CN111517776A - Preparation method of manganese-zinc soft magnetic ferrite material - Google Patents

Preparation method of manganese-zinc soft magnetic ferrite material Download PDF

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CN111517776A
CN111517776A CN202010327093.4A CN202010327093A CN111517776A CN 111517776 A CN111517776 A CN 111517776A CN 202010327093 A CN202010327093 A CN 202010327093A CN 111517776 A CN111517776 A CN 111517776A
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treatment
sintering
soft magnetic
manganese
grinding
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伍波
余文生
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Meishan Yutai Electronic Equipment Co ltd
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Meishan Yutai Electronic Equipment Co ltd
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Abstract

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.

Description

Preparation method of manganese-zinc soft magnetic ferrite material
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.
Example 1
A preparation method of a manganese-zinc soft magnetic ferrite material comprises the following steps:
(1) weighing the main system raw materials:
weighing 52 percent of concentrate iron ore powder and 33 percent of Mn according to mol percentage3O4The balance of ZnO;
(2) weighing the raw materials of a doping system:
weighing 17 percent of CaCO by mass percentage36% of ZrO22% of MoO37% of Bi2O330 percent of CaO, 2 percent of SnO and 5 percent of TiO21% of La2O30.5% 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; controlling the temperature to 1050 ℃ and the duration to 2h during the pre-sintering treatment;
(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 hours to obtain a grinding material for later use; the mass ratio of the doping system raw material to the primary pre-sintering material is 1: 35; the rotating speed of the grinding is controlled to be 340 r/min during the grinding treatment;
(5) preparing slurry:
blending the grinding material obtained in the step (4) with a dispersant solution and deionized water, then carrying out high-speed stirring treatment, and preparing slurry for later use after 25 min; the dispersing agent solution is a PVA solution with the mass fraction of 14%; the corresponding weight ratio of the grinding material to the dispersant solution to the deionized water is 90:2: 40; the rotating speed of stirring is controlled to be 1500 revolutions per minute during the high-speed stirring treatment;
(6) preparing a compact:
performing filter pressing on the slurry obtained in the step (5) to prepare a billet, then placing the billet in a constant-temperature drying oven for drying for 2 hours, and taking out for later use; the drying temperature in the constant-temperature drying box is 90 ℃;
(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; the specific process for the secondary pre-sintering treatment comprises the following steps: controlling the oxygen content of the environment to be 0.12%, heating and preserving heat at 980 ℃ for 35min, then heating and preserving heat at 1200 ℃ for 1.5h, and finally stopping heating and cooling to room temperature along with the furnace;
(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 after 50min to obtain a ball milling material for later use; the rotating speed of ball milling is controlled to be 700 r/min during the ball milling treatment;
(9) sintering and forming:
performing dry pressing molding on the ball-milled material obtained in the step (8), then performing 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; the specific process for the high-temperature sintering treatment comprises the following steps: controlling the oxygen content in the environment to be 0.18%, heating and preserving heat for 35min at 1250 ℃, and then stopping heating and cooling to room temperature along with the furnace.
The manganese-zinc soft magnetic ferrite material prepared in the embodiment 1 of the invention is detected to have the saturation magnetic flux density of 1100-1240 mT at 25 ℃ and 1060-1220 mT at 100 ℃; the power loss under the conditions of 100 ℃, 100kHz and 200mT is not more than 160kW/m3. Therefore, the manganese-zinc soft magnetic ferrite material prepared by the method has good wide temperature range, lower power loss and excellent saturation magnetic flux density.
Example 2
A preparation method of a manganese-zinc soft magnetic ferrite material comprises the following steps:
(1) weighing the main system raw materials:
weighing 54 percent of concentrate iron ore powder and 36 percent of Mn according to mol percentage3O4The balance of ZnO;
(2) weighing the raw materials of a doping system:
weighing 19 percent of CaCO in percentage by mass38% ofZrO23% of MoO39% of Bi2O332 percent of CaO, 4 percent of SnO and 7 percent of TiO21.5% of La2O31% 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; controlling the temperature to be 1080 ℃ and the duration to be 3h during the pre-sintering treatment;
(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 2.5 hours to obtain a grinding material for later use; the mass ratio of the doping system raw material to the primary pre-sintering material is 1: 38; the rotation speed of grinding is controlled to be 360 revolutions per minute during grinding treatment;
(5) preparing slurry:
blending the grinding material obtained in the step (4) with a dispersant solution and deionized water, then carrying out high-speed stirring treatment, and preparing slurry for later use after 27 min; the dispersing agent solution is a PVA solution with the mass fraction of 16%; the corresponding weight ratio of the grinding material to the dispersant solution to the deionized water is 95:4: 42; the rotating speed of stirring is controlled to be 1700 revolutions per minute during the high-speed stirring treatment;
(6) preparing a compact:
performing filter pressing on the slurry obtained in the step (5) to prepare a billet, then placing the billet in a constant-temperature drying oven for drying for 2.6 hours, and taking out for later use; the drying temperature in the constant-temperature drying box is 92 ℃;
(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; the specific process for the secondary pre-sintering treatment comprises the following steps: controlling the oxygen content of the environment to be 0.14%, heating and preserving heat for 40min at the temperature of 1000 ℃, then heating and preserving heat for 2h at the temperature of 1230 ℃, and finally stopping heating and cooling to room temperature along with the furnace;
(8) ball milling treatment:
performing ball milling treatment on the secondary pre-sintered material obtained in the step (7), and taking out the secondary pre-sintered material after 60min to obtain a ball-milled material for later use; the rotating speed of ball milling is controlled to be 740 revolutions per minute during the ball milling treatment;
(9) sintering and forming:
performing dry pressing molding on the ball-milled material obtained in the step (8), then performing 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; the specific process for the high-temperature sintering treatment comprises the following steps: controlling the oxygen content in the environment to be 0.20%, heating and preserving heat for 40min at 1300 ℃, and then stopping heating and cooling to room temperature along with the furnace.
The manganese-zinc soft magnetic ferrite material prepared in the embodiment 2 of the invention is detected to have a saturation magnetic flux density of 1130-1280 mT at 25 ℃ and a saturation magnetic flux density of 1100-1270 mT at 100 ℃; the power loss under the conditions of 100 ℃, 300kHz and 200mT is not more than 150kW/m3. Therefore, the manganese-zinc soft magnetic ferrite material prepared by the method has good wide temperature range, lower power loss and excellent saturation magnetic flux density.
Example 3
A preparation method of a manganese-zinc soft magnetic ferrite material comprises the following steps:
(1) weighing the main system raw materials:
weighing 56% of concentrate iron ore powder and 37% of Mn in mol percentage3O4The balance of ZnO;
(2) weighing the raw materials of a doping system:
weighing 20 percent of CaCO in percentage by mass39% of ZrO24% of MoO310% of Bi2O335 percent of CaO, 5 percent of SnO and 8 percent of TiO22% of La2O31.5% 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; controlling the temperature to be 1100 ℃ during the pre-sintering treatment and the time length to be 4 h;
(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 3 hours to obtain a grinding material for later use; the mass ratio of the doping system raw material to the primary pre-sintering material is 1: 40; the rotating speed of the grinding is controlled to be 380 r/min during the grinding treatment;
(5) preparing slurry:
blending the grinding material obtained in the step (4) with a dispersant solution and deionized water, then carrying out high-speed stirring treatment, and preparing slurry for later use after 30 min; the dispersing agent solution is a PVA solution with the mass fraction of 18%; the corresponding weight ratio of the grinding material to the dispersant solution to the deionized water is 100:5: 45; the rotating speed of stirring is controlled to be 1800 rpm during the high-speed stirring treatment;
(6) preparing a compact:
performing filter pressing on the slurry obtained in the step (5) to prepare a billet, then placing the billet in a constant-temperature drying oven for drying for 3 hours, and taking out for later use; the drying temperature in the constant-temperature drying box is 95 ℃;
(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; the specific process for the secondary pre-sintering treatment comprises the following steps: controlling the oxygen content of the environment to be 0.16%, heating and preserving heat for 45min at 1020 ℃, then heating and preserving heat for 2.5h at 1260 ℃, and finally stopping heating and cooling to room temperature along with the furnace;
(8) ball milling treatment:
performing ball milling treatment on the secondary pre-sintered material obtained in the step (7), and taking out the secondary pre-sintered material after 70min to obtain a ball-milled material for later use; the rotating speed of ball milling is controlled to be 780 revolutions per minute during the ball milling treatment;
(9) sintering and forming:
performing dry pressing molding on the ball-milled material obtained in the step (8), then performing 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; the specific process for the high-temperature sintering treatment comprises the following steps: controlling the oxygen content in the environment to be 0.23%, heating and preserving heat for 45min at 1350 ℃, and then stopping heating and cooling to room temperature along with the furnace.
The manganese-zinc soft magnetic ferrite material prepared in the embodiment 3 of the invention is detected to have a saturation magnetic flux density of 1120-1260 mT at 25 ℃ and a saturation magnetic flux density of 1090-1250 mT at 100 ℃; the power loss under the conditions of 100 ℃, 500kHz and 200mT is not more than 160kW/m3. Therefore, the manganese-zinc soft magnetic ferrite material prepared by the method has good wide temperature range, lower power loss and excellent saturation magnetic flux density.

Claims (8)

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.
CN202010327093.4A 2020-04-23 2020-04-23 Preparation method of manganese-zinc soft magnetic ferrite material Pending CN111517776A (en)

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Application publication date: 20200811