CN102366832A - Preparation method of anisotropic samarium-cobalt/cobalt nano-composite magnet - Google Patents
Preparation method of anisotropic samarium-cobalt/cobalt nano-composite magnet Download PDFInfo
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- CN102366832A CN102366832A CN201110181126XA CN201110181126A CN102366832A CN 102366832 A CN102366832 A CN 102366832A CN 201110181126X A CN201110181126X A CN 201110181126XA CN 201110181126 A CN201110181126 A CN 201110181126A CN 102366832 A CN102366832 A CN 102366832A
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Abstract
The invention discloses a preparation method of an anisotropic samarium-cobalt/cobalt nano-composite magnet. The method mainly comprises the following steps of: performing ball milling on a samarium-cobalt hard magnetic alloy to prepare flaky particles of which the thicknesses are about 10-100 nanometers, putting the powder into an absolute ethyl alcohol solution, ultrasonically and electrically stirring, dissolving chloride hexahydrate and polyvinyl pyrrolidone into the ethyl alcohol solution, and ultrasonically stirring to obtain a mixed solution; and adding solid sodium hydrate and hydrazine hydrate into the mixed solution, reacting, cleaning the product with absolute ethyl alcohol till the pH is neutral, and performing vacuum drying. Raw materials used in the method are readily available, the preparation method is simple and convenient, a reaction product is pure metal cobalt, and the prepared samarium-cobalt/cobalt nano-composite magnet still has higher anisotropism.
Description
Technical fieldThe present invention relates to a kind of preparation method of magnetic material, particularly relate to the preparation method of a kind of anisotropy SmCo/cobalt Nanocomposite magnet.
Background technologyThe Nanocomposite magnet that the soft or hard magnetic nanometer is formed is the novel permanent magnetic material that promises to be permanent-magnet material of future generation most.The theoretical maximum magnetic energy product of this anisotropy compound nano crystal permanent magnetic material can surpass 100 MGOe, far above any single-phase permanent material, is 2 times of commercial neodymium iron boron magnetic body.The preparation method of tradition Nanocomposite magnet mainly comprises fast melt-quenching, mechanical alloying etc., but the magnetic energy product of this Nanocomposite magnet is usually less than 25 MGOe, far below theoretical value.Cause this result's reason to mainly contain two aspects, one: the control of forms such as nanocrystalline size, quantity and distribution; Two: the orientation of permanent magnetism phase increases.In order to solve this two problems, people have been developed heat energy, mechanical energy or heat energy and mechanical energy such Nanocomposite magnet preparation method from big to small that is coupled recently, and as the soft magnetism nano particle wrap up the technology of preparing from small to large of Hard Magnetic phase.For the former,, make permanent magnetism form orientation mutually and still have very big challenge though nanocrystalline form has obtained effective control.For a kind of method in back, though people have been developed some preparation methods from small to large, its used Hard Magnetic phase particle is relatively large, simultaneously, and for the controlled problems that also exist of the form of hard soft magnetism phase.Therefore, the preparation form is controlled and to have anisotropic nanocomposite permanent magnets be a difficult problem that needs to be resolved hurrily.
Summary of the inventionThe object of the present invention is to provide a kind of form controlled and have a preparation method of anisotropic anisotropy SmCo/cobalt Nanocomposite magnet.The present invention mainly adopts the method for liquid-phase reduction; Dispersion technology with ultrasonic agitation; SmCo [(Sm, Pr) Co5 down with] growth one deck is evenly tiny and pattern is controlled on the nano-sheet structural matrix cobalt soft magnetism phase, the prepared nano combined magnetic particle of this method has tangible anisotropy.
Technical scheme of the present invention is following:
1, with SmCo/cobalt magnetically hard alloy ball milling 2～8 h on ball mill, prepares the platy particle that thickness is about 10～100 nm, preferably use the acetone or alcohol ultrasonic cleaning again, get the deposition powder.Adopt above-mentioned ball grinding method to control the form of SmCo magnetically hard alloy well, make it become the less laminated structure of size.
2, get above-mentioned SmCo powder and place absolute ethyl alcohol, both have following relation, and promptly every gram SmCo powder is used the 1000ml absolute ethyl alcohol.Behind ultrasonic (50～60 KHz) and electronic stirring (100～500 rpm) 1～5 min; The SmCo powder is dispersed in the absolute ethyl alcohol; To be that SmCo powder weight 0.8-1.6 cobalt chloride hexahydrate doubly is dissolved in the above-mentioned ethanol with the PVP (polyvinylpyrrolidone) that is SmCo powder weight 15-25 times afterwards; Behind ultrasonic agitation 1～5 min, process mixed solution.Disperse the magnetic nanoparticle of very easily reuniting through the method for above-mentioned simple ultrasonic agitation, the one deck of can on SmCo magnetically hard alloy platy particle matrix, growing is tiny cobalt soft magnetism nano particle evenly.
3, will be that SmCo powder weight 15-25 NaOH (solid sodium hydroxide) and concentration doubly is that 80% hydrazine hydrate adds in the above-mentioned mixed solution; And every gram SmCo powder is used the 25-100ml hydrazine hydrate; Reaction temperature is 20～80 ℃, and the reaction time is 1～60 min; Then product is cleaned with absolute ethyl alcohol and makes PH to neutral, vacuum drying promptly obtain SmCo/cobalt [(Sm, Pr) Co5/Co down with] Nanocomposite magnet.
The present invention compared with prior art has following advantage: raw materials used being easy to get, and the easy and product of preparation method is the simple metal cobalt, the magnetic saturation of prepared SmCo/cobalt Nanocomposite magnet and coercivity be than higher, and still have higher anisotropy.This invention is significant to development high-performance nano built-up magnet.
Description of drawings
Fig. 1 is the field emission scanning electron microscope photo figure of the embodiment of the invention 1 SmCo/cobalt Nanocomposite magnet.
Fig. 2 is the field emission scanning electron microscope photo figure of SmCo behind the embodiment of the invention 2 ball millings 7 h.
Fig. 3 is the field emission scanning electron microscope photo figure of the embodiment of the invention 2 SmCos/cobalt Nanocomposite magnet.
Fig. 4 is the hysteresis curve figure of SmCo/cobalt Nanocomposite magnet powder behind the reaction different time.
Fig. 5 is along parallel (∥) the hysteresis curve figure with vertical (⊥) magnetic aligning direction survey SmCo/cobalt built-up magnet after the reaction different time magnetic aligning.
The specific embodiment
Embodiment 1:
With SmCo magnetically hard alloy ball milling 8 h on ball mill, prepare the platy particle that thickness is about 10 nm.Get above-mentioned SmCo powder 0.02g and place the 20ml absolute ethyl alcohol; At ultrasonic (59 KHz) and electronic stirring (200 rpm) 1min; The SmCo powder is dispersed in the absolute ethyl alcohol; After 0.016g cobalt chloride hexahydrate and 0.5g PVP are dissolved in the above-mentioned ethanol, ultrasonic agitation 1min processes mixed solution.0.5g NaOH and 0.5 ml hydrazine hydrate (80%) are added in the above-mentioned solution, and reaction temperature is that 20 ℃, reaction time are 60 min; Product is cleaned SmCo/cobalt Nanocomposite magnet that the superficial growth that makes extremely neutrality of PH, vacuum drying promptly obtain the SmCo laminated structure goes out a small amount of Co nano particle (see figure 1) with absolute ethyl alcohol.
Embodiment 2:
With SmCo magnetically hard alloy ball milling 7h on ball mill, prepare the platy particle that thickness is about 20nm, surperficial smoother (see figure 2).Use acetone ultrasonic (50 KHz) to clean then.SmCo powder 0.03 g that gets deposition places 30 ml absolute ethyl alcohols; At ultrasonic (50 KHz) and electronic stirring (200 rpm) 1.5min; The SmCo powder is dispersed in the absolute ethyl alcohol; After 0.03g cobalt chloride hexahydrate and 0.6g PVP are dissolved in the above-mentioned ethanol, ultrasonic agitation 1.5min processes mixed solution.0.7g NaOH and 0.8ml hydrazine hydrate (80%) are added in the above-mentioned solution, and reaction temperature is that 30 ℃, reaction time are 50min; Product is cleaned SmCo/cobalt Nanocomposite magnet that the superficial growth that makes extremely neutrality of PH, vacuum drying promptly obtain the SmCo laminated structure goes out the densely covered Co nano particle (see figure 3) of one deck with absolute ethyl alcohol.In the hysteresis curve figure of SmCo shown in Figure 4/cobalt Nanocomposite magnet powder behind the reaction different time, can find out that its magnetic saturation intensity is increased to about 79emu/g by about 61emu/g.After the orientation, its coercivity has 10.4KOe to be reduced to 8.9Koe slightly, and both direction still difference is bigger, explain still to have than the high anisotropy (see figure 5).
Embodiment 3:
With SmCo magnetically hard alloy ball milling 6h on ball mill, prepare the platy particle that thickness is about 35nm, use ethanol ultrasonic (60 KHz) to clean then.The SmCo powder 0.04g that gets deposition places the 40ml absolute ethyl alcohol; At ultrasonic (60KHz) and electronic stirring (500 rpm) 1min; The SmCo powder is dispersed in the absolute ethyl alcohol; After 0.065 g cobalt chloride hexahydrate and 0.7g PVP are dissolved in the above-mentioned ethanol, ultrasonic agitation 2min processes mixed solution.0.8g NaOH and 1ml hydrazine hydrate (80%) are added in the above-mentioned solution, and reaction temperature is that 40 ℃, reaction time are 40 min; Make PH to neutral with the absolute ethyl alcohol cleaning product, vacuum drying promptly obtains SmCo/cobalt Nanocomposite magnet.
Embodiment 4:
With SmCo magnetically hard alloy ball milling 5h on ball mill, prepare the platy particle that thickness is about 45nm, use acetone ultrasonic (55 KHz) to clean then.The SmCo powder 0.05g that gets deposition places the 50ml absolute ethyl alcohol; At ultrasonic (55 KHz) and electronic stirring (100 rpm) 5min; The SmCo powder is dispersed in the absolute ethyl alcohol; After 0.08 g cobalt chloride hexahydrate and 0.8 g PVP are dissolved in the above-mentioned ethanol, ultrasonic agitation 3min processes mixed solution.1g NaOH and 3ml hydrazine hydrate (80%) are added in the above-mentioned solution, and reaction temperature is that 50 ℃, reaction time are 30 min; Make PH to neutral with the absolute ethyl alcohol cleaning product, vacuum drying promptly obtains SmCo/cobalt Nanocomposite magnet.
Embodiment 5:
With SmCo magnetically hard alloy ball milling 4h on ball mill, prepare the platy particle that thickness is about 60nm, use acetone ultrasonic (58 KHz) to clean then.The SmCo powder 0.07g that gets deposition places the 70ml absolute ethyl alcohol; At ultrasonic (58 KHz) and electronic stirring (300 rpm) 3min; The SmCo powder is dispersed in the absolute ethyl alcohol; After 0.96g cobalt chloride hexahydrate and 1.2 g PVP are dissolved in the above-mentioned ethanol, ultrasonic agitation 2.5min processes mixed solution.1.2g NaOH and 5ml hydrazine hydrate (80%) are added in the above-mentioned solution, and reaction temperature is that 60 ℃, reaction time are 20 min; Make PH to neutral with the absolute ethyl alcohol cleaning product, vacuum drying promptly obtains SmCo/cobalt Nanocomposite magnet.
Embodiment 6:
With SmCo magnetically hard alloy ball milling 3h on ball mill, prepare the platy particle that thickness is about 70nm, use ethanol ultrasonic (53 KHz) to clean then.The SmCo powder 0.08g that gets deposition places the 80ml absolute ethyl alcohol; At ultrasonic (53 KHz) and electronic stirring (400 rpm) 3.5min; The SmCo powder is dispersed in the absolute ethyl alcohol; After 0.13 g cobalt chloride hexahydrate and 1.3 g PVP are dissolved in the above-mentioned ethanol, ultrasonic agitation 3min processes mixed solution.1.3g NaOH and 6 ml hydrazine hydrates (80%) are added in the above-mentioned solution, and reaction temperature is that 70 ℃, reaction time are 10 min; Make PH to neutral with the absolute ethyl alcohol cleaning product, vacuum drying promptly obtains SmCo/cobalt Nanocomposite magnet.
Embodiment 7:
With SmCo magnetically hard alloy ball milling 2.5h on ball mill, prepare the platy particle that thickness is about 85nm, use ethanol ultrasonic (56KHz) to clean then.The SmCo powder 0.09g that gets deposition places the 90ml absolute ethyl alcohol; At ultrasonic (56KHz) and electronic stirring (250 rpm) 2.5min; The SmCo powder is dispersed in the absolute ethyl alcohol; After 0.145 g cobalt chloride hexahydrate and 1.4 g PVP are dissolved in the above-mentioned ethanol, ultrasonic agitation 5min processes mixed solution.1.4 g NaOH and 8 ml hydrazine hydrates (80%) are added in the above-mentioned solution, and reaction temperature is that 75 ℃, reaction time are 5min; Make PH to neutral with the absolute ethyl alcohol cleaning product, vacuum drying promptly obtains SmCo/cobalt Nanocomposite magnet.
Embodiment 8:
With SmCo magnetically hard alloy ball milling 2h on ball mill, prepare the platy particle that thickness is about 100 nm, use acetone ultrasonic (57 KHz) to clean then.The SmCo powder 0.1g that gets deposition places the 100ml absolute ethyl alcohol; At ultrasonic (57KHz) and electronic stirring (200 rpm) 5min; The SmCo powder is dispersed in the absolute ethyl alcohol; After 0.16 g cobalt chloride hexahydrate and 1.5g PVP are dissolved in the above-mentioned ethanol, ultrasonic agitation 4min processes mixed solution.1.5g NaOH and 10ml hydrazine hydrate (80%) are added in the above-mentioned solution, and reaction temperature is that 80 ℃, reaction time are 1min; Make PH to neutral with the absolute ethyl alcohol cleaning product, vacuum drying promptly obtains SmCo/cobalt Nanocomposite magnet.
Claims (2)
1. the preparation method of anisotropy SmCo/cobalt Nanocomposite magnet is characterized in that:
(1) with SmCo/cobalt magnetically hard alloy ball milling 2～8 h on ball mill, prepare the platy particle that thickness is about 10～100 nm,
(2) get above-mentioned SmCo powder and place absolute ethyl alcohol; Both have following relation; Being that every gram SmCo powder is used the 1000ml absolute ethyl alcohol, behind ultrasonic and electronic stirring 1～5 min, will be that SmCo powder weight 0.8-1.6 cobalt chloride hexahydrate doubly is dissolved in the above-mentioned ethanol with the polyvinylpyrrolidone that is SmCo powder weight 15-25 times; Ultrasonic agitation 1～5 min processes mixed solution
(3) will be that SmCo powder weight 15-25 solid sodium hydroxide and concentration doubly is that 80% hydrazine hydrate adds in the above-mentioned mixed solution, and every gram SmCo powder uses the 25-100ml hydrazine hydrate, reaction temperature be 20～80 ℃, and the reaction time is 1～60 min; Then product being cleaned with absolute ethyl alcohol makes PH to neutrality, vacuum drying.
2. the preparation method of anisotropy SmCo according to claim 1/cobalt Nanocomposite magnet, it is characterized in that: the platy particle behind the ball milling is used the acetone or alcohol ultrasonic cleaning, gets the deposition powder.
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| CN108630365A (en) * | 2017-03-16 | 2018-10-09 | 中国科学院宁波材料技术与工程研究所 | A kind of nanometer of two-phase composite permanet magnet particle and preparation method thereof |
| CN109884122A (en) * | 2017-12-06 | 2019-06-14 | 天津大学 | Organic gas detection chip based on sulfuration rhenium nano-device |
| CN110586951A (en) * | 2018-06-13 | 2019-12-20 | 中国科学院宁波材料技术与工程研究所 | High-saturation-magnetism ultrafine-grain nano dual-phase permanent magnet material and preparation method thereof |
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| CN110586951B (en) * | 2018-06-13 | 2022-04-12 | 中国科学院宁波材料技术与工程研究所 | High-saturation-magnetism ultrafine-grain nano dual-phase permanent magnet material and preparation method thereof |
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