CN106328893A - Surface modified coated LiNi0.5Mn1.5O4 material, preparation method thereof and lithium battery - Google Patents
Surface modified coated LiNi0.5Mn1.5O4 material, preparation method thereof and lithium battery Download PDFInfo
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- CN106328893A CN106328893A CN201610790144.0A CN201610790144A CN106328893A CN 106328893 A CN106328893 A CN 106328893A CN 201610790144 A CN201610790144 A CN 201610790144A CN 106328893 A CN106328893 A CN 106328893A
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- H—ELECTRICITY
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
- H01M4/505—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
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- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
- H01M4/525—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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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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- H01M2220/00—Batteries for particular applications
- H01M2220/20—Batteries in motive systems, e.g. vehicle, ship, plane
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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
- H01M2220/00—Batteries for particular applications
- H01M2220/30—Batteries in portable systems, e.g. mobile phone, laptop
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- 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
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- 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 invention discloses a surface modified coated LiNi0.5Mn1.5O4 material, a preparation method thereof and a lithium battery. The material LiNi0.5Mn1.5O4 with the surface modified is coated with Li4Ti5O12 adopting a spinel structure. The material is small and uniform in particle size, electrochemical performance of LiNi0.5Mn1.5O4 can be improved, the prepared material with the surface modified is coated with electrochemically inert Li4Ti5O12, so that not only can LiNi0.5Mn1.5O4 have a good spinel structure in charge-discharge processes, but also a side reaction between LiNi0.5Mn1.5O4 and an electrolyte can be inhibited, and compared with materials coated with certain metal oxides, the LiNi0.5Mn1.5O4 material better facilitates conduction of Li ions; the method has the advantages that operation is simple, preparation is convenient and the cost is low, thereby being applicable to industrialized large-scale production.
Description
Technical field
The present invention relates to electrochemical field, be specifically related to the cladded type nickel ion doped material of a kind of surface modification, lithium battery
And preparation method thereof.
Background technology
Relative to conventional batteries, such as lead-acid battery, nickel-cadmium cell and Ni-MH battery, lithium ion battery has energy density
High, have extended cycle life, the outstanding advantage such as self-discharge rate is little, memory-less effect and environmental protection, from the beginning of the nineties by Sony
After developing, lithium ion battery is widely used in the life of people, such as portable type electronic product, new forms of energy
The field such as the vehicles and energy storage.Development along with lithium ion battery technology, it is desirable to lithium ion battery has high-energy-density, height
The feature such as power, low cost.The one-tenth of lithium ion battery is grouped into and generally comprises: positive electrode, negative material, electrolyte, barrier film,
Wherein the performance of positive electrode is the key factor affecting lithium ion battery combination property.At present, business-like lithium ion battery
Positive electrode mainly has cobalt acid lithium (LiCoO2) positive electrode, LiMn2O4 (Li2MnO4) positive electrode, ternary material positive electrode,
Lithium iron phosphate positive material.But, above-mentioned positive electrode has a respective shortcoming:
(1)LiCoO2Positive electrode has shortcomings such as cost is high, environmental pollution is serious, and blanking voltage more than 4.4V with
On, material structure is unstable, the shortcoming that circulation, security performance are deteriorated；
(2)Li2MnO4The high temperature circulation of positive electrode is not good enough with storge quality；
(3) ternary material positive electrode compacted density is on the low side, and its high rate performance is relatively low with security performance；
(4) lithium iron phosphate positive material specific discharge capacity is the highest, and tap density is on the low side, and product exists more serious consistent
Sex chromosome mosaicism.
Spinel nickel manganate cathode material for lithium due to advantages such as its high rate performance are excellent, running voltage is high, with low cost, one
It it is directly the study hotspot of anode material for lithium-ion batteries.But spinel nickel manganate cathode material for lithium surface texture is unstable, follow
The shortcomings such as the manganese metal dissolution during ring seriously inhibit the large-scale application of spinel nickel manganate cathode material for lithium.In order to open
The spinel nickel manganate cathode material for lithium that volatility is excellent, meets the electric motor car requirement to battery high rate performance, and researcher grinds
Send out and disclose multiple technologies means spinel nickel manganate cathode material for lithium is modified.
Method of modifying one: obtained the nickel ion doped material of aluminium hydroxide cladding by liquid phase coating, be subsequently placed in Muffle furnace
The middle 300-450 DEG C of nickel lithium manganate cathode material being thermally treated resulting in aluminium hydroxide coating modification, modified nickel ion doped positive pole
The more uncoated material of material improves about 10%.
Method of modifying two: use sol-gel process to combine with solid phase method, so that at LiNi0.5Mn1.5O4Material bag
The Li covered2TiO3It is evenly distributed, having good uniformity of the final positive electrode prepared so that the positive electrode prepared has well
Cycle performance and high rate performance.
Method of modifying three: by adding microwave susceptor zirconium oxide in presoma preparation process, promote reaction mass
Effectively absorbing microwave to be rapidly heated to reaction temperature 700-950 DEG C, the microwave firing time of notable shortening product was to 1-10 minute；
While at high temperature nickel ion doped material burns till, zirconium oxide and Li source are reacted at nickel ion doped Surface Creation lithium ion conductor
Li2ZrO3Clad, is obviously improved cycle performance and the high rate performance of product.
It is relative complex to there is technique in above method so that it is be difficult to carry out industrialized production, simultaneously for manganese metal dissolution also
Do not have corresponding method to solve, therefore, be badly in need of working out not only can ensure that nickel ion doped has well in charge and discharge process
Lithium ionic mobility and structural stability, and the method for modifying of nickel ion doped and electrolyte generation side reaction can be suppressed.
Summary of the invention
It is an object of the invention to overcome the shortcoming of prior art, it is provided that the cladded type nickel ion doped material of a kind of surface modification
Material；
Another object of the present invention is to provide the preparation method of the cladded type nickel ion doped material of surface modification；
The third object of the present invention is the lithium providing a kind of cladded type nickel ion doped material using surface modification to prepare
Battery.
The purpose of the present invention is achieved through the following technical solutions: the cladded type nickel ion doped material of a kind of surface modification,
Described material is LiNi0.5Mn1.5O4The Li of one layer of spinel structure of cladding of surface modification4Ti5O12。
A kind of preparation method of the cladded type nickel ion doped material of surface modification, it comprises the following steps:
S1. Li is pressed4Ti5O12Lithium source, titanium source and gelatinizing agent dispersion stirring in a solvent is formed colloidal sol by stoichiometric proportion, then
By LiNi0.5Mn1.5O4Join dispersed with stirring in colloidal sol uniform, continue heated and stirred and obtain gel；
S2. by gel drying, burn till, crushing and classification, prepare surface modification cladded type nickel ion doped material.
Further, one during described organic solvent is methanol, ethanol, normal propyl alcohol, isopropanol, ethylene glycol or acetone or
Multiple.
Further, described gelatinizing agent is glacial acetic acid, tartaric acid, oxalic acid, citric acid, ascorbic acid, salicylic acid or propylene
At least one in acid.
Further, described lithium source is lithium salts, and described titanium source is butyl titanate, isopropyl titanate, titanium tetrachloride, sulphuric acid oxygen
At least one in titanium, metatitanic acid methyl ester or iso-butyl titanate.
Further, described at least one used in spray drying, vacuum drying, forced air drying dry.
Further, described in the temperature burnt till be 500～900 DEG C, firing time is 5～24h；Burn till employing Muffle furnace,
Any one in atmosphere furnace, roller kilns or pushed bat kiln burns till.
Further, the pulverizing in described crushing and classification uses mechanical crusher, jet mill, grinder or low temperature
At least one in pulverizer.
A kind of lithium battery, the positive electrode of described lithium battery include above-mentioned surface modification cladded type nickel ion doped material or
By the cladded type nickel ion doped material of the surface modification that preparation method as above prepares.
Further, the negative material of described lithium battery is graphite, silicon, lithium titanate, graphite modified material, Si modification material
Or lithium titanate material modified at least one.
The invention have the advantages that and the invention provides the cladded type nickel ion doped material of a kind of surface modification, lithium electricity
Pond and preparation method thereof, surface modification be coated with Li4Ti5O12Nickel ion doped material particle size little and uniform, be conducive to improve
LiNi0.5Mn1.5O4Chemical property, the cladded type nickel ion doped material surface modifying of the surface modification of preparation be coated with electricity
Chemically inert Li4Ti5O12, not only can ensure that LiNi0.5Mn1.5O4There is in charge and discharge process good spinel structure,
And LiNi can be suppressed0.5Mn1.5O4With electrolyte generation side reaction；Compare some metal-oxides of cladding, material of the present invention
It is more beneficial for the conduction of lithium ion；The method of the cladded type nickel ion doped material preparing this surface modification has simple to operate, system
Standby convenient, low cost, it is adaptable to industrialization large-scale production.
Detailed description of the invention
Below in conjunction with embodiment, the present invention will be further described, and protection scope of the present invention is not limited to following institute
State.
Embodiment 1: the cladded type nickel ion doped material of a kind of surface modification, described material is LiNi0.5Mn1.5O4Surface changes
The Li of one layer of spinel structure of cladding of property4Ti5O12。
The preparation method of the cladded type nickel ion doped material of above-mentioned surface modification, it comprises the following steps:
S1. solid phase method is used to prepare LiNi0.5Mn1.5O4, by Li4Ti5O12Stoichiometric proportion is by Quilonorm (SKB), butyl titanate
Colloidal sol is formed with citric acid dispersion stirring in ethanol, then by LiNi0.5Mn1.5O4Join dispersed with stirring in glue uniform, continue
Continuous heated and stirred obtains gel；
S2. by gel drying, burn till, crushing and classification, prepare surface modification cladded type nickel ion doped material.
Described dry employing is spray-dried；The described temperature burnt till is 700 DEG C, and firing time is 12h；Described crushing and classification
In pulverizing use mechanical crusher, burn till employing Muffle furnace.
Prepare lithium battery: the positive electrode of lithium battery includes using the cladded type nickel ion doped material of above-mentioned surface modification,
The negative material of lithium battery is graphite.
Embodiment 2: the cladded type nickel ion doped material of a kind of surface modification, described material is LiNi0.5Mn1.5O4Surface changes
The Li of one layer of spinel structure of cladding of property4Ti5O12。
The preparation method of the cladded type nickel ion doped material of above-mentioned surface modification, it comprises the following steps:
S1. liquid phase method is used to prepare LiNi0.5Mn1.5O4, by Li4Ti5O12Stoichiometric proportion by lithium nitrate, isopropyl titanate and
Tartaric acid is dispersed in isopropanol stirring and forms colloidal sol, then by LiNi0.5Mn1.5O4Join dispersed with stirring in glue uniform, continue
Continuous heated and stirred obtains gel；
S2. by gel drying, burn till, crushing and classification, prepare surface modification cladded type nickel ion doped material.
Described dry employing is vacuum dried and forced air drying；The described temperature burnt till is 800 DEG C, and firing time is 6h；Institute
State the pulverizing in crushing and classification and use jet mill and grinder, burn till employing atmosphere furnace.
Prepare lithium battery: the positive electrode of lithium battery includes using the cladded type nickel ion doped material of above-mentioned surface modification,
The negative material of lithium battery is lithium titanate.
Embodiment 3: the cladded type nickel ion doped material of a kind of surface modification, described material is LiNi0.5Mn1.5O4Surface changes
The Li of one layer of spinel structure of cladding of property4Ti5O12。
The preparation method of the cladded type nickel ion doped material of above-mentioned surface modification, it comprises the following steps:
S1. solid phase method is used to prepare LiNi0.5Mn1.5O4, by Li4Ti5O12Stoichiometric proportion by Quilonorm (SKB), titanium tetrachloride and
Glacial acetic acid is dispersed in normal propyl alcohol stirring and forms colloidal sol, then by LiNi0.5Mn1.5O4Join dispersed with stirring in glue uniform, continue
Continuous heated and stirred obtains gel；
S2. by gel drying, burn till, crushing and classification, prepare surface modification cladded type nickel ion doped material.
Described dry employing vacuum drying, forced air drying and spray drying；The described temperature burnt till 500 DEG C, firing time
For 24h；Pulverizing in described crushing and classification uses jet mill and Lowtemperaturepulverizer, burns till employing roller kilns.
Prepare lithium battery: the positive electrode of lithium battery includes using the cladded type nickel ion doped material of above-mentioned surface modification,
The negative material of lithium battery is silicon.
Embodiment 4: the cladded type nickel ion doped material of a kind of surface modification, described material is LiNi0.5Mn1.5O4Surface changes
The Li of one layer of spinel structure of cladding of property4Ti5O12。
The preparation method of the cladded type nickel ion doped material of above-mentioned surface modification, it comprises the following steps:
S1. liquid phase method is used to prepare LiNi0.5Mn1.5O4, by Li4Ti5O12Stoichiometric proportion by lithium nitrate, titanyl sulfate and
Ascorbic acid is dispersed in isopropanol stirring and forms colloidal sol, then by LiNi0.5Mn1.5O4Join dispersed with stirring in glue uniform,
Continue heated and stirred and obtain gel；
S2. by gel drying, burn till, crushing and classification, prepare surface modification cladded type nickel ion doped material.
Described dry employing is vacuum dried；The described temperature burnt till is 900 DEG C, and firing time is 6h；Described crushing and classification
In pulverizing use Lowtemperaturepulverizer, burn till employing atmosphere furnace.
Prepare lithium battery: the positive electrode of lithium battery includes using the cladded type nickel ion doped material of above-mentioned surface modification,
The negative material of lithium battery is that lithium titanate is material modified.
Embodiment 5: the cladded type nickel ion doped material of a kind of surface modification, described material is LiNi0.5Mn1.5O4Surface changes
The Li of one layer of spinel structure of cladding of property4Ti5O12。
The preparation method of the cladded type nickel ion doped material of above-mentioned surface modification, it comprises the following steps:
S1. liquid phase method is used to prepare LiNi0.5Mn1.5O4, by Li4Ti5O12Stoichiometric proportion by lithium acetate, metatitanic acid methyl ester and
Salicylic acid is dispersed in ethylene glycol stirring and forms colloidal sol, then by LiNi0.5Mn1.5O4Join dispersed with stirring in glue uniform, continue
Continuous heated and stirred obtains gel；
S2. by gel drying, burn till, crushing and classification, prepare surface modification cladded type nickel ion doped material.
Described dry employing is spray-dried and forced air drying；The described temperature burnt till is 600 DEG C, and firing time is 10h；Institute
State the pulverizing in crushing and classification and use jet mill and Lowtemperaturepulverizer, burn till employing pushed bat kiln.
Prepare lithium battery: the positive electrode of lithium battery includes using the cladded type nickel ion doped material of above-mentioned surface modification,
The negative material of lithium battery is Si modification material.
Embodiment 6: the cladded type nickel ion doped material of a kind of surface modification, described material is LiNi0.5Mn1.5O4Surface changes
The Li of one layer of spinel structure of cladding of property4Ti5O12。
The preparation method of the cladded type nickel ion doped material of above-mentioned surface modification, it comprises the following steps:
S1. liquid phase method is used to prepare LiNi0.5Mn1.5O4, by Li4Ti5O12Stoichiometric proportion is by Quilonorm (SKB), iso-butyl titanate
Colloidal sol is formed with acrylic acid dispersion stirring in acetone, then by LiNi0.5Mn1.5O4Join dispersed with stirring in glue uniform, continue
Continuous heated and stirred obtains gel；
S2. by gel drying, burn till, crushing and classification, prepare surface modification cladded type nickel ion doped material.
Described dry employing is vacuum dried and forced air drying；The described temperature burnt till is 850 DEG C, and firing time is 18h；Institute
State the pulverizing in crushing and classification and use mechanical crusher, jet mill and grinder, burn till employing roller kilns.
Prepare lithium battery: the positive electrode of lithium battery includes using the cladded type nickel ion doped material of above-mentioned surface modification,
The negative material of lithium battery is graphite modified material.
Claims (10)
1. the cladded type nickel ion doped material of a surface modification, it is characterised in that described material is LiNi0.5Mn1.5O4Surface changes
The Li of one layer of spinel structure of cladding of property4Ti5O12。
The preparation method of the cladded type nickel ion doped material of a kind of surface modification the most as claimed in claim 1, it is characterised in that
It comprises the following steps:
S1. Li is pressed4Ti5O12Lithium source, titanium source and gelatinizing agent dispersion stirring in a solvent is formed colloidal sol by stoichiometric proportion, then will
LiNi0.5Mn1.5O4Join dispersed with stirring in colloidal sol uniform, continue heated and stirred and obtain gel；
S2. by gel drying, burn till, crushing and classification, prepare surface modification cladded type nickel ion doped material.
The preparation method of the cladded type nickel ion doped material of a kind of surface modification the most as claimed in claim 2, it is characterised in that
Described organic solvent is one or more in methanol, ethanol, normal propyl alcohol, isopropanol, ethylene glycol or acetone.
The preparation method of the cladded type nickel ion doped material of a kind of surface modification the most as claimed in claim 2, it is characterised in that
Described gelatinizing agent is at least one in glacial acetic acid, tartaric acid, oxalic acid, citric acid, ascorbic acid, salicylic acid or acrylic acid.
The preparation method of the cladded type nickel ion doped material of a kind of surface modification the most as claimed in claim 2, it is characterised in that
Described lithium source is lithium salts, and described titanium source is butyl titanate, isopropyl titanate, titanium tetrachloride, titanyl sulfate, metatitanic acid methyl ester or metatitanic acid
At least one in isobutyl ester.
The preparation method of the cladded type nickel ion doped material of a kind of surface modification the most as claimed in claim 2, it is characterised in that
Described at least one used in spray drying, vacuum drying, forced air drying dry.
The preparation method of the cladded type nickel ion doped material of a kind of surface modification the most as claimed in claim 2, it is characterised in that
The described temperature burnt till is 500～900 DEG C, and firing time is 5～24h, burns till employing Muffle furnace, atmosphere furnace, roller kilns or pushes away
Any one in plate kiln burns till.
The preparation method of the cladded type nickel ion doped material of a kind of surface modification the most as claimed in claim 2, it is characterised in that
In described crushing and classification pulverize in employing mechanical crusher, jet mill, grinder or Lowtemperaturepulverizer at least one
Kind.
9. a lithium battery, it is characterised in that the positive electrode of described lithium battery includes surface modification as claimed in claim 1
Cladded type nickel ion doped material or the surface modification that prepared by preparation method as described in any one in claim 2-8
Cladded type nickel ion doped material.
10. lithium battery as claimed in claim 9 a kind of, it is characterised in that the negative material of described lithium battery be graphite, silicon,
At least one during lithium titanate, graphite modified material, Si modification material or lithium titanate are material modified.
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| CN107154492A (en) * | 2017-05-22 | 2017-09-12 | 东北大学 | A kind of surface modification LATO LNMO electrode materials and preparation method |
| CN107154492B (en) * | 2017-05-22 | 2019-07-09 | 东北大学 | A kind of the LNMO electrode material and preparation method of surface modification LATO |
| CN107293720A (en) * | 2017-06-28 | 2017-10-24 | 合肥国轩高科动力能源有限公司 | A kind of zirconium scandium composite oxides cladding lithium titanate anode material and preparation method thereof |
| CN107658437A (en) * | 2017-08-28 | 2018-02-02 | 河南工程学院 | A kind of preparation method of coating modification high-voltage lithium nickel manganate material |
| CN109904424A (en) * | 2019-02-28 | 2019-06-18 | 河南大学 | The method of one-step method surface cladding and the double modification LNMO positive electrodes of grade doping integration |
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