CN101979194A - Method for synthesizing flower-shaped nickel magnetic powder through mixed solvent hot method - Google Patents
Method for synthesizing flower-shaped nickel magnetic powder through mixed solvent hot method Download PDFInfo
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- CN101979194A CN101979194A CN2010105328940A CN201010532894A CN101979194A CN 101979194 A CN101979194 A CN 101979194A CN 2010105328940 A CN2010105328940 A CN 2010105328940A CN 201010532894 A CN201010532894 A CN 201010532894A CN 101979194 A CN101979194 A CN 101979194A
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Abstract
The invention provides a method for preparing power-shaped nickel magnetic powder by using deionized water and glycol as solvents and nickel chloride as a raw material. The method is implemented by the following simple process steps: firstly, dispersing the nickel chloride into glycol solvent; secondly, dispersing 0.05 to 0.3 percent of sodium hydroxide into the deionized water in percentage by mass to obtain sodium hydroxide solution; thirdly, pouring the two types of solution into polytetrafluoroethylene, wherein the ratio of the deionized water to the glycol is 3:4, the loading level is 4/5, a lining is sleeved and the mixture is placed in an environment at 180 DEG C for 24 hours; and finally, naturally cooling the mixture to the room temperature, collecting mother liquor, then repeatedly washing deposits, and separating, collecting and drying the deposits to obtain black nickel magnetic powder. The invention has the following characteristics: the method is simple and has a high yield, and the product has the advantages of uniform particles, high dispersibility, high crystallinity and the like and can be widely applied to related industries of magnetic liquid, coatings, medicament targeting, heat treatment, rechargeable battery, catalysts and the like; and the method has low raw material price and simple process, and is easy for large-scale industrial production.
Description
Technical field
The present invention be a kind of be the method for the flower-shaped nickel magnetic powder of solvent thermal synthesis under the mixed solvent system about deionized water, ethylene glycol.
Background technology
Nickel is that silvery white metal has ferromagnetism and ductility, can conduct electricity, can heat conduction.Under the normal temperature, nickel surface in humid air forms fine and close oxide-film, not only can stop continuation oxidized, and energy is alkaline-resisting, the corrosion of salting liquid, and it can also high polish and anticorrosive.Therefore, obtained extensive use in fields such as worker's high density magnetic liquid, magnetic carrier, drug targeting, thermotherapy, rechargeable battery and catalyst.At present, prepare in the industry method of nickel a lot of as: gas-phase reaction method, solid reaction process--high-energy ball milling, pyrolytic, liquid phase reactor method a. coprecipitation (industrial synthetic method) b. sol-gal process c. hydro-thermal method d. solvent-thermal method.In said method, the hydro-thermal solvent thermal process has numerous advantages, and is very fast in development in recent years, and it is simple to operate, temperature is low, and environmental pollution is less, and product dispersiveness, homogeneity are good.Because preparation process carries out in totally sealed environment, effectively reduced the effusion and the release of toxic gas in the preparation process, especially practical to the nano material of compound with toxicity.
The performance of nano magnetic material, application and its pattern are closely related, discover that the nano magnetic material (as nano wire, nanometer sheet, nanometer flower) with special appearance shows the performance that is different from and often is better than the ball shaped nano magnetic material.Therefore, pattern control is synthetic is the focus in nano magnetic material field always.People such as L.J.Zhao have reported in the 215-218 page or leaf that in " Materials Letters " the 64th phase in 2010 they utilize solvent heat to send out and have synthesized sub-micron magnetic nickel particle.People such as Hu Yonghong are in " Chinese Journal ofInorganic Chemistry " the 2nd phase in 2006, the 22nd volume, in the 293-297 page or leaf by being that the method for surperficial crystal seed has prepared the nickel hollow ball as template and golden nanometer particle with silicon dioxide granule.People such as Li Qiang are in " Rare Metal Materials and Engineering " the 12nd phase in 2009, and report utilizes improved hydro-thermal method to synthesize thorn-like, nickel powder body chain and spherical in the 38th volume 2080-2084 page or leaf.People such as RezaEmamali Sabzi reported in the 1829-1835 page or leaf with Woelm Alumina and have synthesized the nickel nanosphere for the template electrochemical method, nanometer rods, nanotube in " Electrochimica Acta " the 55th phase in 2010.People such as Liuyang Bai are in " Journal of Crystal Growth " the 331st phase in 2009, and they utilize polyalcohol to synthesize pattern to be dodecahedron in the 2474-2479 page or leaf, the nickel powder body of the spherical and flower-like structure that nanometer sheet is formed.Can see the process more complicated of above-mentioned preparation nickel powder body thus: or need long-time high-energy ball milling; Or the complicated operations process, the auxiliary material that is consumed is various, all is unfavorable for suitability for industrialized production.
It is that the solvent nickel chloride is the flower-shaped nanometer nickel magnetic powder of former preparation with deionized water and ethylene glycol that the present invention proposes a kind of simple solvent-thermal method.
Summary of the invention
The object of the invention is to provide a kind of simple solvent heat to send out the method for preparing high-purity, even monodispersed flower-shaped nickel magnetic powder.The degree of crystallinity height of the flower-shaped nickel magnetic powder that this method is prepared, pattern is even, and the coercivity height can be widely used in relevant industries such as magnetic liquid, thermotherapy, rechargeable battery and catalyst.
This method realizes by following simple process process:
At first, nickel chloride is distributed in the ethylene glycol solution, after be 0.05～0.3 to be distributed to and to obtain sodium hydroxide solution in the deionized water NaOH by quality, again two kinds of solution are poured in the polytetrafluoroethylene (PTFE), the ratio of deionized water and ethylene glycol is 3: 4, loading is 4/5, and lining cover on duty places 180 ℃ of insulations of temperature 24 hours.At last, naturally cool to room temperature, collect behind the mother liquor washing and precipitating thing repeatedly, separate, collect and drying obtains the black nickel magnetic powder with permanent magnet.
Description of drawings
Fig. 1 is the XRD figure spectrum of embodiment 1 product
Fig. 2 is the ESEM picture of embodiment 1 product
Fig. 3 is the ESEM picture of embodiment 1 product
Fig. 4 is the ESEM picture of embodiment 2 products
Fig. 5 is the ESEM picture of embodiment 3 products
Fig. 6 is the ESEM picture of embodiment 4 products
Fig. 7 is the ESEM picture of embodiment 5 products
The specific embodiment
Embodiment 1
The 1.19g nickel chloride is distributed in the ethylene glycol solution, after be 0.3 to be distributed to and to obtain sodium hydroxide solution in the deionized water NaOH by quality, again two kinds of solution are poured in the polytetrafluoroethylene (PTFE), the ratio of deionized water and ethylene glycol is 3: 4, loading is 4/5, lining cover on duty places 180 ℃ of insulations of temperature 24 hours.At last, naturally cool to room temperature, collect behind the mother liquor washing and precipitating thing repeatedly, separate, collect and drying obtains black powder with permanent magnet.The XRD analysis result shows that product is the nickel of face-centred cubic structure, as Fig. 1; ESEM (SEM) analysis result shows that product is monodispersed even floriform appearance, as Fig. 2.Fig. 3 is the SEM picture of high multiple, and product is that diameter is the flower-like structure about 10 μ m as we can see from the figure, and each flower is made up of a lot of small pieces.
The 1.19g nickel chloride is distributed in the ethylene glycol solution, after be 0.2 to be distributed to and to obtain sodium hydroxide solution in the deionized water NaOH by quality, again two kinds of solution are poured in the polytetrafluoroethylene (PTFE), the ratio of deionized water and ethylene glycol is 3: 4, loading is 4/5, lining cover on duty places 180 ℃ of insulations of temperature 24 hours.At last, naturally cool to room temperature, collect behind the mother liquor washing and precipitating thing repeatedly, separate, collect and drying obtains black powder with permanent magnet.ESEM (SEM) analysis result shows that product is that diameter is the monodispersed even floriform appearance of 5-6 μ m, as Fig. 4.
Embodiment 3
The 1.19g nickel chloride is distributed in the ethylene glycol solution, after be 0.15 to be distributed to and to obtain sodium hydroxide solution in the deionized water NaOH by quality, again two kinds of solution are poured in the polytetrafluoroethylene (PTFE), the ratio of deionized water and ethylene glycol is 3: 4, loading is 4/5, lining cover on duty places 180 ℃ of insulations of temperature 24 hours.At last, naturally cool to room temperature, collect behind the mother liquor washing and precipitating thing repeatedly, separate, collect and drying obtains black powder with permanent magnet.ESEM (SEM) analysis result shows that product is that diameter is the monodispersed inhomogeneous sheet pattern of 5-6 μ m, as Fig. 5.
Embodiment 4
The 1.19g nickel chloride is distributed in the ethylene glycol solution, after be 0.1 to be distributed to and to obtain sodium hydroxide solution in the deionized water NaOH by quality, again two kinds of solution are poured in the polytetrafluoroethylene (PTFE), the ratio of deionized water and ethylene glycol is 3: 4, loading is 4/5, lining cover on duty places 180 ℃ of insulations of temperature 24 hours.At last, naturally cool to room temperature, collect behind the mother liquor washing and precipitating thing repeatedly, separate, collect and drying obtains black powder with permanent magnet.ESEM (SEM) analysis result shows that product is monodispersed small pieces and short grained mixing, as Fig. 6.
Embodiment 5
The 1.19g nickel chloride is distributed in the ethylene glycol solution, after be 0.1 to be distributed to and to obtain sodium hydroxide solution in the deionized water NaOH by quality, again two kinds of solution are poured in the polytetrafluoroethylene (PTFE), the ratio of deionized water and ethylene glycol is 3: 4, loading is 4/5, lining cover on duty places 180 ℃ of insulations of temperature 24 hours.At last, naturally cool to room temperature, collect behind the mother liquor washing and precipitating thing repeatedly, separate, collect and drying obtains black powder with permanent magnet.ESEM (SEM) analysis result shows that product is irregular granule, as Fig. 7.
Claims (6)
1. deionized water and ethylene glycol are the method for the flower-shaped nickel magnetic powder of former preparation for the solvent nickel chloride.This method realizes by following simple process process: at first, nickel chloride is distributed in the ethylene glycol solution, after be 0.05～0.3 to be distributed to and to obtain sodium hydroxide solution in the deionized water NaOH by quality, again two kinds of solution are poured in the polytetrafluoroethylene (PTFE), the ratio of deionized water and ethylene glycol is 3: 4, loading is 4/5, and lining cover on duty places 180 ℃ of insulations of temperature 24 hours.At last, naturally cool to room temperature, collect behind the mother liquor washing and precipitating thing repeatedly, separate, collect and drying obtains the black nickel magnetic powder with permanent magnet.
2. the method for claim 1 is characterized in that, used nickel was nickel chloride originally.
3. the method for claim 1 is characterized in that, used NaOH is 0.05～0.3 to be distributed in the deionized water by quality.
4. the method for claim 1 is characterized in that, the used deionized water and the ratio of ethylene glycol are to pour in polytetrafluoroethyllining lining at 3: 4 to be incubated.
5. method as claimed in claim 4 is characterized in that, heating-up temperature is 180 ℃.
6. method as claimed in claim 4 is characterized in that, constant temperature time is 24 hours.
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Cited By (3)
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| CN102363219A (en) * | 2011-11-21 | 2012-02-29 | 新疆大学 | Method for synthesizing floriform cobalt magnetic powder by mixed solvent thermal method |
| CN105834453A (en) * | 2016-06-03 | 2016-08-10 | 大连理工大学 | Preparation method for flower-like cobalt particles |
| CN106424752A (en) * | 2016-09-29 | 2017-02-22 | 清华大学深圳研究生院 | Silver powder with flower-shaped microstructure and preparation method thereof and electric conducting ink |
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| CN102363219A (en) * | 2011-11-21 | 2012-02-29 | 新疆大学 | Method for synthesizing floriform cobalt magnetic powder by mixed solvent thermal method |
| CN105834453A (en) * | 2016-06-03 | 2016-08-10 | 大连理工大学 | Preparation method for flower-like cobalt particles |
| CN106424752A (en) * | 2016-09-29 | 2017-02-22 | 清华大学深圳研究生院 | Silver powder with flower-shaped microstructure and preparation method thereof and electric conducting ink |
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| CN101979194B (en) | 2014-06-25 |
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