CN107248572A - A kind of preparation method of the ultra-thin rich nickel ternary nano piece positive electrode of lithium ion battery - Google Patents

A kind of preparation method of the ultra-thin rich nickel ternary nano piece positive electrode of lithium ion battery Download PDF

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Publication number
CN107248572A
CN107248572A CN201710455902.8A CN201710455902A CN107248572A CN 107248572 A CN107248572 A CN 107248572A CN 201710455902 A CN201710455902 A CN 201710455902A CN 107248572 A CN107248572 A CN 107248572A
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nickel
ultra
preparation
thin
lithium
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曹传宝
吴宇
王然
张君婷
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Beijing Institute of Technology BIT
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Beijing Institute of Technology BIT
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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
    • H01M4/362—Composites
    • H01M4/364—Composites as mixtures
    • 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
    • H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
    • 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
    • H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
    • 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
    • H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
    • H01M4/581—Chalcogenides or intercalation compounds thereof
    • H01M4/5815—Sulfides
    • 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
    • H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
    • H01M4/582—Halogenides
    • 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)
  • Composite Materials (AREA)
  • Battery Electrode And Active Subsutance (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)

Abstract

The present invention relates to a kind of preparation method of the ultra-thin rich nickel ternary nano piece positive electrode of lithium ion battery.Mainly include the following steps that：It is 1 by mol ratio:The nickel salt and alkaline reagent of (1~8) are dissolved in hydrophilic solvent, fully after dissolving, the condensing reflux under microwave-excitation heating condition, naturally cool to after room temperature and be centrifugally separating to obtain ultra-thin nickel hydroxide presoma, then by simple high temperature solid-state method, ultra-thin rich nickel ternary nano piece can be obtained.Preparation method technique of the present invention is simple, and easy to operate, cost is low, has the advantages that controllable preparation, largely synthesizes, beneficial to industrial volume production.

Description

A kind of preparation method of the ultra-thin rich nickel ternary nano piece positive electrode of lithium ion battery
Technical field
The present invention relates to a kind of preparation method of anode material for lithium-ion batteries and application, specially ultra-thin rich nickel ternary is received The preparation method of rice piece, belongs to new energy materialses technology of preparing and application field.
Background technology
One of current lithium ion battery development trend is exactly to improve its energy density, while ensure that there is relatively low price, High heat endurance and the cycle life of length.In LiCoO2Many replacement candidates materials in, LiNiO2Because of its high power capacity, low Cost, of low pollution and paid close attention to by people.However, the LiNiO of metering ratio2It is difficult to prepare to be, and it is poor to there is cycle performance With the defect such as thermal stability difference, almost without actual application value.The Co and Al that adulterates is maximally effective approach, both maintains material The layer structure characteristic of material, improves the cycle performance and high rate performance of material again.
However, traditional block materials have reached their limitations in itself in performance, lasting increasing can not be met Long high-energy and power density requirements.Recently, nano structural material turns into the main drive for solving these limitations.Tool The rich nickel tertiary cathode material for having different nanostructureds has been reported, and these materials have excellent chemical property.It is near Nian Lai, reduction scantling synthesizes the main ultrathin nanometer sheet material being made up of surface, due to being passed there is provided efficient electric charge Defeated and mass transfer, can obtain more excellent performance.Although ultrathin nanometer piece negative material is by wide coverage, Because synthesis positive electrode needs prolonged high-temperature calcination, structural damage can be caused, with ultrathin nanometer chip architecture positive pole Material is not reported also.Applicant is rationally designed, and the rich nickel ternary nano of high-quality ultra-thin has been gone out by Microwave-assisted synthesis Piece.This method operating procedure is simple, raw material is easy to get, and is adapted to industrialized production.Reported as far as the applicant is aware, having no up to now Utilize the method for the ultra-thin rich nickel ternary nano piece of Microwave-assisted synthesis.Prepared ultra-thin rich nickel ternary nano piece can be used as lithium Ion battery positive electrode, and be the electrode material that a class has wide application prospect with good chemical property.
The content of the invention
The purpose of the present invention conveniently, simply, is inexpensively saved with overcoming the defect of above-mentioned prior art presence there is provided one kind Prepare ultra-thin rich nickel ternary nano piece preparation method on a large scale.The present invention is quick by one kind, and simple microwave method can be synthesized Substantial amounts of nickel hydroxide presoma.Then by simple high temperature solid-state method, ultra-thin rich nickel ternary nano piece positive pole can be obtained Material.
The technical scheme of the ultra-thin rich nickel ternary nano piece positive electrode of the present invention is as follows：
(1) it is 1 by mol ratio:The nickel salt and alkaline reagent of (1~8) are dissolved in hydrophilic solvent, fully after dissolving, solution The molar concentration of middle nickel ion is 0.05~2.0mol/L, and the condensing reflux under microwave-excitation heating condition naturally cools to room Ultra-thin nickel hydroxide presoma is centrifugally separating to obtain after temperature.
(2) it is (1-x-y) by mol ratio:(1~1.3):a:B ultra-thin nickel hydroxide presoma and lithium salts, cobalt salt and aluminium Salt is sufficiently mixed in ethanol, wherein 0.1≤x≤0.15,0 ＜ y ＜ 0.1, are then dried under the conditions of 120 DEG C, grinds 30 points Presoma powder is obtained after clock, finally, presoma powder is transferred in high temperature furnace and is heat-treated 1 at a temperature of 500~1000 DEG C ~20 hours, it is cooled to room temperature with furnace temperature and obtains the ultra-thin rich nickel ternary nano piece positive electrode of lithium ion battery.
Above-described nickel salt is：Mixing more than one or both of nickel chloride, nickel nitrate, nickel acetate, nickel sulfate Salt；The alkaline reagent is：Mixed base more than one or both of urea, sodium hydroxide, ammoniacal liquor, ammonium hydrogen carbonate；It is described Hydrophilic agent is：Deionized water, ethanol, ethylene glycol, isopropanol, normal propyl alcohol, n-butanol, one or both of isobutanol with On mixed solvent；The lithium salts is：Lithium acetate, lithium carbonate, lithium hydroxide, the one or more kinds of mixing lithium of lithium nitrate Salt；Described cobalt salt is：Salt-mixture more than one or both of cobalt chloride, cobalt nitrate, cobalt acetate, cobaltous sulfate；The aluminium Salt is：Aluminium acetate, aluminium hydroxide, the one or more kinds of mixing lithium salts of aluminum nitrate.
Obtained ultra-thin rich nickel ternary nano piece better crystallinity degree produced according to the present invention, is a kind of excellent lithium of cycle performance Ion battery positive electrode.In addition, the microwave liquid phase synthesizing method that the present invention is used, reaction time is short, and reaction yield is high, into This is low, and process route is simple, and energy consumption is low, is adapted to industrial volume production.
Brief description of the drawings
Fig. 1 is the X-ray diffractogram (XRD) of ultra-thin rich nickel ternary nano piece in the embodiment of the present invention 1.
Fig. 2 is the transmission electron microscope figure (TEM) of nickel hydroxide in the embodiment of the present invention 1.
Fig. 3 is the transmission electron microscope figure (TEM) of ultra-thin rich nickel ternary nano piece in the embodiment of the present invention 1.
Fig. 4 is the scanning electron microscope diagram (SEM) of ultra-thin rich nickel ternary nano piece in the embodiment of the present invention 1
Fig. 5 is the cycle performance figure of ultra-thin rich nickel ternary nano piece in the embodiment of the present invention 1.
Embodiment
From following examples it will be further appreciated that the present invention, but the claimed scope of the invention is not limited to following reality Apply the express ranges of example.
Embodiment 1
(1) it is 1 by mol ratio:2 nickel nitrate and urea is dissolved in ethylene glycol, fully after dissolving, nickel ion in solution Molar concentration is 0.2mol/L, the condensing reflux under microwave-excitation heating condition, naturally cools to after room temperature and is centrifugally separating to obtain Ultra-thin nickel hydroxide presoma.
(2) it is 0.80 by mol ratio:1.05:0.15:0.05 ultra-thin nickel hydroxide presoma and lithium carbonate, cobalt nitrate and Lithium nitrate is sufficiently mixed in ethanol, is then dried under the conditions of 120 DEG C, and grinding obtains presoma powder after 30 minutes, finally, Presoma powder is transferred in high temperature furnace and is heat-treated 8 hours at a temperature of 700 DEG C, room temperature is cooled to furnace temperature and obtains lithium ion The ultra-thin rich nickel ternary nano piece positive electrode of battery.
Fig. 1 is the X ray diffracting spectrum of the ultra-thin rich nickel ternary nano piece obtained by the present embodiment, the crystal of analysis of material Structure.Fig. 2,3 be the transmission electron micrograph of nickel hydroxide and ultra-thin rich nickel ternary nano piece respectively, it can be seen that Obtained material morphology and size ratio are more uniform, good dispersion.Fig. 4 is the scanning of obtained ultra-thin rich nickel ternary nano piece Electron microscope picture.It is assembled into after battery, ultra-thin rich nickel ternary nano piece has excellent cycle performance (Fig. 5).
Embodiment 2
(1) it is 1 by mol ratio:1 nickel acetate and sodium hydroxide is dissolved in deionized water, fully after dissolving, nickel in solution The molar concentration of ion is 0.05mol/L, and the condensing reflux under microwave-excitation heating condition naturally cools to centrifugation point after room temperature From obtaining ultra-thin nickel hydroxide presoma.
(2) it is 0.85 by mol ratio:1.05:0.10:0.05 ultra-thin nickel hydroxide presoma and lithium hydroxide, cobalt acetate It is sufficiently mixed, is then dried under the conditions of 120 DEG C in ethanol with aluminium acetate, grinding obtains presoma powder after 30 minutes, most Afterwards, presoma powder is transferred in high temperature furnace and be heat-treated 12 hours at a temperature of 600 DEG C, be cooled to room temperature with furnace temperature and obtain lithium The ultra-thin rich nickel ternary nano piece positive electrode of ion battery.
Embodiment 3
(1) it is 1 by mol ratio:3 nickel nitrate and urea is dissolved in deionized water, fully after dissolving, nickel ion in solution Molar concentration be 1mol/L, the condensing reflux under microwave-excitation heating condition naturally cools to after room temperature and is centrifugally separating to obtain Ultra-thin nickel hydroxide presoma.
(2) it is 0.80 by mol ratio:1.10:0.10:0.10 ultra-thin nickel hydroxide presoma and lithium hydroxide, cobalt nitrate It is sufficiently mixed, is then dried under the conditions of 120 DEG C in ethanol with aluminium acetate, grinding obtains presoma powder after 30 minutes, most Afterwards, presoma powder is transferred in high temperature furnace and be heat-treated 6 hours at a temperature of 800 DEG C, be cooled to room temperature with furnace temperature and obtain lithium The ultra-thin rich nickel ternary nano piece positive electrode of ion battery.
Embodiment 4
(1) it is 1 by mol ratio:4 nickel acetate and sodium hydroxide is dissolved in ethylene glycol, fully dissolving after, in solution nickel from The molar concentration of son is 1.5mol/L, and the condensing reflux under microwave-excitation heating condition is naturally cooled to after room temperature and centrifuged Obtain ultra-thin nickel hydroxide presoma.
(2) it is 0.80 by mol ratio:1.05:0.15:0.05 ultra-thin nickel hydroxide presoma and lithium carbonate, cobalt nitrate and Aluminium acetate is sufficiently mixed in ethanol, is then dried under the conditions of 120 DEG C, and grinding obtains presoma powder after 30 minutes, finally, Presoma powder is transferred in high temperature furnace and is heat-treated 4 hours at a temperature of 900 DEG C, room temperature is cooled to furnace temperature and obtains lithium ion The ultra-thin rich nickel ternary nano piece positive electrode of battery.

Claims (7)

1. a kind of preparation method of the ultra-thin rich nickel ternary nano piece positive electrode of lithium ion battery, comprises the following steps：
(1) it is 1 by mol ratio:The nickel salt and alkaline reagent of (1~8) are dissolved in hydrophilic solvent, fully after dissolving, nickel in solution The molar concentration of ion is 0.05~2.0mol/L, and the condensing reflux under microwave-excitation heating condition is naturally cooled to after room temperature It is centrifugally separating to obtain ultra-thin nickel hydroxide presoma.
(2) it is (1-x-y) by mol ratio:(1~1.3):a:B ultra-thin nickel hydroxide presoma and lithium salts, cobalt salt and aluminium salt exist It is sufficiently mixed in ethanol, wherein 0.1≤x≤0.15,0 ＜ y ＜ 0.1, are then dried under the conditions of 120 DEG C, after grinding 30 minutes Presoma powder is obtained, finally, presoma powder is transferred in high temperature furnace at a temperature of 500~1000 DEG C and is heat-treated 1~20 Hour, it is cooled to room temperature with furnace temperature and obtains the ultra-thin rich nickel ternary nano piece positive electrode of lithium ion battery.
2. preparation method as claimed in claim 1, it is characterised in that：The nickel salt is nickel chloride, nickel nitrate, nickel acetate, sulphur Salt-mixture more than one or both of sour nickel.
3. preparation method as claimed in claim 1, it is characterised in that：The alkaline reagent be urea, sodium hydroxide, ammoniacal liquor, Mixed base more than one or both of ammonium hydrogen carbonate.
4. preparation method as claimed in claim 1, it is characterised in that：The hydrophilic agent is deionized water, ethanol, second two Mixed solvent more than one or both of alcohol, isopropanol, normal propyl alcohol, n-butanol, isobutanol.
5. preparation method as claimed in claim 1, it is characterised in that：The lithium salts be lithium acetate, lithium carbonate, lithium hydroxide, The one or more kinds of mixing lithium salts of lithium nitrate.
6. preparation method as claimed in claim 1, it is characterised in that：The cobalt salt is cobalt chloride, cobalt nitrate, cobalt acetate, sulphur Salt-mixture more than one or both of sour cobalt.
7. preparation method as claimed in claim 1, it is characterised in that：The aluminium salt is aluminium acetate, aluminium hydroxide, aluminum nitrate one Plant or two or more mixing lithium salts.
CN201710455902.8A 2017-08-28 2017-08-28 A kind of preparation method of the ultra-thin rich nickel ternary nano piece positive electrode of lithium ion battery Pending CN107248572A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109704413A (en) * 2018-12-07 2019-05-03 北京理工大学 A kind of nickelic positive electrode and the method for improving nickelic positive electrode storge quality

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102074679A (en) * 2010-12-18 2011-05-25 中南大学 Method for preparing spherical aluminum-doped nickel lithium carbonate for lithium ion battery positive electrode material
CN103035898A (en) * 2012-12-21 2013-04-10 深圳市天骄科技开发有限公司 Nano flaky positive electrode material of lithium ion battery and preparation method for positive electrode material
CN103159264A (en) * 2013-03-18 2013-06-19 昆明理工大学 Method for preparing positive material NCA of lithium ion cell by virtue of pure solid phase method
CN103342396A (en) * 2013-06-21 2013-10-09 北京理工大学 Method for microwave liquid-phase synthesis of graphene-like two-dimensional nickel hydroxide nano material

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102074679A (en) * 2010-12-18 2011-05-25 中南大学 Method for preparing spherical aluminum-doped nickel lithium carbonate for lithium ion battery positive electrode material
CN103035898A (en) * 2012-12-21 2013-04-10 深圳市天骄科技开发有限公司 Nano flaky positive electrode material of lithium ion battery and preparation method for positive electrode material
CN103159264A (en) * 2013-03-18 2013-06-19 昆明理工大学 Method for preparing positive material NCA of lithium ion cell by virtue of pure solid phase method
CN103342396A (en) * 2013-06-21 2013-10-09 北京理工大学 Method for microwave liquid-phase synthesis of graphene-like two-dimensional nickel hydroxide nano material

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109704413A (en) * 2018-12-07 2019-05-03 北京理工大学 A kind of nickelic positive electrode and the method for improving nickelic positive electrode storge quality
CN109704413B (en) * 2018-12-07 2021-10-12 北京理工大学 High-nickel anode material and method for improving storage performance of high-nickel anode material

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