CN107739058A - Preparation method of self assembly rhombus flowers Co3O4 nanometer material and products thereof and application - Google Patents
Preparation method of self assembly rhombus flowers Co3O4 nanometer material and products thereof and application Download PDFInfo
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- CN107739058A CN107739058A CN201711066514.7A CN201711066514A CN107739058A CN 107739058 A CN107739058 A CN 107739058A CN 201711066514 A CN201711066514 A CN 201711066514A CN 107739058 A CN107739058 A CN 107739058A
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- rhombus
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G51/00—Compounds of cobalt
- C01G51/04—Oxides; Hydroxides
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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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
- H01M4/48—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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/40—Particle morphology extending in three dimensions prism-like
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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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
- 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 discloses a kind of preparation method of self assembly rhombus flowers Co3O4 nanometer material and products thereof and application, with cobalt salt, water is solvent, and urea, ammonium fluoride are added in whipping process, and continues stirring a period of time.After uniform stirring, ptfe autoclave is transferred to, carries out hydro-thermal reaction in an oven.Centrifuged, washed after the completion of reaction, being dried, then calcined in Muffle furnace high temperature, that is, obtain a kind of rhombus flowers cobaltosic oxide nano composite material.The present invention is using hydro-thermal method synthesis cobaltosic oxide, and the preparation method is simple to operate, and low raw-material cost, reaction temperature is low, and electrochemical properties are excellent, can be widely applied to be catalyzed, senses and the field such as energy stores.
Description
Technical field
The invention belongs to the preparation field of inorganic material, and in particular to a kind of self assembly rhombus flowers cobaltosic oxide nano
Preparation method of material and products thereof and application, a kind of simple hydro-thermal method synthesis Co3O4Rhombus flowers are used as lithium ion battery and born
Pole material.
Background technology
More highlighted using caused environmental problem with the progressively exhausted and fossil fuel of petroleum resources, energy problem
Increasingly receive significant attention, people have to Devoting Major Efforts To Developing find clean reproducible energy.And due to regenerative resource, bag
Include solar energy, wind energy, tide energy etc., there is the energy to provide intermittent feature, it is therefore desirable to be equipped with suitable energy storage and
Conversion equipment.Secondary cell is as a kind of effective energy storage and conversion equipment to high efficiency of energy utilization, environmental protection, economy
Sustainable development is all significant.Lithium ion battery is because of its small in volume, energy density is high, has extended cycle life, memoryless
Effect, temperature range are wide, advantages of environment protection, are developed rapidly.And the capacity of lithium ion battery depends primarily on
Positive and negative pole material, therefore, the bigger positive and negative pole material of development specific capacity are just very necessary.Transition metal oxide material, due to
Its conversion reaction occurs between lithium and transition metal oxide, has higher theoretical capacity, and is widely used in lithium ion
The research of battery electrode material.In the stable phase of numerous cobalt/cobalt oxides, cobaltosic oxide because its have very high reversible capacity,
Excellent cycle performance and cheap, and paid high attention to and widely studied.Shadow of the pattern of nano material to performance
Sound is most important, and nano flower-like material can not only increase the specific surface area of material, and intercrystalline gap be advantageous to lithium from
The diffusion of son, so as to which indelible effect is played in the raising to electrode material capacity and cycle performance.Co3O4As one kind weight
The transition metal oxide wanted, its theoretical specific capacity are 890mAh/g, are traditional negative material graphite（372mAh/g）Twice
More than, therefore the research to cobalt/cobalt oxide gets more and more people's extensive concerning.
The content of the invention
For overcome the deficiencies in the prior art, present invention aims at：A kind of self assembly rhombus flowers cobaltosic oxide is provided
The preparation method of nano material.
Another object of the present invention is：Product prepared by the above method is provided.
A further object of the present invention is：The application of the said goods is provided.
A kind of preparation method of self assembly rhombus flowers Co3O4 nanometer material, it is characterised in that this method it is specific
Step is：
（1）It is soluble in water to weigh a certain amount of cobalt salt, electromagnetic agitation, is allowed to be completely dissolved；
（2）A certain amount of urea, ammonium fluoride are added, lasting stirring a period of time；
（3）Pink mixed solution obtained above is placed in ptfe autoclave, in an oven 100 DEG C~180
Hydro-thermal reaction is carried out at DEG C, the reaction time is 4~10 hours；
（4）After reaction terminates, by solution centrifugal, obtained sediment with ethanol, distillation water washing, dries 10 at 70 DEG C successively
Hour；
（5）By pink powder obtained above, it is placed in Muffle furnace and is calcined 2 hours at 400 DEG C, that is, obtain crystal property very
Good black diamonds Co3O4 nanometer material.
The present invention will prepare cobaltosic oxide nano line on conductive matrices by growth in situ, there is provided a kind of simple side
Method prepares the lithium ion battery negative material with preferable microstructure morphology.
Step（1）In used cobaltatess be cabaltous nitrate hexahydrate Co (NO3)2·6H2O or cobalt chloride hexahydrate CoCl2·
6H2One kind in O.
Step（1）The mol ratio of middle cobalt salt and aqueous solvent is 1:100~1:400.
Step（2）In the mol ratio of used urea and ammonium fluoride be urea：Ammonium fluoride=1: 0.2~0.6.
The present invention provides a kind of self assembly rhombus flowers Co3O4 nanometer material, according to any of the above-described methods described system
It is standby to obtain.
The present invention provides a kind of self assembly rhombus flowers Co3O4 nanometer material and is used as lithium ion battery negative material
Application.
It is of the present invention to belong to technical field of nanometer material preparation, disclose a kind of self assembly rhombus flowers cobaltosic oxide
It is nanocrystalline and preparation method thereof, a kind of simple, economic hydrothermal synthesis method is employed, rhombus flowers cobaltosic oxide is prepared
Nano material.It is characterized in that：First, with cobalt salt, water is solvent, urea, ammonium fluoride is added in whipping process, and persistently stir
Mix a period of time.After uniform stirring, ptfe autoclave is transferred to, carries out hydro-thermal reaction in an oven.After the completion of reaction
Centrifuged, washed, being dried, then calcined in Muffle furnace high temperature, that is, obtain a kind of rhombus flowers cobaltosic oxide nano and answer
Condensation material.The present invention is using hydro-thermal method synthesis cobaltosic oxide, and the preparation method is simple to operate, low raw-material cost, reaction temperature
Spend low, and electrochemical properties are excellent, can be widely applied to be catalyzed, sense and the field such as energy stores.
Brief description of the drawings
Fig. 1：The scanning electron microscope (SEM) photograph of the rhombus flowers Co3O4 nanometer material synthesized for the embodiment of the present invention 1；
Fig. 2：For Co made from the embodiment of the present invention 13O4X-ray powder diffraction pattern；
Fig. 3：For the embodiment of the present invention it is 2-in-1 into rhombus flowers Co3O4 nanometer material scanning electron microscope (SEM) photograph.
Embodiment
The present invention is described in detail by following instantiation, but protection scope of the present invention is not only restricted to these realities
Apply example.
Embodiment 1：
（1）Weigh 2.9105 g cabaltous nitrate hexahydrate Co (NO3)2·6H2O is dissolved in 100 ml distilled water, electromagnetic agitation,
It is allowed to be completely dissolved；
（2）Add 3.003 g urea CO (NH2)2, 0.7408 g ammonium fluorides NH4F, and continue to stir 30 min；
（3）Pink mixed solution obtained above is transferred in 100ml ptfe autoclaves, in an oven 120
Hydro-thermal reaction is carried out at DEG C, the reaction time is 5 hours；
（4）After reaction terminates, by solution centrifugal, sediment is washed with deionized water, ethanol successively, and it is small that 10 are dried at 70 DEG C
When；
（5）By powder sample obtained above, it is placed in Muffle furnace and is calcined 2 hours at 400 DEG C, that is, it is fine to obtain crystal property
Rhombus flowers Co3O4 nanometer material.
From the scanning electron microscope (SEM) photograph and Fig. 2 that Fig. 1 is the rhombus flowers Co3O4 nanometer material that the embodiment of the present invention 1 synthesizes
Co made from the embodiment of the present invention 13O4X-ray powder diffraction pattern shown in, obtained cobaltosic oxide（Co3O4）Crystal formation
With standard powder diffraction card (JCPDS:42-1467) match.
Embodiment 2：
（1）Weigh 2.3284 g cabaltous nitrate hexahydrate Co (NO3)2·6H2O is dissolved in 80ml distilled water, 10 min of ultrasound,
It is allowed to be completely dissolved；
（2）Add 2.4024 g urea CO (NH2)2, 0.5926g ammonium fluorides NH4F, and it is allowed to ultrasonic dissolution；
（3）Pink mixed solution obtained above is transferred in 100ml ptfe autoclaves, in an oven 120
Hydro-thermal reaction is carried out at DEG C, the reaction time is 6 hours；
（4）After reaction terminates, by solution centrifugal, sediment is washed with deionized water, ethanol successively, until supernatant is clarified,
Dried 10 hours at 70 DEG C；
（5）By powder sample obtained above, it is placed in Muffle furnace and is calcined 2 hours at 400 DEG C, that is, it is fine to obtain crystal property
Rhombus flowers Co3O4 nanometer material.
As Fig. 3 embodiment of the present invention it is 2-in-1 into rhombus flowers Co3O4 nanometer material scanning electron microscope (SEM) photograph shown in, institute
Cobaltosic oxide is made（Co3O4）Crystal formation and standard powder diffraction card (JCPDS:42-1467) match.
Embodiment 3：
（1）Weigh 2.2565 g six chloride hydrate Asia cobalt CoCl2·6H2O is dissolved in 100 ml distilled water, electromagnetic agitation,
It is allowed to be completely dissolved；
（2）Add 3.003 g urea CO (NH2)2, 0.7408 g ammonium fluorides NH4F, and continue to stir 30 min；
（3）Pink mixed solution obtained above is transferred in 100ml ptfe autoclaves, in an oven 100
Hydro-thermal reaction is carried out at DEG C, the reaction time is 8 hours；
（4）After reaction terminates, by solution centrifugal, sediment is washed with deionized water, ethanol successively, and it is small that 10 are dried at 70 DEG C
When；
（5）By powder sample obtained above, it is placed in Muffle furnace and is calcined 2 hours at 400 DEG C, that is, it is fine to obtain crystal property
Rhombus flowers Co3O4 nanometer material.
Obtained cobaltosic oxide（Co3O4）Crystal formation and standard powder diffraction card (JCPDS:42-1467) match.
Embodiment 4：
（1）Weigh 0.7275 g cabaltous nitrate hexahydrate Co (NO3)2·6H2O is dissolved in 25ml distilled water, 10 min of ultrasound,
It is allowed to be completely dissolved；
（2）Add 0.7507 g urea CO (NH2)2, 0.1852g ammonium fluorides NH4F, and it is allowed to ultrasonic dissolution；
（3）Pink mixed solution obtained above is transferred in 100ml ptfe autoclaves, in an oven 180
Hydro-thermal reaction is carried out at DEG C, the reaction time is 4 hours；
（4）After reaction terminates, by solution centrifugal, sediment is washed with deionized water, ethanol successively, until supernatant is clarified,
Dried 10 hours at 70 DEG C；
（5）By powder sample obtained above, it is placed in Muffle furnace and is calcined 2 hours at 500 DEG C, that is, it is fine to obtain crystal property
Rhombus flowers Co3O4 nanometer material.
Obtained cobaltosic oxide（Co3O4）Crystal formation and standard powder diffraction card (JCPDS:42-1467) match.
Embodiment 5：
（1）Weigh 1.1642 g cabaltous nitrate hexahydrate Co (NO3)2·6H2O is dissolved in 80ml distilled water, stirs 10 min,
It is allowed to be completely dissolved；
（2）Add 0.6006 g urea CO (NH2)2, 0.2963g ammonium fluorides NH4F, stirring and dissolving；
（3）Pink mixed solution obtained above is transferred in 100ml ptfe autoclaves, in an oven 150
Hydro-thermal reaction is carried out at DEG C, the reaction time is 7 hours；
（4）After reaction terminates, by solution centrifugal, sediment is washed with deionized water, ethanol successively, until supernatant is clarified,
Dried 10 hours at 70 DEG C；
（5）By powder sample obtained above, it is placed in Muffle furnace and is calcined 2 hours at 500 DEG C, that is, it is fine to obtain crystal property
Rhombus flowers Co3O4 nanometer material.
Obtained cobaltosic oxide（Co3O4）Crystal formation and standard powder diffraction card (JCPDS:42-1467) match.
Claims (5)
- A kind of 1. preparation method of self assembly rhombus flowers Co3O4 nanometer material, it is characterised in that the specific step of this method Suddenly it is：（1）Weigh that a certain amount of cobalt salt is soluble in water, the mol ratio of cobalt salt and aqueous solvent is 1:100~1:400, electromagnetic agitation, make Be completely dissolved；（2）A certain amount of urea, ammonium fluoride are added, lasting stirring a period of time；（3）Pink mixed solution obtained above is placed in ptfe autoclave, in an oven 100 DEG C~180 Hydro-thermal reaction is carried out at DEG C, the reaction time is 4~10 hours；（4）After reaction terminates, by solution centrifugal, obtained sediment with ethanol, distillation water washing, dries 10 at 70 DEG C successively Hour；（5）By pink powder obtained above, it is placed in Muffle furnace and is calcined 2 hours at 400 DEG C, that is, obtain crystal property very Good black diamonds Co3O4 nanometer material.
- 2. the preparation method of self assembly rhombus flowers Co3O4 nanometer material according to claim 1, it is characterised in that： Step（1）In used cobaltatess be cabaltous nitrate hexahydrate Co (NO3)2·6H2O or cobalt chloride hexahydrate CoCl2·6H2In O It is a kind of.
- 3. the preparation method of self assembly rhombus flowers Co3O4 nanometer material according to claim 1, it is characterised in that： Step（2）In the mol ratio of used urea and ammonium fluoride be 1: 0.2~0.6.
- 4. a kind of self assembly rhombus flowers Co3O4 nanometer material, it is characterised in that according to claim 1-3 is any Method is prepared.
- 5. a kind of self assembly rhombus flowers Co3O4 nanometer material according to claim 4 is in negative electrode of lithium ion battery material Application in terms of material.
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109534411A (en) * | 2019-01-25 | 2019-03-29 | 安徽益佳通电池有限公司 | A kind of preparation method of the cobaltosic oxide material of morphology controllable |
| CN109650464A (en) * | 2018-12-23 | 2019-04-19 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of cobaltosic oxide nano linear array and products thereof and application |
| CN110284153A (en) * | 2018-03-19 | 2019-09-27 | 天津大学 | A kind of cobalt/cobalt protoxide porous nano-sheet array composite material and its preparation method and application |
| CN110885100A (en) * | 2018-09-07 | 2020-03-17 | 湖北大学 | Preparation method of novel lithium nickel manganese oxide positive electrode material with hierarchical structure |
| CN111003732A (en) * | 2019-12-23 | 2020-04-14 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of cobaltosic oxide nano material, product and application thereof |
| CN111072073A (en) * | 2019-12-20 | 2020-04-28 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of Ni monatomic doped cobaltosic oxide nano material, product and application thereof |
| CN111659466A (en) * | 2020-06-02 | 2020-09-15 | 上海师范大学 | Needle-ball-shaped ZIF-67@ CoO @ Co photoelectric catalytic material and preparation method and application thereof |
| CN112479265A (en) * | 2020-11-16 | 2021-03-12 | 西安理工大学 | Preparation method of cobaltosic oxide nanoparticles |
| CN112960702A (en) * | 2021-04-23 | 2021-06-15 | 华中科技大学 | Preparation method of cobaltosic oxide with thermochemical energy storage performance and product |
| CN113582241A (en) * | 2021-07-21 | 2021-11-02 | 北京化工大学 | Electrocatalytic material echinoid Co for ENRR3O4Preparation method of (1) |
| CN114068914A (en) * | 2021-10-29 | 2022-02-18 | 格林美（江苏）钴业股份有限公司 | Lithium cobaltate positive electrode material and preparation method thereof |
| WO2022142170A1 (en) * | 2020-12-28 | 2022-07-07 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation of manganese(iii) oxide atom cluster modified cobaltosic oxide nano-material for detection, and product and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110284153B (en) * | 2018-03-19 | 2021-06-01 | 天津大学 | Cobalt/cobaltous oxide porous nanosheet array composite material and preparation method and application thereof |
| CN110284153A (en) * | 2018-03-19 | 2019-09-27 | 天津大学 | A kind of cobalt/cobalt protoxide porous nano-sheet array composite material and its preparation method and application |
| CN110885100A (en) * | 2018-09-07 | 2020-03-17 | 湖北大学 | Preparation method of novel lithium nickel manganese oxide positive electrode material with hierarchical structure |
| CN109650464A (en) * | 2018-12-23 | 2019-04-19 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of cobaltosic oxide nano linear array and products thereof and application |
| CN109534411A (en) * | 2019-01-25 | 2019-03-29 | 安徽益佳通电池有限公司 | A kind of preparation method of the cobaltosic oxide material of morphology controllable |
| CN111072073A (en) * | 2019-12-20 | 2020-04-28 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of Ni monatomic doped cobaltosic oxide nano material, product and application thereof |
| CN111003732A (en) * | 2019-12-23 | 2020-04-14 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of cobaltosic oxide nano material, product and application thereof |
| CN111659466A (en) * | 2020-06-02 | 2020-09-15 | 上海师范大学 | Needle-ball-shaped ZIF-67@ CoO @ Co photoelectric catalytic material and preparation method and application thereof |
| CN112479265A (en) * | 2020-11-16 | 2021-03-12 | 西安理工大学 | Preparation method of cobaltosic oxide nanoparticles |
| WO2022142170A1 (en) * | 2020-12-28 | 2022-07-07 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation of manganese(iii) oxide atom cluster modified cobaltosic oxide nano-material for detection, and product and application thereof |
| CN112960702A (en) * | 2021-04-23 | 2021-06-15 | 华中科技大学 | Preparation method of cobaltosic oxide with thermochemical energy storage performance and product |
| CN112960702B (en) * | 2021-04-23 | 2022-02-15 | 华中科技大学 | Preparation method of cobaltosic oxide with thermochemical energy storage performance and product |
| CN113582241A (en) * | 2021-07-21 | 2021-11-02 | 北京化工大学 | Electrocatalytic material echinoid Co for ENRR3O4Preparation method of (1) |
| CN114068914A (en) * | 2021-10-29 | 2022-02-18 | 格林美（江苏）钴业股份有限公司 | Lithium cobaltate positive electrode material and preparation method thereof |
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