CN101979194B - 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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- CN101979194B CN101979194B CN201010532894.0A CN201010532894A CN101979194B CN 101979194 B CN101979194 B CN 101979194B CN 201010532894 A CN201010532894 A CN 201010532894A CN 101979194 B CN101979194 B CN 101979194B
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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 synthetic flower-shaped nickel magnetic powder of solvent heat under 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 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, be widely applied in fields such as work high density magnetic liquid, magnetic carrier, drug targeting, thermotherapy, rechargeable battery and catalyst.At present, in industry, prepare the method for 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, hydro-thermal solvent thermal process has numerous advantages, 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 is carried out in totally sealed environment, effectively reduce effusion and the release of toxic gas in preparation process, especially practical to the nano material of the virose compound of tool.
Performance, application and its pattern of nano magnetic material are closely related, and research finds that the nano magnetic material (as nano wire, nanometer sheet, nano flower) with special appearance shows the performance that is different from and is often better than ball shaped nano magnetic material.Therefore, pattern control is synthetic is the focus in nano magnetic material field always.The people such as L.J.Zhao, in " Materials Letters " the 64th phase in 2010, have reported in 215-218 page that they utilize solvent-thermal method to synthesize sub-micron magnetic nickel particle.The people such as Hu Yonghong are in " Chinese Journal of Inorganic Chemistry " the 2nd phase in 2006, the 22nd volume, in 293-297 page by taking silicon dioxide granule as template and golden nanometer particle prepared nickel hollow ball as the method for surperficial crystal seed.The people such as Li Qiang are in " Rare Metal Materials and Engineering " the 12nd phase in 2009, and in the 38th volume 2080-2084 page, report utilizes improved hydro-thermal method to synthesize thorn-like, nickel powder body chain and spherical.The people such as RezaEmamali Sabzi are " " Electrochimica Acta " the 55th phase in 2010 has reported with Woelm Alumina to be that template electrochemical method has been synthesized nickel nanosphere, nanometer rods, nanotube in 1829-1835 page.The people such as Liuyang Bai are in " Journal of Crystal Growth " the 331st phase in 2009, and in 2474-2479 page, they utilize polyalcohol to synthesize pattern for dodecahedron, the nickel powder body of the flower-like structure of spherical and nanometer sheet composition.Can see thus the above-mentioned process more complicated of preparing nickel powder body: or the long-time high-energy ball milling of needs; Or complicated operating process, the auxiliary material consuming is various, is all unfavorable for suitability for industrialized production.
The present invention proposes a kind of simple solvent-thermal method and prepares flower-shaped nano nickel magnetic powder as source taking deionized water and ethylene glycol as solvent nickel chloride.
Summary of the invention
The object of the invention is to provide a kind of simple solvent-thermal method to prepare the method for high-purity, even monodispersed flower-shaped nickel magnetic powder.The degree of crystallinity of the flower-shaped nickel magnetic powder that this method is prepared is high, and pattern is even, and coercivity is high can be widely used in the relevant industries such as magnetic liquid, thermotherapy, rechargeable battery and catalyst.
The method is by following simple process process implementation:
First, nickel chloride is distributed in ethylene glycol solution, after be 0.05～0.3 to be distributed to and in deionized water, to obtain sodium hydroxide solution NaOH by quality, again two kinds of solution are poured in polytetrafluoroethylene (PTFE), the ratio of deionized water and ethylene glycol is 3: 4, loading is 4/5, and lining cover on duty is placed in 180 DEG C of insulations of temperature 24 hours.Finally, naturally cool to room temperature, collect after mother liquor washing and precipitating thing repeatedly, with permanent magnet separate, collect, and the dry black nickel magnetic powder that obtains.
Brief description of the drawings
Fig. 1 is the XRD collection of illustrative plates 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
Detailed description of the invention
Embodiment 1
1.19g nickel chloride is distributed in ethylene glycol solution, after be 0.3 to be distributed to and in deionized water, to obtain sodium hydroxide solution NaOH by quality, again two kinds of solution are poured in polytetrafluoroethylene (PTFE), the ratio of deionized water and ethylene glycol is 3: 4, loading is 4/5, lining cover on duty, is placed in 180 DEG C of insulations of temperature 24 hours.Finally, naturally cool to room temperature, collect after mother liquor washing and precipitating thing repeatedly, with permanent magnet separate, collect, and the dry black powder that obtains.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 of 10 μ m left and right as we can see from the figure, and each flower is made up of a lot of small pieces.
1.19g nickel chloride is distributed in ethylene glycol solution, after be 0.2 to be distributed to and in deionized water, to obtain sodium hydroxide solution NaOH by quality, again two kinds of solution are poured in polytetrafluoroethylene (PTFE), the ratio of deionized water and ethylene glycol is 3: 4, loading is 4/5, lining cover on duty, is placed in 180 DEG C of insulations of temperature 24 hours.Finally, naturally cool to room temperature, collect after mother liquor washing and precipitating thing repeatedly, with permanent magnet separate, collect, and the dry black powder that obtains.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
1.19g nickel chloride is distributed in ethylene glycol solution, after be 0.15 to be distributed to and in deionized water, to obtain sodium hydroxide solution NaOH by quality, again two kinds of solution are poured in polytetrafluoroethylene (PTFE), the ratio of deionized water and ethylene glycol is 3: 4, loading is 4/5, lining cover on duty, is placed in 180 DEG C of insulations of temperature 24 hours.Finally, naturally cool to room temperature, collect after mother liquor washing and precipitating thing repeatedly, with permanent magnet separate, collect, and the dry black powder that obtains.ESEM (SEM) analysis result shows that product is that diameter is the monodispersed inhomogeneous sheet-like morphology of 5-6 μ m, as Fig. 5.
Embodiment 4
1.19g nickel chloride is distributed in ethylene glycol solution, after be 0.1 to be distributed to and in deionized water, to obtain sodium hydroxide solution NaOH by quality, again two kinds of solution are poured in polytetrafluoroethylene (PTFE), the ratio of deionized water and ethylene glycol is 3: 4, loading is 4/5, lining cover on duty, is placed in 180 DEG C of insulations of temperature 24 hours.Finally, naturally cool to room temperature, collect after mother liquor washing and precipitating thing repeatedly, with permanent magnet separate, collect, and the dry black powder that obtains.ESEM (SEM) analysis result shows that product is monodispersed small pieces and short grained mixing, as Fig. 6.
Embodiment 5
1.19g nickel chloride is distributed in ethylene glycol solution, after be 0.1 to be distributed to and in deionized water, to obtain sodium hydroxide solution NaOH by quality, again two kinds of solution are poured in polytetrafluoroethylene (PTFE), the ratio of deionized water and ethylene glycol is 3: 4, loading is 4/5, lining cover on duty, is placed in 180 DEG C of insulations of temperature 24 hours.Finally, naturally cool to room temperature, collect after mother liquor washing and precipitating thing repeatedly, with permanent magnet separate, collect, and the dry black powder that obtains.ESEM (SEM) analysis result shows that product is irregular granule, as Fig. 7.
Claims (1)
1. a deionized water and ethylene glycol are that solvent nickel chloride is the method that flower-shaped nickel magnetic powder is prepared in source, the method is by following simple process process implementation: first, nickel chloride is distributed in ethylene glycol solution, after be 0.05～0.3 to be distributed to and in deionized water, to obtain sodium hydroxide solution NaOH by quality, pour two kinds of solution into polytetrafluoroethyllining lining again, the ratio of deionized water and ethylene glycol is 3:4, loading is 4/5, steel bushing on neck bush, be placed in 180 DEG C of insulations of temperature 24 hours, finally, naturally cool to room temperature, collect after mother liquor washing and precipitating thing repeatedly, separate with permanent magnet, collect, and the dry black nickel magnetic powder that obtains.
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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 |
| CN105834453B (en) * | 2016-06-03 | 2018-02-16 | 大连理工大学 | A kind of preparation method of flower-shaped cobalt granule |
| CN106424752B (en) * | 2016-09-29 | 2018-10-16 | 清华大学深圳研究生院 | Silver powder with flower shape microstructure and preparation method thereof, electrically conductive ink |
Citations (4)
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| CN101284682A (en) * | 2008-05-21 | 2008-10-15 | 中国科学院上海硅酸盐研究所 | Preparation method for nano multilayer nickelous hydroxide hollow tube |
| 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 |
| CN101555375A (en) * | 2009-05-14 | 2009-10-14 | 上海第二工业大学 | Preparation method for solar selective heat-absorbing paint adopting nano nickel powder as absorber |
| CN101705037A (en) * | 2009-11-19 | 2010-05-12 | 上海第二工业大学 | Method for preparing solar selective heat-absorbing paint |
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| KR20050038142A (en) * | 2003-10-21 | 2005-04-27 | 이태진 | The preparation of metallic tungsten and flower-like structure tungsten materials using co/co2 mixture |
| CN101693616A (en) * | 2009-10-29 | 2010-04-14 | 北京理工大学 | Method for preparing magnetic spinel ferrite hollow ball in one-step method |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101284682A (en) * | 2008-05-21 | 2008-10-15 | 中国科学院上海硅酸盐研究所 | Preparation method for nano multilayer nickelous hydroxide hollow tube |
| 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 |
| CN101555375A (en) * | 2009-05-14 | 2009-10-14 | 上海第二工业大学 | Preparation method for solar selective heat-absorbing paint adopting nano nickel powder as absorber |
| CN101705037A (en) * | 2009-11-19 | 2010-05-12 | 上海第二工业大学 | Method for preparing solar selective heat-absorbing paint |
Non-Patent Citations (3)
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| 吴正翠 等.花状β-氢氧化镍的合成和表征.《无机化学学报》.2006,第22卷(第8期), |
| 崔华莉 等.离子液体辅助合成花状氢氧化镍.《延安大学学报（自然科学版）》.2009,第28卷(第2期), * |
| 花状β-氢氧化镍的合成和表征;吴正翠 等;《无机化学学报》;20060831;第22卷(第8期);1371-1374 * |
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