CN108039488A - Nickelic system's positive electrode and preparation method thereof of high power capacity, high temperature room temperature superior performance - Google Patents

Nickelic system's positive electrode and preparation method thereof of high power capacity, high temperature room temperature superior performance Download PDF

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Publication number
CN108039488A
CN108039488A CN201711129038.9A CN201711129038A CN108039488A CN 108039488 A CN108039488 A CN 108039488A CN 201711129038 A CN201711129038 A CN 201711129038A CN 108039488 A CN108039488 A CN 108039488A
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China
Prior art keywords
positive electrode
nickelic
room temperature
superior performance
power capacity
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CN201711129038.9A
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Inventor
张楠
张亚琳
王宁
吴飞
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Wulong Power (chongqing) Lithium Material Co Ltd
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Wulong Power (chongqing) Lithium Material Co Ltd
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Priority to CN201711129038.9A priority Critical patent/CN108039488A/en
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    • HELECTRICITY
    • H01BASIC ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of or comprising active material
    • H01M4/36Selection of substances as active materials, active masses, active liquids
    • H01M4/48Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/52Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
    • H01M4/525Selection 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
    • HELECTRICITY
    • H01BASIC ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00Secondary cells; Manufacture thereof
    • H01M10/05Accumulators with non-aqueous electrolyte
    • H01M10/052Li-accumulators
    • H01M10/0525Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • HELECTRICITY
    • H01BASIC ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of or comprising active material
    • H01M4/36Selection of substances as active materials, active masses, active liquids
    • H01M4/48Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/50Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
    • H01M4/505Selection 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
    • HELECTRICITY
    • H01BASIC ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of or comprising active material
    • H01M2004/021Physical characteristics, e.g. porosity, surface area
    • HELECTRICITY
    • H01BASIC ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of or comprising active material
    • H01M2004/026Electrodes composed of or comprising active material characterised by the polarity
    • H01M2004/028Positive electrodes
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10Energy storage using batteries

Abstract

The invention discloses a kind of high power capacity, nickelic system's positive electrode of high temperature room temperature superior performance, the granule content in the positive electrode below 7 μm of particle diameter is no more than 6.4%.A kind of preparation method of foregoing positive electrode is also disclosed, the nickelic system's positive electrode of chemical synthesis, the positive electrode after synthesis is classified using dry method mechanical formula grader so that the granule content after classification in product below 7 μm of particle diameter is no more than 6.4%.The high Ni systems positive electrode that the present invention obtains, can produce that cycle-index under capacity big, high temperature and room temperature is more, high performance rechargeable nonaqueous electrolytic battery, apply and meet the high power demand of electric car under various circumstances on electric car.

Description

Nickelic system's positive electrode and preparation method thereof of high power capacity, high temperature room temperature superior performance
Technical field
The invention belongs to the positive electrode technical field of rechargeable nonaqueous electrolytic battery, and in particular to a kind of high power capacity, height Nickelic system's positive electrode of warm room temperature superior performance and preparation method thereof.
Background technology
In recent years, because considering for environmental pollution, electric automobile is by exploitation and practical, in this feelings Under condition, possess that capacity is big, at the same room temperature and high-temperature behavior it is outstanding high Ni systems positive electrode it is of interest by everybody.
High Ni systems positive electrode refers to, ternary system (LiNi0.8Co0.1Mn0.1) and NCA (LiNi0.8Co0.15Al0.05) etc., The ratio of migration W metal accounts for more than 75% positive electrode.The product is crushed after common sintering process, is crushed While can be classified, or directly make product using with the pulverizer of grading function.The particle diameter of the product Size is as the product generally sold currently on the market, average grain diameter D50=9~13 μm or so.
The proportioning of Li somewhat changes a little, and the capacity and cycle performance that can all make product produce very big change.Ability If the scholar in domain thinks that if Li is uniformly mixed into each particle of positive electrode, the Li contents of little particle positive electrode should be Less than the positive electrode of bulky grain.Having document, (Kobe University Guan Ye times, Japanese crystallography can will 49,261-271 (1998)) report that the material of high Ni systems easily becomes the (Li of non-stoichiometric composition1-xNi1+xO2), particularly 700 DEG C of oxygen In gas atmosphere or less than 600 DEG C low temperature close when, positive electrode can be with Li0.996Ni1.004O2Or others Li1- xNi1+xO2The oxide solid solution of form together, if there is the crystallization of this scarce Li in high Ni based materials, can make capacity Decline very much, Li1-xNi1+xO2Capacity it is as shown in table 1 with the change of Li contents:
Table 1.Li1-xNi1+xO2Capacity with Li changes of contents
Li surpluses are for circulating the influence with capacity:If Li superfluous (rich lithium), W metal proportioning is particularly migrated It more than more than 1.2, will raise the internal resistance of material, under common charging voltage (4.2V), capacity can be lower.Li surpluses Particle is easily detected by electric current, so local voltage can be caused to raise, can aggravate positive electrode and electrolyte after voltage rise Side reaction so that circulation be deteriorated.For Li metals ratio more than 1.10, the Li into metal mesh will become more, Li with Ni into After row position exchanges, the Ni deviate from from metal mesh will enter Li layers, so that circulation declines.The influence of Li deficiencies:It is existing Having technology experiment to find no Li has the situation of deficiency, but the situation of the Li deficiencies if there is micron level can make capacity Decline with cycle-index.
The influence of 4 valency Ni:In terms of the price of migration metal, if Li becomes more, because Li is 1 valency, Ni Can be from Ni3+It is changed into Ni4+, the ratio of 4 valency Ni can raise.If 4 valency Ni are excessive when charging, due to jahnteller effects, Crystal structure can change, so that crystal structure becomes unstability, so that circulation is deteriorated, this is known in the field (the WD2014/061654 international patent application dates:On October 15th, 2013).For general knowledge, the positive electrode before charging The inside makes product just contain 4 valency Ni before charge, this influence also exists without 4 valency Ni, but due to the influence of rich lithium It is extended when charging, also, the reactivity of 4 valency Ni is very high, easily decomposes, so that it is anti-with electrolyte to release active oxygen Should, this namely side reaction, the internal resistance of battery can raise after generation side reaction, so as to cause bad shadow to capacity and circulation Ring, this is also knowledge well known in the art.
The content of the invention
Regarding the issue above, the present invention provides a kind of capacity is big, performance is superior at ambient and elevated temperatures Nickelic system's positive electrode and preparation method thereof.
The present invention solves the technical solution that its technical problem uses:
Nickelic system's positive electrode of a kind of high power capacity, high temperature room temperature superior performance, in the positive electrode below 7 μm of particle diameter Granule content be no more than 6.4%.
Nickelic system's positive electrode is ternary system or NCA.
Nickelic system's positive electrode is Li1+xNi1-y-z-pCoyMnzMpO2, wherein, -0.04≤x≤0.06,0≤y≤ At least one of 0.25,0≤z≤0.25,0≤p≤0.25, M Al, Zr, Ti, Mg, Bi, Sb, Mo, B, V.
Nickelic system's positive electrode is 811 or NCA.
A kind of preparation method of above-mentioned positive electrode, the nickelic system's positive electrode of chemical synthesis, to the cathode material after synthesis Material is classified using dry method mechanical formula grader so that the granule content after classification in product below 7 μm of particle diameter is no more than 6.4%.
The dry method mechanical formula grader is telecentricity separate type gas flow sizing machine.
The beneficial effects of the invention are as follows:The high Ni systems positive electrode that the present invention obtains, can produce capacity big, high temperature and Cycle-index is more under room temperature, high performance rechargeable nonaqueous electrolytic battery, applies and meets electric car in different rings on electric car High power demand under border.
Embodiment
With reference to embodiment, the invention will be further described, but not thereby limiting the invention.
The Li contents of the different average grain diameter positive electrodes of embodiment 1
Those skilled in the art know that the proportioning of Li somewhat changes a little, and the capacity and cycle performance that can all make product produce Very big change.What kind of distribution for lithium battery above all Li is, applicant is verified by testing as follows.
D50=10.5 μm is taken, Li contents are 7.4% 811 products, and the sample of different average grain diameters is obtained with grader, The Li contents of each sample are tested.After classification, the relation of D50 and Li weight contents is as shown in table 2 below, it is seen then that D50 Li contents higher in small material.
The Li contents of 2. 811 different-grain diameter material of table
D50(μm) Li contents (%)
0.3 15.1
3.6 11.3
5.1 10.5
7.3 8.02
9.5 7.8
10.3 7.4
11.0 7.3
12.5 7.2
Using same method, the sample of different average grain diameters is obtained to NCA sample classifications, then Li contents are carried out Test, it was found that the trend similar with 811 products.
As it can be seen that with this area scholar is thought in background technology theory on the contrary, finding small in industrial actual production Li contents in grain are of a relatively high rather than lower than the Li contents of bulky grain.This finds to be one for manufacturer A great discovery for having overturned general knowledge.
All the time, it is equally known that the micro mist in product can cause surface area to become larger, because the reason for surface-active, So that the side reaction rise of positive electrode and electrolyte.This is that everybody recognizes the general of micro mist, this reason is not examined Consider the factor of Li contents.But in the case of high Ni systems, from the point of view of situation about being described above, that cognition before is Insufficient.
The reason for presumption generation phenomenon, has very much, such as:Presoma and the particle diameter distribution of Li raw materials that factory uses, Mixed-precision, sintering condition etc..If raw material mixing is uneven, then the presoma of certain small particle is just easy to grow up For the product of rich lithium.In view of the actual temperature and atmosphere in sintering furnace, because the accumulation of powder material, part production Product are easy to the state in anoxic, so as to react incomplete, such part is just easy to produce because reacting incomplete institute The anoxic construction of formation, then the product of the part may become rich lithium and construct.In terms of actual classification experimental result:Totally become Gesture is that rich lithium structure is more readily formed in short grained positive electrode product.High Ni systems product due to containing Ni higher, and Ni with Co and Mn is compared to being easier deoxidation, so a reason of this to be also high Ni systems product be easier anoxic.
The synthesis of embodiment 2 811, NCA samples
In yield following 811 and NCA samples have been synthesized for the pilot scale line sintering furnace (RHK) of the 10.0t/ months.
First, 811 samples are synthesized, are operated in accordance with the following steps:
1) nickel sulfate, cobaltous sulfate, the manganese sulfate solution by concentration for 1.5mol/L, according to Ni:Co:Mn=80:10:10 ratios The aqueous solution of example mixing is put into reactive tank, and puts into the ammonia spirit of 5.0mol/L and the sodium hydroxide solution of 1.5mol/L.Instead Answer and be stirred inside groove using agitating paddle, it is 50 DEG C to keep liquid temperature, is protected using nitrogen, ammonia density exists in retention groove 0.4mol/L, PH=12.2.30 it is small when after liquid in accumulator tank, using filter centrifugal, filtered, then with 15 times Water is cleaned, dry after cleaning.
2) by obtained NiCoMn hydroxide powders and Lithium hydroxide monohydrate (8 μm) according to the proportioning of Li/Me=1.02 After being mixed, under oxygen atmosphere, 800 DEG C 15 sinters when small, is crushed after sintering, and it is Li to obtain composition1。 01Ni0.80Co0.10Mn0.10O2, average grain diameter (D50) is 9.9 μm.Hierarchical test is carried out using the sample.
2nd, NCA samples are synthesized, are operated in accordance with the following steps:
1) by the nickel sulfate that concentration is 1.5mol/L, cobalt sulfate solution, according to Ni:Co=84:16 ratios mix water-soluble Liquid is put into reactive tank, and puts into the ammonia spirit of 5.0mol/L and the sodium hydroxide solution of 1.5mol/L.Used inside reactive tank Agitating paddle is stirred, and it is 50 DEG C to keep liquid temperature, is protected using nitrogen, ammonia density is in 0.4mol/L, PH=11.7 in retention groove. 30 it is small when after liquid in accumulator tank, using filter centrifugal, filtered, then cleaned with 15 times of water, it is dry after cleaning It is dry.
2) the NiCo hydroxide powders that will be obtained, and the aluminium-hydroxide powder of 2.5 μm of average grain diameter, also have average grain diameter After being mixed for 8 μm of Lithium hydroxide monohydrates according to the proportioning of Li/Me=1.02, under oxygen atmosphere, 780 DEG C 15 is burnt when small Knot, sintering are crushed afterwards, and it is Li to obtain composition101Ni0.80Co0.15Al0.05O2, average grain diameter (D50) is 11.2 μm.Make Hierarchical test is carried out with the sample.
Embodiment 3NCA sample different-grain diameters size fractionation is tested
Using the stage division of dry method mechanical formula grader (telecentricity separate type gas flow sizing machine).
The NCA samples synthesized using embodiment 2 carry out different-grain diameter classification experiment, so as to investigate below target grain size Most suitable Cut size of the granule content below 6%.Set Cut size 2,3,6,7,8 μm, grader classification after To eliminate below target grain size in short grained product still containing the little particle below partial target particle diameter (because being not These little particles may be removed completely), the weight for measuring the remaining following particle of target grain size in the product after classification contains Amount, and its performance is tested, the results are shown in Table 3.
The performance test results after table 3.NCA sample different-grain diameters classification processing
Note:The soft-package battery that the battery of test is 1Ah, 1C/1C charge/discharges, 2.75~4.2V.
Tested more than, it is 7 μm to draw most suitable Cut size.
Embodiment 4 811, the test of NCA sample classifications
To embodiment 2 synthesize 811, NCA samples press grain diameter size fractionation, with 7 μm for boundary, be classified, divide After level, the positive electrode of particle different weight content below 7 μm of particle diameter is tested for the property, test result is as shown in table 4.
The performance test results after table 4. 811, the processing of NCA sample classifications
Note:Blank group represents not carry out classification processing.
Granule content below 7 μm of the particle diameter obtained using the present invention is no more than 6.4% high Ni systems positive electrode, Ke Yisheng Output capacity is big, cycle-index is more under high temperature and room temperature, high performance rechargeable nonaqueous electrolytic battery, and apply expires on electric car The high power demand of sufficient electric car under various circumstances.

Claims (6)

  1. A kind of 1. nickelic system's positive electrode of high power capacity, high temperature room temperature superior performance, it is characterised in that:Grain in the positive electrode Granule content below 7 μm of footpath is no more than 6.4%.
  2. 2. nickelic system's positive electrode of high power capacity according to claim 1, high temperature room temperature superior performance, it is characterised in that: Nickelic system's positive electrode is ternary system or NCA.
  3. 3. nickelic system's positive electrode of high power capacity according to claim 2, high temperature room temperature superior performance, it is characterised in that: Nickelic system's positive electrode is Li1+xNi1-y-z-pCoyMnzMpO2, wherein, -0.04≤x≤0.06,0≤y≤0.25,0≤z≤ At least one of 0.25,0≤p≤0.25, M Al, Zr, Ti, Mg, Bi, Sb, Mo, B, V.
  4. 4. nickelic system's positive electrode of high power capacity according to claim 3, high temperature room temperature superior performance, it is characterised in that: Nickelic system's positive electrode is 811 or NCA.
  5. A kind of 5. preparation method of Claims 1-4 any one of them positive electrode, it is characterised in that:Chemical synthesis is nickelic It is positive electrode, the positive electrode after synthesis is classified using dry method mechanical formula grader so that grain in product after classification Granule content below 7 μm of footpath is no more than 6.4%.
  6. 6. the preparation method of the positive electrode according to claim 5, it is characterised in that:The dry method mechanical formula point Level machine is telecentricity separate type gas flow sizing machine.
CN201711129038.9A 2017-11-15 2017-11-15 Nickelic system's positive electrode and preparation method thereof of high power capacity, high temperature room temperature superior performance Pending CN108039488A (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101118964A (en) * 2007-08-31 2008-02-06 深圳市贝特瑞新能源材料股份有限公司 Method for enhancing electrode material performance of lithium ion battery
CN101483265A (en) * 2009-01-13 2009-07-15 深圳市贝特瑞新能源材料股份有限公司 Metal oxide lithium ionic cell positive pole material and preparation thereof
CN101186290B (en) * 2007-12-11 2010-12-15 深圳市贝特瑞新能源材料股份有限公司 Anode material vanadium lithium phosphate and preparation method thereof
CN103066261A (en) * 2012-12-28 2013-04-24 龙能科技(苏州)有限公司 A synthesis method for a high-capacity and high-nickel multi-metal oxide cathode material
CN107342417A (en) * 2016-12-28 2017-11-10 杉杉能源(宁夏)有限公司 A kind of high ni-type precursor of nickel-cobalt-lithium-manganese-oxide with specific morphology and preparation method thereof

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101118964A (en) * 2007-08-31 2008-02-06 深圳市贝特瑞新能源材料股份有限公司 Method for enhancing electrode material performance of lithium ion battery
CN101186290B (en) * 2007-12-11 2010-12-15 深圳市贝特瑞新能源材料股份有限公司 Anode material vanadium lithium phosphate and preparation method thereof
CN101483265A (en) * 2009-01-13 2009-07-15 深圳市贝特瑞新能源材料股份有限公司 Metal oxide lithium ionic cell positive pole material and preparation thereof
CN103066261A (en) * 2012-12-28 2013-04-24 龙能科技(苏州)有限公司 A synthesis method for a high-capacity and high-nickel multi-metal oxide cathode material
CN107342417A (en) * 2016-12-28 2017-11-10 杉杉能源(宁夏)有限公司 A kind of high ni-type precursor of nickel-cobalt-lithium-manganese-oxide with specific morphology and preparation method thereof

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