CN103737016B - The preparation method of thorny magnetic nickel nanowire - Google Patents
The preparation method of thorny magnetic nickel nanowire Download PDFInfo
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- CN103737016B CN103737016B CN201410002979.6A CN201410002979A CN103737016B CN 103737016 B CN103737016 B CN 103737016B CN 201410002979 A CN201410002979 A CN 201410002979A CN 103737016 B CN103737016 B CN 103737016B
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Abstract
The present invention provides the preparation method of a kind of thorny magnetic nickel nanowire: comprise the following steps: step one: configuration nickel salt aqueous solution, and supersound process, mixes; Step 2: add in described nickel salt aqueous solution and go back original reagent, supersound process, mix, obtain solution A; Step 3: pour in reactor by described solution A, puts into the baking oven of externally-applied magnetic field, and heating, reacts, finally obtain thorny magnetic nickel nanowire. The nickel nanowire diameter that the inventive method obtains is 0.5��2 ��m, and length, from tens microns to several millimeters, has extremely high length-to-diameter ratio, and the thorn-like structure on surface can reach 0.3��1 ��m. The diameter of thorny magnetic nickel nanowire, the length of thorn and density are carried out optimising and adjustment by parameters such as nickel ion concentration, reaction times, temperature of reaction and magnetic field sizes in change reaction solution by the present invention. Preparation method of the present invention is novel, technique is simple, energy consumption is low, workable.
Description
Technical field
The present invention relates to the preparation method of a kind of nano material, the preparation method of especially a kind of thorny magnetic nickel nanowire.
Background technology
Nickel (Ni) nano material has the performances such as excellent magnetic, light, point and catalysis, all has broad application prospects in fields such as electronic information, chemical industry, the energy and catalysis. In recent years, the nickel nano material of various shape looks by a large amount of research and preparations, such as Ni nano flower, Ni nano chain, Ni nanometer sheet, Ni nano wire, dendritic structure and hollow structure etc.
Wherein, one dimension nickel nano-material has broader application space compared with zero dimension due to its continuity and high length-to-diameter ratio, and the point effect that the nickel nano wire of thorn-like brings because having the needle point structure of bigger shape anisotropy and surface uniqueness, show excellent electronic conduction and field-causing electron emission characteristic. Therefore aspect is manufactured and designed for its mechanism of crystal growth and advanced material and there is important researching value and meaning.
Through existing literature search being found, preparation method many employings tensio-active agent of thorn-like Ni nano wire, this method needs to adopt extra step to remove tensio-active agent after completing to prepare, and in batch production, operation is loaded down with trivial details and cost is higher.
Summary of the invention
For defect of the prior art, it is an object of the invention to provide the preparation method of a kind of thorny magnetic nickel nanowire.
The present invention is achieved by the following technical solutions:
The present invention provides the preparation method of a kind of thorny magnetic nickel nanowire, and described method comprises the following steps:
Step one: configuration nickel salt aqueous solution, supersound process so that it is be uniformly dissolved; Obtain solution A;
Step 2: add in described solution A and go back original reagent, supersound process so that it is mix, obtain solution B;
Step 3: pour in reaction vessel by described solution B, when putting into externally-applied magnetic field, reacting by heating, finally obtains thorny magnetic nickel nanowire.
Preferably, in step one, the concentration of nickel salt aqueous solution is 0.1��30mol/L.
Preferably, in step one, described nickel salt aqueous solution is nickel chloride aqueous solution or the nickelous acetate aqueous solution.
Preferably, in step 2, described in go back original reagent be hydrazine hydrate.
Preferably, the mass percent concentration going back original reagent described in is 1��30%.
Preferably, in step 2, described solution A is 1:(1��80 with the volume ratio going back original reagent).
Preferably, in step 3, described Heating temperature is 60��100 DEG C, and heat-up time is 0.5��20h.
Preferably, in step 3, described reactive mode is that heating in water bath for reaction and hydro-thermal reaction are closed.
Preferably, in step 3, described applied field strengths is 0.01��4T.
The time of described supersound process is 1��60 minute.
Compared with prior art, the present invention has following useful effect:
(1) preparation method of the present invention is novel, technique is simple, energy consumption is low, workable.
(2) diameter of thorny magnetic nickel nanowire, the length of thorn and density are carried out optimising and adjustment by parameters such as nickel ion concentration, reaction times, temperature of reaction and magnetic field sizes in change reaction solution by the present invention.
(3) the inventive method prepares the nickel nanowire diameter obtained is 0.5��2 ��m, and length, from tens microns to several millimeters, has extremely high length-to-diameter ratio, and the thorn-like structure on surface can reach 0.3��1 ��m.
Accompanying drawing explanation
By reading with reference to the detailed description that non-limiting example is done by the following drawings, the other features, objects and advantages of the present invention will become more obvious:
Fig. 1 is the SEM figure of thorny magnetic nickel nanowire prepared by the embodiment of the present invention 1;
Fig. 2 is the SEM figure of thorny magnetic nickel nanowire prepared by the embodiment of the present invention 2;
Fig. 3 is the SEM figure of thorny magnetic nickel nanowire prepared by the embodiment of the present invention 3;
Fig. 4 is the SEM figure of thorny magnetic nickel nanowire prepared by the embodiment of the present invention 4;
Fig. 5 is the SEM figure of thorny magnetic nickel nanowire prepared by the embodiment of the present invention 5.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in detail. The technician contributing to this area is understood the present invention by following examples further, but does not limit the present invention in any form. It should be appreciated that to those skilled in the art, without departing from the inventive concept of the premise, it is also possible to make some distortion and improvement. These all belong to protection scope of the present invention.
Embodiment 1
The present embodiment relates to the preparation method of a kind of thorn-like nickel nano wire, and concrete steps are as follows:
Step one, the nickel chloride aqueous solution 100mL of configuration 0.01M, supersound process 10min makes it be sufficiently uniformly dissolved, and is designated as solution A;
Step 2, drips in above-mentioned solution A and adds 1mL hydrazine hydrate, and supersound process 10min makes it mix, and obtains solution B.
Step 3, pours into solution B in reactor and is placed in the baking oven in additional 0.5T magnetic field, react 8h at 80 DEG C, and product is taken out after terminating and cleans clean by question response, finally obtains thorn-like nickel nano wire.
As shown in Figure 1, nickel line diameter is 0.8��1.2 ��m to the stereoscan photograph that the present embodiment prepares thorn-like nickel nano wire, and length is 0.5��1 millimeter, and the thorn-like structure on surface can reach 500��700nm.
Embodiment 2
The present embodiment relates to the preparation method of a kind of thorn-like nickel nano wire, and concrete steps are as follows:
Step one, the nickel chloride aqueous solution 100mL of configuration 3M, supersound process 10min makes it be sufficiently uniformly dissolved, and is designated as solution A.
Step 2, drips in above-mentioned solution A and adds 80mL hydrazine hydrate, and supersound process 10min makes it mix, and obtains solution B.
Step 3, pours into solution B in reactor and is placed in the baking oven in additional 0.5T magnetic field, react 20h at 90 DEG C, and product is taken out after terminating and cleans clean by question response, finally obtains thorn-like nickel nano wire.
As shown in Figure 2, nickel line diameter is 1��1.6 ��m to the stereoscan photograph that the present embodiment prepares thorn-like nickel nano wire, and length is 0.5��1.5 millimeter, the nickel Ci Keda 400��700nm on surface.
Embodiment 3
The present embodiment relates to the preparation method of a kind of thorn-like nickel nano wire, and concrete steps are as follows:
Step one, the nickelous acetate aqueous solution 100mL of configuration 0.05M, supersound process 10min makes it be sufficiently uniformly dissolved, and is designated as solution A.
Step 2, drips in above-mentioned solution A and adds 5mL hydrazine hydrate, and supersound process 10min makes it mix, and obtains solution B.
Step 3, pours into solution B in reactor and is placed in the baking oven in additional 4T magnetic field, react 5h at 80 DEG C, and product is taken out after terminating and cleans clean by question response, finally obtains thorn-like nickel nano wire.
As shown in Figure 3, nickel line diameter is about 1.4��2 ��m to the stereoscan photograph that the present embodiment prepares thorn-like nickel nano wire, and long in order straight, length can reach 1��2 millimeter, and the thorn-like structure on surface can reach 0.5��1 ��m.
Embodiment 4
The present embodiment relates to the preparation method of a kind of thorn-like nickel nano wire, and concrete steps are as follows:
Step one, the nickel chloride aqueous solution 100mL of configuration 0.1M, supersound process 10min makes it be sufficiently uniformly dissolved, and is designated as solution A.
Step 2, drips in above-mentioned solution A and adds 10mL hydrazine hydrate, and supersound process 10min makes it mix, and obtains solution B.
Step 3, is placed in solution B in the water-bath in additional 0.1T magnetic field, reacts 3h at 60 DEG C, and product is taken out after terminating and cleans clean by question response, finally obtains thorn-like nickel nano wire.
The stereoscan photograph that the present embodiment prepares thorn-like nickel nano wire is as shown in Figure 4. Nickel nanowire diameter is about 0.8 ��m, and length is 30��50 ��m, and the thorn-like structure on surface reaches 300��500nm.
Embodiment 5
The present embodiment relates to the preparation method of a kind of thorn-like nickel nano wire, and concrete steps are as follows:
Step one, the nickelous acetate aqueous solution 100mL of configuration 0.1M, supersound process 10min makes it be sufficiently uniformly dissolved, and is designated as solution A.
Step 2, drips in above-mentioned solution A and adds 10mL hydrazine hydrate, and supersound process 10min makes it mix, and obtains solution B.
Step 3, is placed in solution B in the water-bath in additional 0.01T magnetic field, reacts 0.5h at 100 DEG C, and product is taken out after terminating and cleans clean by question response, finally obtains thorn-like nickel nano wire.
The stereoscan photograph that the present embodiment prepares thorn-like nickel nano wire is as shown in Figure 5. Nickel nanowire diameter is about 0.5 ��m, and length is 20��40 ��m, and the thorn-like structure on surface is at about 300nm.
In sum: it is 0.5��2 ��m that the inventive method prepares the nickel nanowire diameter obtained, length, from tens microns to several millimeters, has extremely high length-to-diameter ratio, and the thorn-like structure on surface can reach 0.3��1 ��m. The diameter of thorny magnetic nickel nanowire, the length of thorn and density are carried out optimising and adjustment by parameters such as nickel ion concentration, reaction times, temperature of reaction and magnetic field sizes in change reaction solution by the present invention. Preparation method of the present invention is novel, technique is simple, energy consumption is low, workable.
Above specific embodiments of the invention are described. It is understood that the present invention is not limited to above-mentioned particular implementation, those skilled in the art can make various distortion or amendment within the scope of the claims, and this does not affect the flesh and blood of the present invention.
Claims (6)
1. the preparation method of a thorny magnetic nickel nanowire, it is characterised in that, described method comprises the following steps:
Step one: configuration nickel salt aqueous solution, supersound process so that it is be uniformly dissolved, is designated as solution A;
Step 2: add in described solution A and go back original reagent, supersound process so that it is mix, be designated as solution B;
Step 3: described solution B is poured in respective reaction container, when being placed in externally-applied magnetic field, reacting by heating, finally obtains thorny magnetic nickel nanowire; The nickel nanowire diameter obtained is 0.5��2 ��m, and length is from tens microns to several millimeters, and the length of the thorn-like structure on surface reaches 0.3��1 ��m;
Described nickel salt aqueous solution is nickel chloride aqueous solution or the nickelous acetate aqueous solution;
In step 2, described in go back original reagent be hydrazine hydrate;
In step 3, described Heating temperature is 80��100 DEG C, and heat-up time is 0.5��20h.
2. the preparation method of thorny magnetic nickel nanowire according to claim 1, it is characterised in that, in step one, the concentration of nickel salt aqueous solution is 0.1��30mol/L.
3. the preparation method of thorny magnetic nickel nanowire according to claim 1 and 2, it is characterised in that, described in go back original reagent mass percent concentration be 1%��30%.
4. the preparation method of thorny magnetic nickel nanowire according to claim 1, it is characterised in that, in step 2, described solution A is 1:(1��80 with the volume ratio going back original reagent).
5. the preparation method of thorny magnetic nickel nanowire according to claim 1, it is characterised in that, in step 3, described applied field strengths is 0.01��4T.
6. according to the preparation method of thorny magnetic nickel nanowire according to claim 1, it is characterised in that, the time of described supersound process is 1��60 minute.
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