CN102744418A - Method for synthesizing NiCo nano-alloy wire - Google Patents
Method for synthesizing NiCo nano-alloy wire Download PDFInfo
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- CN102744418A CN102744418A CN2012102141787A CN201210214178A CN102744418A CN 102744418 A CN102744418 A CN 102744418A CN 2012102141787 A CN2012102141787 A CN 2012102141787A CN 201210214178 A CN201210214178 A CN 201210214178A CN 102744418 A CN102744418 A CN 102744418A
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Abstract
The invention relates to a method for synthesizing a NiCo nano-alloy wire. The method comprises the following steps: taking a nickel-containing inorganic salt and a cobalt-containing inorganic salt as reaction precursors; placing the reaction precursors, a hydrazine hydrate reducing agent and a reaction medium ethylene glycol into a microwave heating instrument; and heating to 160 DEG C at a certain heating rate and reacting for 3-5 minutes, thereby obtaining the NiCo nano-alloy wire. Compared with the prior art, the method provided by the invention has the advantages of less time consumption, easiness in operation and control, and capability of preparing the NiCo nano-alloy wire with uniform size, magnetism and catalytic activity.
Description
Technical field
The invention belongs to technical field of nano material, relate to a kind of method of synthetic NiCo Nanoalloy line.
Background technology
One dimension Co Base Metal nano material not only has the various special effectses of common nano particle; And have unique shape anisotropy and a magnetic anisotropy; Be the important constituent element of constructing the electromagnet functional material, have important use in fields such as high density magnetic recording, sensitive components, electro-magnetic wave absorption, catalyst, medical science and Biofunctional materials.Wherein the functional material that synthesizes a new generation of Co base Nanoalloy material has been opened up new approach.
Fe, Co, the Ni transition elements is considered to element the most outstanding in above field; Because the material of its one dimension for example nanotube has many excellent properties with nano wire, studying and be applied in the method for preparing on these materials through physics and chemical method has: ball-milling method, electrochemical deposition; Laser ablation, chemical vapour deposition (CVD), sputtering method; Spray-on process, chemical reduction method or the like.These methods prepare not only complex process, are not easy operation and control, and length consuming time.Therefore, how obtaining the NiCo alloy nano-material of one dimension with the method for a kind of simple controllable and weak point consuming time, is a significant research topic.
Summary of the invention
The object of the invention is exactly to have the defective that technology of preparing exists now in order to overcome, and a kind of method of synthetic NiCo alloy wire is provided.
The object of the invention can be realized through following technical scheme:
A kind of method of synthetic NiCo Nanoalloy line; This method is with nickeliferous inorganic salts and contain the cobalt inorganic salts as the reaction precursor body; Reaction precursor body, reducing agent hydrazine hydrate, reaction medium ethylene glycol are placed in the heating using microwave instrument by a certain percentage; Heating rate with 30-60 ℃/min is heated to 160 ℃, through total time be 3-5 minute heating using microwave reaction, prepare the NiCo alloy wire.Concrete steps are following:
(1) with nickeliferous inorganic salts with contain the cobalt inorganic salts and be dissolved in respectively and be mixed with the solution that concentration is 0.60mol/L-0.12mol/L in the deionized water; Add a certain proportion of ethylene glycol and hydrazine hydrate then and be mixed with mixed solution, wherein nickeliferous inorganic salts are 10:1 ~ 1:10 with containing cobalt inorganic salts mole ratio; Ethylene glycol is 50:1 ~ 80:1 with the mol ratio that contains total amount of cobalt inorganic salts and nickeliferous inorganic salts; Hydrazine hydrate and nickeliferous inorganic salts are 1:15 ~ 1:50 with the mol ratio that contains total amount of substance of cobalt inorganic salts;
(2) mixed solution that step (1) is obtained moves in the microwave reaction flask, is heated to 160 ℃ with the heating rate of 30-60 ℃/min, sets to add thermal control program and makes whole heating process continue 3-5 minute.After reaction stops, cooling under field conditions (factors), centrifugation, washing, obtaining end product is black NiCo alloy wire.
Among the present invention, said nickeliferous inorganic salts are nickel chloride or nickel nitrate.The said cobalt inorganic salts that contain are cobalt chloride or cobalt acetate.
Among the present invention, washing described in the step (2) uses deionized water and absolute ethyl alcohol to replace washing.
Compared with prior art, the inventive method weak point consuming time, easy to operate and easy to control can be prepared the size homogeneous, has the NiCo alloy wire of magnetic and excellent degraded catalytic activity.
Description of drawings
Fig. 1 is the sem photograph of the product of embodiment 1.
Fig. 2 is the sem photograph of the product of embodiment 2.
Fig. 3 is a products therefrom power spectrum (EDS) among the embodiment 1.
Fig. 4 is the X-alpha spectrum (XRD) of products therefrom in the instance 1.
The specific embodiment
Below in conjunction with accompanying drawing and specific embodiment the present invention is elaborated.
The first step takes by weighing 0.7470g cobalt acetate (four water) and (AR) is dissolved in the ferric oxalate solution that the 25mL volumetric flask is made into 0.12mol/L, takes by weighing 0.7110g Nickel dichloride hexahydrate (AR) and is dissolved in the Nickel dichloride hexahydrate solution that the 25mL volumetric flask is made into 0.12mol/L.
Second goes on foot, and measures the Nickel dichloride hexahydrate solution of the 0.12mol/L of 1.00mL, and the cobalt acetate solution of the 0.12mol/L of 0.20mL, 20mL ethylene glycol (AR) solution ultrasonic ten minutes, add the 200uL hydrazine hydrate in the 100mL three-neck flask.Again MAS-II type normal pressure microwave synthetic/the extractive reaction work station in, select following microwave heating treatment scheme:
| P/w | T/℃ | t/s |
| 300 | 80 | 60 |
| 300 | 120 | 60 |
| 300 | 160 | 120 |
The 3rd step washed out product with the 10ml ethanolic solution, the black powder deposition in the product mixed liquor, occurs.The sonicated mixed liquor disperses it as far as possible in ethanolic solution, and under 3000 rev/mins speed centrifugal 10 minutes then, discard supernatant liquor, the deionized water that uses the same method, absolute ethyl alcohol alternately washs, centrifugal 5-10 time.Final sample is scattered in the absolute ethyl alcohol, and sample is analyzed.
(Fig. 1) can find out by ESEM, and product is the one dimension linear structure.Can find out that by energy chromatogram (EDS, accompanying drawing 3) product consists of Ni and Co, the copper mesh substrate of using when the Cu among the figure is test causes.Structural characterization XRD figure spectrum (accompanying drawing 4) by the powder x-ray diffraction appearance carries out is visible, and product is the FCC structure of NiCo alloy, and the products therefrom diameter is 50-80nm, and length is for being about 3um.
Measure the Nickel dichloride hexahydrate solution of the 0.12mol/L of 1.00mL, the cobalt acetate solution of the 0.12mol/L of 0.20mL, pvp0.0103g, 20mL ethylene glycol (AR) solution ultrasonic ten minutes, add the 200uL hydrazine hydrate in the 100mL three-neck flask.Again MAS-II type normal pressure microwave synthetic/the extractive reaction work station in, the microwave heating treatment scheme
| P/w | T/ | t/s |
| 300 | 80 | 60 |
| 300 | 120 | 60 |
| 300 | 160 | 120 |
Reaction is cooled to room temperature after finishing, and all the other steps are operated by embodiment 1.
(Fig. 2) can find out by ESEM, and product is the one dimension linear structure.
Claims (4)
1. the method for a synthetic NiCo Nanoalloy line is characterized in that concrete steps are following:
(1) with nickeliferous inorganic salts with contain the cobalt inorganic salts and be dissolved in that to be mixed with concentration in the deionized water be 0.60mol/L-0.12mol/L solution; Add ethylene glycol solvent then and the hydrazine hydrate reduction agent is mixed with mixed solution, wherein nickeliferous inorganic salts are 10:1 ~ 1:10 with containing cobalt inorganic salts mole ratio; Ethylene glycol and nickeliferous inorganic salts are 50:1 ~ 80:1 with the mol ratio that contains total amount of cobalt inorganic salts; The nickeliferous inorganic salts of hydrazine hydrate and presoma are 1:15 ~ 1:50 with the mol ratio that contains total amount of substance of cobalt inorganic salts;
(2) mixed solution that step (1) is obtained moves in the microwave reaction flask, is heated to 160 ℃ with the heating rate of 30-60 ℃/min, sets to add thermal control program and makes whole heating process continue 3-5 minute; After reaction stops, cooling under field conditions (factors), through centrifugation, washing, obtaining end product is black NiCo Nanoalloy line.
2. the method for a kind of synthetic NiCo Nanoalloy line according to claim 1 is characterized in that described nickeliferous inorganic salts are nickel chloride or nickel nitrate.
3. the method for a kind of synthetic NiCo Nanoalloy line according to claim 1 is characterized in that the described cobalt inorganic salts that contain are cobalt chloride or cobalt acetate.
4. the method for a kind of synthetic NiCo Nanoalloy line according to claim 1 is characterized in that use deionized water of washing described in the step (2) and absolute ethyl alcohol replace washing.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105215349A (en) * | 2015-03-02 | 2016-01-06 | 中国科学院理化技术研究所 | Micro-line of a kind of magnetic coupling and preparation method thereof |
| CN107584134A (en) * | 2017-09-20 | 2018-01-16 | 安徽大学 | A kind of microwave spark system for the spherical semi-hard magnet Co Ni non-crystaline amorphous metals of grade method |
Citations (5)
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| US20050056118A1 (en) * | 2002-12-09 | 2005-03-17 | Younan Xia | Methods of nanostructure formation and shape selection |
| CN101028653A (en) * | 2007-04-10 | 2007-09-05 | 北京科技大学 | Chemical production of metal nickel nano-line |
| US20080245186A1 (en) * | 2005-05-13 | 2008-10-09 | University Of Rochester | Synthesis of nano-materials in ionic liquids |
| CN101486102A (en) * | 2009-01-05 | 2009-07-22 | 江苏科技大学 | Method for preparing metallic nickel nano-wire |
| CN101698234A (en) * | 2009-10-21 | 2010-04-28 | 北京科技大学 | Chemical preparation method of metal cobalt nanowire |
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2012
- 2012-06-27 CN CN2012102141787A patent/CN102744418A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20050056118A1 (en) * | 2002-12-09 | 2005-03-17 | Younan Xia | Methods of nanostructure formation and shape selection |
| US20080245186A1 (en) * | 2005-05-13 | 2008-10-09 | University Of Rochester | Synthesis of nano-materials in ionic liquids |
| CN101028653A (en) * | 2007-04-10 | 2007-09-05 | 北京科技大学 | Chemical production of metal nickel nano-line |
| CN101486102A (en) * | 2009-01-05 | 2009-07-22 | 江苏科技大学 | Method for preparing metallic nickel nano-wire |
| CN101698234A (en) * | 2009-10-21 | 2010-04-28 | 北京科技大学 | Chemical preparation method of metal cobalt nanowire |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105215349A (en) * | 2015-03-02 | 2016-01-06 | 中国科学院理化技术研究所 | Micro-line of a kind of magnetic coupling and preparation method thereof |
| CN105215349B (en) * | 2015-03-02 | 2017-08-25 | 中国科学院理化技术研究所 | A kind of magnetic coupling micro-line and preparation method thereof |
| CN107584134A (en) * | 2017-09-20 | 2018-01-16 | 安徽大学 | A kind of microwave spark system for the spherical semi-hard magnet Co Ni non-crystaline amorphous metals of grade method |
| CN107584134B (en) * | 2017-09-20 | 2019-06-21 | 安徽大学 | A kind of microwave spark system for the spherical semi-hard magnet Co-Ni amorphous alloy of grade method |
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Application publication date: 20121024 |