CN103170649A - Preparation method of magnetic nickel nano material - Google Patents
Preparation method of magnetic nickel nano material Download PDFInfo
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- CN103170649A CN103170649A CN2013101310532A CN201310131053A CN103170649A CN 103170649 A CN103170649 A CN 103170649A CN 2013101310532 A CN2013101310532 A CN 2013101310532A CN 201310131053 A CN201310131053 A CN 201310131053A CN 103170649 A CN103170649 A CN 103170649A
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Abstract
The invention discloses a preparation method of a magnetic nickel nano material. According to the preparation method, a chemical reduction method is adopted to reduce a nickel salt precursor by using an organic reducing agent under the condition without inert gas protection, so as to prepare the magnetic nickel nano material. The particle sizes of the particles of the prepared magnetic nickel nano material are uniformly distributed. Compared with the high-temperature organic metal decomposition preparation and the sol-gel process, the preparation method has the advantages of simplicity and convenience in operation, low cost, low requirement on equipment and the like. The magnetic nickel nano material prepared by using the preparation method has wide application prospects in fields of catalysis, biologic techniques, data storage, environmental modification and the like.
Description
Technical field
The present invention relates to a kind of preparation method of nano material, particularly a kind of magnetic nickel nano material preparation method.
Background technology
Nano-nickel powder is high due to surface-active, pore-free permeates, specific area is large, great skin effect and bulk effect are arranged, physicochemical properties with a series of uniquenesses, in many new and high technologies, has important using value as fields such as effective catalyst, fuel cell, nano-coating material, carbide alloy bonding agent and biomedical carriers.To the preparation of nano nickel and the research of structure and performance etc. thereof, enjoyed the concern of domestic and international research institution in recent years.Utilize at present chemical method to prepare nano nickel and mainly take three kinds of methods.(1) carbonyl nickel thermal decomposition method: utilize pyrolysis, laser and the activation means such as ultrasonic, carbonyl nickel is decomposed, and nucleating growth, make the nano metal nickel particle.But the method decomposition temperature is higher, and nickel powder easy-sintering and carbonyl nickel are extremely toxic substances, easily human body and surrounding environment is impacted.(2) sol-gel process: metal alkoxide or inorganic salts through being hydrolyzed direct formation colloidal sol or through separating the solidifying colloidal sol that forms, then making solute polymerization gel, then organic principle is removed in gel drying, roasting, are obtained inorganic material at last.But use metal alkoxide to do raw material, cost is high, and pollution is arranged.(3) reducing process: reducing process is a kind of method that material is reduced into metal-powder in reducing atmosphere.Mainly comprise the methods such as solution reduction, solvothermal method, burning reducing process, hydrazine hydrate reduction method, polyol reduction method.This method compares with front two kinds of methods that to have process simple, is suitable for the advantage of suitability for industrialized production.At present, people have adopted different reducing agents, as hydrazine hydrate [Chen, D.H.; Wu, S.H. Synthesis of nickel nanoparticles in water-in-oil micro-emulsions.
Chem. Mater. 12 (2000) 1354 – 1360] and ethylene glycol [Li, DS; Komarneni, S. Microwave-assisted polyol process for synthesis of Ni nanoparticles.
J. Am. Ceram. Soc. 89 (2006) 1510-1517] prepared the magnetic nickel nano particle.CN200910145026.4 discloses a kind of method for preparing nickel nano particle under hydrothermal synthesizing condition.But the method has adopted strong inorganic reducing agent, highly basic and condition of high voltage, has numerously changed the material preparation operation, has increased preparation cost.
Summary of the invention
The object of the present invention is to provide a kind of need not under the condition of inert gas shielding, utilize the standby magnetic nickel nano material preparation method of organic reducing agent reduced nickel salt precursor system.Magnetic nickel nano material of the present invention has broad application prospects in fields such as catalysis, biotechnology, data storage and environment remediation.
The technical solution that realizes the object of the invention is: a kind of preparation method of magnetic Nano nickel material, and concrete steps are as follows:
A kind of preparation method of magnetic Nano nickel material is characterized in that, concrete steps are as follows:
Step 1 is dissolved in the nickel salt presoma in DMF, stirs, dissolving, then polyvinylpyrrolidone is joined in solution after dissolving, after mixing, refluxes and temperature reaction;
Step 2 treats that the solution that step 1 obtains is cooled to room temperature, and vacuum drying obtains the magnetic nickel nano material.
The present invention need not under the inert gas shielding condition; adopt N; dinethylformamide (DMF) is as the reducing agent of nickel salt presoma; its principle is: under hot conditions; N; dinethylformamide (DMF) is reduced to nickel simple substance with nickel ion in as nickel salt presoma solvent, himself is oxidized to carboxylic acid.Course of reaction can be represented by following chemical equation:
HCONMe
2?+?Ni
2+?+?H
2O→?Ni?+?Me
2NCOOH?+?2H
+
Polyvinylpyrrolidone (PVP) is dissolvable in water DMF (DMF), and the magnetic nickel nano material that produces has been played the effect of stable and protection.Thereby prevented to a certain extent the oxidation of product.
The present invention compared with prior art, its remarkable advantage: (1) is simple to operate, and cost is low, and equipment requirement is easy; (2) make raw material with the nickel salt predecessor, be simple and easy to, pollution-free, DMF (DMF) has good heat and chemical stability, can simultaneously as reducing agent and the solvent of nickel salt presoma, simplify preparation process; (3) with solvent boiling point as reaction temperature, guaranteed the reducing condition of preparation stable system, improved magnetic nickel nano particle growth controllability, be conducive to control its pattern and particle diameter; (4) polyvinylpyrrolidone used in the present invention (PVP) has played certain protective effect in magnetic nickel nano particle forming process, make it be difficult for also having played oxidized the time effect of dispersing nanometer particle.
Below in conjunction with accompanying drawing, the present invention is described in further detail.
Description of drawings
Fig. 1 is SEM (SEM) schematic diagram of magnetic nickel nano material
Fig. 2 is the X-ray powder diffraction schematic diagram of magnetic nickel nano material
Fig. 3 is the room temperature hysteresis curve schematic diagram of magnetic nickel nano material
The specific embodiment
The preparation method of a kind of magnetic Nano nickel material of the present invention, concrete steps are as follows:
1. under room temperature, the nickel salt presoma is dissolved in organic reducing agent, after mechanical agitation to nickel salt presoma dissolves fully, polyvinylpyrrolidone (PVP) is added in solution after dissolving, after mixing, under refluxad be warming up to 153 ℃, reacted 32-40 hour, obtain celadon solution.Wherein, the mass ratio of nickel salt presoma and organic reducing agent is 3:97-3:95; Polyvinylpyrrolidone (PVP) is 0:3-2:3 with the mass ratio of nickel salt presoma; Described nickel salt presoma is nickel chloride, nickelous sulfate, and nickel acetate, its chemical formula is respectively NiCl
2, NiSO
4, Ni (CH
3COO)
2Described organic reducing agent is DMF (DMF).
2. to be cooled to room temperature, with ethanol and deionized water washed product, 50-60 ℃ is dried to constant weight in vacuum drying chamber, and products therefrom is the magnetic nickel nano material.
Embodiment 1
The first step: under room temperature, select the NiCl of 3g
26H
2O is dissolved in 102.65mLN as the nickel salt presoma, and in dinethylformamide (DMF), magnetic agitation obtains being blue-green solution, under refluxad is warming up to 153 ℃, reaction 32h.Obtain celadon solution.
Second step: to be cooled to room temperature, with ethanol and deionized water washed product several, 50 ℃ are dried to constant weight in vacuum drying chamber, and products therefrom is the magnetic nickel nano material.
Embodiment 2
The first step: under room temperature, select the NiCl of 3g
26H
2O is dissolved in 100.53mLN as the nickel salt presoma, in dinethylformamide (DMF), magnetic agitation obtains being blue-green solution, in in churned mechanically situation, 2g polyvinylpyrrolidone (PVP) being added mentioned solution, after mixing, under refluxad be warming up to 153 ℃, reaction 36h.Obtain celadon solution.
Second step: to be cooled to room temperature, with ethanol and deionized water washed product several, 60 ℃ are dried to constant weight in vacuum drying chamber, and products therefrom is the magnetic nickel nano material.
Embodiment 3
The first step: under room temperature, select the NiCl of 3g
26H
2O is dissolved in 101.59mLN as the nickel salt presoma, in dinethylformamide (DMF), magnetic agitation obtains being blue-green solution, in in churned mechanically situation, 1g polyvinylpyrrolidone (PVP) being added mentioned solution, after mixing, under refluxad be warming up to 153 ℃, reaction 40h.Obtain celadon solution.
Second step: to be cooled to room temperature, with ethanol and deionized water washed product several, 55 ℃ are dried to constant weight in vacuum drying chamber, and products therefrom is the magnetic nickel nano material.
With German Brooker X-ray diffractometer, products therefrom of the present invention is carried out phase and identify, as shown in fig. 1, contrast JCPDS standard card (04-0850), all diffraction maximums fit like a glove with the magnetic nano-particle Ni of face-centered cubic phase.
Fig. 2 represents the pattern of the magnetic nickel nano material that the present invention is prepared, and shown in figure, the magnetic nickel nano material particle size distribution homogeneous of gained, particle diameter are the 100nm left and right.
Fig. 3 is the hysteresis curve figure of gained magnetic nickel nano material of the present invention, as seen from the figure: the coercivity (H of magnetic nickel nano material
c) be 125.74Oe, specific saturation magnetization is 22.16emu/g.This material has at room temperature formed complete hysteresis curve, thereby has good ferromagnetism.
Claims (5)
1. the preparation method of a magnetic Nano nickel material, is characterized in that, concrete steps are as follows:
Step 1 is dissolved in the nickel salt presoma in DMF, stirs, dissolving, then polyvinylpyrrolidone is joined in solution after dissolving, mixes, and refluxes and temperature reaction;
Step 2 treats that the solution that step 1 obtains is cooled to room temperature, washing, and vacuum drying obtains the magnetic nickel nano material.
2. the preparation method of magnetic Nano nickel material according to claim 1, is characterized in that, is warming up to 153 ℃ in step 1, and the reaction time is 32-40 hour.
3. the preparation method of magnetic Nano nickel material according to claim 1, is characterized in that, the mass ratio of described nickel salt presoma and DMF is 3:97-3:95; The mass ratio of polyvinylpyrrolidone PVP and nickel salt presoma is 0:3-2:3; Described nickel salt presoma is nickel chloride, nickelous sulfate or nickel acetate.
4. the preparation method of magnetic Nano nickel material according to claim 1, is characterized in that, the solution that obtains with ethanol and deionized water washing step one in step 2.
5. the preparation method of magnetic Nano nickel material according to claim 1, is characterized in that, in step 2, vacuum drying temperature is 50-60 ℃.
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Cited By (4)
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|---|---|---|---|---|
| CN104313728A (en) * | 2014-10-21 | 2015-01-28 | 南京大学（苏州）高新技术研究院 | Exchange bias nickel-base ferromagnetic/antiferromagnetic composite nano fiber and preparation method thereof |
| CN104668577A (en) * | 2015-02-05 | 2015-06-03 | 宁波大学 | Nickel micro nanoparticle and preparation method thereof |
| CN105312589A (en) * | 2014-07-23 | 2016-02-10 | 南京理工大学 | Synthesis method of superfine palladium powder |
| CN104313728B (en) * | 2014-10-21 | 2017-01-04 | 南京大学（苏州）高新技术研究院 | Exchange-biased nickel-based ferromagnetic/antiferromagnetic composite nanofiber and preparation method thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105312589A (en) * | 2014-07-23 | 2016-02-10 | 南京理工大学 | Synthesis method of superfine palladium powder |
| CN104313728A (en) * | 2014-10-21 | 2015-01-28 | 南京大学（苏州）高新技术研究院 | Exchange bias nickel-base ferromagnetic/antiferromagnetic composite nano fiber and preparation method thereof |
| CN104313728B (en) * | 2014-10-21 | 2017-01-04 | 南京大学（苏州）高新技术研究院 | Exchange-biased nickel-based ferromagnetic/antiferromagnetic composite nanofiber and preparation method thereof |
| CN104668577A (en) * | 2015-02-05 | 2015-06-03 | 宁波大学 | Nickel micro nanoparticle and preparation method thereof |
| CN104668577B (en) * | 2015-02-05 | 2019-01-15 | 宁波大学 | A kind of nickel micro-and nano-particles and preparation method thereof |
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Application publication date: 20130626 |