CN110112399A - A kind of effective method of modifying for promoting business tertiary cathode material cyclical stability - Google Patents

A kind of effective method of modifying for promoting business tertiary cathode material cyclical stability Download PDF

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Publication number
CN110112399A
CN110112399A CN201910430068.6A CN201910430068A CN110112399A CN 110112399 A CN110112399 A CN 110112399A CN 201910430068 A CN201910430068 A CN 201910430068A CN 110112399 A CN110112399 A CN 110112399A
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China
Prior art keywords
cathode material
tertiary cathode
ncm622
modifying
cyclical stability
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CN201910430068.6A
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Chinese (zh)
Inventor
李昱
陈良丹
吴亮
邹伟
刘婧
陈丽华
王洪恩
苏宝连
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Wuhan University of Technology WUT
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Wuhan University of Technology WUT
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Priority to CN201910430068.6A priority Critical patent/CN110112399A/en
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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
    • 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
    • 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
    • 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
    • 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

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Composite Materials (AREA)
  • Materials Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Battery Electrode And Active Subsutance (AREA)

Abstract

The invention discloses a kind of method of modifying for effectively promoting business tertiary cathode material cyclical stability, with B2O3For boron source, by itself and the nickelic tertiary cathode material LiNi of business0.6Co0.2Mn0.2O2(NCM622) it is stirred mixing in ethanol, carries out calcination reaction, B in Muffle furnace after high temperature drying and processing2O3Efficient melting diffusion, gained B3+The NCM622 of doping can express excellent chemical property, and the raw material sources being related to are wide, preparation process is simple, be suitble to business promotion application.

Description

A kind of effective method of modifying for promoting business tertiary cathode material cyclical stability
Technical field
It is a kind of effective to promote business tertiary cathode material cyclical stability the present invention relates to technical field of lithium ion Method of modifying.
Background technique
Currently, electric car and hybrid vehicle are in rapid development period, with people to high-energy density and The demand of long circulation life lithium ion battery (LIBs) is constantly promoted, and is dedicated to developing the research of high-performance novel electrode material It is more burning hot.Nickelic tertiary cathode material is due to low cost, high capacity and environmental-friendly intrinsic advantage, it has also become power lithium battery The inexorable trend of pond Materials.Wherein, the nickelic positive electrode LiNi of lithium ion battery0.6Co0.2Mn0.2O2(NCM622) Realize industrial production, it is considered to be most one of the positive electrode of development potentiality.
But currently, nickelic tertiary cathode material still faces many technical bottlenecks: firstly, during charge and discharge cycles, two Highdensity micro-crack can be germinated between secondary particle, this internal stress will lead to intragranular disintegration, and cyclical stability is deteriorated, eventually leads to Battery failure；Second, liquid electrolyte crackle between crystal boundary and second particle permeates, and the side reaction of aggravation and positive electrode is drawn Structural phase transition is sent out, voltage attenuation is caused；In addition, the transition metal ions of high potential causes electricity in high voltage charge and discharge process The continued oxidation for solving liquid decomposes, and aggravates lithium nickel mixing degree, leads to the rapid decay of capacity, the final circulation longevity for reducing battery Life.Therefore, nickelic tertiary cathode material method of modifying is further explored with important research and application value.
Summary of the invention
Based on the above the deficiencies in the prior art, technical problem solved by the invention is to provide a kind of effectively promoted commercially The method of modifying of tertiary cathode material cyclical stability, with B2O3For boron source, by itself and market nickelic tertiary cathode material on sale NCM622 is stirred mixing in ethanol, carries out calcination reaction, B in Muffle furnace after high temperature drying and processing2O3Efficient melting Diffusion, gained B3+Adulterating tertiary cathode material can express excellent chemical property and stability, and the raw material sources being related to Extensively, preparation process is simple, is suitble to commercial introduction application.
Business tertiary cathode material cyclical stability is effectively promoted in order to solve the above technical problem, the present invention provides a kind of Method of modifying, comprise the following steps:
1) by B2O3It is placed in dehydrated alcohol and is stirred dissolution, obtain boracic ethanol solution；
2) commercially available NCM622 is dissolved in and handles acquired solution through step 1), be then stirred at room temperature, Obtain mixed solution；
3) acquired solution heating will be handled through step 2) and carry out drying and processing, obtain the mixing material of boracic；
4) step 3) resulting materials are placed in Muffle furnace, heating carries out high-temperature calcination to get the B3+Doping NCM622 tertiary cathode material.
As a preferred embodiment of the above technical solution, effective promotion business tertiary cathode material cyclical stability provided by the invention Method of modifying further comprise some or all of following technical characteristic:
As an improvement of the above technical solution, in the step 2), NCM622 material and B2O3Mass ratio be 100:(0- 5), mixing time 2-4h.
As an improvement of the above technical solution, in the step 3), drying temperature is 80-100 DEG C, drying time 10- 12h。
As an improvement of the above technical solution, in the step 4), calcination temperature is 450-500 DEG C, time 300- 360min, calcining heating rate are 4-5 DEG C/min.
As an improvement of the above technical solution, the B3+The NCM622 tertiary cathode material of doping is in 2.7-4.3V voltage model Under enclosing, 0.5-5%B2O3The NCM622 positive electrode of volume recycles 100 circles under 0.2C (1C=200mAh/g) current density, Capacity keeps 120-170mAh/g, and capacity retention ratio reaches 60-95%；Pressure is maintained at 3.7-3.8V in its electric discharge, and conservation rate reaches 98-99.5%.
The B3+The NCM622 tertiary cathode material of doping is under 2.7-4.3V voltage range, 5%B2O3Volume NCM622 positive electrode recycles 100 circles under 0.2C (1C=200mAh/g) current density, and capacity keeps 164.8mAh/g, Capacity retention ratio is up to 90.76%；Its discharge in pressure be maintained at 3.77V, conservation rate is up to 99.4%.Electrochemistry loop test result is aobvious Show, electrochemically stable performance significantly improves, and voltage attenuation also obviously weakens.
The principle of the present invention are as follows: the present invention is with B2O3For boron source, it is existed with nickelic tertiary cathode material NCM622 is commercialized It is stirred mixing in ethyl alcohol, carries out calcination reaction in Muffle furnace after high temperature drying and processing.Nickelic tertiary cathode material is tight The capacity attenuation and voltage droop problem of weight restrict its extensive use always, although its intrinsic structure cannot be completely eliminated Unstability, but we can improve the structure of nickelic tertiary cathode material by the micro-structure control measures of element doping Stability.B2O3With relatively low fusing point, boron can be easily melted into material lattice structure, and raw material sources are wide, cost Low, therefore, boron is the preferable candidate in available dopant material.
Compared with prior art, technical solution of the present invention has the following beneficial effects:
1)B2O3With good electrochemical stability, high anti-oxidant current potential, the present invention uses B2O3For boron source, not While changing NCM622 material layer structure, it is effectively incorporated B3+, show the modified tertiary cathode material of gained excellent Stable circulation performance and efficiently solve voltage droop problem in cyclic process.
2) this nonmetalloid is suitable for the modified of tertiary cathode material to adulterate, not only avoids other expensive gold Belong to element, cost is greatly lowered, and raw material sources are wide, environmentally protective.
3) the invention avoids the doping of traditional tertiary cathode material, the synthesis that surface coats and other modified methods are cumbersome Step, no other pollutants generate；Preparation method of the present invention is simple, reaction condition is mild, and repetitive rate is high, is suitble to business Change and promotes and applies.
The above description is only an overview of the technical scheme of the present invention, in order to better understand the technical means of the present invention, And it can be implemented in accordance with the contents of the specification, and in order to allow above and other objects, features and advantages of the invention can It is clearer and more comprehensible, below in conjunction with preferred embodiment, detailed description are as follows.
Detailed description of the invention
In order to illustrate the technical solution of the embodiments of the present invention more clearly, the attached drawing to embodiment is simply situated between below It continues.
Fig. 1 is the XRD diagram of 1 gained NCM622 positive electrode of embodiment 1-2 and comparative example；
Fig. 2 (a) is scanning electron microscope (SEM) photograph of the 1 gained positive electrode of comparative example under 10K amplification factor；
Fig. 2 (b) is scanning electron microscope (SEM) photograph of the 1 gained positive electrode of comparative example under 20K amplification factor；
Fig. 2 (c) is scanning electron microscope (SEM) photograph of the 2 gained positive electrode of embodiment under 20K amplification factor；
Fig. 2 (d) is scanning electron microscope (SEM) photograph of the 1 gained positive electrode of embodiment under 20K amplification factor；
Fig. 3 is the XPS map of the boron element of 1 gained positive electrode of embodiment；
Fig. 4 is the cyclical stability test chart of embodiment 1-2 and 1 gained positive electrode of comparative example under 0.2C multiplying power；
Fig. 5 is embodiment 1 and 1 products therefrom of comparative example pressure-circulation figure in the electric discharge under 0.2C multiplying power.
Specific embodiment
The following detailed description of a specific embodiment of the invention, as part of this specification, by embodiment come Illustrate that the principle of the present invention, other aspects of the present invention, feature and its advantage will become apparent by the detailed description.
Embodiment 1
A kind of effective method of modifying for promoting business tertiary cathode material cyclical stability, preparation method includes following step It is rapid:
1) by 0.01gB2O3(account for NCM622 substrate quality 5%) is dissolved in 15ml dehydrated alcohol, stirring to being completely dissolved, Obtain boracic ethanol solution；
2) 0.2gNCM622 finished product is dissolved in boracic ethanol solution, 2h is stirred at room temperature, obtain mixed solution；
3) acquired solution will be handled through step 2) to be placed in electric heating constant-temperature blowing drying box, 12h is reacted at 80 DEG C, it is dry Mixing material is obtained afterwards；
4) step 3) resulting materials are placed in Muffle furnace, 5h is persistently calcined at 500 DEG C, take out gained after reaction B3+It adulterates NCM622 positive electrode (NCM622-BO5).
The present embodiment products therefrom is shown in Fig. 1, it can be seen from the figure that NCM622 positive electrode is still after adulterating through B element With more sharp diffraction maximum, illustrate that modified ternary material crystalline structure is complete, in the α-NaFeO of stratiform2Type structure, rate Belong to R-3m space group, not impurity peaks appearance in XRD spectra illustrates that the doping of element does not have shadow to the crystalline structure of material It rings.Two groups of division peak (006)/(102) and (108)/(110) splitting are obvious, illustrate the modified tertiary cathode material tool of the present invention There is good layer structure.
The scanning figure of the present embodiment products therefrom is shown in Fig. 2, it can be seen that NCM622 positive electrode is reunited by second particle Made of spherical or spheric granules, size is up to some tens of pm, and the product second particle after doping vario-property becomes large-sized, along diameter To elongated, there is impurity in surface, and edges and corners fog.
The XPS test result of the present embodiment products therefrom is shown in Fig. 3, and the component of B is detected from XPS test spectrum, right The combination answered can be in 192.62eV or so, this result and B2O3In B3+Combination can be corresponding.
Embodiment 2
Method of modifying and the embodiment 1 that commercialization tertiary cathode material cyclical stability is effectively promoted described in embodiment 2 are big Cause it is identical, the difference is that B in step 2)2O3Additive amount accounts for the 2% of NCM622 substrate quality, gained B respectively3+Doping NCM622 positive electrode is labeled as NCM622-BO2.
2 products therefrom of embodiment is subjected to X-ray diffraction analysis, the result is shown in Figure 1, test result and embodiment 1 respectively Test result is almost the same.
SEM sweep test result is shown in Fig. 2, and the test result of test result and embodiment 1 is almost the same.
Comparative example 1
NCM622 positive electrode described in comparative example 1 is commercially available gained, will for the consistency for guaranteeing processing method 0.2gNCM622 finished product is placed in Muffle furnace, and 5h is persistently calcined at 500 DEG C, and the NCM622 after gained high-temperature process is labeled as NCM622-BO0。
The X-ray diffraction analysis test result of comparative example 1 is shown in Fig. 1, the test result one of test result and embodiment 1-2 It causes.
Fig. 2 (a) is scanning electron microscope (SEM) photograph of the 1 gained NCM622-BO0 positive electrode of comparative example under 10K amplification factor；Fig. 2 It (b) is scanning electron microscope (SEM) photograph of the 1 gained NCM622-BO0 positive electrode of comparative example under 20K amplification factor；Fig. 2 (c) is embodiment 2 Scanning electron microscope (SEM) photograph of the gained NCM622-BO2 positive electrode under 20K amplification factor；Fig. 2 (d) is 1 gained NCM622- of embodiment Scanning electron microscope (SEM) photograph of the BO5 positive electrode under 20K amplification factor.SEM sweep test is commercialized purchase described in comparative example 1 as the result is shown The basis material bought is reunited by second particle, and second particle size is smaller and surface is smooth clean.Also, as boron is mixed The size of the increase of amount, second particle is gradually increased, and is radially grown into, and surface impurity is more and more, and corner angle are increasingly It is fuzzy.
Application examples
By B obtained by 1 gained NCM622 of comparative example, embodiment 1-23+Blended positive pole material carries out electrochemical cycle stability respectively Performance test.Specific step is as follows:
Positive electrode, Super P and PVDF are mixed according to the mass ratio of 8:1:1, suitable N- methyl pyrrole is added dropwise Slurry is uniformly coated on aluminium foil by pyrrolidone (NMP), grinding after 30 minutes or so, in 40 DEG C of baking ovens after dry 2h, is set In a vacuum drying oven, 12h is reacted at 120 DEG C.Cathode uses metal lithium sheet, and diaphragm is polypropylene porous film, and electrolyte uses LiPF6Ethylene carbonate (EC) mixed solvent system, battery use 2025 type buttons, followed in 2.7-4.3V voltage range The test of ring stability.
The stable circulation performance test chart of all samples to be tested is shown in Fig. 3, and test result is shown, compared to comparative example 1, Under 0.2C multiplying power, the cyclical stability of embodiment 1-2 products therefrom is obviously improved, and 2 products therefrom of embodiment is in 0.2C electricity 100 circle of circulation, capacity are maintained at 164.8mAh/g under current density, and capacity retention ratio is up to 90.76%.
The electric discharge Medium pressure cycle test chart of comparative example 1 and embodiment 1 is shown in Fig. 4, the results show that in 2.7-4.3V voltage range Under test condition, comparative example 1 is after the circle of circulation 100, and pressure decays to 3.67V in electric discharge；Embodiment 1 under the same test conditions, After the circle of circulation 100, voltage is maintained at 3.77V, and conservation rate is up to 99.4%.
The bound of each raw material cited by the present invention and each raw material of the present invention, section value and technological parameter Bound, the section value of (such as temperature, time) can realize the present invention, embodiment numerous to list herein.
The above is a preferred embodiment of the present invention, cannot limit the right model of the present invention with this certainly It encloses, it is noted that for those skilled in the art, without departing from the principle of the present invention, may be used also To make several improvement and variation, these, which improve and change, is also considered as protection scope of the present invention.

Claims (7)

1. a kind of method of modifying for effectively promoting business tertiary cathode material cyclical stability, which is characterized in that include following step It is rapid:
1) by B2O3It is placed in dehydrated alcohol and is stirred dissolution, obtain boracic ethanol solution；
2) commercially available NCM622 is dissolved in and handles acquired solution through step 1), be then stirred, obtain mixed at room temperature Close solution；
3) acquired solution heating will be handled through step 2) and carry out drying and processing, obtain the mixing material of boracic；
4) step 3) resulting materials are placed in Muffle furnace, heating carries out high-temperature calcination to get the B3+The NCM622 tri- of doping First positive electrode.
2. the method for modifying as described in claim 1 for effectively promoting business tertiary cathode material cyclical stability, feature exist In: in the step 1), B2O3It is 1:(400-800 with ethanol solution mass ratio), mixing time 0.25-1h.
3. the method for modifying as described in claim 1 for effectively promoting business tertiary cathode material cyclical stability, feature exist In: in the step 2), NCM622 material and B2O3Mass ratio be 100:(0.5-5), mixing time 2-4h.
4. the method for modifying as described in claim 1 for effectively promoting business tertiary cathode material cyclical stability, feature exist In: in the step 3), drying temperature is 80-100 DEG C, drying time 10-12h.
5. the method for modifying as described in claim 1 for effectively promoting business tertiary cathode material cyclical stability, feature exist In: in the step 4), calcination temperature is 450-500 DEG C, time 300-360min, and calcining heating rate is 4-5 DEG C/min.
6. effective method of modifying for promoting business tertiary cathode material cyclical stability as claimed in claims 1-5, feature It is: the B3+The NCM622 tertiary cathode material of doping is under 2.7-4.3V voltage range, 0.5-5%B2O3Volume NCM622 positive electrode recycles 100 circles under 0.2C current density, and capacity keeps 120-170mAh/g, and capacity retention ratio reaches 60-95%；Pressure is maintained at 3.7-3.8V in its electric discharge, and conservation rate reaches 98-99.5%.
7. effective method of modifying for promoting business tertiary cathode material cyclical stability as claimed in claims 1-5, feature It is: the B3+The NCM622 tertiary cathode material of doping is under 2.7-4.3V voltage range, 5%B2O3The NCM622 of volume is just Pole material recycles 100 circles under 0.2C current density, and capacity keeps 164.8mAh/g, and capacity retention ratio is up to 90.76%；Its Pressure is maintained at 3.77V in electric discharge, and conservation rate is up to 99.4%.
CN201910430068.6A 2019-05-22 2019-05-22 A kind of effective method of modifying for promoting business tertiary cathode material cyclical stability Pending CN110112399A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112599781A (en) * 2020-12-15 2021-04-02 荆门市格林美新材料有限公司 Double-concentration gradient doped lithium ion battery anode material and preparation method thereof

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103022499A (en) * 2012-12-03 2013-04-03 东莞新能源科技有限公司 Mixed positive-pole material for lithium ion battery
CN103236521A (en) * 2013-04-17 2013-08-07 天津华夏泓源实业有限公司 Nickel-cobalt-lithium manganese positive electrode material with boron-lithium composite oxide clad on surface, and preparation method thereof
US20180090753A1 (en) * 2016-09-27 2018-03-29 Contemporary Amperex Technology Co., Limited Positive electrode material for li-ion battery, method for preparing the same, and li-ion power battery containing the same

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103022499A (en) * 2012-12-03 2013-04-03 东莞新能源科技有限公司 Mixed positive-pole material for lithium ion battery
CN103236521A (en) * 2013-04-17 2013-08-07 天津华夏泓源实业有限公司 Nickel-cobalt-lithium manganese positive electrode material with boron-lithium composite oxide clad on surface, and preparation method thereof
US20180090753A1 (en) * 2016-09-27 2018-03-29 Contemporary Amperex Technology Co., Limited Positive electrode material for li-ion battery, method for preparing the same, and li-ion power battery containing the same

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112599781A (en) * 2020-12-15 2021-04-02 荆门市格林美新材料有限公司 Double-concentration gradient doped lithium ion battery anode material and preparation method thereof

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Application publication date: 20190809