CN106517360B - A kind of particle self assembly cobaltosic oxide micron spherical powder and preparation method thereof - Google Patents
A kind of particle self assembly cobaltosic oxide micron spherical powder and preparation method thereof Download PDFInfo
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- CN106517360B CN106517360B CN201611011874.2A CN201611011874A CN106517360B CN 106517360 B CN106517360 B CN 106517360B CN 201611011874 A CN201611011874 A CN 201611011874A CN 106517360 B CN106517360 B CN 106517360B
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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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- 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 present invention relates to cobaltosic oxide micro-powder preparing technical field, more particularly to a kind of particle self assembly cobaltosic oxide micron spherical powder and preparation method thereof.It is formed by cobaltosic oxide nano particles self assemble, and the grain size of spherical powder is 1~10 μm, and the pattern of spherical powder is uniform.Preparation method is：The aqueous solution of soluble cobalt is placed on through ultrasonic mixing in constant temperature blast drying oven with the aqueous solution of glycine-NaOH to be reacted；After the reaction was complete cobaltosic oxide micron spherical powder is obtained through post-processing.The present invention successfully obtains a kind of particle self assembly cobaltosic oxide micron spherical shape powder body material by glycine biomolecule assisting alcohol-hydrothermal method.By series show glycine be used as the particle self assembly cobaltosic oxide micron spherical powder that is obtained in template and raw material reaction system with narrower particle size distribution, topographic profile is uniform and the performances such as controllably.
Description
Technical field
The present invention relates to cobaltosic oxide micro-powder preparing technical field, more particularly to a kind of particle self assembly four aoxidizes
Three cobalt micron spherical powders and preparation method thereof.
Background technology
Cobaltosic oxide is as a kind of anti-magnetic phase p-type semiconductor material, in semi-conducting material, ceramic material, catalyst, biography
The application of sensor etc. is very extensive.Cobaltosic oxide is in the electrode material as lithium ion battery, different synthesis sides
Method and the diverse microcosmic structure of material have a great impact to its chemical property.
The preparation method of cobaltosic oxide mainly has at present：Microemulsion method, template, sol-gel method etc..Huang Kelong etc.
It is prepared for pure phase cubic cobaltosic oxide using solvent-thermal method, dispersant is made with polyethylene glycol, is changed as solvent just
The ratio of fourth alcohol and water can reach to pure phase Co3O4Pattern and particle size control.Yang Huaming etc. is first with solid phase
Reaction method synthesizes unformed presoma, then by presoma by roasting synthesis Co3O4Nano-powder.Chen Youcun etc. utilizes solvent
The method of heat, with Co (NO3)2·6H2O is cobalt source, H2O2It is molten with the mixed solution of n-dodecane hydrocarbon and oleic acid for oxidant
Agent is successfully prepared for Co3O4Nanometer rods.These report majorities are all to synthesize Co3O4Receive, micron particles, and synthesize grain
Sub- self assembly Co3O4Spherical powder is rarely reported.
Invention content
The purpose of the present invention is to propose to a kind of particle self assembly cobaltosic oxide micron spherical powder and preparation method thereof, with
Overcome the defect in the prior art, a new way is provided for industrial-scale production cobaltosic oxide micron spherical powder.
To realize the purpose, present invention employs following technical schemes：
A kind of particle self assembly cobaltosic oxide micron spherical powder, is formed by cobaltosic oxide nano particles self assemble,
The grain size of spherical powder is 1~10 μm, and the pattern of spherical powder is uniform.
A kind of particle self assembly cobaltosic oxide micron spherical shape raw powder's production technology, the aqueous solution of soluble cobalt with it is sweet
The aqueous solution of propylhomoserin-NaOH, which is placed on through ultrasonic mixing in constant temperature blast drying oven, to be reacted, and reaction temperature is 160~200
DEG C, the reaction time is 12~36h, and the molar ratio between glycine and the cobalt ions of soluble cobalt is 1：1~20：1；It has reacted
Quan Houjing post-processes to obtain cobaltosic oxide micron spherical powder.
Preferably, soluble cobalt is cabaltous nitrate hexahydrate, cobalt acetate or cobalt chloride.Soluble cobalt is in its aqueous solution
In a concentration of 0.1~1mol/L of molal volume.The molal volume of glycine a concentration of 0.1 in the aqueous solution of glycine-NaOH
A concentration of 0.02~1mol/L of molal volume of~5mol/L, NaOH.
As a further improvement, post-processing is to use absolute ethyl alcohol and deionized water after being separated by solid-liquid separation reaction product respectively
It alternately washs, is subsequently placed in thermostatic drying chamber and is dried.Drying temperature is 20~60 DEG C in thermostatic drying chamber, drying time
For 3~10h.
The particle self assembly cobaltosic oxide micron spherical powder and preparation method thereof of the present invention, mainly passes through sweet ammonia
Acid, Co (NO3)2·6H2The soluble cobalts such as O and NaOH are raw material, and carrying out hydro-thermal reaction again after mixing is stirred by ultrasonic prepares grain
Sub- self assembly cobaltosic oxide micron spherical powder.The present invention successfully obtains one by glycine biomolecule assisting alcohol-hydrothermal method
Kind particle self assembly cobaltosic oxide micron spherical shape powder body material.Show to be used as template and raw material in glycine by series
The particle self assembly cobaltosic oxide micron spherical powder obtained in reaction system has narrower particle size distribution, topographic profile uniform
With the performances such as controllable.This simple synthetic method can also be used as a kind of general strategy to synthesize the flower-shaped of other self assemblies
Micro-, nano material.Beneficial effects of the present invention are also manifested by：
1) the present invention, which realizes, utilizes glycine and Co (NO3)2·6H2The soluble cobalts such as O pass through water as presoma
Hot method quickly obtains particle self assembly cobaltosic oxide micron spherical powder, and one is provided for similar micro-, nano material synthesis
The new approach of kind.
2) the present invention it is simple for process, entire preparation system be easy structure, easy to operate, condition is easily-controllable, it is of low cost,
Product composition is easily-controllable, product is evenly distributed, is not easy to reunite, is suitable for large-scale industrial production.
3) the present invention is not add other auxiliary in preparation process as reactant using conventional soluble cobalt salt
The by-product of substance, generation is few, and environmental pollution is smaller, is a kind of environment-friendly type synthesis technology.
4) product prepared by the present invention has preferable water-soluble, good biocompatibility, can be used in lithium ion battery
Electrode material etc..
Description of the drawings
Fig. 1 is the XRD diagram of embodiment 1 (product 1) and embodiment 2 (product 2) products therefrom.
Fig. 2 a-2b are followed successively by low, the high magnification FE-SEM figures of 1 products therefrom of embodiment.
Fig. 2 c are that the EDS of 1 products therefrom of embodiment schemes.
Fig. 3 a-3b are followed successively by low, the high magnification FE-SEM figures of 2 products therefrom of embodiment.
Specific implementation mode
It is spherical below by way of the specific embodiment particle self assembly cobaltosic oxide micron that present invention be described in more detail
Powder and preparation method thereof.
Embodiment 1
The preparation of particle self assembly cobaltosic oxide micron spherical powder：
(1) it weighs 30mmol glycine and 3mmol NaOH is poured into beaker, 15mL deionized water dissolvings are added, and be placed on
30min is stirred on magnetic stirring apparatus, forms solution A.Weigh 3mmol Co (NO3)2·6H2O is poured into beaker, and 10mL is added and goes
Ionized water is dissolved, and maintains like condition, and stir 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 transferred in 50mL reaction kettles washed in advance, then is poured into after being rinsed beaker with 5mL deionized waters
In reaction kettle；Reaction kettle is covered and is put into constant temperature blast drying oven, setting temperature is 180 DEG C, and reaction is for 24 hours；To the end of reaction
Afterwards, reaction kettle, the powder centrifuge that will be generated after reaction are taken out, and is alternately washed with absolute ethyl alcohol and deionized water respectively
It washs for several times, then obtaining black cobaltosic oxide powder i.e. particle self assembly four in thermostatic drying chamber with 40 DEG C of dry 6h aoxidizes
Three cobalt micron spherical powders.
Fig. 2 a-2b are that the FE-SEM of 1 products therefrom of embodiment schemes.By Fig. 2 a of low range it is found that obtained Co3O4Powder
Bodily form looks are uniform, and average particle size is 5 μm, and good crystallinity；By powerful Fig. 2 b it is found that obtained rough,
Assembled by more tiny nano particle；The EDS figures (Fig. 2 c) of product show that obtained product is made of Co and O, Si's
Substrate of the peak from experiment, and when the peak of Pt is then sample preparation caused by metal spraying.
Embodiment 2
The preparation of particle self assembly cobaltosic oxide micron spherical powder：
(1) it weighs 30mmol glycine and 4mmol NaOH is poured into beaker, 20mL deionized water dissolvings are added, and be placed on
30min is stirred on magnetic stirring apparatus, forms solution A.It weighs 4mmol cobalt acetates to pour into beaker, 10mL deionized waters are added will
It is dissolved, and maintains like condition, and stir 30min, forms solution B.Solution A after stirring is added be put into solution B it is super
Ultrasound 30min in sound wave washer forms solution C.
(2) solution C is transferred in 50mL reaction kettles washed in advance, then is poured into after being rinsed beaker with 5mL deionized waters
In reaction kettle；Reaction kettle is covered and is put into constant temperature blast drying oven, setting temperature is 180 DEG C, reacts 12h；To the end of reaction
Afterwards, reaction kettle, the powder centrifuge that will be generated after reaction are taken out, and is alternately washed with absolute ethyl alcohol and deionized water respectively
It washs for several times, then obtaining black cobaltosic oxide powder i.e. particle self assembly four in thermostatic drying chamber with 40 DEG C of dry 6h aoxidizes
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 it is found that have diffraction maximum appearance at 30.8 °, 35.3 °, 46.8 °, 54.6 °, correspond to respectively
(220), (311), (400), (511) crystal face show that product is spinel-type Co3O4, product purity is higher.
Fig. 3 a-3b are that the FE-SEM of 2 products therefrom of embodiment schemes.By Fig. 3 a of low range it is found that obtained Co3O4Powder
Bodily form looks are uniform, and average particle size is 3 μm, and good crystallinity；By powerful Fig. 3 b it is found that obtained rough,
Assembled by more tiny nano particle.
Embodiment 3
The preparation of particle self assembly cobaltosic oxide micron spherical powder：
(1) it weighs 30mmol glycine and 5mmol NaOH is poured into beaker, 10mL deionized water dissolvings are added, and be placed on
30min is stirred on magnetic stirring apparatus, forms solution A.It weighs 5mmol cobalt chlorides to pour into beaker, 10mL deionized waters are added will
It is dissolved, and maintains like condition, and stir 30min, forms solution B.Solution A after stirring is added be put into solution B it is super
Ultrasound 30min in sound wave washer forms solution C.
(2) solution C is transferred in 50mL reaction kettles washed in advance, then is poured into after being rinsed beaker with 5mL deionized waters
In reaction kettle；Reaction kettle is covered and is put into constant temperature blast drying oven, setting temperature is 200 DEG C, reacts 10h；To the end of reaction
Afterwards, reaction kettle, the powder centrifuge that will be generated after reaction are taken out, and is alternately washed with absolute ethyl alcohol and deionized water respectively
It washs for several times, then obtaining black cobaltosic oxide powder i.e. particle self assembly four in thermostatic drying chamber with 50 DEG C of dry 5h aoxidizes
Three cobalt micron spherical powders.
It should be pointed out that the present invention is not limited only to embodiment listed above, it is every can be direct from the content of present invention
Export or enlightenment, which join conceivable the relevant technologies, should all belong to the range that the present invention covers protection.
Claims (1)
1. a kind of particle self assembly cobaltosic oxide micron spherical shape raw powder's production technology, it is characterised in that：Steps are as follows：
(1) it weighs 30mmol glycine and 3mmol NaOH is poured into beaker, 15mL deionized water dissolvings are added, and be placed on magnetic force
30min is stirred on blender, forms solution A；Weigh 3mmol Co (NO3)2·6H2O is poured into beaker, and 10mL deionizations are added
Water is dissolved, and maintains like condition, and stir 30min, forms solution B；Solution A after stirring is added and is put into solution B
To ultrasound 30min in ultrasonic cleaner, solution C is formed；
(2) solution C is transferred in 50mL reaction kettles washed in advance, then pours into reaction after being rinsed beaker with 5mL deionized waters
In kettle；Reaction kettle is covered and is put into constant temperature blast drying oven, setting temperature is 180 DEG C, and reaction is for 24 hours；It waits for after reaction, taking
Go out reaction kettle, the powder centrifuge that will be generated after reaction, and absolute ethyl alcohol and deionized water alternately washing number are used respectively
It is secondary, then black cobaltosic oxide powder i.e. particle self assembly cobaltosic oxide is obtained with 40 DEG C of dry 6h in thermostatic drying chamber
Micron spherical powder；
The particle self assembly cobaltosic oxide micron spherical powder is formed by spinel-type cobaltosic oxide nano particles self assemble,
The grain size of spherical powder is 5 μm, and the pattern of spherical powder is uniform；Spinel-type cobaltosic oxide nano rough, by
More tiny nano particle assembles；There is diffraction maximum appearance at 30.8 °, 35.3 °, 46.8 °, 54.6 °, corresponds to respectively
(220), (311), (400), (511) crystal face.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
| 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 |
| 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 |
| 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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| CN101434416A (en) * | 2008-11-28 | 2009-05-20 | 宁波金和新材料有限公司 | Hydroxy spherical cobaltosic oxide and preparation thereof |
| CN101585559A (en) * | 2009-06-14 | 2009-11-25 | 宁波科博特钴镍有限公司 | Preparation method of spherical cobaltosic oxide with high battery security |
| CN102134105A (en) * | 2011-05-09 | 2011-07-27 | 四川大学 | Method for accessorily preparing nanometer cobaltosic oxide granules at room temperature by utilizing amino acids |
| CN103771539A (en) * | 2012-10-19 | 2014-05-07 | 宁波科博特钴镍有限公司 | Method and apparatus for preparing large particle size spherical tricobalt tetreoxide |
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| CN101434416A (en) * | 2008-11-28 | 2009-05-20 | 宁波金和新材料有限公司 | Hydroxy spherical cobaltosic oxide and preparation thereof |
| CN101585559A (en) * | 2009-06-14 | 2009-11-25 | 宁波科博特钴镍有限公司 | Preparation method of spherical cobaltosic oxide with high battery security |
| CN102134105A (en) * | 2011-05-09 | 2011-07-27 | 四川大学 | Method for accessorily preparing nanometer cobaltosic oxide granules at room temperature by utilizing amino acids |
| CN103771539A (en) * | 2012-10-19 | 2014-05-07 | 宁波科博特钴镍有限公司 | Method and apparatus for preparing large particle size spherical tricobalt tetreoxide |
Non-Patent Citations (1)
| Title |
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| "Synthesis and catalytic property of facetcontrolled Co3O4 structures enclosed by (111) and (113) facets";Hai Zhou et al.;《CrystEngComm》;20160531;第18卷;第5456–5462页 * |
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