阅读说明：本技术 一种锰锌软磁铁氧体材料的制备方法 (Preparation method of manganese-zinc soft magnetic ferrite material ) 是由 伍波 余文生 于 2020-04-23 设计创作，主要内容包括：本发明公开了一种锰锌软磁铁氧体材料的制备方法,属于锰锌软磁铁氧体材料加工制造技术领域,包括如下步骤：(1)主体体系原料称取、(2)掺杂体系原料称取、(3)一次预烧处理、(4)共混研磨处理、(5)浆料制备、(6)坯块制备、(7)二次预烧处理、(8)球磨处理、(9)烧结成型。本发明方法整体工艺简单,各步骤搭配合理,成本较低,便于推广应用,制得的锰锌软磁铁氧体具有较好的宽温性、较低的功率损耗以及优异的饱和磁通密度。(The invention discloses a preparation method of a manganese-zinc soft magnetic ferrite material, belonging to the technical field of processing and manufacturing of manganese-zinc soft magnetic ferrite materials, comprising the following steps: (1) weighing main body system raw materials, (2) weighing doping system raw materials, (3) primary pre-sintering treatment, (4) blending and grinding treatment, (5) slurry preparation, (6) billet preparation, (7) secondary pre-sintering treatment, (8) ball milling treatment and (9) sintering and forming. The method has the advantages of simple overall process, reasonable matching of all steps, lower cost and convenient popularization and application, and the prepared manganese-zinc soft magnetic ferrite has better wide temperature property, lower power loss and excellent saturation magnetic flux density.)

1. A preparation method of a manganese-zinc soft magnetic ferrite material is characterized by comprising the following steps:

(1) weighing the main system raw materials:

weighing 52-56% of fine iron ore powder and 33-37% of Mn in mol percentage₃O₄The balance of ZnO;

(2) weighing the raw materials of a doping system:

weighing 17-20% of CaCO by mass percent₃6 to 9% of ZrO₂2-4% of MoO₃7 to 10% of Bi₂O₃30-35% of CaO, 2-5% of SnO and 5-8% of TiO₂1-2% of La₂O₃0.5 to 1.5% of Y₂O₃And the balance graphene;

(3) primary pre-sintering treatment:

mixing all the main system raw materials weighed in the step (1) together, and then carrying out primary pre-sintering treatment on the mixture to obtain a primary pre-sintering material for later use;

(4) blending and grinding treatment:

blending and grinding all the doping system raw materials weighed in the step (2) and the primary pre-sintered material obtained in the step (3), and continuously grinding for 2-3 hours to obtain a grinding material for later use;

(5) preparing slurry:

blending the grinding material obtained in the step (4) with a dispersant solution and deionized water, and then carrying out high-speed stirring treatment for 25-30 min to obtain slurry for later use;

(6) preparing a compact:

performing filter pressing on the slurry obtained in the step (5) to prepare a blank block, then placing the blank block in a constant-temperature drying box for drying for 2-3 hours, and taking out for later use;

(7) and (3) secondary pre-sintering treatment:

performing secondary pre-sintering treatment on the briquette obtained in the step (6) to obtain a secondary pre-sintering material for later use;

(8) ball milling treatment:

performing ball milling treatment on the secondary pre-sintering material obtained in the step (7), and taking out the secondary pre-sintering material for 50-70 min to obtain a ball milling material for later use;

(9) sintering and forming:

and (4) carrying out dry pressing molding on the ball-milled material obtained in the step (8), then carrying out high-temperature sintering treatment on the ball-milled material, and finally taking out the ball-milled material and naturally cooling the ball-milled material to room temperature.

2. The method for preparing a manganese-zinc soft magnetic ferrite material according to claim 1, wherein the temperature of the one-time pre-sintering treatment in the step (3) is controlled to be 1050-1100 ℃ for 2-4 hours.

3. The preparation method of the manganese-zinc soft magnetic ferrite material according to claim 1, wherein the mass ratio of the doping system raw material to the primary pre-sintering material in the step (4) is 1: 35-40; and during the grinding treatment, the rotating speed of grinding is controlled to be 340-380 r/min.

4. The preparation method of the manganese-zinc soft magnetic ferrite material according to claim 1, wherein the dispersant solution in the step (5) is a PVA solution with a mass fraction of 14-18%; the corresponding weight ratio of the grinding material to the dispersant solution to the deionized water is 90-100: 2-5: 40-45; and the rotating speed of stirring is controlled to be 1500-1800 rpm during the high-speed stirring treatment.

5. The method for preparing a Mn-Zn soft magnetic ferrite material according to claim 1, wherein the drying temperature in the constant temperature drying oven in the step (6) is 90-95 ℃.

6. The method for preparing a manganese-zinc soft magnetic ferrite material according to claim 1, wherein the specific process for the secondary pre-sintering treatment in step (7) is as follows: controlling the oxygen content of the environment to be 0.12-0.16%, heating and preserving heat for 35-45 min at 980-1020 ℃, then heating and preserving heat for 1.5-2.5 h at 1200-1260 ℃, and finally stopping heating and cooling to room temperature along with the furnace.

7. The method for preparing a manganese-zinc soft magnetic ferrite material according to claim 1, wherein the rotation speed of ball milling is controlled to 700-780 rpm during the ball milling treatment in step (8).

8. The method for preparing a manganese-zinc soft magnetic ferrite material according to claim 1, wherein the specific process for the high temperature sintering treatment in step (9) is as follows: controlling the oxygen content in the environment to be 0.18-0.23%, heating and preserving heat for 35-45 min at 1250-1350 ℃, and then stopping heating and cooling to room temperature along with the furnace.

Technical Field

The invention belongs to the technical field of processing and manufacturing of manganese-zinc soft magnetic ferrite materials, and particularly relates to a preparation method of a manganese-zinc soft magnetic ferrite material.

Background

The use of soft magnetic materials in industry has emerged with the rise of electrical and telecommunications technology, the first applications started at the end of the nineteenth century. The soft magnetic material can be applied to the fields of household appliances, informationization, automobiles and other matching fields. With the rapid development of modern electronic technology, the high-permeability manganese-zinc ferrite in the soft magnetic material is developed rapidly, the application range is gradually expanded from the original pulse transformer to the fields of electromagnetic filters, chokes, inductors and the like, the application field is wider and wider, the market demand thereof is increased year by year, the product types are increased day by day, and the high-permeability manganese-zinc ferrite becomes a bright point for the development of the magnetic material industry.

With the expansion of the application range of ferrite materials and the development of electronic equipment, the performance requirements of ferrite materials, such as frequency stability, temperature stability, time stability and the like, are higher and higher, so as to meet the development requirements of the electronic industry and the challenges of the application environment changes on the product adaptability.

Disclosure of Invention

The invention aims to provide a preparation method of a manganese-zinc soft magnetic ferrite material, and the prepared manganese-zinc soft magnetic ferrite material has the characteristics of low loss and high use stability.

The technical purpose of the invention is realized by the following technical scheme:

a preparation method of a manganese-zinc soft magnetic ferrite material comprises the following steps:

(1) weighing the main system raw materials:

weighing 52-56% of fine iron ore powder and 33-37% of Mn in mol percentage₃O₄The balance of ZnO;

(2) weighing the raw materials of a doping system:

weighing 17-20% of CaCO by mass percent₃6 to 9% of ZrO₂2-4% of MoO₃7 to 10% of Bi₂O₃30-35% of CaO, 2-5% of SnO and 5-8% of TiO₂1-2% of La₂O₃0.5 to 1.5% of Y₂O₃And the balance graphene;

(3) primary pre-sintering treatment:

mixing all the main system raw materials weighed in the step (1) together, and then carrying out primary pre-sintering treatment on the mixture to obtain a primary pre-sintering material for later use;

(4) blending and grinding treatment:

blending and grinding all the doping system raw materials weighed in the step (2) and the primary pre-sintered material obtained in the step (3), and continuously grinding for 2-3 hours to obtain a grinding material for later use;

(5) preparing slurry:

blending the grinding material obtained in the step (4) with a dispersant solution and deionized water, and then carrying out high-speed stirring treatment for 25-30 min to obtain slurry for later use;

(6) preparing a compact:

performing filter pressing on the slurry obtained in the step (5) to prepare a blank block, then placing the blank block in a constant-temperature drying box for drying for 2-3 hours, and taking out for later use;

(7) and (3) secondary pre-sintering treatment:

performing secondary pre-sintering treatment on the briquette obtained in the step (6) to obtain a secondary pre-sintering material for later use;

(8) ball milling treatment:

performing ball milling treatment on the secondary pre-sintering material obtained in the step (7), and taking out the secondary pre-sintering material for 50-70 min to obtain a ball milling material for later use;

(9) sintering and forming:

and (4) carrying out dry pressing molding on the ball-milled material obtained in the step (8), then carrying out high-temperature sintering treatment on the ball-milled material, and finally taking out the ball-milled material and naturally cooling the ball-milled material to room temperature.

Further, the temperature is controlled to be 1050-1100 ℃ during the primary pre-sintering treatment in the step (3), and the time duration is 2-4 hours.

Further, the mass ratio of the doping system raw materials in the step (4) to the primary pre-sintering material is 1: 35-40; and during the grinding treatment, the rotating speed of grinding is controlled to be 340-380 r/min.

Further, the dispersant solution in the step (5) is a PVA solution with the mass fraction of 14-18%; the corresponding weight ratio of the grinding material to the dispersant solution to the deionized water is 90-100: 2-5: 40-45; and the rotating speed of stirring is controlled to be 1500-1800 rpm during the high-speed stirring treatment.

Further, the drying temperature in the constant-temperature drying oven in the step (6) is 90-95 ℃.

Further, the specific process for the secondary pre-sintering treatment in the step (7) is as follows: controlling the oxygen content of the environment to be 0.12-0.16%, heating and preserving heat for 35-45 min at 980-1020 ℃, then heating and preserving heat for 1.5-2.5 h at 1200-1260 ℃, and finally stopping heating and cooling to room temperature along with the furnace.

Further, the rotating speed of ball milling in the step (8) is controlled to be 700-780 rpm.

Further, the specific process for the high-temperature sintering treatment in the step (9) is as follows: controlling the oxygen content in the environment to be 0.18-0.23%, heating and preserving heat for 35-45 min at 1250-1350 ℃, and then stopping heating and cooling to room temperature along with the furnace.

Compared with the prior art, the invention has the following advantages:

the invention provides a preparation method of a manganese-zinc soft magnetic ferrite material, which optimizes and improves the traditional process method and effectively improves the quality of the material; in the preparation process, the main system raw material and the doping system raw material are compounded to prepare the material, and particularly, La is added into the doping system raw material₂O₃、Y₂O₃The added lanthanum ions can be segregated among crystal boundaries of the manganese-zinc ferrite and form a barrier layer with silicon and the like, so that the resistivity of the crystal boundaries can be improved, the yttrium ions and titanium dioxide can form a composite titanium type high-resistance layer at the crystal boundaries together, and meanwhile, graphene particles can be fixed among the crystal boundaries and are stabilized at ferrous ions to form a static resistance, so that the overall reaction activity is improved, and the wide-temperature performance of the ferrite is improved; finally, the components are matched with the raw material components of the doping system and the raw material components of the main body system, so that the saturation magnetic flux density of the ferrite material is effectively improved, the power loss characteristic is optimized, the use stability is enhanced, and the service life is prolonged. The method has the advantages of simple overall process, reasonable matching of all steps, lower cost and convenient popularization and application, and the prepared manganese-zinc soft magnetic ferrite has better wide temperature property, lower power loss and excellent saturation magnetic flux density and has great market competitiveness.

Detailed Description

The following detailed description of the preferred embodiments of the present invention is provided to enable those skilled in the art to readily understand the advantages and features of the present invention, and to clearly and unequivocally define the scope of the present invention.