the side
Method includes the following steps：
Step S1, the oxide of tin oxide and niobium manganese is weighed, low-temperature treatment after mixing obtains niobium manganese oxidation tin mixture；
Step S2, nickel-cobalt-manganese ternary material is weighed in proportion, and be sufficiently mixed uniformly with niobium manganese oxidation tin mixture,
Obtain mixture；
Step S3, the obtained mixtures of step S2 are encased in saggar, are sintered, obtain the modified oxidized tin cladding of niobium manganese
Nickel-cobalt lithium manganate cathode material.
2. the preparation method of the nickel-cobalt lithium manganate cathode material of the modified oxidized tin cladding of niobium manganese as described in claim 1, feature
It is, in the oxide of the tin oxide that step S1 is weighed and niobium manganese, the molar ratio Sn of tin niobium manganese：Nb：Mn=1:(0.1~0.3)：
(0.2~0.5), ranging from 200-500 DEG C of low-temperature treatment.
3. the preparation method of the nickel-cobalt lithium manganate cathode material of the modified oxidized tin cladding of niobium manganese as claimed in claim 2, feature
It is, in step S2, niobium manganese oxidation tin mixture accounts for the 0.05-0.4% of nickel-cobalt-manganese ternary material and weighs nickel cobalt manganese in mass ratio
Ternary material.
4. the preparation method of the nickel-cobalt lithium manganate cathode material of the modified oxidized tin cladding of niobium manganese as described in claim 1, feature
It is, in step S3, the sintering temperature of sintering process is 600-1000 DEG C, sintering time 4-12h.
5. a kind of nickel-cobalt lithium manganate cathode material of the modified oxidized tin cladding of niobium manganese, which is characterized in that the nickle cobalt lithium manganate is just
Pole material uses any one of claim 1-4 the method to be such as prepared, and material matrix is nickel-cobalt-manganese ternary material, material shell
Layer is the compound coating layer of tin oxide-manganese-niobium.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111769260A (en) * | 2020-03-20 | 2020-10-13 | 浙江南都电源动力股份有限公司 | High specific energy lithium ion battery and preparation method thereof |
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