CN107381660A - Sb, Mn codope cobaltosic oxide nano flower-like microsphere preparation method - Google Patents
Sb, Mn codope cobaltosic oxide nano flower-like microsphere preparation method Download PDFInfo
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Abstract
The invention discloses a kind of Sb, Mn codope cobaltosic oxide nano flower-like microsphere preparation methods, CTAB is dissolved in ethanol solution, and antimonic salt, manganese salt and cobalt salt are added in above-mentioned solution and obtain solution A；Ammonium fluoride, urea, which add, obtains solution B into solution A；Solution B is placed in ptfe autoclave, after reaction terminates, sediment is washed into drying and calcining, finally gives the Sb of crystallization, Mn codopes Co3O4Nanometer sheet self aggregation nano flower-like microballoon.Hydro-thermal method and double ion original position doping method are combined by the present invention, by antimony and additive Mn in cobaltosic oxide nano oxide, this method has preparation technology simple, pattern is easy to the advantages such as regulation and control, resulting composite has the characteristics that specific surface area is big, product stability is high, is such as catalyzed in various fields, there is great application value in energy storage, sensing field.
Description
Technical field
The invention belongs to nano composite material technical field, especially a kind of Sb, Mn- codopes cobaltosic oxide nano flower
Shape microballoon preparation method, specially in nano-cobaltic-cobaltous oxide（Co3O4）The preparation side of situ codope two kinds of metallic elements of Sb, Mn
Method, and products thereof and application.
Background technology
Small size effect, skin effect, quantum size effect, the macro quanta tunnel effect that nano material possesses, and
Dielectric confinement effect etc., and there is numerous characteristics and essential characteristic, this also causes nano material in optics, calorifics, catalysis, light
Electrochemistry and chemical property etc. show to be different from general block materials characteristic.
Energy problem, it is the topic that people compare concern always.And energy storage is also considered new energy by the external world
Develop last one kilometer problem to be solved, meanwhile, the utilization of energy technology, be also considered as New Energy Industry last
Block cake.Nanometer technology is applied to new energy field, is one of the emphasis direction of researchers' research.Lithium ion battery works
Principle is that charge-discharge principle is：In charging, positive pole has lithium ion generation, and negative pole is reached by electrolyte.After reaching negative pole, lithium
Ion is embedded in negative material, and embedded is more, and charging capacity is higher.Discharge process is exactly the mistake that lithium ion reaches positive pole from negative pole
Journey.And nano material has that size is small, the big grade of specific surface area some it is exclusive the characteristics of, then when it is applied to electrode material, than
Surface area increases, and can shorten lithium ion transport path, and can make the advantages such as Volume Changes reduction.
Transition metal oxide is a kind of compound combined by transition metal atoms with oxygen atom, and they generally have general
The characteristic that logical nano material is connected with（Quantum size effect etc.）, it is universal due to its superior catalytic activity and semiconductor property
Use.And design and prepare multicomponent nanocomposite electrode material, advantageously reduce the surface energy of active material and reduce in electrolyte
Agglomeration between the generation of irreversible side reaction and active component.
The content of the invention
For overcome the deficiencies in the prior art, present invention aims at：Provide a kind of Sb, Mn- codope cobaltosic oxides
Nano flower-like microballoon preparation method.
Another object of the present invention is：The product that above-mentioned preparation method obtains is provided.
A further object of the present invention is：The application that above-mentioned preparation method obtains product is provided.
The object of the invention is realized by following proposal：
A kind of Sb, Mn- codope Co3O4The preparation method of nano flower-like microballoon, comprises the steps：
1）Surfactant CTAB is dissolved in ethanol solution, and antimonic salt, manganese salt and cobalt salt are added in above-mentioned solution and obtain solution
A；
2）Ammonium fluoride, urea, which add, obtains solution B into solution A, wherein, Surfactant CTAB used, antimonic salt, manganese salt,
The mol ratio of ammonium fluoride, urea and cobalt salt is antimonic salt：Manganese salt：Ammonium fluoride：Urea：Mol ratio=0.002 ~ 0.008 of cobalt salt:
0.001~0.005:0.1~3:15~36；
3）Solution B is placed in ptfe autoclave, after reaction terminates, sediment is washed into drying and calcining, finally gives crystalline substance
The Sb of change, Mn- codope Co3O4Nanometer sheet self aggregation nano flower-like microballoon.
Hydro-thermal method and double ion original position doping method are combined by the present invention, by antimony and additive Mn in cobaltosic oxide nano oxygen
In compound, this method has that preparation technology is simple, and pattern, which is easy to advantage, the resulting composites such as regulation and control, has specific surface area
Greatly, the features such as product stability is high.
The present invention is specifically, in the steps below：
（1）Weigh 0.3 g Surfactant CTABs to be dissolved in 100 ml ethanol solutions, stir 30 min, be completely dissolved it；
（2）Antimonic salt, manganese salt and cobalt salt are added in above-mentioned solution according to a certain percentage, and by the solution magnetic agitation 30 ~ 60
Min, obtain uniform settled solution A；
（3）Weigh a certain amount of ammonium fluoride, urea is added into solution A, stirring, obtain solution B；
（4）Solution B obtained above is placed in ptfe autoclave, is carried out at a temperature of 100 DEG C ~ 160 DEG C anti-
Should, the reaction time was controlled at 3 ~ 10 hours；
（5）After reaction terminates, by sediment successively with ethanol, distillation water washing, dried 8 hours at a temperature of 90 DEG C, Ran Houjin
One step is calcined 2 hours at a temperature of obtained solid powder is placed in into 450 DEG C, finally gives the Sb of crystallization, Mn- codopes
Co3O4Nanometer sheet self aggregation nano flower-like microballoon.
On the basis of such scheme, described antimonic salt is one kind in antimony chloride or nitric acid antimony.
On the basis of such scheme, described cobalt salt is cabaltous nitrate hexahydrate Co (NO3)2·6H2O or cobalt acetate Co
(CH3COO)2·4H2O。
The present invention provides a kind of a kind of Sb obtained according to above-mentioned preparation method, Mn- codopes Co3O4Nano flower-like microspheres product.
For Sb, Mn- codopes Co3O4Nanometer sheet self aggregation nano flower-like microballoon.The present invention proposes that a kind of simple, economic double ion is former
Position doping method, using solvent heat means, a step realizes the Effective Doping of two kinds of elements, and structure is multilevel hierarchy, by particle group
Into the further autohemagglutination of laminated structure integrate flower-like microsphere.
The present invention is also provided according to application of the product that above-mentioned preparation method obtains as lithium ion battery negative material.
Hydro-thermal method and double ion original position doping method are combined by the present invention, by antimony and additive Mn in cobaltosic oxide nano oxygen
In compound, a kind of simple, economic double ion original position doping method is proposed, using solvent heat means, a step realizes two kinds of elements
Effective Doping, structure is multilevel hierarchy, and the further autohemagglutination of the laminated structure being made up of particle integrates flower-like microsphere, obtains Sb,
Mn- codopes Co3O4Nanometer sheet self aggregation nano flower-like microballoon.Present invention process is simple, and pattern is easy to the advantages such as regulation and control, gained
To composite have the characteristics that specific surface area is big, product stability is high, be such as catalyzed in various fields, energy storage, sensing neck
There is great application value in domain.And the Sb, Mn- codopes Co of this method synthesis3O4Compound, by nanometer sheet self aggregation nanometer
Flower-like microsphere, three-dimensional structure is formed, the specific surface area of material can be increased.Electrochemistry during as lithium ion battery negative material
Performance improves, it is considered to be a kind of material with good prospect.
Brief description of the drawings
Fig. 1 is the Sb, Mn- codopes Co that the embodiment of the present invention 1 synthesizes3O4The scanning electron microscope (SEM) photograph of nano flower-like microballoon；
Fig. 2 be the embodiment of the present invention it is 2-in-1 into Sb, Mn codopes Co3O4The scanning electron microscope (SEM) photograph of nano flower-like microballoon；
Fig. 3 be the embodiment of the present invention it is 2-in-1 into Sb, Mn codopes Co3O4The chemical property figure of nano flower-like microballoon.
Embodiment
The present invention is described in detail by following instantiation, but protection scope of the present invention is not only restricted to these implementations
Example.
A kind of Sb, Mn- codope Co3O4The preparation method of nano flower-like microballoon, it is characterised in that comprise the following steps：
1）Surfactant CTAB is dissolved in ethanol solution, and antimonic salt, manganese salt and cobalt salt are added in above-mentioned solution and obtain solution
A；
2）Ammonium fluoride, urea, which add, obtains solution B into solution A, wherein, Surfactant CTAB used, antimonic salt, manganese salt,
The mol ratio of ammonium fluoride, urea and cobalt salt is antimonic salt：Manganese salt：Ammonium fluoride：Urea：Mol ratio=0.002 ~ 0.008 of cobalt salt:
0.001~0.005:0.1~3:15~36；
3）Solution B is placed in ptfe autoclave, after reaction terminates, sediment is washed into drying and calcining, finally gives crystalline substance
The Sb of change, Mn- codope Co3O4Nanometer sheet self aggregation nano flower-like microballoon.
Embodiment 1
（1）Weigh 0.3 g Surfactant CTABs to be dissolved in 100 ml ethanol solutions, stir 30 min, be completely dissolved it；
（2）Weigh 2.9105 g cabaltous nitrate hexahydrate Co (NO3)2·6H2O, 0.1825 g antimony chlorides and 0.0016 g permanganic acid
Potassium
To adding in above-mentioned solution, and by the solution magnetic agitation 50 min, uniform settled solution A is obtained；
（3）Weigh 1.11 g ammonium fluorides and 9.00 g urea are added into solution A, stir, obtain solution B；
（4）Solution B obtained above is placed in ptfe autoclave, is reacted at a temperature of 160 DEG C, during reaction
Between control at 3 hours；
（5）After reaction terminates, by sediment successively with ethanol, distillation water washing, dried 8 hours at a temperature of 90 DEG C, Ran Houjin
One step is calcined 2 hours at a temperature of obtained solid powder is placed in into 450 DEG C, finally gives the Sb of crystallization, Mn- codopes
Co3O4Nanometer sheet self aggregation nano flower-like microballoon.
Fig. 1 is the stereoscan photograph of the material.
Embodiment 2
（1）Weigh 0.3 g Surfactant CTABs to be dissolved in 100 ml ethanol solutions, stir 30 min, be completely dissolved it；
（2）Claim 2.4908 g cobalt acetate Co (CH3COO)2·4H2O, 0.0062 g nitric acid antimony and 0.0016 g potassium permanganate
To adding in above-mentioned solution, and by the solution magnetic agitation 60 min, uniform settled solution A is obtained；
（3）Weigh 0.037 g ammonium fluorides and 21.6216 g urea are added into solution A, stir, obtain solution B；
（4）Solution B obtained above is placed in ptfe autoclave, is reacted at a temperature of 100 DEG C, during reaction
Between control at 10 hours；
（5）After reaction terminates, by sediment successively with ethanol, distillation water washing, dried 8 hours at a temperature of 90 DEG C, Ran Houjin
One step is calcined 2 hours at a temperature of obtained solid powder is placed in into 450 DEG C, finally gives the Sb of crystallization, Mn- codopes
Co3O4Nanometer sheet self aggregation nano flower-like microballoon.
Fig. 2 is the stereoscan photograph of the material.
Embodiment 3
（1）Weigh 0.3 g Surfactant CTABs to be dissolved in 100 ml ethanol solutions, stir 30 min, be completely dissolved it；
（2）Claim 2.4908 g cobalt acetate Co (CH3COO)2·4H2O, 0.1539 g nitric acid antimony and 0.0016 g potassium permanganate
To adding in above-mentioned solution, and by the solution magnetic agitation 30 min, uniform settled solution A is obtained；
（3）Weigh 0.37 g ammonium fluorides and 9.6096 g urea are added into solution A, stir, obtain solution B；
（4）Solution B obtained above is placed in ptfe autoclave, is reacted at a temperature of 150 DEG C, during reaction
Between control at 6 hours；
（5）After reaction terminates, by sediment successively with ethanol, distillation water washing, dried 8 hours at a temperature of 90 DEG C, Ran Houjin
One step is calcined 2 hours at a temperature of obtained solid powder is placed in into 450 DEG C, finally gives the Sb of crystallization, Mn- codopes
Co3O4Nanometer sheet self aggregation nano flower-like microballoon.
Fig. 2 is the stereoscan photograph of the material.
Claims (6)
1. a kind of Sb, Mn- codope cobaltosic oxide nano flower-like microsphere preparation method, it is characterised in that comprise the following steps：
1）Surfactant CTAB is dissolved in ethanol solution, and antimonic salt, manganese salt and cobalt salt are added in above-mentioned solution and obtain solution
A；
2）Ammonium fluoride, urea, which add, obtains solution B into solution A, wherein, Surfactant CTAB used, antimonic salt, manganese salt,
The mol ratio of ammonium fluoride, urea and cobalt salt is antimonic salt：Manganese salt：Ammonium fluoride：Urea：Mol ratio=0.002 ~ 0.008 of cobalt salt:
0.001~0.005:0.1~3:15~36；
3）Solution B is placed in ptfe autoclave, after reaction terminates, sediment is washed into drying and calcining, finally gives crystalline substance
The Sb of change, Mn- codope Co3O4Nanometer sheet self aggregation nano flower-like microballoon.
2. Sb according to claim 1, Mn- codope cobaltosic oxide nano flower-like microsphere preparation method, it is characterised in that tool
Body step is as follows：
（1）Weigh 0.3 g Surfactant CTABs to be dissolved in 100 ml ethanol solutions, stir 30 min, be completely dissolved it；
（2）Antimonic salt, manganese salt and cobalt salt are added in above-mentioned solution according to a certain percentage, and by the solution magnetic agitation 30 ~ 60
Min, obtain uniform settled solution A；
（3）Weigh a certain amount of ammonium fluoride, urea is added into solution A, stirring, obtain solution B；
（4）Solution B obtained above is placed in ptfe autoclave, is carried out at a temperature of 100 DEG C ~ 160 DEG C anti-
Should, the reaction time was controlled at 3 ~ 10 hours；
（5）After reaction terminates, by sediment successively with ethanol, distillation water washing, dried 8 hours at a temperature of 90 DEG C, Ran Houjin
One step is calcined 2 hours at a temperature of obtained solid powder is placed in into 450 DEG C, finally gives the Sb of crystallization, Mn- codopes
Co3O4Nanometer sheet self aggregation nano flower-like microballoon.
3. Sb according to claim 1 or 2, Mn- codope cobaltosic oxide nano flower-like microsphere preparation method, its feature exist
In described antimonic salt is one kind in antimony chloride or nitric acid antimony.
4. Sb according to claim 1 or 2, Mn- codope cobaltosic oxide nano flower-like microsphere preparation method, its feature exist
In described cobalt salt is cabaltous nitrate hexahydrate Co (NO3)2·6H2O or cobalt acetate Co (CH3COO)2·4H2O。
5. a kind of Sb obtained according to any preparation methods of claim 1-4, Mn- codope cobaltosic oxide nano flower-like microsphere
Product.
6. a kind of Sb according to claim 5, Mn- codope cobaltosic oxide nano flower-like microsphere are born as lithium ion battery
The application of pole material.
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Cited By (6)
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| CN108483513A (en) * | 2018-06-27 | 2018-09-04 | 台州聚合科技有限公司 | A kind of preparation method of three-dimensional flower-shaped cobaltosic oxide |
| 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 |
| CN114668850A (en) * | 2022-03-17 | 2022-06-28 | 中山市华舜科技有限责任公司 | Preparation method of capacitance antibacterial material |
| 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 |
| CN114804222A (en) * | 2022-06-16 | 2022-07-29 | 荆门市格林美新材料有限公司 | Nickel-manganese bimetal doped large-particle cobalt carbonate and preparation method and application thereof |
| CN115215381A (en) * | 2022-07-22 | 2022-10-21 | 广东邦普循环科技有限公司 | Manganese-doped cobaltosic oxide and preparation method and application thereof |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108483513A (en) * | 2018-06-27 | 2018-09-04 | 台州聚合科技有限公司 | A kind of preparation method of three-dimensional flower-shaped cobaltosic oxide |
| CN108483513B (en) * | 2018-06-27 | 2020-01-10 | 台州聚合科技有限公司 | Preparation method of three-dimensional flower-like cobaltosic oxide |
| 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 |
| 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 |
| CN114668850A (en) * | 2022-03-17 | 2022-06-28 | 中山市华舜科技有限责任公司 | Preparation method of capacitance antibacterial material |
| CN114668850B (en) * | 2022-03-17 | 2024-04-19 | 中山市华舜科技有限责任公司 | Preparation method of capacitor antibacterial material |
| CN114804222A (en) * | 2022-06-16 | 2022-07-29 | 荆门市格林美新材料有限公司 | Nickel-manganese bimetal doped large-particle cobalt carbonate and preparation method and application thereof |
| CN115215381A (en) * | 2022-07-22 | 2022-10-21 | 广东邦普循环科技有限公司 | Manganese-doped cobaltosic oxide and preparation method and application thereof |
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