CN103170646A - Synthetic method of nanometer materials of cobalt fractal structure - Google Patents
Synthetic method of nanometer materials of cobalt fractal structure Download PDFInfo
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- CN103170646A CN103170646A CN2013101049330A CN201310104933A CN103170646A CN 103170646 A CN103170646 A CN 103170646A CN 2013101049330 A CN2013101049330 A CN 2013101049330A CN 201310104933 A CN201310104933 A CN 201310104933A CN 103170646 A CN103170646 A CN 103170646A
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Abstract
The invention discloses a synthetic method of nanometer materials of a cobalt fractal structure and relates to preparation of cobalt nanometer materials. The synthetic method solves the problem that a preparation method of cobalt-based nanometer materials of a fractal structure does not exist in the prior art. The method comprises the following steps of (1) taking cobalt salt and reducing agent as a mixed precursor, dissolving the mixed precursor in alkaline deionized water solution, and stirring until fully dissolved; (2) transferring the obtained precursor solution into a reaction kettle to conduct temperature rising reaction; (3) cooling to indoor temperature, using deionized water to wash an obtained product, then conducting centrifugation and vacuum drying, and manufacturing the nanometer materials of the cobalt fractal structure. The method is low in material cost, simple in the synthetic method and easy to operate. Adjusting of the reaction speed is easily achieved by controlling concentration, temperature and potential of hydrogen (PH) value of a reactant, and therefore, the nanometer materials of the cobalt fractal structure is obtained, and the product shapes and sizes of the nanometer materials of the cobalt fractal structure are effectively controlled.
Description
Technical field
The present invention relates to metallic cobalt (Co) preparations of nanomaterials method, be specifically related to a kind of hydrothermal synthesis method of metallic cobalt fractal structure nano material.
Background technology
Cobalt is a kind of ash gray transitional metal, has ferromagnetism, and matter is hard and crisp, and chemical stability is good in normal temperature atmosphere, and its Main physical, chemical parameters and iron, nickel approach, and belong to iron family element.Due to its good physics, chemistry and mechanical performance, it is the important source material of producing the materials such as high temperature resistant, corrosion-resistant, high strength and ferromagnetism.The largest application areas of cobalt is secondary cell.The research and development competition of lithium secondary battery is very fierce, all synthetic chemical property is superior and security performance the is good lithium ion secondary battery anode material emphasis as research and development, the positive electrode of exploitation has cobalt acid lithium or lithiated nickel dioxide cobalt or lithium cobalt oxide manganese to World Developed Countries.Due to the advantageous property of cobalt, be difficult to be replaced by other metals aspect high temperature resistant, corrosion resisting alloy making, superalloy is the second largest application of cobalt at present.In addition, cobalt powder is used as high temperature alloy adhesive, rare earth permanent magnet functional material and industrial catalyst etc. widely.
Than block materials, the cobalt nano material shows unique magnetics, catalytic performance due to the impact of the microeffects such as small-size effect, skin effect.This makes it have more wide potential using value at aspects such as magnetic inductor, high density magnetic storage medium, catalysis.Up to now, the nano material of the multiple special appearances such as the nano particle of metal cobalt, rod, nano wire, nano chain, nanotube, nano flower has all been furtherd investigate, but the cobalt-based preparations of nanomaterials method with fractal structure has no report.
Summary of the invention
The object of the invention is to overcome the shortcoming of prior art, a kind of synthetic method of metallic cobalt fractal structure nano material is provided, solve the technical problem that prior art there is no the cobalt-based preparation method of nano material of fractal structure.
The present invention is achieved by the following technical solutions:
A kind of synthetic method of metallic cobalt fractal structure nano material, step is as follows:
1) take cobalt salt and reducing agent as mixing presoma, it is dissolved in alkaline deionized water solution, is stirred to dissolving fully;
2) the gained precursor solution is moved in reactor temperature reaction;
3) be cooled to room temperature, products therefrom is washed rear centrifugal, vacuum drying with deionized water, can make the nano material of the fractal structures such as metallic cobalt nanometer blade, nanometer snowflake, nanometer tree branches.
Described cobalt salt is cobalt chloride, cobaltous sulfate, cobalt carbonate, cobalt oxalate, cobalt acetate or basic cobaltous carbonate.
Described reducing agent is hydrazine hydrate or sodium borohydride.
The mass ratio of described cobalt salt and reducing agent is 1:10～100, and the consumption of deionized water is cobalt salt and reducing agent gross mass 5～20 times.
Described alkaline deionized water solution is the deionized water solution of NaOH or potassium hydroxide, and the molar concentration of NaOH or potassium hydroxide is 0～5mol/L, and the solution pH value is 7～14.
The reaction temperature of described precursor solution is 90～180 ℃, and the reaction time is 2～4 hours.
The washing of described deionized water, centrifugal 3 times, centrifuge speed 15000rad/min; Vacuum drying is carried out in the electric vacunm drying case, and vacuum is-0.1MPa.
The invention has the advantages that the persursor material cost is low, synthetic method is simple, easy operating; Be easy to realize adjusting to reaction speed by the control to reactant concentration, temperature of reaction system, pH value, and then obtain the nano material of the effectively controlled metallic cobalt fractal structure of product pattern, size.
Description of drawings
Fig. 1 is the SEM figure of a kind of flakes nanometer cobalt elemental crystal of making of the present invention;
Fig. 2 is the SEM figure of a kind of dendroid nanometer cobalt elemental crystal of making of the present invention;
Fig. 3 is the XRD figure of a kind of foliaceous nanometer cobalt elemental crystal of making of the present invention.
The specific embodiment
Embodiment 1:
Take 0.143g cobalt chloride, 4ml hydrazine hydrate, add in 40ml NaOH deionized water solution, the NaOH molar concentration is 1.5mol/L, and the solution pH value is 7, and it is dissolved fully, stirs half an hour at normal temperatures, and precursor solution is fully mixed; The precursor solution that mixes is transferred in reactor, is heated to 180 ℃ of reactions 3 hours with thermostatic drying chamber; Be cooled to room temperature, with products therefrom with deionized water washing, centrifugal 3 times, centrifuge speed 15000rad/min, dry in the electric vacunm drying case afterwards, vacuum is-0.1MPa to make flakes nanometer cobalt elemental crystal (see figure 1).
Embodiment 2:
Take 0.143g cobalt chloride, 1.9g sodium borohydride, add in 40ml NaOH deionized water solution, naoh concentration is 5mol/L, and the solution pH value is 9, and it is dissolved fully, stirs half an hour at normal temperatures, and precursor solution is fully mixed; The precursor solution that mixes is transferred in reactor, is heated to 100 ℃ of reactions 4 hours with thermostatic drying chamber; Be cooled to room temperature, with products therefrom with deionized water washing, centrifugal 3 times, centrifuge speed 15000rad/min, dry in the electric vacunm drying case afterwards, vacuum is-0.1MPa to make dendroid nanometer cobalt elemental crystal (see figure 2).
Embodiment 3:
Take 0.72g cobalt acetate, 4ml hydrazine hydrate, add in 40ml potassium hydroxide deionized water solution, concentration of potassium hydroxide is 1.5mol/L, and the solution pH value is 8, and it is dissolved fully, stirs half an hour at normal temperatures, and precursor solution is fully mixed; The precursor solution that mixes is transferred in reactor, utilizes thermostatic drying chamber to be heated to 120 ℃ of reactions 2 hours; Be cooled to room temperature, with products therefrom with deionized water washing, centrifugal 3 times, centrifuge speed 15000rad/min, dry in the electric vacunm drying case afterwards, vacuum is-0.1MPa to make foliaceous nanometer cobalt elemental crystal (see figure 3).
Fig. 3 is the XRD figure of resulting materials, adopts X ' Pert Pro MPD X-ray diffractometer (Cu target K
αRay, wavelength X=0.154nm).The reference standard card can find out, synthetic material is the cobalt elemental crystal of the six close pile structures of side.
Embodiment 4:
Take 0.143g cobaltous sulfate, 4ml hydrazine hydrate, add in 40ml NaOH deionized water solution, the NaOH molar concentration is 1.5mol/L, and the solution pH value is 7, and it is dissolved fully, stirs half an hour at normal temperatures, and precursor solution is fully mixed; The precursor solution that mixes is transferred in reactor, is heated to 90 ℃ of reactions 4 hours with thermostatic drying chamber; Be cooled to room temperature, with products therefrom with deionized water washing, centrifugal 3 times, centrifuge speed 15000rad/min, dry in the electric vacunm drying case afterwards, vacuum is-0.1MPa to make flakes nanometer cobalt elemental crystal (see figure 1).
Embodiment 5:
Take 0.143g cobalt carbonate, 1.9g sodium borohydride, add in 40ml NaOH deionized water solution, naoh concentration is 5mol/L, and the solution pH value is 9, and it is dissolved fully, stirs half an hour at normal temperatures, and precursor solution is fully mixed; The precursor solution that mixes is transferred in reactor, is heated to 100 ℃ of reactions 4 hours with thermostatic drying chamber; Be cooled to room temperature, with products therefrom with deionized water washing, centrifugal 3 times, centrifuge speed 15000rad/min, dry in the electric vacunm drying case afterwards, vacuum is-0.1MPa to make dendroid nanometer cobalt elemental crystal (see figure 2).
Embodiment 6:
Take 0.72g cobalt oxalate, 72ml hydrazine hydrate, add in 360ml potassium hydroxide deionized water solution, concentration of potassium hydroxide is 1.5mol/L, and the solution pH value is 14, and it is dissolved fully, stirs half an hour at normal temperatures, and precursor solution is fully mixed; The precursor solution that mixes is transferred in reactor, utilizes thermostatic drying chamber to be heated to 120 ℃ of reactions 2 hours; Be cooled to room temperature, with products therefrom with deionized water washing, centrifugal 3 times, centrifuge speed 15000rad/min, dry in the electric vacunm drying case afterwards, vacuum is-0.1MPa to make foliaceous nanometer cobalt elemental crystal (see figure 3).
Embodiment 7:
Take 0.143g basic cobaltous carbonate, 4ml hydrazine hydrate, add in 40ml NaOH deionized water solution, the NaOH molar concentration is 1.5mol/L, the solution pH value is 7, and it is dissolved fully, and stir half an hour at normal temperatures, precursor solution is fully mixed; The precursor solution that mixes is transferred in reactor, is heated to 90 ℃ of reactions 4 hours with thermostatic drying chamber; Be cooled to room temperature, with products therefrom with deionized water washing, centrifugal 3 times, centrifuge speed 15000rad/min, dry in the electric vacunm drying case afterwards, vacuum is-0.1MPa to make flakes nanometer cobalt elemental crystal (see figure 1).
Claims (7)
1. the synthetic method of a metallic cobalt fractal structure nano material, step is as follows:
1) take cobalt salt and reducing agent as mixing presoma, it is dissolved in alkaline deionized water solution, is stirred to dissolving fully;
2) the gained precursor solution is moved in reactor temperature reaction;
3) be cooled to room temperature, products therefrom is washed rear centrifugal, vacuum drying with deionized water, can make the nano material of metallic cobalt fractal structure.
2. the synthetic method of metallic cobalt fractal structure nano material according to claim 1, it is characterized in that: described cobalt salt is cobalt chloride, cobaltous sulfate, cobalt carbonate, cobalt oxalate, cobalt acetate or basic cobaltous carbonate.
3. the synthetic method of metallic cobalt fractal structure nano material according to claim 1, it is characterized in that: described reducing agent is hydrazine hydrate or sodium borohydride.
4. the synthetic method of metallic cobalt fractal structure nano material according to claim 1, it is characterized in that: the mass ratio of described cobalt salt and reducing agent is 1:10～100, the consumption of deionized water is cobalt salt and reducing agent gross mass 5～20 times.
5. the synthetic method of metallic cobalt fractal structure nano material according to claim 1, it is characterized in that: described alkaline deionized water solution is the deionized water solution of NaOH or potassium hydroxide, the molar concentration of NaOH or potassium hydroxide is 0～5mol/L, and the solution pH value is 7～14.
6. the synthetic method of metallic cobalt fractal structure nano material according to claim 1, it is characterized in that: the reaction temperature of described precursor solution is 90～180 ℃, the reaction time is 2～4 hours.
7. the synthetic method of metallic cobalt fractal structure nano material according to claim 1 is characterized in that: described deionized water washing, centrifugal 3 times, centrifuge speed 15000rad/min; Vacuum drying is carried out in the electric vacunm drying case, and vacuum is-0.1MPa.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103341641A (en) * | 2013-07-24 | 2013-10-09 | 厦门大学 | Preparing method for CoSb3 thermoelectric nanometer powder materials |
| CN104368825A (en) * | 2014-11-24 | 2015-02-25 | 中国人民解放军军械工程学院 | Preparation method for shape-controllable ferrocobalt magnetic nanoparticles |
| CN104550995A (en) * | 2013-10-23 | 2015-04-29 | 同济大学 | Gold-silver composite nano chain antibacterial agent synthesizing method |
| CN107584137A (en) * | 2017-09-14 | 2018-01-16 | 浙江大学 | A kind of method that solwution method prepares metallic cobalt |
| CN108500291A (en) * | 2018-03-16 | 2018-09-07 | 南京工业大学 | The preparation method of sheet cobalt powder in a kind of alkaline medium |
| CN113084183A (en) * | 2021-03-17 | 2021-07-09 | 电子科技大学 | Cunninghamia lanceolata leaf-shaped cobalt particles and method for preparing magnetic composite material by using same |
| CN116145175A (en) * | 2023-02-22 | 2023-05-23 | 兰州大学 | Electrocatalyst, preparation method and application thereof |
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| CN101537500A (en) * | 2009-04-24 | 2009-09-23 | 华东师范大学 | Novel three-dimensional flower-shaped metallic cobalt particle and preparation method thereof |
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2013
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101537500A (en) * | 2009-04-24 | 2009-09-23 | 华东师范大学 | Novel three-dimensional flower-shaped metallic cobalt particle and preparation method thereof |
Non-Patent Citations (3)
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| LIU ZHAO-TIE, ETAL.: "Synthesis and catalytic behaviors of cobalt nanocrystals with special morphologies", 《POWDER TECHNOLOGY》 * |
| QIAO RU, ETAL.: "Preparation of three-dimensional leaflike cobalt microcrystals and decoration of their surface with silver nanoparticles", 《JOURNAL OF NANOPARTICLE RESEARCH》 * |
| ZHU LU-PING, ETAL.: "Synthesis and characterization of novel three-dimensional metallic Co dendritic superstrctures by a simple hydrothermal reduction route", 《CRYSTAL GROWTH & DESIGN》 * |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103341641A (en) * | 2013-07-24 | 2013-10-09 | 厦门大学 | Preparing method for CoSb3 thermoelectric nanometer powder materials |
| CN104550995A (en) * | 2013-10-23 | 2015-04-29 | 同济大学 | Gold-silver composite nano chain antibacterial agent synthesizing method |
| CN104550995B (en) * | 2013-10-23 | 2016-08-03 | 同济大学 | A kind of synthetic method of gold silver composite Nano chain antibacterial |
| CN104368825A (en) * | 2014-11-24 | 2015-02-25 | 中国人民解放军军械工程学院 | Preparation method for shape-controllable ferrocobalt magnetic nanoparticles |
| CN107584137A (en) * | 2017-09-14 | 2018-01-16 | 浙江大学 | A kind of method that solwution method prepares metallic cobalt |
| CN107584137B (en) * | 2017-09-14 | 2020-04-03 | 浙江大学 | Method for preparing metal cobalt by solution method |
| CN108500291A (en) * | 2018-03-16 | 2018-09-07 | 南京工业大学 | The preparation method of sheet cobalt powder in a kind of alkaline medium |
| CN113084183A (en) * | 2021-03-17 | 2021-07-09 | 电子科技大学 | Cunninghamia lanceolata leaf-shaped cobalt particles and method for preparing magnetic composite material by using same |
| CN113084183B (en) * | 2021-03-17 | 2022-03-15 | 电子科技大学 | Cunninghamia lanceolata leaf-shaped cobalt particles and method for preparing magnetic composite material by using same |
| CN116145175A (en) * | 2023-02-22 | 2023-05-23 | 兰州大学 | Electrocatalyst, preparation method and application thereof |
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Application publication date: 20130626 |