CN107732181A - Nickel cobalt manganese anode material for lithium-ion batteries of samarium doping and preparation method thereof - Google Patents
Nickel cobalt manganese anode material for lithium-ion batteries of samarium doping and preparation method thereof Download PDFInfo
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- CN107732181A CN107732181A CN201710891921.5A CN201710891921A CN107732181A CN 107732181 A CN107732181 A CN 107732181A CN 201710891921 A CN201710891921 A CN 201710891921A CN 107732181 A CN107732181 A CN 107732181A
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- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
- 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 invention discloses a kind of nickel cobalt manganese anode material for lithium-ion batteries of samarium doping, its molecular formula is LiaNixCoyMnzSmbO2;The invention also discloses the preparation method of the positive electrode.The present invention by the oxide of nickel cobalt manganese monocrystalline composite precursor and nanoscale samarium by carrying out ultrahigh speed premixing, again by the compound of nickel cobalt manganese monocrystalline composite precursor and the oxide of nanoscale samarium and common nickel cobalt manganese polycrystalline composite precursor mixed at high speed, improve mixed effect, because monocrystalline composite precursor high mechanical strength, ultra-high-speed mixing can be used and be unlikely to broken, monocrystalline composite precursor can play a part of collision medium simultaneously, the oxide of nanoscale samarium is fully broken up, is sufficiently mixed doped chemical and host element.
Description
Technical field
The invention belongs to anode material for lithium-ion batteries manufacturing technology field, and in particular to a kind of nickel cobalt manganese lithium of samarium doping
Ion battery positive electrode and preparation method thereof.
Background technology
Nickel-cobalt-manganese ternary anode material for lithium-ion batteries is due to higher energy density and relatively simple system
It is widely used in IT product and new-energy automobile field for technique.But simple nickle cobalt lithium manganate (LNCM) is due to structure
Stability is not good enough, is easy to make due to the deintercalation of Li ions and the change of Ni, Co, Mn ionic valence condition in charge and discharge process
Into collapsing for material structure, so as to cause greatly to endanger to the cycle life and security of material, regarding to the issue above typically
Improved by the way of appropriate Sm ions are mixed.Due to Sm3+With Ni3+Valence state it is identical, the Sm of incorporation3+Occupy Ni3+
Position, in charging process, Ni can occur for Ni ions3+To Ni4+Transformation, and with volume contraction, if charging voltage mistake
Height, depth of charge are excessive, and the volume contraction of material will be irreversible, and finally loses electro-chemical activity, and Sm3+In discharge and recharge
Fixed price in journey, it is electrochemicaUy inert, the change of valence state does not occur in discharge and recharge, thus the change of volume does not occur yet,
Skeleton, stable crystal structure, the cycle life and security performance for improving material can be played a part of.
As can be seen here, Sm incorporation has significant improvement result, but simultaneously because incorporation to the structural stability of material
Be all non-electroactive material, mutually tackle material specific discharge capacity cause necessarily to influence.If incorporation is too high, put
Capacitance will significantly reduce;If incorporation is insufficient, the stability of material cannot effectively improve.Therefore, doping member
Element is to realize an important factor for specific discharge capacity reaches balance with stability with uniform mix of host element.It is and more in the prior art
Using simple mixing oxides method incorporation in general Sm2O3, it is extremely difficult to doped chemical and is mixed with the uniform of host element.
The content of the invention
An object of the present invention is to provide a kind of nickel cobalt manganese anode material for lithium-ion batteries of samarium doping, mesh of the invention
Two preparation methods for being to provide the positive electrode, solve doped chemical in the prior art and uneven ask mixed with host element
Topic.
The technical solution adopted in the present invention is:
A kind of nickel cobalt manganese anode material for lithium-ion batteries of samarium doping, its molecular formula are LiaNixCoyMnzSmbO2, wherein, 1
≤a≤1.2;0.3≤x≤0.98;0.01≤y≤0.6;0.001≤z≤0.6;B is 4/3-a/3-x-y-z, 0.00001≤b
≤0.03。
The present invention another technical scheme be:
The preparation method of the nickel cobalt manganese anode material for lithium-ion batteries of samarium doping, it comprises the following steps:
Step 1, nickel cobalt manganese polycrystalline composite precursor, nickel cobalt manganese monocrystalline composite precursor, nanometer samarium source and lithium are weighed respectively
Source;
Step 2, the nickel cobalt manganese monocrystalline composite precursor weighed in the step 1 and nanometer samarium source are subjected to ultrahigh speed mixed
Close, the first mixture is made;
It is step 3, obtained first mixture in the step 2 and the nickel cobalt manganese polycrystalline weighed in the step 1 is compound
Presoma and lithium source carry out mixed at high speed, and the second mixture is made;
Step 4, obtained second mixture in the step 3 is encased in porcelain boat be calcined, that is, samarium doping is made
Nickel cobalt manganese anode material for lithium-ion batteries.
The characteristics of another technical scheme of the invention, also resides in:
In the step 1, the nickel cobalt manganese polycrystalline composite precursor and nickel cobalt manganese monocrystalline composite precursor be nickel, cobalt,
At least one of the composite oxides of manganese, complex hydroxide, compound oxyhydroxide, wherein, nickel, cobalt, the mol ratio of manganese
For Ni:Co:Mn=0.3-0.98:0.01-0.6:0.001-0.6.
In the step 1, the nanometer samarium source is the oxide or hydroxide of nanoscale samarium.
In the step 1, the mass ratio of the nickel cobalt manganese polycrystalline composite precursor and nickel cobalt manganese monocrystalline composite precursor is
2-20:1。
In the step 2, the ultra-high-speed mixing uses ternary material ultrahigh speed blender, and the rotating speed of ultra-high-speed mixing is
5500-20000r/min。
In the step 3, the lithium source is lithium carbonate or lithium hydroxide.
In the step 3, the mixed at high speed uses ternary material high speed blender, and the rotating speed of mixed at high speed is 1000-
10000r/min。
It is described to be roasted in the step 4:6h-36h is calcined at 600 DEG C -1200 DEG C.
Compared with prior art, the present invention is using the oxide of nanoscale samarium as Sm sources, and the method for using mixed at high speed
Solid phase mixing mixes Sm, and this method is simple to operation, and Sm incorporation easily accurately controls, and the Sm sources of nano-scale are beneficial to Sm
Be uniformly distributed;The present invention by the oxide of nickel cobalt manganese monocrystalline composite precursor and nanoscale samarium by carrying out ultrahigh speed premix
Close, then by the compound of nickel cobalt manganese monocrystalline composite precursor and the oxide of nanoscale samarium and common nickel cobalt manganese polycrystalline compound precursor
Body mixed at high speed, mixed effect is improved, can be unlikely using ultra-high-speed mixing because monocrystalline composite precursor high mechanical strength
In broken, while monocrystalline composite precursor can play a part of collision medium, and the oxide of nanoscale samarium is fully broken up, and make
Doped chemical and host element are sufficiently mixed.
Embodiment
The present invention is described in further detail with reference to embodiment:
A kind of nickel cobalt manganese anode material for lithium-ion batteries of samarium doping, its molecular formula are LiaNixCoyMnzSmbO2, wherein, 1
≤a≤1.2;0.3≤x≤0.98;0.01≤y≤0.6;0.001≤z≤0.6;B is 4/3-a/3-x-y-z, 0.00001≤b
≤0.03。
A kind of preparation method of the nickel cobalt manganese anode material for lithium-ion batteries of above-mentioned samarium doping, it comprises the following steps:
Step 1, nickel cobalt manganese polycrystalline composite precursor, nickel cobalt manganese monocrystalline composite precursor, nanometer samarium source and lithium are weighed respectively
Source;The nickel cobalt manganese polycrystalline composite precursor and nickel cobalt manganese monocrystalline composite precursor are the composite oxides, multiple of nickel, cobalt, manganese
At least one of hydroxide, compound oxyhydroxide are closed, wherein, nickel, cobalt, the mol ratio of manganese are Ni:Co:Mn=0.3-
0.98:0.01-0.6:0.001-0.6;The nanometer samarium source is the oxide or hydroxide of nanoscale samarium;The nickel cobalt manganese is more
The mass ratio of brilliant composite precursor and nickel cobalt manganese monocrystalline composite precursor is 2-20:1;
The advantages of step 1, is:Using the oxide of nanoscale samarium as Sm sources so that Sm incorporation easily accurately controls,
The Sm sources of nano-scale are advantageous to being uniformly distributed for Sm;The monocrystalline composite precursor of use is especially suitable for ultra-high-speed mixing, and single
Brilliant composite precursor is solid, ultra-high-speed mixing when do not break up, while monocrystalline composite precursor can play the work of collision medium
With, mixed nanometer element is fully broken up, then again with remaining conventional polycrystalline composite precursor carry out mixed at high speed, reach more
Good mixed effect.
Step 2, the nickel cobalt manganese monocrystalline composite precursor weighed in the step 1 and nanometer samarium source are subjected to ultrahigh speed mixed
Close, the first mixture is made;The ultra-high-speed mixing uses ternary material ultrahigh speed blender, and the rotating speed of ultra-high-speed mixing is
5500-20000r/min;
In step 2, ultrahigh speed is carried out to monocrystalline composite precursor and nanometer samarium source using ternary material high speed blender and mixed
Close, because monocrystalline composite precursor high mechanical strength, ultra-high-speed mixing can be used and be unlikely to broken, while before monocrystalline is compound
Collision medium can be played a part of by driving body, and the oxide of nanoscale samarium is fully broken up, makes doped chemical and host element abundant
Mixing.
It is step 3, obtained first mixture in the step 2 and the nickel cobalt manganese polycrystalline weighed in the step 1 is compound
Presoma and lithium source carry out mixed at high speed, and the second mixture is made;The lithium source is lithium carbonate or lithium hydroxide;The high speed is mixed
Conjunction uses ternary material high speed blender, and the rotating speed of mixed at high speed is 1000-10000r/min;
Step 4, obtained second mixture in the step 3 is encased in porcelain boat be calcined at 600 DEG C -1200 DEG C
6h-36h, that is, the nickel cobalt manganese anode material for lithium-ion batteries of samarium doping is made.
Embodiment 1:
A kind of nickel cobalt manganese anode material for lithium-ion batteries of samarium doping, its molecular formula are LiaNixCoyMnzSmbO2, wherein, 1
≤a≤1.2;0.3≤x≤0.98;0.01≤y≤0.6;0.001≤z≤0.6;B is 4/3-a/3-x-y-z, 0.00001≤b
≤0.03。
A kind of molecular formula is Li1.2Ni0.3Co0.6Mn0.001Sm0.029O2Samarium doping nickel cobalt manganese lithium ion cell positive material
The preparation method of material, it comprises the following steps:
Step 1, nickel cobalt manganese polycrystalline composite precursor, nickel cobalt manganese monocrystalline composite precursor, nanometer Sm are weighed respectively2O3And lithium
Source;Wherein, nickel cobalt manganese polycrystalline composite precursor and nickel cobalt manganese monocrystalline composite precursor are the composite oxides, multiple of nickel, cobalt, manganese
At least one of hydroxide, compound oxyhydroxide are closed, nickel, cobalt, the mol ratio of manganese are Ni:Co:Mn=0.3:0.6:
0.001;The mass ratio of nickel cobalt manganese polycrystalline composite precursor and nickel cobalt manganese monocrystalline composite precursor is 2:1;
Step 2, by the nickel cobalt manganese monocrystalline composite precursor weighed in the step 1 and nanometer Sm2O3Ultrahigh speed is carried out to mix
Close, the first mixture is made;The ultra-high-speed mixing uses ternary material ultrahigh speed blender, and the rotating speed of ultra-high-speed mixing is
5500r/min;
It is step 3, obtained first mixture in the step 2 and the nickel cobalt manganese polycrystalline weighed in the step 1 is compound
Presoma and lithium source carry out mixed at high speed, and the second mixture is made;The lithium source is lithium carbonate or lithium hydroxide;The high speed is mixed
Conjunction uses ternary material high speed blender, and the rotating speed of mixed at high speed is 1000r/min;
Step 4, obtained second mixture in step 3 is encased in porcelain boat at 600 DEG C it is calcined 36h, that is, samarium is made
The nickel cobalt manganese anode material for lithium-ion batteries of doping.
Above-mentioned anode material for lithium-ion batteries, metal lithium sheet are that negative pole assembles button cell progress discharge and recharge contrast test,
First discharge specific capacity can reach 152.5mAh/g under 0.5C multiplying powers, capability retention 98.1% after 100 charge and discharges circulation,
And common positive electrode first discharge specific capacity is 153mAh/g, capability retention 96.9% after 100 charge and discharges circulation.
Embodiment 2:
A kind of nickel cobalt manganese anode material for lithium-ion batteries of samarium doping, its molecular formula are LiaNixCoyMnzSmbO2, wherein, 1
≤a≤1.2;0.3≤x≤0.98;0.01≤y≤0.6;0.001≤z≤0.6;B is 4/3-a/3-x-y-z, 0.00001≤b
≤0.03。
A kind of molecular formula is LiNi0.98Co0.01Mn0.008Sm0.002O2Samarium doping nickel cobalt manganese lithium ion cell positive material
The preparation method of material, it comprises the following steps:
Step 1, nickel cobalt manganese polycrystalline composite precursor, nickel cobalt manganese monocrystalline composite precursor, nanometer Sm are weighed respectively2O3And lithium
Source;Wherein, nickel cobalt manganese polycrystalline composite precursor and nickel cobalt manganese monocrystalline composite precursor are the composite oxides, multiple of nickel, cobalt, manganese
At least one of hydroxide, compound oxyhydroxide are closed, nickel, cobalt, the mol ratio of manganese are Ni:Co:Mn=0.98:0.01:
0.008;The mass ratio of nickel cobalt manganese polycrystalline composite precursor and nickel cobalt manganese monocrystalline composite precursor is 10:1;
Step 2, by the nickel cobalt manganese monocrystalline composite precursor weighed in step 1 and nanometer Sm2O3Carry out ultra-high-speed mixing, system
Obtain the first mixture;The ultra-high-speed mixing uses ternary material ultrahigh speed blender, and the rotating speed of ultra-high-speed mixing is 10000r/
min;
Step 3, the nickel cobalt manganese polycrystalline compound precursor that will be weighed in obtained first mixture in step 2 and the step 1
Body and lithium source carry out mixed at high speed, and the second mixture is made;The lithium source is lithium carbonate or lithium hydroxide;The mixed at high speed is adopted
With ternary material high speed blender, the rotating speed of mixed at high speed is 5000r/min;
Step 4, obtained second mixture in step 3 is encased in porcelain boat at 835 DEG C it is calcined 16h, that is, samarium is made
The nickel cobalt manganese anode material for lithium-ion batteries of doping.
Above-mentioned anode material for lithium-ion batteries, metal lithium sheet are that negative pole assembles button cell progress discharge and recharge contrast test,
First discharge specific capacity can reach 201.5mAh/g under 0.5C multiplying powers, capability retention 97.1% after 100 charge and discharges circulation,
And common positive electrode first discharge specific capacity is 204.5mAh/g, capability retention 94.7% after 100 charge and discharges circulation.
Embodiment 3:
A kind of nickel cobalt manganese anode material for lithium-ion batteries of samarium doping, its molecular formula are LiaNixCoyMnzSmbO2, wherein, 1
≤a≤1.2;0.3≤x≤0.98;0.01≤y≤0.6;0.001≤z≤0.6;B is 4/3-a/3-x-y-z, 0.00001≤b
≤0.03。
A kind of molecular formula is Li1.06Ni0.35Co0.02Mn0.6Sm0.01O2Samarium doping nickel cobalt manganese lithium ion cell positive material
The preparation method of material, it comprises the following steps:
Step 1, nickel cobalt manganese polycrystalline composite precursor, nickel cobalt manganese monocrystalline composite precursor, nanometer Sm are weighed respectively2O3And lithium
Source;Wherein, nickel cobalt manganese polycrystalline composite precursor and nickel cobalt manganese monocrystalline composite precursor are the composite oxides, multiple of nickel, cobalt, manganese
At least one of hydroxide, compound oxyhydroxide are closed, nickel, cobalt, the mol ratio of manganese are Ni:Co:Mn=0.35:0.02:
0.6;The mass ratio of nickel cobalt manganese polycrystalline composite precursor and nickel cobalt manganese monocrystalline composite precursor is 20:1;
Step 2, by the nickel cobalt manganese monocrystalline composite precursor weighed in step 1 and nanometer Sm2O3Carry out ultra-high-speed mixing, system
Obtain the first mixture;The ultra-high-speed mixing uses ternary material ultrahigh speed blender, and the rotating speed of ultra-high-speed mixing is 20000r/
min;
Step 3, by obtained first mixture in step 2 and the nickel cobalt manganese polycrystalline composite precursor that is weighed in step 1 and
Lithium source carries out mixed at high speed, and the second mixture is made;Wherein, lithium source is lithium carbonate or lithium hydroxide;Mixed at high speed uses ternary
Material high speed blender, the rotating speed of mixed at high speed is 10000r/min;
Step 4, obtained second mixture in step 3 is encased in porcelain boat at 1200 DEG C it is calcined 6h, that is, samarium is made
The nickel cobalt manganese anode material for lithium-ion batteries of doping.
Above-mentioned anode material for lithium-ion batteries, metal lithium sheet are that negative pole assembles button cell progress discharge and recharge contrast test,
First discharge specific capacity can reach 153.5mAh/g under 0.5C multiplying powers, capability retention 98.8% after 100 charge and discharges circulation,
And common positive electrode first discharge specific capacity is 154mAh/g, capability retention 98.2% after 100 charge and discharges circulation.
The present invention is with nanometer Sm2O3Method solid phase mixing for Sm sources, and use mixed at high speed mixes Sm, this method
Simple to operation, Sm incorporation easily accurately controls, Sm sources being uniformly distributed beneficial to Sm of nano-scale;What the present invention used
Monocrystalline composite precursor is especially suitable for ultra-high-speed mixing, and monocrystalline composite precursor is solid, ultra-high-speed mixing when do not break up, together
Shi Danjing composite precursors can play a part of collision medium, and mixed nanometer element is fully broken up, then again with remaining
Conventional polycrystalline composite precursor carries out mixed at high speed, reaches more preferable mixed effect.
Claims (9)
1. the nickel cobalt manganese anode material for lithium-ion batteries of a kind of samarium doping, it is characterised in that its molecular formula is
LiaNixCoyMnzSmbO2, wherein, 1≤a≤1.2;0.3≤x≤0.98;0.01≤y≤0.6;0.001≤z≤0.6;B is 4/
3-a/3-x-y-z, 0.00001≤b≤0.03.
2. a kind of preparation method of the nickel cobalt manganese anode material for lithium-ion batteries of samarium doping as described in the appended claim 1, its feature
It is, it comprises the following steps:
Step 1, nickel cobalt manganese polycrystalline composite precursor, nickel cobalt manganese monocrystalline composite precursor, nanometer samarium source and lithium source are weighed respectively;
Step 2, the nickel cobalt manganese monocrystalline composite precursor weighed in the step 1 and nanometer samarium source are carried out to ultra-high-speed mixing, system
Obtain the first mixture;
Step 3, the nickel cobalt manganese polycrystalline compound precursor that will be weighed in obtained first mixture in the step 2 and the step 1
Body and lithium source carry out mixed at high speed, and the second mixture is made;
Step 4, obtained second mixture in the step 3 is encased in porcelain boat be calcined, that is, the nickel of samarium doping is made
Cobalt manganese anode material for lithium-ion batteries.
3. a kind of preparation method of the nickel cobalt manganese anode material for lithium-ion batteries of samarium doping according to claim 2, it is special
Sign is, in the step 1, the nickel cobalt manganese polycrystalline composite precursor and nickel cobalt manganese monocrystalline composite precursor are nickel, cobalt, manganese
Composite oxides, complex hydroxide, at least one of compound oxyhydroxide, wherein, nickel, cobalt, the mol ratio of manganese are
Ni:Co:Mn=0.3-0.98:0.01-0.6:0.001-0.6.
4. a kind of preparation method of the nickel cobalt manganese anode material for lithium-ion batteries of samarium doping according to claim 2, it is special
Sign is, in the step 1, the nanometer samarium source is the oxide or hydroxide of nanoscale samarium.
A kind of 5. preparation of the nickel cobalt manganese anode material for lithium-ion batteries of samarium doping according to any one of claim 2-4
Method, it is characterised in that in the step 1, the nickel cobalt manganese polycrystalline composite precursor and nickel cobalt manganese monocrystalline composite precursor
Mass ratio is 2-20:1.
A kind of 6. preparation of the nickel cobalt manganese anode material for lithium-ion batteries of samarium doping according to any one of claim 2-4
Method, it is characterised in that in the step 2, the ultra-high-speed mixing uses ternary material ultrahigh speed blender, ultra-high-speed mixing
Rotating speed be 5500-20000r/min.
A kind of 7. preparation of the nickel cobalt manganese anode material for lithium-ion batteries of samarium doping according to any one of claim 2-4
Method, it is characterised in that in the step 3, the lithium source is lithium carbonate or lithium hydroxide.
A kind of 8. preparation of the nickel cobalt manganese anode material for lithium-ion batteries of samarium doping according to any one of claim 2-4
Method, it is characterised in that in the step 3, the mixed at high speed uses ternary material high speed blender, the rotating speed of mixed at high speed
For 1000-10000r/min.
A kind of 9. preparation of the nickel cobalt manganese anode material for lithium-ion batteries of samarium doping according to any one of claim 2-4
Method, it is characterised in that described to be roasted in the step 4:6h-36h is calcined at 600 DEG C -1200 DEG C.
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CN113036115A (en) * | 2021-02-07 | 2021-06-25 | 东莞市创明电池技术有限公司 | Graded high-nickel ternary composite material, preparation method thereof and lithium secondary battery |
CN113113580A (en) * | 2021-03-12 | 2021-07-13 | 江门市力源电子有限公司 | Special high-rate high-capacity high-platform lithium ion battery for electronic cigarette |
CN113113580B (en) * | 2021-03-12 | 2022-06-07 | 江门市力源电子有限公司 | Special high-rate high-capacity high-platform lithium ion battery for electronic cigarette |
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