CN106517360A - Particle self-assembly type micro-spherical tricobalt tetroxide powder and preparation method thereof - Google Patents
Particle self-assembly type micro-spherical tricobalt tetroxide powder and preparation method thereof Download PDFInfo
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- CN106517360A CN106517360A CN201611011874.2A CN201611011874A CN106517360A CN 106517360 A CN106517360 A CN 106517360A CN 201611011874 A CN201611011874 A CN 201611011874A CN 106517360 A CN106517360 A CN 106517360A
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- tricobalt tetroxide
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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
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/85—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by XPS, EDX or EDAX data
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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
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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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
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
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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
Abstract
The invention relates to the technical field of micro-spherical tricobalt tetroxide powder, in particular to particle self-assembly type micro-spherical tricobalt tetroxide powder and a preparation method thereof. The particle self-assembly type micro-spherical tricobalt tetroxide powder is prepared from tricobalt tetroxide nano-particles by means of self-assembly, the particle size of the spherical powder is 1-10 micrometers, and the spherical powder is morphologically uniform. The preparation method includes ultrasonically mixing a soluble cobalt salt water solution with a glycine-NaOH water solution, and disposing a mixture in a constant-temperature blast air oven for reaction; conducting treatment after complete reaction so as to obtain the micro-spherical tricobalt tetroxide powder. The particle self-assembly type micro-spherical tricobalt tetroxide powder is obtained successfully through a glycine biomolecule assisted hydrothermal process. A series of characteristics indicate that the particle self-assembly type micro-spherical tricobalt tetroxide powder is narrow in particle size distribution, uniform in morphological distribution and controllable in a raw material reaction system with the glycine as a template.
Description
Technical field
The present invention relates to Cobalto-cobaltic oxide micro-powder preparing technical field, a kind of more particularly to particle self assembly four is aoxidized
Three cobalt micron spherical powders and preparation method thereof.
Background technology
Cobalto-cobaltic oxide as a kind of anti-magnetic phase p-type semiconductor material, in semi-conducting material, ceramic material, catalyst, biography
The application of the aspects such as sensor is quite varied.Cobalto-cobaltic oxide in the electrode material as lithium ion battery, different synthesis sides
The diverse microcosmic structure of method and material has a great impact to its chemical property.
The preparation method of Cobalto-cobaltic oxide mainly has at present：Microemulsion method, template, sol-gel process etc..Huang Kelong etc.
Pure phase cubic Cobalto-cobaltic oxide is prepared for using solvent-thermal method, dispersant is made with Polyethylene Glycol, just changed as solvent
The ratio of fourth alcohol and water, can reach to pure phase Co3O4Pattern and size control.Yang Huaming etc. is first with solid phase
Reaction method synthesizes unformed presoma, then presoma is synthesized Co through roasting3O4Nano-powder.Chen Youcun etc. utilizes solvent
The method of heat, with Co (NO3)2·6H2O is cobalt source, H2O2For oxidant, with the mixed solution of n-dodecane hydrocarbon and Oleic acid as molten
Agent, is successfully prepared for Co3O4Nanometer rods.These report majorities are all to synthesize Co3O4Receive, micron particle, and synthesize grain
Sub- self assembly Co3O4Spherical powder body is rarely reported.
The content of the invention
The purpose of the present invention is to propose to a kind of particle self assembly Cobalto-cobaltic oxide micron spherical powder and preparation method thereof, with
Overcome the defect in prior art, a new way is provided for industrial-scale production Cobalto-cobaltic oxide micron spherical powder.
For realizing the purpose, technical scheme below is present invention employs：
A kind of particle self assembly Cobalto-cobaltic oxide micron spherical powder, is formed by cobaltosic oxide nano particles self assemble,
The particle diameter of spherical powder is 1～10 μm, and the pattern of spherical powder is uniform.
A kind of spherical raw powder's production technology of particle self assembly Cobalto-cobaltic oxide micron, the aqueous solution of soluble cobalt with it is sweet
The aqueous solution of propylhomoserin NaOH is placed in constant temperature blast drying oven Jing after ultrasonic mixing and is reacted, and reaction temperature is 160～200
DEG C, the response time is 1 for the mol ratio between the cobalt ion of 12～36h, glycine and soluble cobalt：1～20：1；React
Jing post processings after complete obtain Cobalto-cobaltic oxide micron spherical powder.
Preferably, soluble cobalt is cabaltous nitrate hexahydrate, cobalt acetate or cobaltous chloride.Soluble cobalt is in its aqueous solution
In molal volume concentration be 0.1～1mol/L.In the aqueous solution of glycine NaOH, the molal volume concentration of glycine is 0.1
The molal volume concentration of～5mol/L, NaOH is 0.02～1mol/L.
Used as further improving, post processing is will to use dehydrated alcohol and deionized water after product solid-liquid separation respectively
Alternately wash, be dried in being subsequently placed in thermostatic drying chamber.In thermostatic drying chamber, baking temperature is 20～60 DEG C, drying time
For 3～10h.
Particle self assembly Cobalto-cobaltic oxide micron spherical powder of the present invention and preparation method thereof, mainly by sweet ammonia
Acid, Co (NO3)2·6H2The soluble cobalts such as O and NaOH are raw material, carry out hydro-thermal reaction again and prepare grain after mixing ultrasonic agitation
Sub- self assembly Cobalto-cobaltic oxide micron spherical powder.The present invention successfully obtains one by glycine biomolecule assisting alcohol-hydrothermal method
Plant the spherical powder body material of particle self assembly Cobalto-cobaltic oxide micron.Show to be used as template and raw material in glycine by series
The particle self assembly Cobalto-cobaltic oxide micron spherical powder obtained in reaction system has narrower particle size distribution, topographic profile homogeneous
With the performance such as controllable.This simple synthetic method can also synthesize the flower-shaped of other self assemblies as a kind of general strategy
Micro-, nano material.Beneficial effects of the present invention are also manifested by：
1). present invention achieves utilizing glycine and Co (NO3)2·6H2The soluble cobalts such as O as presoma, by water
Full-boiled process quickly obtains particle self assembly Cobalto-cobaltic oxide micron spherical powder, and the synthesis for being similar to micro-, nano material provides one
Plant new approach.
2). the process is simple of the present invention, whole preparation system easily builds, easy to operate, condition is easily-controllable, with low cost,
The product easily-controllable, products distribution of composition is uniform, be difficult to reunite, be suitable for large-scale industrial production.
3). the present invention is as reactant, without other auxiliary in preparation process using conventional soluble cobalt salt
Material, the by-product of generation are few, and environmental pollution is less, are a kind of environment-friendly type synthesis techniques.
4). product prepared by the present invention has preferable water solublity, good biocompatibility, can be used in lithium ion battery
The aspects such as electrode material.
Description of the drawings
Fig. 1 is the XRD figure of embodiment 1 (product 1) and embodiment 2 (product 2) products therefrom.
Fig. 2 a-2b are followed successively by the low of 1 products therefrom of embodiment, high magnification FE-SEM figures.
Fig. 2 c are schemed for the EDS of 1 products therefrom of embodiment.
Fig. 3 a-3b are followed successively by the low of 2 products therefrom of embodiment, high magnification FE-SEM figures.
Specific embodiment
The particle self assembly Cobalto-cobaltic oxide micron that the present invention is further described below by way of specific embodiment is spherical
Powder body and preparation method thereof.
Embodiment 1
The preparation of particle self assembly Cobalto-cobaltic oxide micron spherical powder：
(1) weigh 30mmol glycine and 3mmol NaOH are poured in beaker, add 15mL deionized water dissolving, and be placed on
30min is stirred on magnetic stirring apparatuss, forms solution A.Weigh 3mmol Co (NO3)2·6H2O is poured in beaker, adds 10mL to go
Ionized water is dissolved, and is maintained like condition, and is stirred 30min, forms solution B.Solution A after stirring is added to solution B
In be put into ultrasound 30min in ultrasonic cleaner, form solution C.
(2) solution C is proceeded in 50mL reactors washed in advance, then is poured into after rinsed beaker
In reactor；Reactor is covered and is put in constant temperature blast drying oven, it is 180 DEG C to arrange temperature, reacts 24h；Question response terminates
Afterwards, reactor is taken out, by the powder centrifuge generated after reaction, and is washed with dehydrated alcohol and deionized water alternating respectively
Wash for several times, then 6h is dried with 40 DEG C in thermostatic drying chamber and obtains i.e. four oxidation of particle self assembly of black cobaltosic oxide powder
Three cobalt micron spherical powders.
Fig. 2 a-2b are schemed for the FE-SEM of 1 products therefrom of embodiment.From Fig. 2 a of low range, resulting Co3O4Powder
Bodily form looks are homogeneous, and particle mean size is 5 μm, and good crystallinity；From powerful Fig. 2 b, resulting rough,
Assembled by more tiny nano-particle；Product obtained by EDS figures (Fig. 2 c) of product shows is made up of Co and O, Si's
Substrate of the peak from experiment, and the peak of Pt when being then sample preparation metal spraying cause.
Embodiment 2
The preparation of particle self assembly Cobalto-cobaltic oxide micron spherical powder：
(1) weigh 30mmol glycine and 4mmol NaOH are poured in beaker, add 20mL deionized water dissolving, and be placed on
30min is stirred on magnetic stirring apparatuss, forms solution A.Weigh 4mmol cobalt acetates to pour in beaker, addition 10mL deionized waters will
Its dissolving, maintains like condition, and stirs 30min, forms solution B.Solution A after stirring is added be put into into solution B it is super
Ultrasound 30min in sound wave washer, forms solution C.
(2) solution C is proceeded in 50mL reactors washed in advance, then is poured into after rinsed beaker
In reactor；Reactor is covered and is put in constant temperature blast drying oven, it is 180 DEG C to arrange temperature, reacts 12h；Question response terminates
Afterwards, reactor is taken out, by the powder centrifuge generated after reaction, and is washed with dehydrated alcohol and deionized water alternating respectively
Wash for several times, then 6h is dried with 40 DEG C in thermostatic drying chamber and obtains i.e. four oxidation of particle self assembly of black cobaltosic oxide powder
Three cobalt micron spherical powders.
Fig. 1 is the XRD spectrum of embodiment 1 (product 1) and embodiment 2 (product 2) products therefrom.Itself and standard card
JCPDS No.43-1003 compare and understand, have diffraction maximum to occur, correspond at 30.8 °, 35.3 °, 46.8 °, 54.6 ° respectively
(220), (311), (400), (511) crystal face, show that product is spinel-type Co3O4, product purity is higher.
Fig. 3 a-3b are schemed for the FE-SEM of 2 products therefrom of embodiment.From Fig. 3 a of low range, resulting Co3O4Powder
Bodily form looks are homogeneous, and particle mean size is 3 μm, and good crystallinity；From powerful Fig. 3 b, resulting rough,
Assembled by more tiny nano-particle.
Embodiment 3
The preparation of particle self assembly Cobalto-cobaltic oxide micron spherical powder：
(1) weigh 30mmol glycine and 5mmol NaOH are poured in beaker, add 10mL deionized water dissolving, and be placed on
30min is stirred on magnetic stirring apparatuss, forms solution A.Weigh 5mmol cobaltous chlorides to pour in beaker, addition 10mL deionized waters will
Its dissolving, maintains like condition, and stirs 30min, forms solution B.Solution A after stirring is added be put into into solution B it is super
Ultrasound 30min in sound wave washer, forms solution C.
(2) solution C is proceeded in 50mL reactors washed in advance, then is poured into after rinsed beaker
In reactor；Reactor is covered and is put in constant temperature blast drying oven, it is 200 DEG C to arrange temperature, reacts 10h；Question response terminates
Afterwards, reactor is taken out, by the powder centrifuge generated after reaction, and is washed with dehydrated alcohol and deionized water alternating respectively
Wash for several times, then 5h is dried with 50 DEG C in thermostatic drying chamber and obtains i.e. four oxidation of particle self assembly of black cobaltosic oxide powder
Three cobalt micron spherical powders.
It is pointed out that the present invention is not limited only to embodiment listed above, it is every can be direct from present invention
Derive or enlighten the conceivable correlation technique of connection and all should belong to the scope that the present invention covers protection.
Claims (7)
1. a kind of particle self assembly Cobalto-cobaltic oxide micron spherical powder, it is characterised in that：By cobaltosic oxide nano granule certainly
Assemble, the particle diameter of spherical powder is 1～10 μm, and the pattern of spherical powder is uniform.
2. the spherical raw powder's production technology of a kind of particle self assembly Cobalto-cobaltic oxide micron as claimed in claim 1, its feature exist
In：The aqueous solution of soluble cobalt is placed in constant temperature blast drying oven Jing after ultrasonic mixing with the aqueous solution of glycine NaOH
Row reaction, reaction temperature are 160～200 DEG C, and the response time is between the cobalt ion of 12～36h, glycine and soluble cobalt
Mol ratio be 1：1～20：1；Jing post processings after reaction completely obtain Cobalto-cobaltic oxide micron spherical powder.
3. preparation method as claimed in claim 2, it is characterised in that：Soluble cobalt be cabaltous nitrate hexahydrate, cobalt acetate or
Cobaltous chloride.
4. preparation method as claimed in claim 2, it is characterised in that：Molal volume of the soluble cobalt in its aqueous solution is dense
Spend for 0.1～1mol/L.
5. preparation method as claimed in claim 2, it is characterised in that：In the aqueous solution of glycine NaOH glycine mole
Volumetric concentration is 0.1～5mol/L, and the molal volume concentration of NaOH is 0.02～1mol/L.
6. preparation method as claimed in claim 2, it is characterised in that：Post processing is will to be made after product solid-liquid separation respectively
Alternately washed with dehydrated alcohol and deionized water, be dried in being subsequently placed in thermostatic drying chamber.
7. preparation method as claimed in claim 6, it is characterised in that：In thermostatic drying chamber, baking temperature is 20～60 DEG C, is done
The dry time is 3～10h.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107098390A (en) * | 2017-04-20 | 2017-08-29 | 合肥学院 | One kind simply prepares the adjustable sheet self assembly MoS of particle diameter2The method of bobbles shape powder |
| CN109422293A (en) * | 2017-09-05 | 2019-03-05 | 中国科学院大连化学物理研究所 | A kind of preparation method of micron-size spherical cobaltosic oxide material |
| CN109422294A (en) * | 2017-09-05 | 2019-03-05 | 中国科学院大连化学物理研究所 | A kind of preparation method for the cobaltosic oxide nano particle that size is controllable |
| CN115092970A (en) * | 2022-02-22 | 2022-09-23 | 广东邦普循环科技有限公司 | Aluminum-doped needle-like cobaltosic oxide and preparation method thereof |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107098390A (en) * | 2017-04-20 | 2017-08-29 | 合肥学院 | One kind simply prepares the adjustable sheet self assembly MoS of particle diameter2The method of bobbles shape powder |
| CN107098390B (en) * | 2017-04-20 | 2018-10-16 | 合肥学院 | One kind simply preparing the adjustable sheet self assembly MoS of grain size2The method of bobbles shape powder |
| CN109422293A (en) * | 2017-09-05 | 2019-03-05 | 中国科学院大连化学物理研究所 | A kind of preparation method of micron-size spherical cobaltosic oxide material |
| CN109422294A (en) * | 2017-09-05 | 2019-03-05 | 中国科学院大连化学物理研究所 | A kind of preparation method for the cobaltosic oxide nano particle that size is controllable |
| CN109422293B (en) * | 2017-09-05 | 2021-09-17 | 中国科学院大连化学物理研究所 | Preparation method of micron-sized spherical cobaltosic oxide material |
| CN109422294B (en) * | 2017-09-05 | 2021-09-17 | 中国科学院大连化学物理研究所 | Preparation method of size-controllable cobaltosic oxide nanoparticles |
| CN115092970A (en) * | 2022-02-22 | 2022-09-23 | 广东邦普循环科技有限公司 | Aluminum-doped needle-like cobaltosic oxide and preparation method thereof |
| CN115092970B (en) * | 2022-02-22 | 2023-06-13 | 广东邦普循环科技有限公司 | Aluminum-doped needle-shaped cobaltosic oxide and preparation method thereof |
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