CN110518209A - Method for preparing anode material and the positive electrode of preparation - Google Patents
Method for preparing anode material and the positive electrode of preparation Download PDFInfo
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- CN110518209A CN110518209A CN201910798461.0A CN201910798461A CN110518209A CN 110518209 A CN110518209 A CN 110518209A CN 201910798461 A CN201910798461 A CN 201910798461A CN 110518209 A CN110518209 A CN 110518209A
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- lithium
- cobalt
- anode material
- preparing anode
- nickel
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- 238000000034 method Methods 0.000 title claims abstract description 51
- 239000010405 anode material Substances 0.000 title claims abstract description 36
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 239000000463 material Substances 0.000 claims abstract description 81
- KFDQGLPGKXUTMZ-UHFFFAOYSA-N [Mn].[Co].[Ni] Chemical compound [Mn].[Co].[Ni] KFDQGLPGKXUTMZ-UHFFFAOYSA-N 0.000 claims abstract description 56
- 229910000480 nickel oxide Inorganic materials 0.000 claims abstract description 49
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 claims abstract description 37
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 30
- 229910017052 cobalt Inorganic materials 0.000 claims abstract description 29
- 239000010941 cobalt Substances 0.000 claims abstract description 29
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims abstract description 29
- 229910052744 lithium Inorganic materials 0.000 claims abstract description 29
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims abstract description 25
- 239000002243 precursor Substances 0.000 claims abstract description 25
- 238000005245 sintering Methods 0.000 claims abstract description 23
- 229910052787 antimony Inorganic materials 0.000 claims abstract description 20
- 229910052749 magnesium Inorganic materials 0.000 claims abstract description 20
- 238000012545 processing Methods 0.000 claims abstract description 18
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 16
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 claims abstract description 16
- 230000008569 process Effects 0.000 claims abstract description 15
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 14
- 229910052726 zirconium Inorganic materials 0.000 claims abstract description 14
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000000126 substance Substances 0.000 claims abstract description 7
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 claims description 24
- 229910052808 lithium carbonate Inorganic materials 0.000 claims description 24
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 claims description 21
- 239000000843 powder Substances 0.000 claims description 12
- 239000011572 manganese Substances 0.000 claims description 11
- PQXKHYXIUOZZFA-UHFFFAOYSA-M lithium fluoride Chemical compound [Li+].[F-] PQXKHYXIUOZZFA-UHFFFAOYSA-M 0.000 claims description 10
- 238000012216 screening Methods 0.000 claims description 8
- 229910021503 Cobalt(II) hydroxide Inorganic materials 0.000 claims description 5
- 230000037396 body weight Effects 0.000 claims description 5
- ASKVAEGIVYSGNY-UHFFFAOYSA-L cobalt(ii) hydroxide Chemical compound [OH-].[OH-].[Co+2] ASKVAEGIVYSGNY-UHFFFAOYSA-L 0.000 claims description 5
- SAXCKUIOAKKRAS-UHFFFAOYSA-N cobalt;hydrate Chemical compound O.[Co] SAXCKUIOAKKRAS-UHFFFAOYSA-N 0.000 claims description 5
- XIXADJRWDQXREU-UHFFFAOYSA-M lithium acetate Chemical compound [Li+].CC([O-])=O XIXADJRWDQXREU-UHFFFAOYSA-M 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 3
- 230000003647 oxidation Effects 0.000 claims description 3
- 238000007254 oxidation reaction Methods 0.000 claims description 3
- 235000013495 cobalt Nutrition 0.000 claims 4
- 229910001416 lithium ion Inorganic materials 0.000 abstract description 10
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 abstract description 9
- 230000008901 benefit Effects 0.000 abstract description 4
- 230000008961 swelling Effects 0.000 abstract description 4
- 238000001816 cooling Methods 0.000 description 25
- 239000004615 ingredient Substances 0.000 description 24
- UBEWDCMIDFGDOO-UHFFFAOYSA-N cobalt(2+);cobalt(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[Co+2].[Co+3].[Co+3] UBEWDCMIDFGDOO-UHFFFAOYSA-N 0.000 description 22
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 20
- 239000002994 raw material Substances 0.000 description 18
- 238000000498 ball milling Methods 0.000 description 13
- 230000000052 comparative effect Effects 0.000 description 12
- NIPNSKYNPDTRPC-UHFFFAOYSA-N N-[2-oxo-2-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 NIPNSKYNPDTRPC-UHFFFAOYSA-N 0.000 description 4
- 239000002253 acid Substances 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 238000009831 deintercalation Methods 0.000 description 3
- 230000005611 electricity Effects 0.000 description 3
- 229910052759 nickel Inorganic materials 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000005253 cladding Methods 0.000 description 2
- 239000002019 doping agent Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000003780 insertion Methods 0.000 description 2
- 230000037431 insertion Effects 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000003672 processing method Methods 0.000 description 2
- 201000009032 substance abuse Diseases 0.000 description 2
- 229910052727 yttrium Inorganic materials 0.000 description 2
- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- PNEFIWYZWIQKEK-UHFFFAOYSA-N carbonic acid;lithium Chemical compound [Li].OC(O)=O PNEFIWYZWIQKEK-UHFFFAOYSA-N 0.000 description 1
- 238000005056 compaction Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 229910052733 gallium Inorganic materials 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 229910000625 lithium cobalt oxide Inorganic materials 0.000 description 1
- BFZPBUKRYWOWDV-UHFFFAOYSA-N lithium;oxido(oxo)cobalt Chemical compound [Li+].[O-][Co]=O BFZPBUKRYWOWDV-UHFFFAOYSA-N 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- 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
- H01M4/366—Composites as layered products
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—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
- H01M4/525—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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- 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
-
- Y—GENERAL 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The present invention provides a kind of method for preparing anode material, include the following steps: that the first lithium source and the cobalt source of doping are made A through mixed processing, sintering processes and expected by A.；B. B material is made through mixed processing, sintering processes in the second lithium source, nickel manganese cobalt ternary precursor and nickel oxide；C. by A material, B material and covering through mixed processing, sintering processes；Wherein, the doped chemical for adulterating the cobalt source includes at least one of Mg, Al, Ti and Zr and Sb, and covering includes at least one of aluminium oxide, lanthana and yttrium oxide and nickel oxide.The positive electrode of method for preparing anode material preparation of the present invention has many advantages, such as that specific capacity height, good cycle, high-temperature storage thickness swelling are small and energy density is high, is able to satisfy the demand in the market to high capacity high performance lithium ion battery positive electrode.
Description
Technical field
The present invention relates to positive electrode preparation technical field more particularly to a kind of method for preparing anode material and its preparations
Positive electrode.
Background technique
Lithium ion battery has obtained in the small portables electric appliance such as laptop, mobile phone, Video Camera extensively
Using, and various 3C electronic products develop to more lightening direction, the update of 3C Product is more and more frequent, and exploitation energy is close
Du Genggao, cycle performance are more preferable, the lower anode material for lithium-ion batteries of cost becomes the target that lithium electricity industry is mutually chased unexpectedly.
Anode material for lithium ion battery plays a decisive role to lithium ion battery overall performance, cost performance.3C class electricity at present
The positive electrode that pond product uses also has still based on high voltage lithium cobalt oxide anode using high voltage ternary material substitution portion
Divide the blended anode material of high voltage cobalt acid lithium material.But with the raising of charge cutoff voltage, when charging in positive electrode
A large amount of abjection Li+Afterwards, the layer structure that will lead to positive electrode is collapsed, so that the cycle performance of material be made to deteriorate.In view of existing
The problems such as layer structure for having positive electrode to occur easily is collapsed, and cycle performance deteriorates, need to develop a kind of high performance lithium from
Sub- positive electrode for battery material.
Summary of the invention
The purpose of the present invention is to provide a kind of method for preparing anode material and the positive electrode of preparation, with overcome it is existing just
The problems such as layer structure that the lithium battery of pole material preparation occurs easily is collapsed, and cycle performance deteriorates.
Technical scheme is as follows:
The present invention provides a kind of method for preparing anode material, includes the following steps:
A. A is made through mixed processing, sintering processes in the first lithium source and the cobalt source of doping to expect；
B. B material is made through mixed processing, sintering processes in the second lithium source, nickel manganese cobalt ternary precursor and nickel oxide；
C. A material, B material and covering are subjected to mixed processing, sintering processes；
Wherein, the doped chemical for adulterating the cobalt source includes at least one of Mg, Al, Ti and Zr and Sb, covering packet
Include at least one of aluminium oxide, lanthana and yttrium oxide and nickel oxide.
The present invention also provides a kind of positive electrodes prepared using above-mentioned method for preparing anode material.
Method for preparing anode material of the present invention, in step A, using Mg, Al, Ti or Zr be at least one and the cobalt of Sb doping
Source, this doping enable doped chemical to be preferably distributed in cobalt source, thus can be more uniformly when synthesizing cobalt acid lithium
It is distributed in cobalt acid lithium crystal structure, the cobalt acid lithium material stratiform structure sheaf spacing after doping increases, and is conducive to the embedding of lithium ion
Enter/deintercalation, improve the diffusion coefficient of lithium ion in the material, is conducive to the specific discharge capacity for improving material；And make cobalt
Structural stability of sour lithium material during lithium ion insertion/deintercalation increases, so that the security performance of material and long-term circulation
Performance is effectively improved；In step B, nickel oxide is added, carries out Ni element bulk phase-doped, can not only promote material
Specific capacity, and can suitably improve material impedance, Ni enters Li layers and also functions to supporting role, it is more advantageous to deintercalation/insertion of Li,
Promote cycle performance；In step C, nickel oxide is added and carries out surface cladding, can react with the extra lithium of material surface to drop
The alkalinity of low material surface, Al, Ga or Y element, which is added, can prevent the structure collapses under high-voltage case, improve cycle performance.
In the method for preparing anode material, addition in Y-oxides doping in cobalt source doping, step B and step C is coated in step A
Agent, these three processing methods cooperate, and dopant and covering mutually promote, play a role jointly, the positive material of preparation
Material has many advantages, such as that specific capacity height, good cycle, high-temperature storage thickness swelling are small and energy density is high, is able to satisfy in the market
Demand to high capacity high performance lithium ion battery positive electrode.
Specific embodiment
The present invention provides the positive electrode of a kind of method for preparing anode material and its preparation, below to positive electrode preparation side
Method and its positive electrode of preparation be relatively described in detail.
A kind of method for preparing anode material, includes the following steps:
A. A is made through mixed processing, sintering processes in the first lithium source and the cobalt source of doping to expect；
B. B material is made through mixed processing, sintering processes in the second lithium source, nickel manganese cobalt ternary precursor and nickel oxide；
C. by A material, B material and covering through mixed processing, sintering processes；
Wherein, the doped chemical for adulterating cobalt source includes at least one of Mg, Al, Ti and Zr and Sb, and covering includes oxygen
Change at least one of aluminium, lanthana and yttrium oxide and nickel oxide.
It should be noted that step A and step B have no successive point, being doped to cobalt source be can be doped chemical
Mixed with cobalt source, be sintered 1-2h at 750-920 DEG C after ball milling, adulterate cobalt source doped chemical can be Mg and Sb, Al and Sb,
Ti and Sb, Zr and Sb or Mg, Al, Ti and Sb, covering can be aluminium oxide and nickel oxide, lanthana and nickel oxide, oxidation
Yttrium and nickel oxide or aluminium oxide, lanthana and nickel oxide, in nickel manganese cobalt ternary precursor the ratio of nickel manganese cobalt can be 424,
333,523,701 or 515.
Preferably, further include in step A by A feed powder mill handle be made partial size D50 be 10-25 μm；Further include in step B by
It is 3-8 μm that B feed powder mill, which handles and partial size D50 is made,.It is mixed in a certain ratio using the A material of larger particles and the B material of smaller particle,
The pole piece compaction density of positive electrode not only can be improved, but also the advantage of the two can be protruded, show material higher
Specific capacity, better cycle performance, lower cost.Specifically, it can be 10 μm, 15 μm that A feed powder mill, which handles and partial size D50 is made,
With 25 μm, B feed powder mill handle be made partial size D50 can be 3 μm, 4 μm and 8 μm.
Preferably, in step A, cobalt source include but is not limited to one of cobaltosic oxide, hydroxyl cobalt and cobalt hydroxide or
The molar ratio of a variety of mixtures, Li and Co are 1.03-1.2, and sintering temperature is 950-1100 DEG C.Cobalt source is preferably four oxidations three
One of cobalt, hydroxyl cobalt and cobalt hydroxide or a variety of mixtures, but the selection of cobalt source is not limited to these raw materials.Specifically,
The molar ratio of Li and Co can be 1.03,1.07 or 1.2, and sintering temperature can be 950 DEG C, 1000 DEG C or 1100 DEG C.
Preferably, the doping of Sb is the 0.02-0.5% of the molal quantity of Co in step A, one in Mg, Al, Ti and Zr
The 0.02-0.5% for the molal quantity that kind or a variety of dopings are Co.Specifically, the doping of Sb is the molal quantity of Co
0.02%, 0.2%, 0.3% or 0.5%, one of Mg, Al, Ti and Zr or a variety of dopings are the molal quantity of Co
0.02%, 0.2%, 0.3% or 0.5%.
Preferably, Li: the molar ratio of (Ni+Co+Mn) is 1.03-1.2, and nickel oxide accounts for nickel-cobalt-manganese ternary forerunner in step B
The 3-7% of body weight.The preferred nanoscale of nickel oxide, specifically, Li: the molar ratio of (Ni+Co+Mn) can for 1.03,1.1 or
1.2, nickel oxide accounts for 3%, 4%, the 7% of nickel-cobalt-manganese ternary forerunner's body weight.
Preferably, the weight ratio of A material and B material is (60-90): (40-10), sintering temperature 800- in step C
950℃.Specifically, the weight ratio of A material and B material can be 60:40,90:10,90:40 or 60:10 etc., and sintering temperature can
Think 800 DEG C, 880 DEG C or 950 DEG C
Preferably, the weight ratio of covering and A material is 0.05-1% in step C, sintering temperature is 850-950 DEG C.Specifically
The weight ratio of ground, covering and A material can be 0.05%, 0.8% or 1%, and sintering temperature can be 850 DEG C, 900 DEG C or 950
℃。
Preferably, the first lithium source is selected from one of lithium carbonate, lithium fluoride, lithium hydroxide, lithium acetate or a variety of, the second lithium
Source is selected from one of lithium carbonate, lithium fluoride, lithium hydroxide, lithium acetate or a variety of.The selection of first lithium source and the second lithium source can
Be it is identical be also possible to difference, the selection of the first lithium source and the second lithium source is not limited to these raw materials.
Preferably, step C processing further includes crushing and screening processing.
It is a kind of according to positive electrode prepared by above-mentioned method for preparing anode material.
To make the purpose of the present invention, technical solution and effect clearer, clear and definite, referring to embodiment to the present invention into
One step is described in detail.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, it is not used to limit this
Invention.
Embodiment 1
A kind of method for preparing anode material, includes the following steps:
A. A material will be made through mixed processing, sintering processes with lithium carbonate after Sb and Zr doped cobaltic-cobaltous oxide；
B. B material is made through mixed processing, sintering processes in lithium carbonate, nickel manganese cobalt ternary precursor and nickel oxide；
C. by A material, B material, yttrium oxide and nickel oxide mixed processing, sintering processes.
Embodiment 2
A kind of method for preparing anode material, includes the following steps:
A. it will be uniformly mixed after Sb and Mg doped cobaltic-cobaltous oxide with lithium carbonate, be sintered 2h, ball after cooling at 1030 DEG C
The A that partial size D50 is 25 μm is worn into expect；
B. lithium carbonate, nickel manganese cobalt (523) ternary precursor and nano-nickel oxide are uniformly mixed, are sintered at 900 DEG C
10h, ball milling is expected at the B that partial size D50 is 8 μm after cooling；
C. A material, B material, nickel oxide and aluminium oxide are uniformly mixed, 900 DEG C at a temperature of keep the temperature 8 hours, it is cooling after powder
Broken screening；
Wherein, in step A, the doping of Sb and Mg are respectively 0.1% and 0.15%, cobaltosic oxide of the molal quantity of Co
Raw material is 1.05 progress ingredients according to Li: Co molar ratio；In step B, lithium carbonate, nickel cobalt manganese (523) ternary precursor, nano oxygen
Change nickel raw material according to Li: (Ni+Co+Mn) molar ratio is 1.05 progress ingredients, and wherein the weight of nickel oxide accounts for nickel cobalt manganese (523) three
The 5% of first forerunner's body weight；In step C, the weight ratio of A material and B material is 80:20 ingredient, and the weight ratio that covering and A expect is
1%.
Embodiment 3
A kind of method for preparing anode material, includes the following steps:
A. it will be uniformly mixed after Sb, Al and Mg doping hydroxyl cobalt with lithium hydroxide, be sintered 2.5h at 950 DEG C, after cooling
Ball milling is expected at the A that partial size D50 is 20 μm；
B. lithium hydroxide, nickel manganese cobalt (523) ternary precursor and nano-nickel oxide are uniformly mixed, are sintered at 900 DEG C
10h, ball milling is expected at the B that partial size D50 is 5 μm after cooling；
C. A material, B material, nickel oxide and aluminium oxide are uniformly mixed, 950 DEG C at a temperature of keep the temperature 6 hours, it is cooling after powder
Broken screening；
Wherein, in step A, the doping of Sb is the molal quantity that the doping of 0.5%, the Al and Mg of the molal quantity of Co are Co
0.5%, hydroxyl cobalt raw material according to Li: Co molar ratio be 1.2 carry out ingredients；In step B, lithium hydroxide, nickel cobalt manganese (523) three
First presoma, nano-nickel oxide raw material are according to Li: (Ni+Co+Mn) molar ratio is 1.2 progress ingredients, wherein the weight of nickel oxide
Account for the 7% of nickel cobalt manganese (523) ternary precursor weight；In step C, A material with B material weight ratio be 90:10 ingredient, covering and
The weight ratio of A material is 0.05%.
Embodiment 4
A kind of method for preparing anode material, includes the following steps:
A. it will be uniformly mixed after Sb and Zr doped cobaltic-cobaltous oxide with lithium carbonate, be sintered 2h, ball after cooling at 1000 DEG C
The A that partial size D50 is 20 μm is worn into expect；
B. lithium carbonate, nickel manganese cobalt (523) ternary precursor and nano-nickel oxide are uniformly mixed, are sintered at 900 DEG C
10h, ball milling is expected at the B that partial size D50 is 5 μm after cooling；
C. A material, B material, nickel oxide and lanthana are uniformly mixed, 900 DEG C at a temperature of keep the temperature 6 hours, it is cooling after powder
Broken screening；
Wherein, in step A, the doping of Sb is the molal quantity that the doping of 0.3%, Zr of the molal quantity of Co is Co
0.4%, cobaltosic oxide raw material is 1.08 progress ingredients according to Li: Co molar ratio；In step B, lithium carbonate, nickel cobalt manganese (523)
Ternary precursor, nano-nickel oxide raw material are according to Li: (Ni+Co+Mn) molar ratio is 1.15 progress ingredients, wherein the weight of nickel oxide
Amount accounts for the 6% of nickel cobalt manganese (523) ternary precursor weight；In step C, the weight ratio of A material and B material is 90:20 ingredient, covering
Weight ratio with A material is 0.08%.
Embodiment 5
A kind of method for preparing anode material, includes the following steps:
A. it will be uniformly mixed after Sb and Ti doping cobalt hydroxide with lithium fluoride, be sintered 2h, ball milling after cooling at 1100 DEG C
Expect at the A that partial size D50 is 10 μm；
B. lithium carbonate, nickel manganese cobalt (523) ternary precursor and nano-nickel oxide are uniformly mixed, are sintered at 800 DEG C
11h, ball milling is expected at the B that partial size D50 is 3 μm after cooling；
C. A material, B material, nickel oxide and yttrium oxide are uniformly mixed, 800 DEG C at a temperature of keep the temperature 8 hours, it is cooling after powder
Broken screening；
Wherein, in step A, the doping of Sb is the molal quantity that the doping of 0.02%, Ti of the molal quantity of Co is Co
0.02%, cobalt hydroxide raw material is 1.03 progress ingredients according to Li: Co molar ratio；In step B, lithium carbonate, nickel cobalt manganese (523) three
First presoma, nano-nickel oxide raw material are according to Li: (Ni+Co+Mn) molar ratio is 1.03 progress ingredients, wherein the weight of nickel oxide
Account for the 3% of nickel cobalt manganese (523) ternary precursor weight；In step C, A material with B material weight ratio be 60:40 ingredient, covering and
The weight ratio of A material is 1%.
Embodiment 6
A kind of method for preparing anode material, includes the following steps:
A. it will be uniformly mixed after Sb, Mg, Al, Ti and Zr doped cobaltic-cobaltous oxide with lithium acetate, be sintered 3h at 950 DEG C,
Ball milling is expected at the A that partial size D50 is 15 μm after cooling；
B. lithium carbonate, nickel manganese cobalt (523) ternary precursor and nano-nickel oxide are uniformly mixed, are sintered at 850 DEG C
10h, ball milling is expected at the B that partial size D50 is 7 μm after cooling；
C. by A material, B material, nickel oxide, aluminium oxide, lanthana and yttrium oxide be uniformly mixed, 950 DEG C at a temperature of keep the temperature 6
Hour, it is crushed and screened after cooling；
Wherein, in step A, the doping of Sb is the 0.2% of the molal quantity of Co, and the doping of Mg, Al, Ti and Zr are Co's
Molal quantity 0.3%, cobaltosic oxide raw material according to Li: Co molar ratio be 1.1 carry out ingredients；In step B, lithium carbonate, nickel cobalt
Manganese (523) ternary precursor, nano-nickel oxide raw material are according to Li: (Ni+Co+Mn) molar ratio is 1.1 progress ingredients, wherein aoxidizing
The weight of nickel accounts for the 5% of nickel cobalt manganese (523) ternary precursor weight；In step C, the weight ratio of A material and B material is 70:40 ingredient,
The weight ratio of covering and A material is 1%.
Comparative example 1
A kind of method for preparing anode material, includes the following steps:
A. it will be uniformly mixed after cobaltosic oxide with lithium carbonate, be sintered 2h at 1030 DEG C, ball milling is at partial size D50 after cooling
Expect for 25 μm of A；
B. lithium carbonate, nickel manganese cobalt (523) ternary precursor and nano-nickel oxide are uniformly mixed, are sintered at 900 DEG C
10h, ball milling is expected at the B that partial size D50 is 8 μm after cooling；
C. A material, B material, nickel oxide and aluminium oxide are uniformly mixed, 900 DEG C at a temperature of keep the temperature 8 hours, it is cooling after powder
Broken screening；
Wherein, in step A, cobaltosic oxide raw material is 1.05 progress ingredients according to Li: Co molar ratio；In step B, carbonic acid
Lithium, nickel cobalt manganese (523) ternary precursor, nano-nickel oxide raw material are according to Li: (Ni+Co+Mn) molar ratio is 1.05 progress ingredients,
Wherein the weight of nickel oxide accounts for the 5% of nickel cobalt manganese (523) ternary precursor weight；In step C, A material is with the B weight ratio expected
The weight ratio of 80:20 ingredient, covering and A material is 1%.
Comparative example 2
A kind of method for preparing anode material, includes the following steps:
A. it will be uniformly mixed after Sb and Mg doped cobaltic-cobaltous oxide with lithium carbonate, be sintered 2h, ball after cooling at 1030 DEG C
The A that partial size D50 is 25 μm is worn into expect；
B. lithium carbonate and nickel manganese cobalt (523) ternary precursor are uniformly mixed, are sintered 10h, ball milling after cooling at 900 DEG C
Expect at the B that partial size D50 is 8 μm；
C. A material, B material, nickel oxide and aluminium oxide are uniformly mixed, 900 DEG C at a temperature of keep the temperature 8 hours, it is cooling after powder
Broken screening；
Wherein, in step A, the doping of Sb and Mg are respectively 0.1% and 0.15%, cobaltosic oxide of the molal quantity of Co
Raw material is 1.05 progress ingredients according to Li: Co molar ratio；In step B, lithium carbonate, nickel cobalt manganese (523) ternary precursor raw material are pressed
According to Li: (Ni+Co+Mn) molar ratio is 1.05 progress ingredients；In step C, the weight ratio of A material and B material is 80:20 ingredient, cladding
The weight ratio of agent and A material is 1%.
Comparative example 3
A kind of method for preparing anode material, includes the following steps:
A. it will be uniformly mixed after Sb and Mg doped cobaltic-cobaltous oxide with lithium carbonate, be sintered 2h, ball after cooling at 1030 DEG C
The A that partial size D50 is 25 μm is worn into expect；
B. lithium carbonate, nickel manganese cobalt (523) ternary precursor and nano-nickel oxide are uniformly mixed, are sintered at 900 DEG C
10h, ball milling is expected at the B that partial size D50 is 8 μm after cooling；
C. A material and B material are uniformly mixed, 900 DEG C at a temperature of keep the temperature 8 hours, crushed and screened after cooling；
Wherein, in step A, the doping of Sb and Mg are respectively 0.1% and 0.15%, cobaltosic oxide of the molal quantity of Co
Raw material is 1.05 progress ingredients according to Li: Co molar ratio；In step B, lithium carbonate, nickel cobalt manganese (523) ternary precursor, nano oxygen
Change nickel raw material according to Li: (Ni+Co+Mn) molar ratio is 1.05 progress ingredients, and wherein the weight of nickel oxide accounts for nickel cobalt manganese (523) three
The 5% of first forerunner's body weight；In step C, the weight ratio of A material and B material is 80:20 ingredient.
According to the method for preparing anode material of embodiment 1-6 and comparative example 1-3 prepare positive electrode be made into full battery into
Row detection, testing result is as shown in table 1-2:
1 embodiment 1-5 battery performance of table
2 embodiment 6 of table and comparative example 1-3 battery performance
From table 1-2 it is found that the full battery of embodiment 1-6 preparation recycles 400 weeks capacity retention ratios, full electricity in 1C specific volume, 1C
It measures thickness swelling after 85 DEG C of state storage 4h are cooling and 3C5V overcharges good more of equal aspect of performance comparison comparative example 1-3, in fact
It applies 135 DEG C of a 1-6 and comparative example 1-2 heat abuses to be not much different, embodiment 1-6 is than 135 DEG C of heat abuses of comparative example 3 better
It is more.
This is because: in embodiment 1-6, step A is using being doped with nickel oxide in the cobalt source of doping, step B and C is walked
It is rapid to be added covering, to adding covering in Y-oxides doping in cobalt source doping, step B and step C in step A, at these three
Reason method cooperates, and dopant and covering mutually promote, play a role jointly, and the positive electrode of preparation has specific capacity
The advantages that height, good cycle, high-temperature storage thickness swelling are small and energy density is high.And step A does not use in comparative example 1
The cobalt source of doping, only nickel oxide and covering play a role, and step B is not doped with nickel oxide in comparative example 2, only adulterate
Cobalt source and covering play a role, in comparative example 3 step C be added covering, the nickel oxide of the cobalt source and doping only adulterated
It plays a role, comparative example 1-3 lacks the collective effect of three kinds of processing methods, makes specific capacity, the cyclicity of the positive electrode of preparation
The state that the comprehensive performances such as energy, high-temperature storage performance and energy density cannot be optimal.
It should be understood that the application of the present invention is not limited to the above for those of ordinary skills can
With improvement or transformation based on the above description, all these modifications and variations all should belong to the guarantor of appended claims of the present invention
Protect range.
Claims (10)
1. a kind of method for preparing anode material, which comprises the steps of:
A. A is made through mixed processing, sintering processes in the first lithium source and the cobalt source of doping to expect；
B. B material is made through mixed processing, sintering processes in the second lithium source, nickel manganese cobalt ternary precursor and nickel oxide；
C. A material, B material and covering are subjected to mixed processing, sintering processes；
Wherein, the doped chemical for adulterating the cobalt source includes at least one of Mg, Al, Ti and Zr and Sb, the covering packet
Include at least one of aluminium oxide, lanthana and yttrium oxide and nickel oxide.
2. method for preparing anode material according to claim 1, which is characterized in that further including in step A will be at A feed powder mill
Managing and partial size D50 is made is 10-25 μm；Further include in step B by B feed powder mill handle be made partial size D50 be 3-8 μm.
3. method for preparing anode material according to claim 1, which is characterized in that in step A, the cobalt source is four oxidations
The molar ratio of one of three cobalts, hydroxyl cobalt and cobalt hydroxide or a variety of mixtures, Li and Co are 1.03-1.2, and sintering temperature is
950-1100℃。
4. method for preparing anode material according to claim 1, which is characterized in that in step A, the doping of Sb is Co's
The 0.02- for the molal quantity that the 0.02-0.5% of molal quantity, one of Mg, Al, Ti and Zr or a variety of dopings are Co
0.5%.
5. method for preparing anode material according to claim 1, which is characterized in that in step B, Li: (Ni+Co+Mn's)
Molar ratio is 1.03-1.2, and the nickel oxide accounts for the 3-7% of the nickel-cobalt-manganese ternary forerunner body weight.
6. method for preparing anode material according to claim 1, which is characterized in that in step C, the A material and B material
Weight ratio be (60-90): (40-10).
7. method for preparing anode material according to claim 1, which is characterized in that in step C, the covering and described
The weight ratio of A material is 0.05-1%, and sintering temperature is 850-950 DEG C.
8. method for preparing anode material according to claim 1, which is characterized in that first lithium source be selected from lithium carbonate,
One of lithium fluoride, lithium hydroxide, lithium acetate are a variety of, second lithium source be selected from lithium carbonate, lithium fluoride, lithium hydroxide,
One of lithium acetate is a variety of.
9. method for preparing anode material according to claim 1, which is characterized in that step C further includes crushing and screening processing.
10. a kind of positive electrode, which is characterized in that according to the method for preparing anode material institute as described in claim 1-9 is any
Preparation.
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