CN106935848A - A kind of preparation method for improving trielement composite material cycle performance - Google Patents
A kind of preparation method for improving trielement composite material cycle performance Download PDFInfo
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- CN106935848A CN106935848A CN201710181956.XA CN201710181956A CN106935848A CN 106935848 A CN106935848 A CN 106935848A CN 201710181956 A CN201710181956 A CN 201710181956A CN 106935848 A CN106935848 A CN 106935848A
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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
- 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
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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
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
- H01M4/1391—Processes of manufacture of electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
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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
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- H01M4/366—Composites as layered products
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- H—ELECTRICITY
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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
- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
- H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
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Abstract
The invention belongs to field of lithium ion battery material preparation, a kind of preparation method of raising trielement composite material cycle performance, its trielement composite material is presented core shell structure, and kernel is ternary material, and shell clad is lithium powder complex, and its cladding thickness is 0.5~2 μm；By weight percentage, its lithium powder complex is by 40~60% lithium powder, 5~10% conductive agents, 30~55% polymer composition；Its preparation method is to configure lithium efflorescence polymer solution first, is mixed with ternary material afterwards, and the trielement composite material that shell is coated with lithium powder polymer is prepared by spray drying technology.The present invention, has the advantages that conductance is high, imbibition ability is strong, is applied to the characteristics such as lithium ion battery has good cycle, high rate performance good and its energy density is high, is particularly suitable for pure electric automobile field.
Description
Technical field
The invention belongs to field of lithium ion battery material preparation, a kind of raising trielement composite material cyclicity is particularly said
The preparation method of energy.
Background technology
Lithium ion battery as a kind of new secondary cell, with height ratio capacity, have extended cycle life, the spy such as security is good
Point, is widely used in the driving power supply of the portable electronics such as mobile phone, notebook computer.With the continuous upgrading of electronic product
Regenerate, and electric automobile, hybrid vehicle development, requirement to battery energy density improves constantly.
Under the premise of same capacity is played, market needs to improve constantly the volume energy density of battery, that is, improves
The unit volume loading of cell active materials.Commercial anode material for lithium-ion batteries is broadly divided into three classes, olivine at present
The LiFePO 4 of structure, specific energy is high, cheap, but its own tap density is low；The mangaic acid of spinel structure
Lithium, simple production process is safe, but its in use capacity attenuation it is very fast, particularly high temperature cyclic performance is poor；
Stratiform cobalt acid lithium, is that existing market uses widest positive electrode, but cobalt resource is rare, and price is high, and toxicity is big, battery peace
Full property is poor.Novel anode trielement composite material nickle cobalt lithium manganate, due to cheap, good cycle, structural stability is good, shake
Real density is high, as more satisfactory positive electrode.But the high temperature cyclic performance deviation of material, limits it and uses field, its
Improving ternary material cycle performance main method has：Material coating modification and its material doped, and material doped is most simple at present
Single method.Such as patent（CN1036823199A）Disclose high temperature circulation nickle cobalt lithium manganate NCM523 ternary materials long and
Its preparation method, aluminium salt or its oxide are mainly added, mixed using dry method batch mixing by it by material sintering process
It is sintered again after uniform, the high-temperature behavior of nickle cobalt lithium manganate NCM523 is improved by Al ion dopings, is effectively being solved
The poor problem of nickle cobalt lithium manganate high temperature cyclic performance, the high-temperature storage performance of having determined, but its structural stability difference and its multiplying power
Poor performance, influences the performance of its other performance.And coating modification can then be improved under conditions of material internal structure is not influenceed
The compatibility of material surface and electrolyte, and improve the performances such as the circulation of material, multiplying power.At present carried out in material surface
Carbon coating, reduces the Probability of its side reaction and improves its cycle performance, but its big high rate performance and its peace to material
Full performance is unfavorable.And it is a kind of new technique for growing up in recent years to mend lithium technology, i.e., lithium is mended by pole piece or material surface
The transmission rate and its efficiency first of its lithium ion are improved, and improves the performances such as its circulation, multiplying power, domestic lithium of mending is mainly at present
Benefit lithium is carried out to pole piece, and ternary material surface is carried out to mend lithium then domestic no report.
The content of the invention
For the defect that current ternary material cycle performance and its high rate performance aspect are present, the purpose of the present invention is to pass through
Ternary material coats lithium powder complex, improves circulation, the high rate performance of its ternary material.
The technical scheme is that be accomplished by the following way：A kind of system for improving trielement composite material cycle performance
Preparation Method, its trielement composite material is presented core shell structure, and kernel is ternary material, and shell clad is lithium powder complex, its bag
Thickness is covered for 0.5~2 μm；By weight percentage, its lithium powder complex is by 40~60% lithium powder, 5~10% conductive agents, 30
~55% polymer composition；Its preparation method, configures lithium efflorescence polymer solution first, mixes with ternary material afterwards, and pass through
Spray drying technology prepares the trielement composite material that shell is coated with lithium powder polymer, it is characterised in that：
1）, lithium powder composite solution configuration：
30~55g polymeric materials are dissolved in 1000ml organic solvents first, after being uniformly dispersed, 5~10g are added successively and is led
Electric agent, 40~60g lithium powder, and stir, obtain lithium powder composite solution A；
2）, trielement composite material preparation：
200~300g ternary materials are added in lithium powder composite solution A, after being uniformly dispersed, by spray dryer, are prepared
Spherical trielement composite material.
Described step 1）Middle polymer is polymethyl methacrylate, polyethyl methacrylate, polymethylacrylic acid
Butyl ester, polyisobutyl methacrylate, poly hydroxy ethyl acrylate, polyethylene glycol methyl methacrylate, polyethylene glycol two
Methacrylate, poly- 3- methoxy-methyl acrylates, PMA, polyethyl acrylate, polymethylacrylic acid bay
Any one in ester, polyacrylic acid trifluoro ethyl ester, poly (glycidyl methacrylate) etc., its molecular weight is 1~100,000；
Described step 1）Middle organic solvent is carbon tetrachloride, tetrahydrofuran, N-N- dimethylformamides, acetone, N, N- diformazans
One kind in yl acetamide, dichloromethane, dichloroethanes, toluene, ethyl acetate, n-hexane, hexamethylene.
Described step 1）Middle conductive agent is fibrous conductive agent, is CNT, gas-phase growth of carbon fibre, and solid carbon is fine
One kind in dimension.
Described step 1）In ternary material be LiNixCoyMn1-x-yO2（X >=0.3, y≤0.3）,LiNixCoyAL1-x- yO2（X >=0.3, y≤0.3）In one kind.
Beneficial effects of the present invention：1st, in ternary material Surface coating lithium powder complex, its material is made in charge and discharge process
It is middle that sufficient lithium ion is provided, the transmission rate of its lithium ion is improved, and improve its high rate performance；Simultaneously because material discharge and recharge
During form SEI films and consume a part of lithium ion, and SEI to belong to semiconductor resistor larger, and pass through to supplement lithium ion, can be with
To provide the lithium ion of abundance in charge and discharge process, its cycle performance is improved.2nd, the polymeric material of lithium powder complex surfaces cladding
Material does not dissolve in 1-METHYLPYRROLIDONE, and is coated on the outside processing characteristics for improving its preceding operation, and in lithium ion battery liquid injection
Afterwards, polymer is dissolved in the solvent of electrolyte, and its lithium powder is coated on ternary material surface, improves the transmission speed of its lithium ion
Rate, while there is fibrous carbon conductive agent on the one hand to improve its electronic conductivity in lithium powder complex, on the other hand in complex
Middle formation conductive network, improves the structural stability of its clad.
Brief description of the drawings
Fig. 1 is the SEM pictures of the trielement composite material that embodiment 1 is prepared.
Fig. 2 is that embodiment 1-3 compares with the high rate performance of comparative example.
Specific embodiment
A kind of preparation method for improving trielement composite material cycle performance, its trielement composite material is presented core shell structure, interior
Core is ternary material, and shell clad is lithium powder complex, and its cladding thickness is 0.5~2 μm；By weight percentage, its lithium
Powder complex is by 40~60% lithium powder, 5~10% conductive agents, 30~55% polymer composition.Its preparation method is by following step
Suddenly：1）The configuration of lithium powder composite solution；2）The preparation of trielement composite material.
Embodiment 1：
Know that a kind of preparation method for improving trielement composite material cycle performance is comprised the following steps by Fig. 1：
1st, the configuration of lithium powder composite solution：40g polymethyl methacrylate materials are dissolved in 1000ml carbon tetrachloride first,
After being uniformly dispersed, the agent of 10g carbon nanotube conductings, 50g lithium powder are added successively, and stirred, obtain lithium powder composite solution A；
2nd, the preparation of trielement composite material：By 250gLiNi0.5Co0.2Mn0.3O2Ternary material is added to lithium powder composite solution A
In, after being uniformly dispersed, by spray dryer（Spray drying intake air temperature is set to 150 DEG C, and air outlet temperature is set as 100
DEG C, prepare spherical trielement composite material.
Embodiment 2：
1st, the configuration of lithium powder composite solution：30g polybutyl methacrylate materials are dissolved in 1000mlN-N- dimethyl first
In formamide, after being uniformly dispersed, 5g gas-phase growth of carbon fibre, 60g lithium powder are added successively, and stirred, obtain lithium powder and be combined
Solution A；
2nd, the preparation of trielement composite material：Afterwards by 200gLiNi0.5Co0.2Mn0.3O2Ternary material be added to lithium powder be combined it is molten
In liquid A, after being uniformly dispersed, by spray dryer（Spray drying intake air temperature is set to 150 DEG C, and air outlet temperature is set as
100 DEG C, prepare spherical trielement composite material.
Embodiment 3：
1st, the configuration of lithium powder composite solution：55g polyisobutyl methacrylate materials are dissolved in 1000ml n-hexanes first,
After being uniformly dispersed, 10g solid carbon fibers, 40g lithium powder are added successively, and stirred, obtain lithium powder composite solution A；
2nd, the preparation of trielement composite material：Afterwards by 300gLiNi0.5Co0.2Mn0.3O2Ternary material be added to lithium powder be combined it is molten
In liquid A, after being uniformly dispersed, by spray dryer（Spray drying intake air temperature is set to 150 DEG C, and air outlet temperature is set as
100 DEG C, prepare spherical trielement composite material.
Comparative example：The LiNi purchased with the market0.5Co0.2Mn0.3O2As a comparison, producer：Xinxiang day power lithium energy share has
Limit company, model：TLM510.
1) SEM tests：
As can be seen from Figure, the trielement composite material that embodiment 1 is prepared is presented spherical, and particle diameter exists（5-20）Between μm,
Size distribution is uniform.
2）Electrochemical property test：
2.1 make button cell test.
Known by Fig. 2, be that embodiment 1-3 compares with the high rate performance of comparative example.
Button cell is dressed up as follows to the trielement composite material that embodiment 1-3 and comparative example are prepared and is surveyed
Examination：
1）In adding 220mLN- methyl pyrrolidones in 95g positive electrodes, 1g Kynoar, 4g conductive agents SP, stirring is equal
It is even to prepare anode sizing agent, it is coated on Copper Foil, to dry, roll pressing obtains positive pole.
Electrolyte uses LiPF6It is electrolyte, concentration is 1.3mol/L, and volume ratio is 1:1 EC and DEC is solvent, gold
Used as to electrode, barrier film uses polyethylene (PE), polypropylene (PP) or poly- second propylene (PEP) composite membrane, is being flushed with hydrogen gas category lithium piece
Glove box according to existing method assembling button cell A1, A2, A3 and B1.
2）Above-mentioned button cell is tested on new prestige 5V/10mA type cell testers, charging/discharging voltage scope 3-4.3V,
Charge-discharge magnification 0.1C, test result is as shown in table 1.
The button cell test result of table 1
| The electric battery of button | A1 | A2 | A3 | B1 |
| Discharge capacity first（mAh/g） | 169.1 | 168.7 | 167.1 | 160.1 |
| Efficiency first（%） | 97.1 | 96.9 | 96.8 | 92.1 |
As can be seen from Table 1, embodiment prepares the gram volume of trielement composite material and its efficiency is better than comparative example first, and it is former
Because lithium flour complexes have lithium ion conducting rate characteristic high in clad, be provide in charge and discharge process the lithium of abundance from
Son, so as to improve the performance of its ternary material gram volume and its efficiency first.
2.2 soft-package batteries are tested
1）High rate performance
The material prepared using embodiment 1~3 and comparative example is used as positive electrode.With Delanium as negative pole, with LiPF6It is (molten
Agent is EC+DEC, volume ratio 1：1, concentration 1.3mol/l) it is electrolyte, celegard2400 prepares 5Ah Soft Rolls electricity for barrier film
Pond C1, C2, C3 and D.Charged with 0.3C multiplying powers afterwards, blanking voltage 4.2V, afterwards with 0.3C, 1.0C, 2.0C,
3.0C, 4.0C, 6.0C are discharged, discharge cut-off voltage 3.0V, finally prepare soft-package battery.
Table 2, embodiment compares with the high rate performance of comparative example
As can be seen from Table 2, the high rate performance of the lithium ion battery that embodiment 1-3 is prepared is substantially better than comparative example, its reason
For the surface coated lithium flour complexes of ternary material provide sufficient lithium ion, are offer abundance during high rate charge-discharge
Lithium ion, and therefore improve its high rate performance.
2）Cycle performance
The cycle performance of its soft-package battery is tested afterwards, and wherein test parameter is：Rate of charge is 1.0C, and discharge-rate is
1.0C, voltage range 3.0V-4.2V, cycle-index 500 times.
The recycle ratio of the embodiment of table 3 and comparative example compared with
| Sequence number | Discharge capacity first（Ah） | 500 discharge capacities（Ah） | Capability retention |
| Embodiment 1 | 5.23 | 4.97 | 95.1% |
| Embodiment 2 | 5.27 | 4.99 | 94.8% |
| Embodiment 3 | 5.26 | 4.92 | 93.7% |
| Comparative example | 5.19 | 4.68 | 90.3% |
As can be seen from Table 3, the cycle performance of the soft-package battery that embodiment is prepared is substantially better than comparative example, and its reason is,
During lithium ion battery charge and discharge cycles, the trielement composite material Surface coating prepared by embodiment has lithium flour complexes,
After fluid injection chemical conversion, polymer is dissolved, and its lithium powder is coated on ternary material surface, and and electrolyte contacts, discharge
More lithium ion, the lithium ion that SEI consumption is formed in lithium ion battery charge and discharge process is supplemented in time, and is therefore carried
Its cycle performance high.
Claims (5)
1. it is a kind of improve trielement composite material cycle performance preparation method, its trielement composite material present core shell structure, kernel
It is ternary material, shell clad is lithium powder complex, its cladding thickness is 0.5~2 μm；By weight percentage, its lithium powder
Complex is by 40~60% lithium powder, 5~10% conductive agents, 30~55% polymer composition；Its preparation method is to configure first
Lithium efflorescence polymer solution, mixes with ternary material afterwards, and preparing shell by spray drying technology is coated with lithium powder polymer
Trielement composite material, it is characterised in that：
1）, lithium powder composite solution configuration：30~55g polymeric materials are dissolved in 1000ml organic solvents first, are disperseed
After uniform, 5~10g conductive agents, 40~60g lithium powder are added successively, and stirred, obtain lithium powder composite solution A；
2）, trielement composite material preparation：200~300g ternary materials are added in lithium powder composite solution A, are uniformly dispersed
Afterwards, by spray dryer, spherical trielement composite material is prepared.
2. it is according to claim 1 it is a kind of improve trielement composite material cycle performance preparation method, it is characterised in that：Institute
The step of stating 1）In polymer be polymethyl methacrylate, polyethyl methacrylate, polybutyl methacrylate, poly- first
Base isobutyl acrylate, poly hydroxy ethyl acrylate, polyethylene glycol methyl methacrylate, glycol dimethacrylates
Ester, poly- 3- methoxy-methyl acrylates, PMA, polyethyl acrylate, polylauryl methacrylate, polyacrylic acid
Any one in trifluoro ethyl ester, poly (glycidyl methacrylate) etc., its molecular weight is 1~100,000.
3. it is according to claim 1 it is a kind of improve trielement composite material cycle performance preparation method, it is characterised in that：Institute
The step of stating 1）Middle organic solvent is carbon tetrachloride, tetrahydrofuran, N-N- dimethylformamides, acetone, N, N- dimethylacetamides
One kind in amine, dichloromethane, dichloroethanes, toluene, ethyl acetate, n-hexane, hexamethylene.
4. it is according to claim 1 it is a kind of improve trielement composite material cycle performance preparation method, it is characterised in that：Institute
The step of stating 1）Middle conductive agent is fibrous conductive agent, is CNT, gas-phase growth of carbon fibre, in solid carbon fiber one
Kind.
5. it is according to claim 1 it is a kind of improve trielement composite material cycle performance preparation method, it is characterised in that：Institute
The step of stating 1）In ternary material be LiNixCoyMn1-x-yO2（X >=0.3, y≤0.3）,LiNixCoyAL1-x-yO2（x≥
0.3, y≤0.3）In one kind.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108448076A (en) * | 2018-02-09 | 2018-08-24 | 山东丰元化学股份有限公司 | The method of modifying of nickle cobalt lithium manganate trielement composite material |
| CN109873148A (en) * | 2019-03-06 | 2019-06-11 | 昆明理工大学 | The preparation method of the modified nickelic ternary lithium battery composite positive pole of conducting polymer base |
| CN111430710A (en) * | 2020-03-17 | 2020-07-17 | 桂林电子科技大学 | Modified nickel cobalt lithium manganate ternary cathode material and preparation method and application thereof |
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| CN101488568A (en) * | 2008-01-14 | 2009-07-22 | 中国科学院物理研究所 | Surface modification process used for lithium secondary battery positive pole active material |
| CN104332657A (en) * | 2014-08-20 | 2015-02-04 | 东莞新能源科技有限公司 | Lithium ion battery lithium-enriching technology and lithium ion battery prepared by the technology |
| CN106410120A (en) * | 2016-10-27 | 2017-02-15 | 东莞塔菲尔新能源科技有限公司 | Method for supplementing lithium to lithium ion battery pole piece |
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2017
- 2017-03-24 CN CN201710181956.XA patent/CN106935848A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101488568A (en) * | 2008-01-14 | 2009-07-22 | 中国科学院物理研究所 | Surface modification process used for lithium secondary battery positive pole active material |
| CN104332657A (en) * | 2014-08-20 | 2015-02-04 | 东莞新能源科技有限公司 | Lithium ion battery lithium-enriching technology and lithium ion battery prepared by the technology |
| CN106410120A (en) * | 2016-10-27 | 2017-02-15 | 东莞塔菲尔新能源科技有限公司 | Method for supplementing lithium to lithium ion battery pole piece |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108448076A (en) * | 2018-02-09 | 2018-08-24 | 山东丰元化学股份有限公司 | The method of modifying of nickle cobalt lithium manganate trielement composite material |
| CN109873148A (en) * | 2019-03-06 | 2019-06-11 | 昆明理工大学 | The preparation method of the modified nickelic ternary lithium battery composite positive pole of conducting polymer base |
| CN111430710A (en) * | 2020-03-17 | 2020-07-17 | 桂林电子科技大学 | Modified nickel cobalt lithium manganate ternary cathode material and preparation method and application thereof |
| CN111430710B (en) * | 2020-03-17 | 2021-06-11 | 桂林电子科技大学 | Modified nickel cobalt lithium manganate ternary cathode material and preparation method and application thereof |
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