阅读说明：本技术 一种低磁滞损耗的磁性材料制备方法 (Preparation method of magnetic material with low hysteresis loss ) 是由 时乾中 朱平 于 2018-06-12 设计创作，主要内容包括：本发明公开了一种低磁滞损耗的磁性材料制备方法,包括如下步骤：(1)、准备；(2)、混料；(3)、一次熔炼；(4)、二次熔炼；(5)、三次熔炼；(6)、退火；(7)、粉碎；(8)、压制；(9)、烧结。本发明,设计合理,通过三次熔炼、三次退火和两次粉碎和两次压制,有效提高磁密度,所制得的磁体具有良好的磁性能,居里温度超过280℃,具有良好的温度稳定性和较高的磁感应强度,其功率损耗通现有技术相比低得多；本发明提供的磁性材料制备方法,工艺简单,生产成本低,操作安全,适合工业化生产。(The invention discloses a preparation method of a magnetic material with low hysteresis loss, which comprises the following steps: (1) preparing; (2) mixing materials; (3) and smelting for the first time; (4) and smelting for the second time; (5) and smelting for the third time; (6) annealing; (7) crushing; (8) pressing; (9) and sintering. The invention has reasonable design, effectively improves the magnetic density by three times of smelting, three times of annealing, two times of crushing and two times of pressing, and the prepared magnet has good magnetic performance, the Curie temperature is over 280 ℃, good temperature stability and higher magnetic induction intensity are realized, and the power loss is much lower compared with the prior art; the preparation method of the magnetic material provided by the invention has the advantages of simple process, low production cost and safe operation, and is suitable for industrial production.)

1. A preparation method of a magnetic material with low hysteresis loss is characterized by comprising the following steps:

(1) and (3) preparation: weighing the following raw materials in percentage by mass: 0.003-0.005% of graphene, 1.17-1.23% of silver, 3.38-3.46% of sodium chloride, 4.59-4.85% of chromium, and the balance of iron and inevitable impurities;

(2) mixing materials: weighing sodium chloride according to the mass percent, dissolving the sodium chloride in water to prepare a sodium chloride solution with the concentration of 0.5-0.8mol/L, then placing the iron, chromium and sodium chloride solution into a reaction kettle according to the mass percent, sealing, heating to 380-400 ℃ within 30-40min, stirring at the temperature for 10-20min, vacuumizing the reaction kettle by a vacuum pump, and continuously heating at the temperature for 15-25 min; thus obtaining a treated mixture A;

(3) and primary smelting: putting the mixture A into a smelting furnace, heating to 1590-1595 ℃, and smelting for 30-35min to obtain a mixture B;

(4) and secondary smelting: adding silver into the mixture B, heating to 1610-;

(5) and smelting for the third time: adding graphene into the mixture C, continuously smelting for 33-35min at the temperature of 3850-3855 ℃, and slagging off to prepare a mixture D;

(6) and annealing: placing the mixture D in a resistance furnace for homogenizing annealing to obtain a mixture E;

(7) and crushing: placing the mixture B in a hydrogen crushing furnace for twice crushing, and carrying out air milling on the obtained product in an air flow mill to prepare powder with the particle size of 3.6-4.0 mu m;

(8) and pressing: placing the powder obtained in the step (7) in a magnetic field, orienting the powder under 770-800 MPa, and pressing a blank;

(9) and sintering: preheating the blank at 820-880 ℃ for 90-120 min, placing the blank in a mold with heat, pressurizing at 250-285 MPa to improve the density of the magnet, then preserving the heat at 1150-1250 ℃ for 190-230 min, tempering, introducing steam for air cooling, and cooling to room temperature.

2. The method for preparing the magnetic material with low hysteresis loss according to claim 1, wherein in the steps (3), (4) and (5), inert gas is introduced during the mixing process, the inert gas is continuously introduced for 2-3 min after the addition is finished, and then the steps of vacuumizing and smelting are carried out.

3. The method as claimed in claim 2, wherein the inert gas is argon.

4. The method as claimed in claim 2, wherein the degree of vacuum of the vacuum is 3 x 10^-2～5×10^-2Pa。

5. The method for preparing a magnetic material with low hysteresis loss according to claim 1, wherein the tempering process in the step (9) is as follows: and cooling the heated blank to 850-900 ℃, preserving the heat for 190-230 min, slowly cooling to 550-600 ℃, and preserving the heat for 250-280 min.

6. The method for preparing a magnetic material with low hysteresis loss according to claim 1, wherein the annealing process in the step (6) is as follows: the first-stage annealing temperature is 655-658 ℃, and the temperature is kept for 2.5-3h at the temperature; the second-stage annealing temperature is 445-448 ℃, and the temperature is kept for 4.5-5 h; the third-stage annealing temperature is 512-515 ℃, and the temperature is kept for 6-6.5h at the temperature.

Technical Field

The invention relates to the field of magnetic materials, in particular to a preparation method of a magnetic material with low hysteresis loss.

Background

The magnetic material has wide application, is mainly applied to matched products such as induction cookers, air conditioners, computer communication, electronic transformers and the like, and can also be applied to the fields of automotive electronics, power motors and the like. The preparation method of the magnetic material can be divided into a solid phase method, a gas phase method and a liquid phase method. The solid phase method is simple in process, but the reaction is carried out at a temperature higher than 600 ℃ and the magnetic material obtained is easily agglomerated and is not easily dispersed. The vapor phase method is a chemical vapor deposition method, the method needs to carry out reaction at the temperature higher than 200 ℃, the reaction condition is harsh, the processing window is small, and the mass production is not easy. The liquid phase method requires sintering the initial product at a temperature higher than 400 ℃ at a high temperature to obtain a magnetic material with high purity.

The energy crisis is a practical problem faced by all countries in the world, and energy conservation is an important way to solve energy shortage, so that the great advocation and development of energy-saving products not only have important practical significance, but also have profound social significance. The magnetic product is a typical energy-saving and material-saving product and plays an irreplaceable role in energy conservation of the traditional industry. However, in the prior art, the magnetic material has the defects of low magnetoelectric conversion efficiency, high manufacturing cost and high energy consumption in various applied electrical equipment due to poor temperature stability and low magnetic induction intensity in the application process.

Disclosure of Invention

The present invention is directed to a method for preparing a magnetic material with low hysteresis loss, so as to solve the problems mentioned in the background art.

In order to achieve the purpose, the invention provides the following technical scheme:

a preparation method of a magnetic material with low hysteresis loss comprises the following steps:

(1) and (3) preparation: weighing the following raw materials in percentage by mass: 0.003-0.005% of graphene, 1.17-1.23% of silver, 3.38-3.46% of sodium chloride, 4.59-4.85% of chromium, and the balance of iron and inevitable impurities;

(2) mixing materials: weighing sodium chloride according to the mass percent, dissolving the sodium chloride in water to prepare a sodium chloride solution with the concentration of 0.5-0.8mol/L, then placing the iron, chromium and sodium chloride solution into a reaction kettle according to the mass percent, sealing, heating to 380-400 ℃ within 30-40min, stirring at the temperature for 10-20min, vacuumizing the reaction kettle by a vacuum pump, and continuously heating at the temperature for 15-25 min; thus obtaining a treated mixture A;

(3) and primary smelting: putting the mixture A into a smelting furnace, heating to 1590-1595 ℃, and smelting for 30-35min to obtain a mixture B;

(4) and secondary smelting: adding silver into the mixture B, heating to 1610-;

(5) and smelting for the third time: adding graphene into the mixture C, continuously smelting for 33-35min at the temperature of 3850-3855 ℃, and slagging off to prepare a mixture D;

(6) and annealing: placing the mixture D in a resistance furnace for homogenizing annealing to obtain a mixture E;

(7) and crushing: placing the mixture B in a hydrogen crushing furnace for twice crushing, and carrying out air milling on the obtained product in an air flow mill to prepare powder with the particle size of 3.6-4.0 mu m;

(8) and pressing: placing the powder obtained in the step (7) in a magnetic field, orienting the powder under 770-800 MPa, and pressing a blank;

(9) and sintering: preheating the blank at 820-880 ℃ for 90-120 min, placing the blank in a mold with heat, pressurizing at 250-285 MPa to improve the density of the magnet, then preserving the heat at 1150-1250 ℃ for 190-230 min, tempering, introducing steam for air cooling, and cooling to room temperature.

As a further scheme of the invention: and (3), in the steps (4) and (5), introducing inert gas in the mixing process, continuously introducing the inert gas for 2-3 min after the material is added, and then vacuumizing and smelting.

As a further scheme of the invention: the inert gas is argon.

As a further scheme of the invention: the vacuum degree of the vacuum pumping is 3 multiplied by 10^-2～5×10^-2Pa。

As a further scheme of the invention: the tempering process in the step (9) comprises the following steps: and cooling the heated blank to 850-900 ℃, preserving the heat for 190-230 min, slowly cooling to 550-600 ℃, and preserving the heat for 250-280 min.

As a further scheme of the utility model: the annealing process in the step (6) comprises the following steps: the first-stage annealing temperature is 655-658 ℃, and the temperature is kept for 2.5-3h at the temperature; the second-stage annealing temperature is 445-448 ℃, and the temperature is kept for 4.5-5 h; the third-stage annealing temperature is 512-515 ℃, and the temperature is kept for 6-6.5h at the temperature.

Compared with the prior art, the invention has the beneficial effects that:

the preparation method of the magnetic material with low hysteresis loss is reasonable in design, the magnetic density is effectively improved through three times of smelting, three times of annealing, two times of crushing and two times of pressing, the prepared magnet has good magnetic performance, the Curie temperature exceeds 280 ℃, the temperature stability is good, the magnetic induction intensity is high, and the power loss is much lower compared with that of the prior art; the preparation method of the magnetic material provided by the invention has the advantages of simple process, low production cost and safe operation, and is suitable for industrial production.

Detailed Description

The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.