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High-saturation-magnetic ultra-fine grain nano two-phase permanent magnet material and preparation method thereof

A technology of permanent magnetic materials and ultra-fine crystals, which is applied in the direction of magnetic materials, inorganic materials, magnetic objects, etc., can solve the problem of limiting the exchange coupling effect and magnetic energy product of nano-two-phase materials, difficulty in reaching ultra-fine nanoscale, complicated procedures, etc. problem, to achieve the effect of avoiding the growth and coarsening of soft magnetic particles, avoiding high temperature treatment process, and simple preparation process

Active Publication Date: 2019-12-20
NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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  • Application Information

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Problems solved by technology

At present, liquid phase synthesis of high-temperature annealing method is the most widely used method for preparing high-saturation ultra-fine-grained nano-double-phase permanent magnet particles. In addition, there are mechanical alloying high-temperature annealing methods, high-temperature and high-pressure pressing methods, and plasma sintering methods. However, the above-mentioned methods all include high-temperature Processing technology, complex process and high cost
In recent years, the chemical liquid phase encapsulation method developed in a homogeneous solution can assemble soft magnetic particles on hard magnetic particles at room temperature to below 80°C to prepare dual-phase nanocomposites, avoiding the traditional high temperature technology, but when the soft magnetic particles When the magnetic content increases from 3% to 10% and exceeds 10%, the deposited soft magnetic particles are easy to grow to 19-80nm, and it is difficult to reach the ultra-fine nanoscale below 10nm (see F.Q.Wang, X.J.Hu, G.W.Huang, F.C.Hou, X.Y.Zhang.Journal of Alloys and Compounds,2015,626:212-216; N.Poudyal,K.Elkins,K.Gandha,J.P.Liu,IEEE Transactions on magnetics 51(2015)2104704), thus limiting the low-temperature preparation of nano Further improvement of exchange coupling effect and magnetic energy product of dual-phase materials

Method used

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  • High-saturation-magnetic ultra-fine grain nano two-phase permanent magnet material and preparation method thereof

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preparation example Construction

[0029] Another aspect of the embodiments of the present invention provides a method for preparing a high-saturated ultrafine-grained nano-dual-phase permanent magnet material, comprising:

[0030] The hard magnetic particles are surface activated with an acidic substance to obtain activated hard magnetic particles;

[0031] In a protective atmosphere, at a temperature of 20-70 °C, the activated hard magnetic particles are uniformly dispersed in the mixture of oil phase solvent and co-surfactant to form a dispersion of activated hard magnetic particles, and then slowly Add soft magnetic precursor material, and add alkaline agent and reducing agent at the same time, mix and react to form a water-in-oil microemulsion with ultra-fine bubbles, so that soft magnetic particles self-assemble on the surface of activated hard magnetic particles to obtain high saturation magnetic ultrafine Crystal nano duplex permanent magnet material.

[0032] As one of the preferred solutions, the pre...

Embodiment 1

[0069] (1) Under the protection of high-purity Ar gas, 0.12g of SmCo with a saturation magnetization of 90emu / g 5 The magnetic powder and 60 ml of anhydrous ethanol were put into a four-necked flask, and the hard magnetic powder was uniformly dispersed by ultrasonic and mechanical stirring in a 60°C water bath, and then 0.5 ml of dilute hydrochloric acid was added to activate the hard magnetic powder. After activating for 10 minutes, the acid solution was removed to obtain Activated hard magnetic particles.

[0070] (2) Under the protection of high-purity Ar gas, select oleic acid as the oil phase solvent and absolute ethanol as the co-surfactant, and use ultrasonic and mechanical stirring to remove the activated SmCo 5 The hard magnetic powder is uniformly dispersed in the mixed solution of oil phase solvent and co-surfactant with a ratio of 1:60. FeCl 2 ·4H 2 O and CoCl 2 ·6H 2 O soft magnetic raw material, NaOH alkaline agent, and hydrazine hydrate reducing agent with a...

Embodiment 2

[0074] In the present embodiment, the raw materials are exactly the same as the raw materials in Example 1, as follows:

[0075] (1) identical with the step (1) of embodiment 1;

[0076] (2) It is basically the same as step (2) in Example 1, except that when the soft magnetic phase is assembled by the mixed reaction, the ratio of the oil phase solvent to the cosurfactant is 1:30.

[0077] This example obtains SmCo 5 / Fe-Co nano-dual-phase composite permanent magnetic particles, the size and magnetic properties of the soft magnetic particles are shown in Table 1.

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Abstract

The invention discloses a high-saturation-magnetic ultra-fine grain nano two-phase permanent magnet material and a preparation method thereof. The preparation method comprises the following steps of performing surface activating treatment on hard magnetic particles with an acidic material to obtain activated hard magnetic particles; and then promoting high-content soft magnetic particles to be nucleated on the surfaces of the activated hard magnetic particles by adopting a reducing technology of a microemulsion with ultra-fine fine bubbles and inhibiting the growth of the high-content soft magnetic particles to achieve the self-assembly of the high-content ultra-fine grain soft magnetic particles on the activated hard magnetic particles, thereby finally obtaining the high-saturation-magnetic ultra-fine grain nano two-phase permanent magnet material. The preparation method provided by the invention avoids high temperature operation, the preparation technology is simple, low in cost, andeasy to produce on a large scale, the phenomenon that in a conventional low-temperature liquid-phase preparation condition, higher soft magnetic content causes growing and coarsening of soft magneticparticles is avoided, the obtained nano two-phase permanent magnet material has the characteristics of higher soft magnetic content, ultra-fine soft magnetic size and more uniform soft magnetic distribution, and the strong-coupling, high-saturation-magnetic and high-energy-product nano two-phase permanent magnet material is beneficially prepared.

Description

technical field [0001] The invention relates to a preparation method of a magnetic material, in particular to a high-saturated magnetic ultrafine crystal nano-dual-phase composite permanent magnetic material and a preparation method thereof, belonging to the technical field of preparation of dual-phase composite materials. Background technique [0002] Nano-composite permanent magnetic materials rely on the unique magnetic coupling effect of nano-scale hard magnetic particles and soft magnetic particles, and have an ultra-high theoretical magnetic energy product. Refining high-content soft magnetic particles to ultra-fine sizes below 10 nm and uniformly distributing them around the hard magnetic phase is an important link to enhance the dual-phase coupling effect and obtain nano-dual-phase materials with high magnetic energy product. At present, the liquid-phase synthesis high-temperature annealing method is the most widely used to prepare ultra-fine-grained nano-dual-phase ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B22F9/24B22F1/02H01F1/03
CPCB22F9/24H01F1/0306B22F1/17
Inventor 杜娟王凤青姚璐璐郑强刘平
Owner NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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