CN104505508A - Preparation method of nickel cobalt oxide electrode material - Google Patents

Preparation method of nickel cobalt oxide electrode material Download PDF

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Publication number
CN104505508A
CN104505508A CN201410778878.8A CN201410778878A CN104505508A CN 104505508 A CN104505508 A CN 104505508A CN 201410778878 A CN201410778878 A CN 201410778878A CN 104505508 A CN104505508 A CN 104505508A
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electrode material
nickel
cobalt
preparation
salt
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CN201410778878.8A
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Inventor
金玉红
王莉
何向明
李建军
尚玉明
张玉峰
赵鹏
张艳丽
高剑
王要武
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JIANGSU HEZHI LITHIUM-SULFUR BATTERY TECHNOLOGY Co Ltd
Tsinghua University
Jiangsu Huadong Institute of Li-ion Battery Co Ltd
Original Assignee
JIANGSU HEZHI LITHIUM-SULFUR BATTERY TECHNOLOGY Co Ltd
Tsinghua University
Jiangsu Huadong Institute of Li-ion Battery Co Ltd
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Priority to CN201410778878.8A priority Critical patent/CN104505508A/en
Publication of CN104505508A publication Critical patent/CN104505508A/en
Priority to PCT/CN2015/095405 priority patent/WO2016095669A1/en
Pending legal-status Critical Current

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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
    • H01M4/52—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
    • H01M4/36—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
    • 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
    • H01M4/131—Electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
    • 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
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

Abstract

The invention relates to a preparation method of a Ni1.5Co1.5O4 electrode material, which comprises the following steps: providing a nickel salt, a cobalt salt, hexamethylenetetramine, ethanol and water, wherein the mass ratio of the ethanol to the water is greater than 1:1 and less than or equal to 4:1; mixing the nickel salt, cobalt salt, hexamethylenetetramine, ethanol and water, and dissolving the nickel salt, cobalt salt and hexamethylenetetramine to obtain a mixed solution; carrying out solvothermal reaction on the mixed solution to obtain a precursor; and sintering the precursor in an oxygen-containing atmosphere to obtain the Ni1.5Co1.5O4 electrode material, wherein the Ni1.5Co1.5O4 electrode material is a plurality of three-dimensional flower-like structures which are self-assembled by Ni1.5Co1.5O4 nanosheets.

Description

The preparation method of nickel cobalt oxide electrode material
Technical field
The present invention relates to a kind of preparation method of electrode material, particularly relate to a kind of Ni 1.5co 1.5o 4the preparation method of electrode material.
Background technology
Good conductivity, theoretical ratio capacitance are high owing to having for nickel cobalt oxide, good cycle and advantages of environment protection and become a kind of ideal electrode material for lithium ion battery and ultracapacitor that can meet practical application.But be used as the nickel cobalt oxide mainly cobalt acid nickel (NiCo of lithium ion battery and electrode material for super capacitor at present 2o 4), also not by other nickel cobalt oxides as Ni 1.5co 1.5o 4as the research of lithium ion battery and electrode material for super capacitor.
But, people study nickel cobalt oxide is used as energy gap larger semi-conducting material time, find Ni 1.5co 1.5o 4have and compare NiCo 2o 4better electric conductivity.Conductivity is higher, and the performance used as electrode material is also better, but prior art is mainly by Ni 1.5co 1.5o 4film is used as semi-conducting material, due to this Ni 1.5co 1.5o 4film does not almost have duct, and specific area is less, is unfavorable for that the diffusion of lithium ion and electrochemical reaction active site fully react, very limited to the memory capacity of lithium ion, therefore directly by this Ni 1.5co 1.5o 4when film uses as electrode material, its chemical property is poor.
Summary of the invention
In view of this, necessaryly provide a kind of and be beneficial to lithium ion diffusion and the Ni that fully reacts of electrochemical reaction active site 1.5co 1.5o 4the preparation method of electrode material.
A kind of Ni 1.5co 1.5o 4the preparation method of electrode material, comprising:
There is provided nickel salt, cobalt salt, hexa, ethanol and water, wherein, the mass ratio of described second alcohol and water is greater than 1:1 and is less than or equal to 4:1;
Described nickel salt, cobalt salt, hexa, ethanol and water are mixed, and described nickel salt, cobalt salt, hexa are dissolved, obtain a mixed solution;
Make described mixed solution carry out hydro-thermal reaction, obtain presoma; And
Carry out under an oxygen-containing atmosphere sintering described presoma, obtain described Ni 1.5co 1.5o 4electrode material, described Ni 1.5co 1.5o 4electrode material is by Ni 1.5co 1.5o 4the multiple three-dimensional flower-shaped structure that nanometer sheet self assembly is formed.
Ni provided by the invention 1.5co 1.5o 4the preparation method of electrode material, selects hexa to carry out co-precipitation to nickel ion and cobalt ions, can obtain nickel element and cobalt element mol ratio is the Ni of 1:1 1.5co 1.5o 4electrode material, selects ethanol water and hexa to cooperatively interact to Ni simultaneously 1.5co 1.5o 4the pattern of electrode material regulates and controls, and can prepare the Ni of three-dimensional flower-shaped structure 1.5co 1.5o 4electrode material.The Ni of this three-dimensional flower-shaped structure 1.5co 1.5o 4electrode material specific area is huge, high adsorption capacity, release stress process in change in volume less, the diffusion and the electrochemical reaction active site that are more conducive to lithium ion fully react, to the raising of lithium ion memory capacity, the modification of change in volume in adsorption/desorption lithium process, the raising of speed have important meaning.This preparation method's technique is simple, environmental protection, cost are lower, can carry out large-scale production.
Accompanying drawing explanation
Fig. 1 is Ni of the present invention 1.5co 1.5o 4the flow chart of electrode material preparation method.
Fig. 2 a and Fig. 2 b is respectively the green precursor powder of the embodiment of the present invention 1 preparation and the XRD spectra of black solid powder.
Fig. 3 is the energy dispersion EDX elementary analysis figure of black solid powder prepared by the embodiment of the present invention 1.
Fig. 4 a, 4b, 4c and 4d are respectively the field emission scanning electron microscope of black solid powder under different multiplying (FESEM) figure prepared by the embodiment of the present invention 1.
Embodiment
Refer to Fig. 1, the embodiment of the present invention provides a kind of Ni 1.5co 1.5o 4the preparation method of electrode material, comprising:
S1, provides nickel salt, cobalt salt, hexa, ethanol and water, and wherein, the mass ratio of described second alcohol and water is greater than 1:1 and is less than or equal to 4:1;
S2, mixes described nickel salt, cobalt salt, hexa, ethanol and water, and described nickel salt, cobalt salt, hexa is dissolved, obtain a mixed solution;
S3, makes described mixed solution carry out hydro-thermal reaction, obtains presoma; And
S4, carries out under an oxygen-containing atmosphere sintering described presoma, obtains described Ni 1.5co 1.5o 4electrode material, described Ni 1.5co 1.5o 4electrode material is by Ni 1.5co 1.5o 4the multiple three-dimensional flower-shaped structure that nanometer sheet self assembly is formed.
In step sl, described nickel salt can be one or more in nickel nitrate, nickel chloride, nickel acetate and nickelous sulfate.Described cobalt salt can be one or more in nickel nitrate, nickel chloride, cobalt acetate and cobaltous sulfate.The mixed proportion of described nickel salt and described cobalt salt is not limit, and under any mixed proportion, all can obtain nickel element and cobalt element mol ratio is the Ni of 1:1 1.5co 1.5o 4electrode material.Preferably, in described nickel salt and described cobalt salt, the mixed proportion of nickel element and cobalt element can be 1:4 ~ 4:1.More preferably, in described nickel salt and described cobalt salt, the mixed proportion of nickel element and cobalt element can be 1:2 ~ 2:1.Within the scope of aforementioned proportion, nickel salt and cobalt salt can be utilized fully, reduce the waste of raw material.
In step s 2, described mixed solution is the settled solution of transparent and homogeneous.In described mixed solution, described second alcohol and water forms a mixed solvent, and this mixed solvent is the reaction medium of described hydro-thermal reaction.Described nickel salt, cobalt salt and hexa are dissolved in described mixed solvent.Described nickel salt and cobalt salt form nickel ion and cobalt ions after dissolving in described mixed solvent respectively.
First described second alcohol and water can be mixed to form described mixed solvent, more described nickel salt, cobalt salt and hexa are added in described mixed solvent simultaneously mix.Also first by described nickel salt, cobalt salt, the mixing of second alcohol and water, and then described hexa can be added mix.The mode of described mixing is not limit, such as, stirring or ultrasonic mode can be used to mix.
In step s3, described presoma is shallow green powder, and this shallow green powder is nickel cobalt hydroxide.In described hydrothermal reaction process, described hexa makes described nickel ion and described cobalt ions be converted to nickel cobalt hydroxide precipitation as precipitation reagent, and due to the Precipitation Potential of described hexa to described nickel ion and described cobalt ions close, therefore in this nickel cobalt hydroxide, the mol ratio of nickel element and cobalt element is 0.91 ~ 1.09.Preferably, the quality of described hexa and the quality of described nickel salt and cobalt salt and ratio be 1:1 ~ 3:1, the hexa in this proportion can make described nickel ion and cobalt ions precipitate fully.
Described hexa and described mixed solvent also have the effect of pattern guiding agent, under the cooperatively interacting of the two, can obtain the nickel cobalt hydroxide of three-dimensional flower-shaped structure, the nickel cobalt hydroxide of this three-dimensional flower-shaped structure is formed by the self assembly of nickel cobalt hydroxide nanometer sheet.In the sintering process of subsequent step S4, described nickel cobalt hydroxide is oxidized to Ni 1.5co 1.5o 4, and this three-dimensional flower-shaped structure remains unchanged, thus obtain the Ni of three-dimensional flower-shaped structure 1.5co 1.5o 4electrode material.When the mass ratio of described second alcohol and water is greater than 1:1 and is less than or equal to 4:1, the Ni of described three-dimensional flower-shaped structure of regular appearance, size uniformity can be formed 1.5co 1.5o 4electrode material, and the Ni of this three-dimensional flower-shaped structure 1.5co 1.5o 4electrode material is by tens Ni 1.5co 1.5o 4the spherical structure of nanometer sheet composition, in this spherical structure, each described Ni 1.5co 1.5o 4the center of nanometer sheet all from this spherical structure as petal stretches out, and multiple described Ni 1.5co 1.5o 4nanometer sheet partial intersection, this spherical structure all has in all directions by described Ni 1.5co 1.5o 4the space that nanometer sheet is formed and duct.The Ni of this three-dimensional flower-shaped structure 1.5co 1.5o 4electrode material specific area is huge, high adsorption capacity, release stress process in change in volume less, the diffusion and the electrochemical reaction active site that are more conducive to lithium ion fully react, to the raising of lithium ion memory capacity, the modification of change in volume in adsorption/desorption lithium process, the raising of speed have important meaning.Preferably, the mass ratio of described second alcohol and water is more than or equal to 2:1 and is less than or equal to 3:1.Preferably, the quality of described hexa and the quality of described ethanol and water and ratio be 1:4 ~ 1:2.
Described mixed solution can be transferred in steel lining polytetrafluoroethylene reactor and carry out hydro-thermal reaction.The reaction temperature of described hydro-thermal reaction is 80 DEG C ~ 260 DEG C, and reaction temperature is too low, and the dissociation constant of described hexa is also lower, thus does not have the effect of precipitation reagent and pattern guiding agent, and reaction temperature is too high, and described hexa can be made to decompose.Preferably, described reaction temperature is 100 DEG C ~ 140 DEG C, and this temperature range is more conducive to the nickel cobalt hydroxide forming the described three-dimensional flower-shaped structure that pattern is homogeneous, consistency is good.The described hydro-thermal reaction time is greater than 2 hours, to make described hydro-thermal reaction more abundant.Preferably, the described hydro-thermal reaction time is 2 hours ~ 8 hours.
After obtaining described presoma by described step S3, can this presoma of separating-purifying further.The mode of described separation can for filtering or centrifugation.Presoma after described separation can wash further.Water and absolute ethyl alcohol is adopted repeatedly to wash this presoma respectively in the embodiment of the present invention.Presoma after described separating-purifying can carry out drying further to remove solvent.This drying can be vacuum filtration or heat drying.
In step s 4 which, described sintering temperature can be 300 DEG C ~ 500 DEG C, and described sintering time can be 2 hours ~ 10 hours.Oxidation reaction is there is and forms described Ni in described nickel cobalt hydroxide in described sintering process 1.5co 1.5o 4electrode material.Described Ni 1.5co 1.5o 4electrode material is black powder.
Embodiment 1
By the Ni (NO of 1mmol 3) 26H 2co (the NO of O and 2mmol 3) 26H 2o joins in the mixed solvent of second alcohol and water, stirs 30 minutes, and the mixed proportion of second alcohol and water is 2:1, then adds hexa (HMT) lentamente, the quality of hexa and Ni (NO 3) 26H 2o and Co (NO 3) 26H 2o quality and ratio be 2:1, stir 30 minutes, form homogeneous pink mixed solution;
Above-mentioned mixed solution is transferred in steel lining polytetrafluoroethylene reactor, 90 DEG C of heating 4 hours, then room temperature is cooled to the furnace, take out, wash through vacuum filtration-three washing-vacuum filtrations-three ethanol and purification process is carried out to prepared sample, at 60 DEG C, vacuumize 12 hours, can obtain light green color precursor powder;
The described green precursor powder of preparation is placed in Muffle furnace, in air atmosphere, is raised to 350 DEG C with 1 DEG C of heating rate per minute, keeps 3 hours, then cool to room temperature with the furnace, black solid powder can be obtained.
Refer to Fig. 2, by known to the analysis of XRD collection of illustrative plates, described green presoma is cobalt nickel hydroxide structure, and described black solid powder is spinel-type cobalt-nickel oxide structure.Refer to Fig. 3 and following table, analyzed by EDX, can determine that Co/Ni atomic ratio is 1:1, therefore can infer that the structural formula of this spinel-type cobalt-nickel oxide is Ni 1.5co 1.5o 4.Refer to Fig. 4, can find out, described black solid powder be pattern homogeneous by Ni 1.5co 1.5o 4the three-dimensional flower-shaped structure that nanometer sheet self assembly is formed.
Element Percentage by weight (%) Atomicity percentage (%)
O 32.94 64.36
Co 34.98 18.55
Ni 32.09 17.09
Total amount 100.00 100.00
Ni provided by the invention 1.5co 1.5o 4the preparation method of electrode material, selects hexa to carry out co-precipitation to nickel ion and cobalt ions, can obtain nickel element and cobalt element mol ratio is the Ni of 1:1 1.5co 1.5o 4electrode material, selects ethanol water and hexa to cooperatively interact to Ni simultaneously 1.5co 1.5o 4the pattern of electrode material regulates and controls, and can prepare the Ni of three-dimensional flower-shaped structure 1.5co 1.5o 4electrode material.The Ni of this three-dimensional flower-shaped structure 1.5co 1.5o 4electrode material specific area is huge, high adsorption capacity, release stress process in change in volume less, the diffusion and the electrochemical reaction active site that are more conducive to lithium ion fully react, to the raising of lithium ion memory capacity, the modification of change in volume in adsorption/desorption lithium process, the raising of speed have important meaning.This preparation method's technique is simple, environmental protection, cost are lower, can carry out large-scale production.
In addition, those skilled in the art can also do other change in spirit of the present invention, and certainly, these changes done according to the present invention's spirit, all should be included within the present invention's scope required for protection.

Claims (9)

1. a Ni 1.5co 1.5o 4the preparation method of electrode material, comprising:
There is provided nickel salt, cobalt salt, hexa, ethanol and water, wherein, the mass ratio of described second alcohol and water is greater than 1:1 and is less than or equal to 4:1;
Described nickel salt, cobalt salt, hexa, ethanol and water are mixed, and described nickel salt, cobalt salt, hexa are dissolved, obtain a mixed solution;
Make described mixed solution carry out hydro-thermal reaction, obtain presoma; And
Carry out under an oxygen-containing atmosphere sintering described presoma, obtain described Ni 1.5co 1.5o 4electrode material, described Ni 1.5co 1.5o 4electrode material is by Ni 1.5co 1.5o 4the multiple three-dimensional flower-shaped structure that nanometer sheet self assembly is formed.
2. Ni as claimed in claim 1 1.5co 1.5o 4the preparation method of electrode material, is characterized in that, described presoma is nickel cobalt hydroxide, and in described nickel cobalt hydroxide, the mol ratio of nickel element and cobalt element is 0.91 ~ 1.09.
3. Ni as claimed in claim 1 1.5co 1.5o 4the preparation method of electrode material, is characterized in that, the mass ratio of described second alcohol and water is 2:1 ~ 3:1.
4. Ni as claimed in claim 1 1.5co 1.5o 4the preparation method of electrode material, is characterized in that, the quality of described hexa and the quality of described second alcohol and water and ratio be 1:4 ~ 1:2.
5. Ni as claimed in claim 1 1.5co 1.5o 4the preparation method of electrode material, is characterized in that, the reaction temperature of described hydro-thermal reaction is 100 DEG C ~ 140 DEG C.
6. Ni as claimed in claim 1 1.5co 1.5o 4the preparation method of electrode material, is characterized in that, described hexa and described nickel salt and cobalt salt quality and mass ratio be 1:1 ~ 3:1.
7. Ni as claimed in claim 1 1.5co 1.5o 4the preparation method of electrode material, is characterized in that, described nickel salt is one or more in nickel nitrate, nickel chloride, nickel acetate and nickelous sulfate, and described cobalt salt is one or more in cobalt nitrate, cobalt chloride, cobalt acetate and cobaltous sulfate.
8. Ni as claimed in claim 1 1.5co 1.5o 4the preparation method of electrode material, is characterized in that, described sintering temperature is 300 ~ 500 DEG C, and described sintering time is 2 ~ 8 hours.
9. Ni as claimed in claim 1 1.5co 1.5o 4the preparation method of electrode material, is characterized in that, each three-dimensional flower-shaped structure is by tens Ni 1.5co 1.5o 4the spherical structure of nanometer sheet composition, in this spherical structure, each described Ni 1.5co 1.5o 4the center of nanometer sheet all from this spherical structure as petal stretches out, and multiple described Ni 1.5co 1.5o 4nanometer sheet partial intersection, this spherical structure all has in all directions by described Ni 1.5co 1.5o 4the space that nanometer sheet is formed and duct.
CN201410778878.8A 2014-12-17 2014-12-17 Preparation method of nickel cobalt oxide electrode material Pending CN104505508A (en)

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CN105399151A (en) * 2015-11-24 2016-03-16 青岛能迅新能源科技有限公司 Preparation method of NiCo2O4 nano-material
CN105399152A (en) * 2015-11-24 2016-03-16 青岛能迅新能源科技有限公司 Solvent thermal preparation method of NiCo2O4 nano-material
CN105399149A (en) * 2015-11-24 2016-03-16 青岛能迅新能源科技有限公司 Preparation method of supercapacitor electrode material
CN105399150A (en) * 2015-11-24 2016-03-16 青岛能迅新能源科技有限公司 NiCo2O4 nano-material as well as preparation method and application thereof
CN106450300A (en) * 2016-11-01 2017-02-22 中南大学 Na2Fe2P2O7 material with flower-like structure and preparation method and application thereof
CN106450300B (en) * 2016-11-01 2019-05-03 中南大学 A kind of ferric sodium pyrophosphate material and its preparation method and application with flower-like structure
CN107522241A (en) * 2017-08-20 2017-12-29 桂林理工大学 A kind of preparation method and applications of nickel cobalt double-metal hydroxide
CN108598502A (en) * 2018-03-23 2018-09-28 广东工业大学 A kind of Ni-Co metal oxides air cell electrode catalyst and its preparation method and application
CN108470628A (en) * 2018-04-17 2018-08-31 吉林大学 A kind of combination electrode material and preparation method thereof
CN109167074A (en) * 2018-08-08 2019-01-08 东华大学 The nitrogen-doped carbon nanocomposite of hollow additive Mn cobalt oxide nickel coated and preparation
CN115849461A (en) * 2022-11-30 2023-03-28 陕西科技大学 Hollow cage-shaped nickel-cobalt bimetallic oxide and preparation method and application thereof

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