阅读说明：本技术 一种高温高Bs低损耗软磁铁氧体材料及其制备方法 (High-temperature high-BsLow-loss soft magnetic ferrite material and preparation method thereof ) 是由 顾张新 邢冰冰 李小龙 张强原 缪思敏 宋岩岩 于 2020-05-19 设计创作，主要内容包括：本发明提供了一种高温高B<Sub>s</Sub>低损耗软磁铁氧体材料及其制备方法,铁氧体材料由主成分和副成分组成,所述主成分以各自氧化物计算分别为Fe<Sub>2</Sub>O<Sub>3</Sub>：56.5 mol％～57.5mol％,ZnO：7.0 mol％～9.0mol％,NiO：3.5 mol％～5.0mol％,余量为MnO；所述副成分包括CaCO<Sub>3</Sub>、Nb<Sub>2</Sub>O<Sub>5</Sub>、Li<Sub>2</Sub>CO<Sub>3</Sub>和MgO中的一种或几种。其制备方法包括配料、混合、预烧、砂磨、造粒、成型、烧结。本发明主要选用高铁配方,在主成分中添加NiO,并控制主成分、副成分的组成含量,特别是添加比磁化强度较高的Li<Sub>2</Sub>CO<Sub>3</Sub>、MgO添加剂以及采用低温致密化烧结工艺,使软磁铁氧体材料同时具备高温高B<Sub>s</Sub>、低损耗的性能。(The invention provides a high-temperature high-B s A low-loss soft magnetic ferrite material and a preparation method thereof, wherein the ferrite material consists of a main component and a secondary component, and the main component is Fe respectively calculated by respective oxides 2 O 3 : 56.5 mol% -57.5 mol%, ZnO: 7.0 mol% -9.0 mol%, NiO: 3.5mol% -5.0 mol%, and the balance being MnO; the secondary component comprises CaCO 3 、Nb 2 O 5 、Li 2 CO 3 And one or more of MgO. The preparation method comprises the steps of proportioning, mixing, presintering, sanding, granulating, molding and sintering. The invention mainly selects a high-iron formula, NiO is added into the main component, the composition contents of the main component and the auxiliary component are controlled, and particularly Li with higher specific magnetization intensity is added 2 CO 3 MgO additive and low-temperature densification sintering process are adopted to enable the soft magnetic ferrite material to have high temperature and high B s Low loss performance.)

1. High-temperature high-B_sThe low-loss soft magnetic ferrite material consists of main component and subsidiary component, and features that the main component is quaternary system and the main material includes Fe₂O₃: 56.5 mol% -57.5 mol%, ZnO: 7.0 mol% -9.0 mol%, NiO: 3.5mol% -5.0 mol%, and the balance being MnO; the secondary component comprises CaCO₃：0.04 wt%～0.12wt%、Nb₂O₅：0.01 wt%～0.03wt%、Li₂CO₃:0.01wt% -0.14 wt%, MgO: 0.005wt% -0.03 wt% of one or more of the following steps:

1) preparing materials: adopting quaternary system formula according to main formula Fe₂O₃Weighing ZnO, NiO and MnO in proportion, mixing and crushing;

2) pre-burning: pre-burning the mixed powder;

3) sanding: adding the additive into the pre-sintered material, performing vibration grinding and then performing secondary mixing treatment, wherein the sand grinding time is 60-100 min, and the particle size is 0.4-1.5 um;

4) and (3) granulation: drying the ground slurry and then granulating;

5) molding: pressing the granulated particles to obtain a required blank;

6) and (3) sintering: the blank is sintered in a kiln by adopting balanced oxygen partial pressure, the oxygen content is 0.1-0.5 percent at the temperature rising section of 800-1200 ℃, and the sintering temperature is 1340-1390 ℃.

2. High temperature high saturation magnetic flux density B according to claim 1_sThe low-loss soft magnetic ferrite material is characterized in that: the pre-sintering temperature in the step 2) is 850-1000 ℃, and the heat preservation is carried out for 1-2 h.

3. High temperature high saturation magnetic flux density B according to claim 1_sThe low-loss soft magnetic ferrite material is characterized in that: the sintering temperature in the step 5) is 1350-1390 ℃, the equilibrium oxygen content is 1.0-4.0 percent, and the heat preservation time is 4-6 hours.

Technical Field

The invention belongs to the technical field of soft magnetic ferrite materials, and particularly relates to a high-temperature high-B ferrite material_sA low-loss soft magnetic ferrite material and a preparation method thereof.

Background

With the rapid development of personal computers, information appliances, automotive electronics, and the like, demands for miniaturization and flattening of electronic devices have been made. Increase the high-temperature saturation magnetic flux density B of the magnetic core_sThe converter is beneficial to reducing the volume of the converter and ensuring the normal operation of electronic devices under complex conditions such as high temperature and the like. Meanwhile, the high-temperature power consumption of the material is not too high, the power consumption is required to be a negative temperature coefficient in order to avoid the rapid increase of the temperature rise caused by the power consumption, and the temperature at the lowest point of the power consumption is higher than the working temperature, so that the electronic device is in a low-loss state when working at the working temperature, and the vicious circle between the power consumption and the temperature rise caused by the power consumption is prevented.

In recent years, high temperature high B_sLow-loss soft magnetic ferrite materials have become a focus of attention in the magnetic industry.

In a Chinese published patent CN101090017A, a high saturation magnetic flux density low loss MnZn power ferrite and a preparation method thereof are disclosed, the invention relates to a high saturation magnetic flux density low loss MnZn power ferrite and a preparation method thereof; the invention develops the power consumption valley point of less than or equal to 260mW/cm under the conditions of 90 ℃, 100kHz and 200mT by accurately controlling the components and the preparation method of the material³A MnZn power ferrite having a saturation magnetic flux density of 530mT or more at 25 ℃ under 1000A/m and 50Hz and a saturation magnetic flux density of 420mT or more at 100 ℃ under 1000A/m and 50 Hz.

In chinese published patent CN102054552A, a NiMnZn ferrite material is disclosed, which is composed of a main component and an accessory component, and is characterized in that: the main component raw materials are as follows: fe₂O₃53.2-55.7 mol%, ZnO 2-11 mol%, NiO 0-2.5 mol% but not 0, and the balance MnO; what is needed isThe accessory ingredient raw materials comprise the following components in percentage by weight of the total weight of the main ingredient raw materials: SiO 2₂50～200ppm，CaCO₃200～1500ppm，ZrO₂50～500ppm，Nb₂O₅50 to 500ppm and Na₂O₅0 to 300 ppm. The invention also provides a preparation method of the NiMnZn ferrite material, wherein in the sintering procedure, the heating rate is 4-7 ℃/min in the temperature rise stage of 1000-1300 ℃, and the oxygen partial pressure concentration is below 0.2%; the temperature is 1300-1350 ℃, and the sintering time is 2-8 hours. The ferrite core provided by the invention has a saturation magnetic flux density of more than 450mT at 100 ℃ and a loss of 320KW/m at 100 DEG C³The following.

In chinese published patent CN102690106A, a high saturation magnetic flux density MnZn ferrite material is disclosed, which is composed of a main component and a subcomponent, wherein the main component and the content are calculated as oxides: fe₂O₃60-68 mol%, 10-20 mol% of ZnO and the balance of MnO; the auxiliary components based on the total weight of the main components are as follows: SiO 2₂50～200ppm、CaCO₃200～1500ppm、ZrO₂50～500ppm、Nb₂O₅50 to 500ppm and V₂O₅50 to 500 ppm. The invention also provides a preparation method of the ferrite material. The ferrite core provided by the invention has a saturation magnetic flux density of above 560mT at 25 ℃ and above 460mT at 100 ℃; volume loss at 25 ℃ is 1800kW/m³The volume loss at 100 ℃ is below 1600kW/m³The following.

Disclosure of Invention

The invention aims to solve the technical problem of providing a high-temperature high-B_sA low-loss soft magnetic ferrite material and its preparing process, wherein the high-iron formula is mainly selected, NiO is added to main component, and the contents of main and auxiliary components are controlledIn particular, addition of Li having a higher specific magnetization₂CO₃MgO additive and low-temperature densification sintering process are adopted to enable the soft magnetic ferrite material to have high temperature and high B_sLow loss performance.

The technical scheme adopted by the invention for solving the technical problem is as follows: high-temperature high-B_sThe low-loss soft magnetic ferrite material consists of main component and subsidiary component, the main component is quaternary system, and each main material includes Fe₂O₃: 56.5 mol% -57.5 mol%, ZnO: 7.0 mol% -9.0 mol%, NiO: 3.5mol% -5.0 mol%, and the balance being MnO; the secondary component comprises CaCO₃：0.04 wt%～0.12wt%、 Nb₂O₅：0.01wt%～0.03wt%、Li₂CO₃:0.01wt% -0.14 wt%, MgO: 0.005wt% -0.03 wt% of one or more of the components.

A high temperature high B_sThe preparation method of the low-loss soft magnetic ferrite material comprises the following steps:

1) preparing materials: adopting quaternary system formula according to main formula Fe₂O₃Weighing ZnO, NiO and MnO in proportion, mixing and crushing;

2) pre-burning: pre-burning the mixed powder;

3) sanding: adding the additive into the pre-sintered material, performing vibration grinding and then performing secondary mixing treatment, wherein the sand grinding time is 60-100 min, and the particle size is 0.4-1.5 um;

4) and (3) granulation: drying the ground slurry and then granulating;

5) molding: pressing the granulated particles to obtain a required blank;

6) and (3) sintering: the blank is sintered in a kiln by adopting balanced oxygen partial pressure, the oxygen content is 0.1-0.5 percent at the temperature rising section of 800-1200 ℃, and the sintering temperature is 1340-1390 ℃.

Preferably, the pre-sintering temperature in the step 2) is 850-1000 ℃, and the temperature is kept for 1-2 h.

Preferably, the sintering temperature in the step 5) is 1350-1390 ℃, the equilibrium oxygen content is 1.0-4.0%, and the heat preservation time is 4-6 h.

The invention has the beneficial effects that: by controlling the composition and content of the main component and the subcomponent, Li having a high specific magnetization is added₂CO₃MgO additive and high-temperature high-B prepared by adopting low-temperature densification sintering process_sThe power consumption of the low-loss soft magnetic ferrite core is less than 550kW/m at 100kHz and 200mT at 100 DEG C³B at 100 ℃ at 1kHz,1194A/m_sReaching 480mT, and the soft magnetic ferrite material has high temperature and high B_sLow loss performance.

Detailed Description

The present invention will be described below with reference to specific examples, but the present invention is not limited to these examples.