阅读说明：本技术 一种软磁性材料试剂熔盐配置及使用方法 (Soft magnetic material reagent molten salt preparation and use method ) 是由 徐灿华 于 2019-11-11 设计创作，主要内容包括：本发明涉及软磁性材料试剂的制备及使用方法,公开了一种软磁性材料试剂熔盐配置及使用方法,其原料由：AgCl、CaCl<Sub>2</Sub>、NaCl、NaF、SiO<Sub>2</Sub>组成,其中AgCl、CaCl<Sub>2</Sub>、NaCl、NaF按照0.02～0.06：0.5：1：3的摩尔比称取,再加入占总试剂熔盐介质质量分数的8～12％的粉状SiO<Sub>2</Sub>单独烘干,研磨成粉状混合均匀即可。(The invention relates to a preparation and use method of a soft magnetic material reagent, and discloses a preparation and use method of a soft magnetic material reagent molten salt, which comprises the following raw materials: AgCl, CaCl 2 、NaCl、NaF、SiO 2 Composition of which AgCl and CaCl 2 NaCl and NaF are mixed according to the weight ratio of 0.02-0.06: 0.5: 1: 3, adding powdery SiO accounting for 8-12% of the mass fraction of the total reagent molten salt medium 2 Oven drying separately, grinding into powder, and mixing.)

1. A method for preparing and using soft magnetic material reagent molten salt is characterized in that the reagent molten salt is prepared from the following components in percentage by weight: AgCl, CaCl₂、NaCl、NaF、SiO₂Composition of which AgCl and CaCl₂NaCl and NaF are weighed according to the molar ratio of 0.02-0.06: 0.5: 1: 3, and SiO accounting for 8-12% of the mass fraction of the total reagent molten salt medium is added₂And (3) powder.

2. A soft magnetic material reagent molten salt preparation and use method according to claim 1, characterized in that each raw material of the reagent is dried for 8 hours at 200 ℃, respectively ground into powder, and then mixed uniformly.

3. A method for preparing and using a molten salt of a soft magnetic material reagent according to claim 1, wherein Si in the molten salt of the reagent is silicon steel with a cathode containing 4.5%, a thickness of 1.2-4.5mm and SiO₂The size of the powdery particles is 270-300 meshes.

4. A method of preparing and using soft magnetic material reagent molten salt according to claim 1, wherein the reagent molten salt is analytically pure.

5. A method for preparing and using a soft magnetic material reagent molten salt according to claim 1, characterized in that when the temperature of the alloy ribbon is reduced to 650-750 ℃, the temperature is kept for 20min, the alloy ribbon is immersed in the reagent molten salt, the reagent molten salt is connected with a direct current power supply, pulse power supply is adopted, and the average current density is controlled to be 60mA/cm₂The alloy belt moves at a constant speed in the molten salt, the advancing speed is 0.03-0.096/min, and the residence time of each point of the alloy belt in the molten salt is 30-35 min.

6. A soft magnetic material reagent molten salt configuration and use method according to one of claims 1 to 5, characterized In that the reagent immersed alloy strip has raw materials consisting of Pd, Ni, In, Ga, Ge, Be, Ce, Au, Fe with purity of more than 99.9%, B is added In the form of ferroboron, wherein the weight percentage of B is 24%.

The technical field is as follows:

the invention relates to the technical field of preparation processes for manufacturing magnetic materials, in particular to preparation and use methods of soft magnetic material reagent molten salt.

Background art:

the yield of the permanent magnet and soft magnet ferrites in China accounts for 68-72% of the global yield since 2011, the market supply of the magnetic product raw materials in China is sufficient, and the magnetic material is supported by a huge application market and is a genuine large country for producing and manufacturing the magnetic materials.

From the production aspect, the global production of magnetic materials is mainly focused on Japan and China at present, from the technical and productivity aspects, Japan is a magnetic material technology capturer, and the productivity of the magnetic materials in China is the top world, and about 68-75% of the world magnets are produced every year. But most of them are hard magnetic material products using rare earth ore.

In terms of product competition, the international market is leading in japan, the united states and a part of european countries. The countries start early in the production of magnetic materials, the development capability of new products is strong, the technical content is high, the competition of high-grade ferrite magnetic materials in the international market is mainly concentrated in the countries, and a large number of enterprises participate in the international market competition of high-grade magnetic materials in China. With the continuous development of new application markets, such as new markets in the development of automotive electronics, LEDTV, LED lighting, EMC, 4C (computer, communication, radio and television, content service) fusion, 4G and 5G communication, smart grid, Internet of things, new energy automobiles and the like, more new development opportunities are provided for the development of the Chinese magnetic material industry, and the utilization of a large amount of rare earth ores can be saved.

The invention content is as follows:

in view of the above problems, the present invention provides a soft magnetic material reagent molten salt preparation and use method, wherein the reagent molten salt is prepared from: AgCl, CaCl₂、NaCl、NaF、SiO₂Composition of which AgCl and CaCl₂NaCl and NaF are weighed according to the molar ratio of 0.02-0.06: 0.5: 1: 3, and SiO accounting for 8-12% of the mass fraction of the total reagent molten salt medium is added₂And (3) powder.

Furthermore, all raw materials of the reagent are dried for 8 hours at 200 ℃, ground into powder respectively and then mixed evenly.

Furthermore, the preparation and use method of the soft magnetic material reagent molten salt is characterized in that Si in the reagent molten salt is silicon steel with 4.5% of cathode content, thickness of 1.2-4.5mm and SiO content₂The size of the powdery particles is 270-300 meshes.

Furthermore, the preparation and use method of the soft magnetic material reagent molten salt is characterized in that the reagent molten salt is analytically pure.

Further, when the temperature of the alloy belt is reduced to 650-750 ℃, keeping the temperature for 20min, immersing the alloy belt into the reagent molten salt, switching on a direct-current power supply, adopting pulse power supply, controlling the average current density to be 60mA/cm2, enabling the master alloy belt to move at a constant speed in the molten salt, enabling the running speed to be 0.03-0.096/min, and ensuring that the residence time of each point of the master alloy belt in the molten salt is 30-35 min.

Furthermore, the raw materials of the alloy strip immersed In the reagent comprise Pd, Ni, In, Ga, Ge, Be, Ce, Au and Fe with the purity of more than 99.9%, and B is added In the form of ferroboron, wherein the weight percentage of B is 24%.

Description of the drawings:

FIG. 1 is a linear plot of the saturation magnetic flux density coercivity;

FIG. 2 is a graph showing the change in coercive force versus Cu concentration;

fig. 3 is a comparison of the metallographic structure of the ratios of the four components.

The specific implementation mode is as follows:

weighing raw materials of each component according to the molar ratio of AgCl, CaCl2, NaCl and NaF of 0.02-0.06: 0.5: 1: 3, drying reagents of the raw materials at 200 ℃ for 8h respectively, adding powdery SiO2 accounting for 8-12% of the mass fraction of the molten salt medium, separately grinding, and uniformly mixing for later use.

The cathode is Fe-based iron plate with the thickness of 1.2-4.5 mm; the powder particle size of the SiO2 is 270-300 meshes.

When the furnace temperature reaches 650-750 ℃, keeping the temperature for 20min, and beginning to immerse the alloy strip into the molten salt; meanwhile, a direct current power supply is switched on, pulse power supply is adopted, and the average current density is controlled to be 60mA/cm 2.

The alloy belt moves at a constant speed in the molten salt, and the advancing speed is 0.03-0.096/min; the residence time of each point of the alloy strip in the molten salt is kept between 30 and 35 minutes.

And after the alloy strip is extracted from the molten salt, the alloy strip is wound into a coil by a belt winding machine, and the material preparation is finished.

Further, the low-temperature treatment temperature is-100 ℃ to-130 ℃, and the heat preservation time is 15-0 min; then standing for 1-2 hours at room temperature; and then, preserving the heat for 2 to 4 hours at the temperature of between 200 and 250 ℃, and then cooling the mixture to room temperature along with the furnace.

The invention has the beneficial technical effects that:

in the invention, the Ge and the second transition system Pd can effectively inhibit the growth of crystal grains, are beneficial to obtaining a finer and uniform crystal grain structure and can improve the thermal stability of the magnet. In, Ga, Au and B act together to improve amorphous forming ability. Si, Be and Ce can prevent the crystal grains from growing up in the heat treatment, and the crystal grains are refined, so that the resistivity is improved, and the loss is reduced. The Ni of the first transition system inhibits the growth of grains at the grain intersection and refines the grains, thereby inhibiting the enhancement of stray fields around the grains and further improving the magnetic performance.

The alloy of the invention adopts a mode of combining rapid cooling, heat treatment and alloying in solidification, which not only effectively reduces the phase size in the alloy, ensures the uniform distribution of chemical components in the material, ensures the magnetic property of the alloy, but also greatly reduces the internal stress caused by rapid cooling through gradient treatment, and also ensures the mechanical property of the alloy.

The product obtained by the invention has excellent soft magnetic performance, heavy rare earth elements are not used in the preparation, the used rare earth elements are trace, and the cost of other raw materials is lower. The alloy is rapidly cooled in the preparation process, so that the uniformity of the components, the structure and the performance of the alloy is ensured, and the quality of the alloy is ensured. The alloy has simple preparation process and simple process, and the produced alloy has good performance and is very convenient for industrial production. The material prepared by the invention can be applied to magnetic devices in the fields of information, communication and the like.

Then placing the alloy strip in a liquid nitrogen atmosphere for low-temperature treatment at the temperature of-100 to-130 ℃, and preserving heat for 15 to 0 minutes; then standing for 1-2 hours at room temperature; and then, preserving the heat for 2 to 4 hours at the temperature of between 200 and 250 ℃, and then cooling the mixture to room temperature along with the furnace.