CN109950498A - A kind of nickelic positive electrode and preparation method thereof with uniform clad - Google Patents
A kind of nickelic positive electrode and preparation method thereof with uniform clad Download PDFInfo
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Abstract
The invention discloses a kind of nickelic positive electrode and preparation method thereof with uniform clad, the preparation method include the following steps: that (1) is uniform by nickelic positive electrode and lithium source and nanometer covering material solid phase mixing, are sieved, obtain mixture；(2) step (1) described mixture is placed in saggar, high temperature sintering is carried out under the Muffle furnace oxygen atmosphere of preheating, it is cooling, it is crushed, sieving obtains the nickelic positive electrode with uniform clad.The present invention then adds additional lithium source by coating outside one layer of oxide cladding layers on nickelic positive electrode surface, obtains that stability is good by high temperature sintering, the high positive electrode of specific capacity.The present invention passes through solid phase mixing covering material, nickelic positive electrode and lithium source, easy to operate, low in cost, it is easy to accomplish large-scale production.
Description
Technical field
The present invention relates to technical field of lithium ion, and in particular to a kind of nickelic positive electrode with uniform clad
And preparation method thereof.
Background technique
In recent years, the energy has become the important bottleneck for restricting social progress and development.It is produced in national energy security, automobile
Under the backgrounds such as industry bend overtakes other vehicles, environmental protection, China's new energy related industry is rapidly flourished.Lithium ion battery due to
Have the characteristics that high working voltage, high-energy density and long-life and is used widely.Positive electrode directly determines lithium
The main performance of ion battery.Requirement with market to course continuation mileage and energy density is higher and higher, has at low cost, electric discharge
Stratiform high-nickel material (the LiNi for the advantages that capacity is big, energy density is highxMyO2, wherein 0.5≤x <, 1,0 < y < 0.5, x+y=
1, M is one or more kinds of metallic elements) have become most promising Olivine-type Cathode Material in Li-ion Batteries
One of.
But high-nickel material often has the shortcomings that cyclicity is poor, safety is low, thermal runaway thermal discharge is big.Meanwhile it is nickelic
Ternary material generally requires the lithium source (such as lithium hydroxide or lithium carbonate) of excessive addition, lamellar compound structure during the preparation process
In lithium be also easy abjection side reaction occur with water and carbon dioxide in air to generate remaining lithium hydroxide and lithium carbonate, increase
Material pH value destroys the structural stability of material and causes a series of problems of battery, as internal resistance increase, capacity attenuation are too fast
Deng.Therefore, a kind of long circulating is developed, the nickelic tertiary cathode material of high safety becomes more and more urgent task.
Chinese patent CN106960958A discloses a kind of positive electrode active materials covering liquid and preparation method thereof and anode
The method for coating of active material, the invention include solvent and the Phosphate coating predecessor that can be dissolved in the solvent, and feature exists
In the solvent includes at least alcohols solvent, which generates monophosphate Al by heat treatmentmMnPO4,
Middle M is the alkali earth metal or transiting group metal elements that one or more valence states are k, 1,0 n≤1 < 0≤m < and 3m+kn=
3；The invention further includes positive electrode active materials covering liquid, which is characterized in that for a kind of homogeneous clear solution, including phosphoric acid ester
Mixing of the compound of compound, aluminium salt and modifying element in alcohols solvent, or including in phosphoric acid and phosphorus pentoxide extremely
Mixing of the compound of a kind of few, aluminium salt and modifying element in alcohols solvent.The preparation method of positive electrode active materials covering liquid,
Include the following steps:
Phosphate compounds are added in S1 in alcohols solvent, obtain phosphate ester solution；And
The compound of aluminium salt and modifying element, the chemical combination of the aluminium salt and modifying element is added in S2 in the phosphate ester solution
Object is dissolved in the alcohols solvent, and reacts to obtain positive electrode active materials covering liquid with the phosphate compounds；
Positive electrode active materials are uniformly mixed with the positive electrode active materials covering liquid, obtain a solidliquid mixture by S3；And
S4 by solidliquid mixture drying and is sintered, obtains anode composite material, which includes that anode is living
Property material and the clad for being coated on the surface of positive electrode active material.
The method that solution is dried is obtained cladding active material by patent disclosure covering liquid liquid phase coating.This side
The clad that method obtains is smaller to the removal effect of the residual lithium in nickelic (nickel content >=50%) surface, and material in the solution for a long time
High temperature drying can generate certain destruction to structure, technology difficulty production is larger, needs to use larger amount of organic solvent, leads
Cost is caused to increase.
Application No. is the Chinese patents of CN108336348A to disclose a kind of alumina-coated anode material for lithium-ion batteries
Method.Aluminium hydroxide is dissolved in glacial acetic acid, colourless transparent solution is obtained, dehydrated alcohol dilution is then added into the solution；
Anode material for lithium-ion batteries is weighed, dehydrated alcohol is added, opens stirring；Two kinds of solution of above-mentioned gained are mixed；It heats and holds
Continuous stirring, until evaporating completely；It is dry, heat treatment.The invention method for coating using aluminium oxide to positive electrode into
Row cladding.But lithium abjection in layer structure easily occurs during Post isothermal treatment and occurs instead with aluminium oxide for such method
It answers, positive electrode activity lithium content is reduced, to reduce energy density.
Summary of the invention
The technical problem to be solved by the present invention is to overcome the technological deficiency of background technique, provide a kind of with uniformly cladding
The nickelic positive electrode and preparation method thereof of layer.The present invention is by coating one layer of oxide cladding layers on nickelic positive electrode surface
Outside, it then adds additional lithium source (lithium hydroxide or lithium carbonate), obtains that stability is good by high temperature sintering, the high anode of specific capacity
Material.The present invention passes through solid phase mixing covering material, nickelic positive electrode and lithium source, easy to operate, low in cost, it is easy to accomplish
Large-scale production.
It is as follows that the present invention solves technical solution used by above-mentioned technical problem:
A kind of preparation method of the nickelic positive electrode with uniform clad, includes the following steps:
(1) nickelic positive electrode and lithium source and nanometer covering material solid phase mixing is uniform, sieving obtains mixture；
(2) step (1) described mixture is placed in saggar, high temperature burning is carried out under the Muffle furnace oxygen atmosphere of preheating
Knot, it is cooling, it is crushed, sieving obtains the nickelic positive electrode with uniform clad；
In the step (1), the molecular formula of the nickelic positive electrode is LiNixMvO2, wherein 0.5≤x <, 1,0 < y <
0.5, x+y=1, the M are any one or a few in Co, Mn, Al, Ti, Mg；
In the step (1), the lithium source is lithium hydroxide or lithium carbonate；
In the step (1), the nanometer covering material is the compound that can be reacted with elemental lithium, including but not
It is limited to metal phosphate, metal sulfate, metal oxide, any one or a few in metal hydroxides, boron oxide；Institute
State metal phosphate and the metal oxide metal include but is not limited to Al, Zr, Mg, Ti, Mn, Ni, Sn, Co, Zn, Ca,
One or more of Sr, Ba, Y, V, Nb, Ce and La.
Preferably, in the step (1), the M is Co, Mn or the M is Co, Al.
It is highly preferred that the M is Co, Mn in the step (1).
Preferably, in the step (1), the nickelic positive electrode is LiNi0.88Co0.09Mn0.03O2Or
LiNi0.80Co0.10Mn0.10O2。
Preferably, in the step (1), the lithium source and the nanometer covering material are stoichiometrically just completely anti-
It answers.
Preferably, in the step (1), by molar amount, the additional amount of the nanometer covering material: the nickelic anode
The additional amount of material is 0.001~0.05.
Preferably, in the step (1), the nanometer covering material is nano aluminium oxide, nano zircite, nano oxidized
Any one or a few in gallium, nano indium oxide.
Preferably, in the step (2), concentration >=80% of the oxygen.
Preferably, in the step (2), the temperature of the sintering is 300~900 DEG C, the time of the sintering is 4~
15h。
It is highly preferred that the temperature of the sintering is 700 DEG C in the step (2), the time of the sintering is 10h.
A kind of nickelic positive electrode with uniform clad, is prepared using preparation method as described above.
Basic principle of the invention:
Since high temperature sintering will lead to the cladding compound and nickelic positive electrode surface residual on nickelic positive electrode surface
Lithium (lithium hydroxide or lithium carbonate) even crystals lithium reacts, and leads to the missing of active lithium, specific capacity is caused to reduce, and ties
The problems such as structure is undergone phase transition.
The present invention is by nickelic positive electrode (LiNixMyO2, wherein 0.5≤x < 1,0 < y < 0.5, x+y=1, M are one kind
Or more than one metallic element) with supplement lithium source (such as lithium hydroxide or lithium carbonate) and nanometer covering material is after mixing
It is placed in saggar, high temperature sintering, obtains the nickelic positive electrode of high capacity with uniform clad, uniform clad is also effective
Improve nickelic positive electrode cyclical stability.
For the present invention by additionally supplementing lithium source, the effective loss for alleviating lithium in crystal structure improves positive electrode
Structural stability improves the performances such as specific capacity.
Compared with prior art, the beneficial effects of the present invention are:
(1) present invention avoids crystal knot due to making covering material react with the lithium source additionally supplemented at high temperature
The excessive loss of lithium in structure improves specific capacity；
(2) material prepared by the present invention provides guarantor for the safety and stability of battery due to the stability of crystal structure
Barrier；
(3) present invention will form one layer of new lithium salts structure on active positive electrode material surface, guarantee material by high temperature sintering
Expect to improve lithium ion mobility rate while structural stability；
(4) present invention is uniform by simple solid phase mixing, reduces production cost and time.
Detailed description of the invention
Fig. 1 is the SEM figure of the nickelic positive electrode obtained with uniform clad of the embodiment of the present invention 1；
Fig. 2 is the height with (188.7mAh/g) before uniformly cladding (209.8mAh/g) afterwards obtained of the embodiment of the present invention 1
Button electricity specific volume spirogram of nickel positive electrode under the conditions of 0.2C/0.2C charge and discharge before and after cladding；
Fig. 3 is to have the nickelic positive electrode (online in figure) of uniform clad made from the embodiment of the present invention 2 and do not wrap
The powder conductivity rate performance map of the nickelic cell positive material (offline in figure) covered at various pressures；
Fig. 4 is the 1C/1C item before and after cladding of the nickelic positive electrode with uniform clad obtained of the embodiment of the present invention 3
Charge and discharge cycles situation map under part；
Fig. 5 is that the nickelic positive electrode obtained with uniform clad of the embodiment of the present invention 4 is rectangular complete before and after cladding
The comparison of battery direct current resistance numerical value；
Fig. 6 is that the 1C/1C before and after cladding of the nickelic positive electrode with uniform clad obtained of the embodiment of the present invention 5 fills
It discharges, the loop condition figure under the conditions of 45 DEG C.
Specific embodiment
In order to better understand the content of the present invention, it is described further combined with specific embodiments below with attached drawing.Ying Li
Solution, these embodiments are only used for that the present invention is further described, rather than limit the scope of the invention.In addition, it should also be understood that,
After having read content of the present invention, person skilled in art makes some nonessential changes or adjustment to the present invention,
Still fall within protection scope of the present invention.
Embodiment 1
By positive electrode active materials LiNi0.88Co0.09Mn0.03O21kg and nano aluminium oxide 2.89g, monohydrate lithium hydroxide
2.33g ball grinding stirring is uniform, and sieving is placed in saggar, (oxygen concentration >=80%) 560 under the Muffle furnace oxygen atmosphere of preheating
DEG C sintering reaction 6h.Slow cooling, broken sieving obtain the active substances in cathode materials with uniform clad.
Embodiment 2
By positive electrode active materials LiNi0.80Co0.10Mn0.10O21kg and nano zircite 3.49g, monohydrate lithium hydroxide
2.33g ball grinding stirring is uniform, and sieving is placed in saggar, (oxygen concentration >=80%) 720 under the Muffle furnace oxygen atmosphere of preheating
DEG C sintering reaction 7h.Slow cooling, broken sieving obtain the active substances in cathode materials with uniform clad.
Embodiment 3
By positive electrode active materials LiNi0.80Co0.10Mn0.10O21kg and Nanometer gallium oxide 5.31g, monohydrate lithium hydroxide
2.33g ball grinding stirring is uniform, and sieving is placed in saggar, (oxygen concentration >=80%) 500 under the Muffle furnace oxygen atmosphere of preheating
DEG C sintering reaction 4h.Slow cooling, broken sieving obtain the active substances in cathode materials with uniform clad.
Embodiment 4
By positive electrode active materials LiNi0.80Co0.10Mn0.10O21kg and nano indium oxide 7.87g, monohydrate lithium hydroxide
2.33g ball grinding stirring is uniform, and sieving is placed in saggar, (oxygen concentration >=80%) 600 under the Muffle furnace oxygen atmosphere of preheating
DEG C sintering reaction 5h.Slow cooling, broken sieving obtain the active substances in cathode materials with uniform clad.
Embodiment 5
By positive electrode active materials LiNi0.80Co0.10Mn0.10O21kg and nano indium oxide 7.87g, lithium carbonate 2.05g ball milling
It stirs evenly, is sieved, is placed in saggar, (oxygen concentration >=80%) 700 DEG C of sintering are anti-under the Muffle furnace oxygen atmosphere of preheating
Answer 10h.Slow cooling, broken sieving obtain the active substances in cathode materials with uniform clad.
Effect example
(1) preparation of button CR2032 battery:
Using the technical solution well known to those skilled in the art that positive electrode is prepared into lithium ion battery, by embodiment
Nickelic positive electrode obtained in 1~5 is assembled into button cell, method particularly includes: there is uniform clad just by obtained
Pole material, acetylene black and Kynoar (PVDF) are weighed by 94: 3: 3 mass ratioes, are uniformly mixed, and NMP is added and stirs 2h, at viscous
Thick shape slurry, is uniformly coated on aluminium foil, rear 80 DEG C of vacuum bakeouts, tabletting, cuts the positive plate that diameter is 14mm.With diameter
The pour lithium slice of 16mm is as negative electrode tab, with 1mol/L LiPF6+ DEC/EC (volume ratio 1: 1) mixed solution is electrolyte, with poly-
Celgard propylene microcellular film is diaphragm, carries out being assembled into button CR2032 battery in the glove box full of argon gas.
(2) preparation of rectangular aluminum-shell battery:
A certain amount of NMP is added after de-airing mixer is sufficiently stirred in conductive agent and binder according to a certain percentage, is added
Enter pre-dry positive electrode (anode: binder: conductive agent=94.5: 2.5: 3) to stir evenly completely (uniform, stable
Paste), uniformly coating is cut by roll-in after pole piece vacuum drying in current collector aluminum foil, pole piece is cut out after slurry sieving
At the small pole piece of 374 × 41mm, weld after aluminium strip tab and graphite cathode piece well prepared in advance, diaphragm (401 × 42mm) into
Row winding is assembled into battery core, battery core is fitted into the aluminum-shell battery of 053048 model, using laser-beam welding machine by nut cap and battery
Case weld is secured, and 80 DEG C of dryings of vacuum are not less than 4 hours progress fluid injection (LiF of 1mol/L6PO4), normal temperature environment soaks after fluid injection
Profit 24 hours upper cabinet partial volumes, then seal liquid injection hole using the stainless steel steel ball that diameter is 1.3mm.
As shown in Figure 1, can see apparent uniform coating in particle surface.
Positive electrode be prepared into the first discharge specific capacity of CR2032 half-cell as shown in Fig. 2, cladding after material specific capacity
209.8mAh/g is increased to by 188.7.
Positive electrode powder conductivity rate at various pressures is as shown in figure 3, it can be seen that powder after its material cladding
Conductivity is significantly improved, and is increased to the 0.094S/cm after cladding by 0.069 before coating at 20kN.
As shown in figure 4, positive electrode cladding front and back is in 1C/1C charge and discharge cycles situation, it can be seen that hold after 300 circle circulations
Amount keeps obviously increasing to 93.0% after coating from 91.3% before cladding.
As shown in figure 5, prepared positive electrode, which does after squarely full battery DCR, is reduced to cladding by 35.6 before coating
27.1m Ω afterwards.
As shown in fig. 6, loop condition of the positive electrode cladding front and back at 45 DEG C of 1C/1C charge and discharge, it can be seen that 300 circles
Capacity keeps obviously increasing to 90.9% after coating from 89.0% before cladding after circulation.
The present invention is by supplementing lithium source and and lithium to the anode material for lithium-ion batteries such as nickle cobalt lithium manganate or nickel cobalt lithium aluminate
The covering material dry mixed sintering that source reacts, it is excellent big with specific capacity to prepare the cycle performance with special clad
Nickelic positive electrode, specifically:
(1) present invention reacts by additionally supplementing lithium source (lithium hydroxide or lithium carbonate) and coating and reduces structurally live
The missing of property lithium, increases the specific discharge capacity and stability of nickelic positive electrode；
(2) present invention can reduce nickelic positive electrode surface lithium hydroxide and lithium carbonate and pH without washing；
(3) present invention is by physical mixed, and cost is relatively low, easy to operate, is easy to industrialization large-scale production；
(4) present invention inhibits nickelic positive electrode because the structure collapses that active lithium missing occurs, improve nickelic anode
Structural stability of material during charge and discharge cycles, also improves the cycle performance of nickelic positive electrode.
Above description is not limitation of the present invention, and the present invention is also not limited to the example above.The art it is common
Within the essential scope of the present invention, the variations, modifications, additions or substitutions made also should belong to protection of the invention to technical staff
Range.
Claims (9)
1. a kind of preparation method of the nickelic positive electrode with uniform clad, which comprises the steps of:
(1) nickelic positive electrode and lithium source and nanometer covering material solid phase mixing is uniform, sieving obtains mixture；
(2) step (1) described mixture is placed in saggar, high temperature sintering is carried out under the Muffle furnace oxygen atmosphere of preheating, it is cold
But, it is crushed, sieving obtains the nickelic positive electrode with uniform clad；
In the step (1), the molecular formula of the nickelic positive electrode is LiNixMyO2, wherein 0.5≤x <, 1,0 < y < 0.5,
X+y=1, the M are any one or a few in Co, Mn, Al, Ti, Mg；
In the step (1), the lithium source is lithium hydroxide or lithium carbonate；
In the step (1), the nanometer covering material is the compound that can be reacted with elemental lithium, including but not limited to
Metal phosphate, metal sulfate, metal oxide, any one or a few in metal hydroxides, boron oxide；The gold
Belong to phosphate and the metal oxide metal include but is not limited to Al, Zr, Mg, Ti, Mn, Ni, Sn, Co, Zn, Ca, Sr,
One or more of Ba, Y, V, Nb, Ce and La.
2. a kind of preparation method of the nickelic positive electrode with uniform clad as described in claim 1, which is characterized in that
In the step (1), the M is Co, Mn or the M is Co, Al.
3. a kind of preparation method of the nickelic positive electrode with uniform clad as described in claim 1, which is characterized in that
In the step (1), the nickelic positive electrode is LiNi0.88Co0.09Mn0.03O2Or LiNi0.80Co0.10Mn0.10O2。
4. a kind of preparation method of the nickelic positive electrode with uniform clad as described in claim 1, which is characterized in that
In the step (1), the lithium source is stoichiometrically reacted completely just with the nanometer covering material.
5. a kind of preparation method of the nickelic positive electrode with uniform clad as described in claim 1, which is characterized in that
In the step (1), by molar amount, the additional amount of the nanometer covering material: the additional amount of the nickelic positive electrode is
0.001~0.05.
6. a kind of preparation method of the nickelic positive electrode with uniform clad as described in claim 1, which is characterized in that
In the step (1), the nanometer covering material is nano aluminium oxide, in nano zircite, Nanometer gallium oxide, nano indium oxide
Any one or a few.
7. a kind of preparation method of the nickelic positive electrode with uniform clad as described in claim 1, which is characterized in that
In the step (2), concentration >=80% of the oxygen.
8. a kind of preparation method of the nickelic positive electrode with uniform clad as described in claim 1, which is characterized in that
In the step (2), the temperature of the sintering is 300~900 DEG C, and the time of the sintering is 4~15h.
9. a kind of nickelic positive electrode with uniform clad, which is characterized in that using as claim 1~8 any one
The preparation method is prepared.
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| CN110844945A (en) * | 2019-11-07 | 2020-02-28 | 昆山宝创新能源科技有限公司 | High-nickel ternary cathode material and preparation method and application thereof |
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| CN110844945A (en) * | 2019-11-07 | 2020-02-28 | 昆山宝创新能源科技有限公司 | High-nickel ternary cathode material and preparation method and application thereof |
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| CN111434618A (en) * | 2020-01-17 | 2020-07-21 | 蜂巢能源科技有限公司 | Cobalt-free layered positive electrode material, preparation method and lithium ion battery |
| CN111799465A (en) * | 2020-04-21 | 2020-10-20 | 广西大学 | Composite coating method for manganese-based lithium battery electrode material |
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| CN111769288B (en) * | 2020-08-13 | 2022-05-03 | 哈尔滨工业大学 | Method for in-situ lithium supplement of lithium ion battery anode material |
| CN112490444A (en) * | 2020-10-27 | 2021-03-12 | 北京泰丰先行新能源科技有限公司 | Lithium ion secondary battery positive electrode material and preparation method thereof |
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| CN114560511A (en) * | 2022-01-26 | 2022-05-31 | 泾河新城陕煤技术研究院新能源材料有限公司 | High-nickel cathode material with high cycle stability and preparation method thereof |
| CN114899376A (en) * | 2022-05-11 | 2022-08-12 | 井冈山大学 | Lithium aluminum phosphate fluoride-coated positive electrode material and preparation method thereof |
| CN116332146A (en) * | 2023-03-10 | 2023-06-27 | 无锡晶石新型能源股份有限公司 | Method for improving specific surface of lithium iron manganese phosphate by fusion cladding method |
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Address after: Jia Ling Road 315400 Yuyao City, Zhejiang province Ningbo City No. 39 Applicant after: Ningbo new energy Polytron Technologies Inc Address before: 315400 Cao'e Village, Xiaocao'e Town, Yuyao City, Ningbo City, Zhejiang Province Applicant before: Ningbo new energy Polytron Technologies Inc |
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Application publication date: 20190628 |