CN109360948A - The nickelic multicomponent material presoma of one type monocrystalline type - Google Patents
The nickelic multicomponent material presoma of one type monocrystalline type Download PDFInfo
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- CN109360948A CN109360948A CN201811059154.2A CN201811059154A CN109360948A CN 109360948 A CN109360948 A CN 109360948A CN 201811059154 A CN201811059154 A CN 201811059154A CN 109360948 A CN109360948 A CN 109360948A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
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- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
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- H—ELECTRICITY
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- 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
- H01M4/502—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese for non-aqueous cells
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
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- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
- H01M4/523—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron for non-aqueous cells
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- H—ELECTRICITY
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
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Abstract
The present invention provides the nickelic multicomponent material presomas of a type monocrystalline type, it is characterised in that: the chemical general formula of the presoma is Ni(1‑a‑b)CoaMnb(OH)2, wherein 1 > 1-a-b >=0.6,0.4 >=a >=0,1 >=b > 0.The nickelic multicomponent material presoma of class monocrystalline type of the present invention is started with from the microstructure of material, the growth for controlling presoma coprecipitation reaction early period by adding dispersing agent in reaction kettle bottom liquid, increase nucleation amount, it avoids generating common needle-shaped or dotted primary particle pattern presoma, using cellulose thickener in salting liquid, characteristic forms primary particle radially growth under lower ph at high speed simultaneously, ultimately forms sheet-like morphology structure.
Description
Technical field
The invention belongs to field of lithium ion battery, more particularly, to the nickelic multicomponent material presoma of a type monocrystalline type.
Background technique
Nickle cobalt lithium manganate polynary positive pole material (hereinafter referred to as polynary positive pole material) is a kind of novel high-capacity lithium-ion electric
Pond positive electrode, general nickel is main electroactive substance in multicomponent material, and cobalt can reduce material electrochemical and polarize and mention
Structural stability and thermal stability can be improved in high magnification, manganese, thus in nickel cobalt manganese the synergistic effect of two or three of element make it is polynary
Positive electrode have good structural stability and comprehensive electrochemical, security performance, cycle performance and in terms of
With some superiority, the material safety can be good, and price is relatively low, and good with the compatibility of electrolyte, cycle performance is excellent, because
This was used as vehicle mounted dynamic battery positive electrode gradually to be received by market in recent years.And with a series of new energy national in recent years
The issuing and implementation of source automobile policy, according to route map to the year two thousand twenty, power battery specific energy reach 300 watt-hours/kilogram, cost
Within 0.8 yuan/watt-hour, positive electrode corresponding to this target is exactly nickelic ternary.Also let us is seen for the success of tesla
High-nickel material is applied to completely may be implemented on vehicle mounted dynamic battery.
But the nickelic multicomponent material as power battery anode material still has some problems: (1) material is mostly
Secondary agglomeration ball, internal, external primary particle size is small and fault of construction is more, under the conditions of high voltage or larger current charge and discharge easily
Recurring structure collapses；(2) polynary positive pole material internal void is big, and volume energy density is low and internal particle is difficult to coat, and is filling
During discharge cycles, electrolyte is gradually immersed into porous anode material internal and interface side reaction occurs with electrolyte, causes material
Expect that structure is destroyed, metal cation dissolution is serious, eventually leads to circulation (especially high temperature circulation) performance and security performance decline.
(3) the secondary agglomeration structure of polynary positive pole material is easily crushed in battery anode slice preparation process, leads to the interior of material
Portion's particle is exposed, and interface side reaction and digestion of metallic ion aggravation cause battery capacity during high temperature circulation and substantially decay.
Researcher attempts to solve the above problems by preparation big crystal grain or large single crystal polynary positive pole material.Most techniques
By way of after carrying out ball mill crushing after by presoma and lithium salts dry mixed and preparing micron particles by high-temperature roasting
Prepare class single crystal grain, this preparation method is on 333 and 523 type ternary materials using commonplace.But due to the party
The maturing temperature that method uses is higher, and the serious high capacity characteristics for destroying high-nickel material are not applied for high-nickel material by high temperature
On.
Meanwhile nickelic multicomponent material has higher ph since rich nickel characteristic roasting rear surface residual lithium salt is more, continues
Water suction, has larger impact to homogenate technique.Most of manufacturer reduces high-nickel material surface by means such as washing or pickling
Lithium salts, studies have shown that washing can reduce high-nickel material cyclical stability and high rate performance, this is to power battery in this way to the longevity
Life and power-performance have the positive electrode of high request to be difficult to functionization.Meanwhile cladding and repeatedly roasting are carried out after washing again
Burning will increase extra cost.
Summary of the invention
In view of this, the present invention is directed to propose the nickelic multicomponent material presoma of a type monocrystalline type, drops without using washing
The high rate performance of material is improved while low surface residual lithium.
In order to achieve the above objectives, the technical scheme of the present invention is realized as follows:
The nickelic multicomponent material presoma of one type monocrystalline type, the chemical general formula of the presoma are Ni(1-a-b)CoaMnb(OH)2,
Wherein, 1 > 1-a-b >=0.6,0.4 >=a >=0,1 >=b > 0.
Further, the shape characteristic of the presoma are as follows: by the length of primary particle for 1-5um, with a thickness of 0.1-
Second particle of the granularity D50 that the flaky material of 0.5um is polymerized in 2-8um.
Further, the second particle surface is coated with M element oxide cladding layers；The M element be Zr, Nb or
One of Al.
Further, the presoma is made by the method included the following steps:
(1) additive A is added in the reaction kettle bottom liquid of nitrogen protection atmosphere；
(2) mixed solution of nickel-cobalt-manganese ternary salting liquid and additive B is added into reaction kettle, wherein nickel-cobalt-manganese ternary
In salting liquid the molar ratio of Ni, Co, Mn be 1-a-b:a:b, 1 > 1-a-b >=0.6,0.4 >=a >=0,1 >=b > 0, nickel cobalt manganese three
The mass ratio of first salting liquid and additive B is 1:(0.01%-0.1%), pH value is controlled by the aqueous slkali containing ammonium hydroxide and is carried out
Coprecipitation reaction；
(3) nitrate solution containing metal ion is added with the ammonium bicarbonate soln of same concentrations with identical speed simultaneously
Enter in reaction kettle, solidliquid mixture is obtained after reaction；
(4) solidliquid mixture in step (3) is separated by centrifugal filtration, is dried at 60-200 DEG C after washing to neutrality
Dry 4-10h, obtains the nickelic multicomponent material presoma of class monocrystalline type.
Further, the additive A in the step (1) is one of citric acid, sodium citrate or ethylene glycol or two
Kind or more mixture；The additive amount of additive A in the step (1) is the 0.05- of the reaction kettle bottom liquid quality
0.1%.
Further, the additive B in the step (2) is methylcellulose, hydroxypropyl methyl cellulose, carboxymethyl fibre
Tie up the mixture of one or more of plain sodium or hydroxyethyl cellulose.
Further, the pH value in the step (2) is 10.5-11.
Further, the metal ion in the step (3) is the combination of one or more of Zr, Nb, Al.
Further, the molar ratio of the metal ion and the total ion of nickel cobalt manganese is (0.05%-0.5%): 1.
The revolving speed of the reaction kettle is 500-1000rpm.
Compared with the existing technology, the nickelic multicomponent material presoma of class monocrystalline type of the present invention has the advantage that
(1) the nickelic multicomponent material presoma of class monocrystalline type of the present invention is started with from the microstructure of material, by
The growth that dispersing agent control presoma coprecipitation reaction early period is added in reaction kettle bottom liquid, increases nucleation amount, avoids generating common
Needle-shaped or dotted primary particle pattern presoma, at the same using cellulose thickener in salting liquid at high speed characteristic compared with
Primary particle is formed under low ph value radially to increase, and ultimately forms sheet-like morphology structure；The structure can at a lower temperature (750 DEG C)
The multicomponent material to form class monocrystalline shape characteristic is reacted with lithium salts.Regulated and controled by special appearance, reduces roasting monocrystal material
Maximum temperature avoids destruction of the high temperature to high-nickel material high capacity characteristics.After liquid phase method presoma cladding can reduce roasting
The surface residual lithium salts of material reduces the interfacial reaction of electrolyte and surface nickel ion, simultaneously because selected metal ion
The oxide cladding layers of formation can form ionic conductor material with lithium ion, can effectively improve the ion-conductance of material after roasting
It leads.And due to being arranged cladding process at presoma, the degree of being evenly coated can be improved, be not required to after being washed and being coated
After baking technique, can be effectively reduced process costs.
(2) the nickelic multicomponent material presoma of class monocrystalline type of the present invention has carried out element-specific cladding, covering material
Lithium ion conductor clad will be formed with residual lithium salt in mixed lithium roasting process, be mentioned while being coated to high-nickel material
The high ionic conductivity of material surface, improves the forthright again of material while reducing surface residual lithium without using washing
Energy.
(3) the nickelic multicomponent material presoma of class monocrystalline type of the present invention prepares sheet by special technology controlling and process
Shape primary particle polymerization second particle presoma, the presoma after being mixed with lithium salts can at a lower temperature (be less than etc.
In 780 DEG C) formed class monocrystalline pattern nickelic polynary positive pole material.It can be obtained simultaneously guaranteeing the advantage with monocrystalline pattern
Gram volume identical with second particle high-nickel material.
(4) preparation method of the nickelic multicomponent material presoma of class monocrystalline type of the present invention carries out presoma packet simultaneously
It covers, reduces the surface residual lithium salts of high-nickel material after roasting, reach and mix phase after lithium roasting is washed with other technique persursor materials
As residual lithium salt content.
(5) the nickelic multicomponent material presoma of class monocrystalline type of the present invention can make monocrystalline high-nickel material while have list
The high-pressure solid of brilliant material, high pressure resistant, low yield gas, high circulation and high-nickel material high capacity characteristics.
Detailed description of the invention
Fig. 1 be the embodiment of the present invention 1 described in the 811 nickelic multicomponent material presomas of type class monocrystalline type SEM figure (× 5,
000)；
Fig. 2 be the embodiment of the present invention 1 described in the 622 nickelic multicomponent material presomas of type class monocrystalline type SEM figure (× 1,
000)。
Specific embodiment
In addition to being defined, technical term used in following embodiment has universal with those skilled in the art of the invention
The identical meanings of understanding.Test reagent used in following embodiment is unless otherwise specified conventional biochemical reagent；It is described
Experimental method is unless otherwise specified conventional method.
Below with reference to examples and drawings, the present invention will be described in detail.
Embodiment 1
The nickelic multicomponent material presoma of one type monocrystalline type, the chemical formula of the presoma are Ni8.2Co1Mn0.8(OH)2。
The presoma is made by the method included the following steps:
(1) bottom 5L liquid and 5g sodium citrate are added in the reaction kettle bottom liquid of nitrogen protection atmosphere；
(2) the nickel-cobalt-manganese ternary salting liquid that configuration 20L concentration is 2M, nickel cobalt manganese molar ratio is 8.2:1:0.8, to reaction kettle
In in revolving speed 600rpm, configured nickel-cobalt-manganese ternary salting liquid is at the uniform velocity added with 1L/h rate and 35g methylcellulose stirs
To being completely dissolved, while the sodium hydroxide solution control pH value containing ammonium hydroxide is added 10.6 ± 0.02, until salting liquid is complete
It squeezes into entirely；
(3) the nitric acid niobium of 0.5M is added with 0.5M ammonium bicarbonate soln with phase same rate, until niobium ion and nickel cobalt manganese gold
Belong to when ion molar ratio is 0.5% and stops liquid feeding；
(4) solidliquid mixture is separated by centrifugal filtration, dries 4h at 120 DEG C after washing to neutrality, after sieving i.e.
The nickelic presoma of the 811 type class monocrystalline can be obtained.
As shown in Figure 1, material primary particle is 2-3um, thickness 0.5um or so sheet, second particle granularity D50 is
6.32um, particle surface have obvious coating.
Embodiment 2
The nickelic multicomponent material presoma of one type monocrystalline type, the chemical formula of the presoma are Ni6Co2Mn2(OH)2。
The presoma is made by the method included the following steps:
(1) bottom 5L liquid and 5g citric acid are added in the reaction kettle bottom liquid of nitrogen protection atmosphere；
(2) configuration 20L concentration be 2M nickel-cobalt-manganese ternary salting liquid, nickel cobalt manganese molar ratio be 6:2:2, into reaction kettle
Revolving speed 800rpm, configured nickel-cobalt-manganese ternary salting liquid is added at the uniform velocity with 1L/h rate and 35g methylcellulose is stirred to complete
Fully dissolved, while the sodium hydroxide solution control pH value containing ammonium hydroxide is added 10.95 ± 0.02, until salting liquid is beaten completely
Enter；
(3) zirconium nitrate of 0.5M is added with 0.5M ammonium bicarbonate soln with phase same rate, until zirconium ion and nickel cobalt manganese gold
Belong to when ion molar ratio is 0.3% and stops liquid feeding；
(4) solidliquid mixture is separated by centrifugal filtration, dries 4h at 120 DEG C after washing to neutrality, after sieving i.e.
The nickelic presoma of the 622 type class monocrystalline can be obtained.
Material primary particle is 1.5-3.5um, and thickness 0.5um or so sheet, second particle granularity D50 is 7.1um, particle
There is obvious coating on surface.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Within mind and principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (9)
1. the nickelic multicomponent material presoma of a type monocrystalline type, it is characterised in that: the chemical general formula of the presoma is Ni(1-a-b)
CoaMnb(OH)2, wherein 1 > 1-a-b >=0.6,0.4 >=a >=0,1 >=b > 0.
2. the nickelic multicomponent material presoma of class monocrystalline type according to claim 1, it is characterised in that: the presoma
Shape characteristic are as follows: by the length of primary particle be 1-5um, with a thickness of the granularity D50 that is polymerized of flaky material of 0.1-0.5um
In the second particle of 2-8um.
3. the nickelic multicomponent material presoma of class monocrystalline type according to claim 2, it is characterised in that: the second particle
Surface is coated with M element oxide cladding layers；The M element is one of Zr, Nb or Al.
4. the nickelic multicomponent material presoma of class monocrystalline type according to claim 1, it is characterised in that: the presoma by
The method included the following steps is made:
(1) additive A is added in the reaction kettle bottom liquid of nitrogen protection atmosphere；
(2) mixed solution of nickel-cobalt-manganese ternary salting liquid and additive B is added into reaction kettle, wherein nickel-cobalt-manganese ternary salt is molten
The molar ratio of Ni, Co, Mn are 1-a-b:a:b, 1 > 1-a-b >=0.6,0.4 >=a >=0,1 >=b > 0, nickel-cobalt-manganese ternary salt in liquid
The mass ratio of solution and additive B is 1:(0.01%-0.1%), it is coprecipitated that pH value progress is controlled by the aqueous slkali containing ammonium hydroxide
It forms sediment and reacts；
(3) nitrate solution containing metal ion is added with the ammonium bicarbonate soln of same concentrations with identical speed simultaneously anti-
It answers in kettle, solidliquid mixture is obtained after reaction；
(4) solidliquid mixture in step (3) is separated by centrifugal filtration, dries 4- at 60-200 DEG C after washing to neutrality
10h obtains the nickelic multicomponent material presoma of class monocrystalline type.
5. the nickelic multicomponent material presoma of class monocrystalline type according to claim 4, it is characterised in that: the step (1)
In additive A be one or more of citric acid, sodium citrate or ethylene glycol mixture；The step (1)
In additive A additive amount be the reaction kettle bottom liquid quality 0.05-0.1%.
6. the nickelic multicomponent material presoma of class monocrystalline type according to claim 4, it is characterised in that: the step (2)
In additive B be one of methylcellulose, hydroxypropyl methyl cellulose, sodium carboxymethylcellulose or hydroxyethyl cellulose
Or two or more mixture.
7. the nickelic multicomponent material presoma of class monocrystalline type according to claim 4, it is characterised in that: the step (2)
In pH value be 10.5-11.
8. the nickelic multicomponent material presoma of class monocrystalline type according to claim 4, it is characterised in that: the step (3)
In metal ion be one or more of Zr, Nb, Al combination.
9. the nickelic multicomponent material presoma of class monocrystalline type according to claim 8, it is characterised in that: the metal ion
Molar ratio with the total ion of nickel cobalt manganese is (0.05%-0.5%): 1.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112047397A (en) * | 2020-09-15 | 2020-12-08 | 天津市捷威动力工业有限公司 | High-power ternary material precursor and preparation method thereof |
| CN112054184A (en) * | 2020-09-15 | 2020-12-08 | 天津市捷威动力工业有限公司 | High-power multi-element material and preparation method thereof |
| CN114709413A (en) * | 2022-04-14 | 2022-07-05 | 远景动力技术(江苏)有限公司 | Ternary material and application thereof |
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| CN106505193A (en) * | 2017-01-12 | 2017-03-15 | 宁波金和锂电材料有限公司 | Monocrystalline nickel-cobalt lithium manganate cathode material and preparation method thereof and lithium ion battery |
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| CN114709413A (en) * | 2022-04-14 | 2022-07-05 | 远景动力技术(江苏)有限公司 | Ternary material and application thereof |
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