WO2023045074A1 - Ultra-high-frequency high-permeability low-loss manganese-zinc soft magnetic ferrite and preparation method - Google Patents

Ultra-high-frequency high-permeability low-loss manganese-zinc soft magnetic ferrite and preparation method Download PDF

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WO2023045074A1
WO2023045074A1 PCT/CN2021/134490 CN2021134490W WO2023045074A1 WO 2023045074 A1 WO2023045074 A1 WO 2023045074A1 CN 2021134490 W CN2021134490 W CN 2021134490W WO 2023045074 A1 WO2023045074 A1 WO 2023045074A1
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ultra
temperature
soft magnetic
permeability
frequency
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French (fr)
Chinese (zh)
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张志新
张强原
邢冰冰
王鸿健
徐涛
缪思敏
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天通控股股份有限公司
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Priority to DE112021008262.0T priority Critical patent/DE112021008262T5/en
Publication of WO2023045074A1 publication Critical patent/WO2023045074A1/en

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Definitions

  • the invention relates to an ultra-high frequency, high magnetic permeability, low loss manganese zinc soft magnetic ferrite and a preparation method, belonging to the technical field of magnetic materials.
  • SiC silicon carbide
  • GaN gallium nitride
  • the operating frequency of high-frequency transformers is higher than 1MHz.
  • NiZn ferrite is a commonly used material with a frequency above 5MHz, but its cost is much higher than that of MnZn ferrite.
  • the Chinese patent with the authorized announcement number CN106830913B discloses a method for making MnZn ferrite with high frequency, high saturation magnetic flux density and low loss. 6MHz.
  • the Chinese patent with the publication number CN112759379A discloses a tempering process for reducing the loss of high-frequency MnZn ferrite sintered magnetic core. improved, but did not account for changes in other magnetic properties. It is very different from the annealing method of the present invention, and the present invention can not only improve the loss but also increase the magnetic permeability, so that the magnetic permeability of the magnetic core does not deteriorate under ultra-high frequency.
  • the present invention provides a manganese-zinc soft magnetic ferrite with ultra-high frequency and high magnetic permeability and a preparation method.
  • the invention adopts suitable main components and doping, adopts low Zn main formula, improves the material cut-off frequency, and makes it have lower loss under the frequency characteristic of 6-8MHz.
  • Doping the low-melting-point material MoO 3 in the main formula can help dissolve, reduce the sintering temperature and accelerate the reaction speed, reduce the grain size and reduce the high-frequency loss. Due to the low Zn formula and the doping of co-solvent, the magnetic permeability of the material is reduced. In order to further reduce the loss and increase the magnetic permeability, it is annealed at 600-900°C.
  • Annealing can not only eliminate the internal stress of the magnetic core and increase the magnetic permeability, but also make the liquid phase distribution more uniform, increase the resistivity and reduce the loss. Finally, a manganese-zinc soft ferrite with ultra-high frequency and high magnetic permeability is obtained.
  • Step 1 Ingredients: Weigh Fe2O3 according to the proportion: 73.5 ⁇ 76.5wt%, ZnO: 0 ⁇ 3.0wt%, MoO3 : 0.01 ⁇ 0.04wt %, the rest is Mn3O4 , and then carry out wet sanding Mixing, the mixing time is 10-20min;
  • Step 2 Pre-burning: Pre-burning the mixture obtained in step 1 after drying, and pre-burning in the air, the pre-burning temperature is 800-1000°C, and the heating rate is 3-5°C/min;
  • Step 3 Sanding: vibrate and grind the calcined material obtained in Step 2, and then add auxiliary components according to the proportion: CaCO 3 : 400-600ppm, ZrO 2 : 100-300ppm, TiO 2 : 500-800ppm, Co 2 O 3 : 1500 ⁇ 4000ppm, CuO: 50 ⁇ 200ppm, sanding and sanding time is 30 ⁇ 90min;
  • Step 4 Granulation: According to the total weight of the powder obtained after grinding, add 15wt% polyvinyl alcohol, grind and sieve into particles of a certain size, dry and granulate the slurry after sanding;
  • Step 5 Press molding: press into a circular green body with a size of ⁇ 12.5mm* ⁇ 7.5mm*7mm;
  • Step 6 sintering, the sintering temperature is 1000-1200°C, the holding time is 4-8 hours, and the equilibrium oxygen content is 1.5-3.0%;
  • Step 7 annealing, annealing the fired product under vacuum condition.
  • the heating process first raise the temperature to 250-400°C at 3-5°C/min, keep it warm for 30-60min, then raise the temperature at 1-3°C to 600-900°C, keep it warm for 2-4h, and then gradually cool down, and the cooling rate starts at 1-3°C/min to 300-500°C, and then to room temperature at 5-8°C.
  • the main components of an ultra-high-frequency high-permeability low-loss manganese-zinc ferrite include Fe 2 O 3 : 74.0-75.5wt%, ZnO: 1.4-3.0wt%, MoO 3 : 0.03-0.04wt% %, the rest is Mn 3 O 4 ; auxiliary components: CaCO 3 : 400-600ppm, ZrO 2 : 100-300ppm, TiO 2 : 500-800ppm, Co 2 O 3 : 1500-2000ppm, CuO: 50-200ppm.
  • the sintering temperature in step 6 is 1050-1150° C., and the grain size after sintering is 2-4 ⁇ m.
  • the manganese-zinc soft magnetic ferrite of the present invention has lower loss and high magnetic permeability under the frequency characteristics of 6-8 MHz, and the technical performance, index and parameters are as follows:
  • the ultra-high-frequency high-permeability low-loss manganese-zinc soft magnetic ferrite of the present invention can not only replace part of NiZn ferrite, meet the requirements of magnetic devices for ultra-high frequencies, greatly reduce material costs, but also help reduce The size of the device and the number of winding turns reduce the line loss and temperature rise, and can be widely used in miniaturized devices, making a good material reserve for future device miniaturization.
  • the ultra-high frequency high magnetic permeability low loss manganese zinc soft ferrite material prepared by the present invention and the preparation process are further specifically described below through specific implementation cases.
  • Two MnZn soft ferrite materials of Example 1 and Example 2 and four MnZn soft ferrite materials of Comparative Example 1, Comparative Example 2, Comparative Example 3 and Comparative Example 4 were prepared according to the following preparation methods.
  • Embodiment 1 A manganese-zinc soft magnetic ferrite with high magnetic permeability and low loss at ultra-high frequency is composed of a main component and an auxiliary component.
  • the preparation method is as follows:
  • Step 1 Ingredients: Fe 2 O 3 : 74.3wt%, ZnO: 1.8wt%, MoO 3 : 0.04wt% and the rest of Mn 3 O 4 ingredients, and then mixed by wet ball milling, the mixing time is 15min;
  • Step 2 Pre-burning: pre-burn the mixture obtained in step 1 after drying, the pre-burning temperature is 900°C, and the heating rate is 5°C/min;
  • Step 3 Sanding: vibrating the obtained calcined material, then adding auxiliary components: CaCO 3 : 600ppm, ZrO 2 : 200ppm, TiO 2 : 800ppm, Co 2 O 3 : 1800ppm, CuO: 50-200ppm, sanding for 70min ;
  • Step 4 Granulation: according to the total weight of the powder obtained after grinding, add 15wt% polyvinyl alcohol, grind and sieve into particles of a certain size;
  • Step 5 Press molding: press into a circular green body with a size of ⁇ 12.5mm* ⁇ 7.5mm*7mm;
  • Step 6 Sintering: the sintering temperature is 1120°C, the holding time is 6h, and the equilibrium oxygen content is 1.6%;
  • Step 7 Annealing: raise the temperature to 700° C. at a certain rate under vacuum conditions, keep it for 2 hours, and then gradually lower it to room temperature at a certain rate.
  • Embodiment 2 A manganese-zinc soft magnetic ferrite material with high magnetic permeability and low loss at ultra-high frequency, which is composed of main components and auxiliary components, and the preparation method is as follows:
  • Step 1 Ingredients: Fe 2 O 3 : 74.8wt%, ZnO: 2.4wt%, MoO 3 : 0.04wt% and the rest of Mn 3 O 4 ingredients, and then mixed by wet ball milling, the mixing time is 15min;
  • Step 2 Pre-burning: pre-burn the mixture obtained in step 1 after drying, the pre-burning temperature is 900°C, and the heating rate is 5°C/min;
  • Step 3 sanding: vibrating the obtained calcined material, then adding auxiliary components: CaCO 3 : 600ppm, ZrO 2 : 200ppm, TiO 2 : 800ppm, Co 2 O 3 : 1800ppm, CuO: 80ppm, sanding for 70min;
  • Step 4 Granulation: according to the total weight of the powder obtained after grinding, add 15wt% polyvinyl alcohol, grind and sieve into particles of a certain size;
  • Step 5 Press molding: press into a circular green body with a size of ⁇ 12.5mm* ⁇ 7.5mm*7mm;
  • Step 6 Sintering: the sintering temperature is 1120°C, the holding time is 6h, and the equilibrium oxygen content is 1.6%;
  • Step 7 Annealing: raise the temperature to 700° C. at a certain rate under vacuum conditions, keep it for 2 hours, and then gradually lower it to room temperature at a certain rate.
  • Embodiment 3 An ultra-high frequency high magnetic permeability low loss manganese zinc soft magnetic ferrite material is composed of main components and auxiliary components.
  • the preparation method is as follows:
  • Step 1 Ingredients: Fe 2 O 3 : 75.2wt%, ZnO: 2.8wt%, MoO 3 : 0.03wt% and the rest of Mn 3 O 4 ingredients, and then mixed by wet ball milling, the mixing time is 15min;
  • Step 2 Pre-burning: pre-burn the mixture obtained in step 1 after drying, the pre-burning temperature is 900°C, and the heating rate is 5°C/min;
  • Step 3 Sanding: vibrating the obtained calcined material, then adding auxiliary components: CaCO 3 : 600ppm, ZrO 2 : 200ppm, TiO 2 : 800ppm, Co 2 O 3 : 1800ppm, CuO: 80ppm, and sanding for 70min.
  • Step 4 Granulation: according to the total weight of the powder obtained after grinding, add 15wt% polyvinyl alcohol, grind and sieve into particles of a certain size;
  • Step 5 Press molding: press into a circular green body with a size of ⁇ 12.5mm* ⁇ 7.5mm*7mm;
  • Step 6 Sintering: the sintering temperature is 1120°C, the holding time is 6h, and the equilibrium oxygen content is 1.6%;
  • Step 7 Annealing: raise the temperature to 800° C. at a certain rate under vacuum conditions, keep it for 2 hours, and then gradually lower it to room temperature at a certain rate.
  • Comparative Example 1 A manganese-zinc soft magnetic ferrite material is composed of a main component and an auxiliary component.
  • the preparation method is as follows:
  • Step 1 Ingredients: Fe 2 O 3 : 74.3wt%, ZnO: 2.2wt%, MoO 3 : 0.04wt% and the rest of Mn 3 O 4 ingredients, and then mixed by wet ball milling, the mixing time is 15min;
  • Step 2 Pre-burning: pre-burn the mixture obtained in step 1 after drying, the pre-burning temperature is 900°C, and the heating rate is 5°C/min;
  • Step 3 Sanding: vibrating the obtained calcined material, then adding auxiliary components: CaCO 3 : 600ppm, ZrO 2 : 200ppm, TiO 2 : 800ppm, Co 2 O 3 : 1800ppm, CuO: 50-200ppm, sanding for 70min ;
  • Step 4 Granulation: according to the total weight of the powder obtained after grinding, add 15wt% polyvinyl alcohol, grind and sieve into particles of a certain size;
  • Step 5 Press molding: press into a circular green body with a size of ⁇ 12.5mm* ⁇ 7.5mm*7mm;
  • Step 6 Sintering: the sintering temperature is 1120° C., the holding time is 6 hours, and the equilibrium oxygen content is 1.6%.
  • Comparative Example 2 A manganese-zinc soft magnetic ferrite material is composed of a main component and an auxiliary component.
  • the preparation method is as follows:
  • Step 1 Ingredients: Fe 2 O 3 : 74.6wt%, ZnO: 3.4wt%, MoO 3 : 0.04wt% and the rest of Mn 3 O 4 ingredients, and then mixed by wet ball milling, the mixing time is 15min;
  • Step 2 Pre-burning: pre-burn the mixture obtained in step 1 after drying, the pre-burning temperature is 900°C, and the heating rate is 5°C/min;
  • Step 3 Sanding: vibrating the obtained calcined material, then adding auxiliary components: CaCO 3 : 600ppm, ZrO 2 : 200ppm, TiO 2 : 800ppm, Co 2 O 3 : 1800ppm, CuO: 50-200ppm, sanding for 70min ;
  • Step 4 Granulation: according to the total weight of the powder obtained after grinding, add 15wt% polyvinyl alcohol, grind and sieve into particles of a certain size;
  • Step 5 Press molding: press into a circular green body with a size of ⁇ 12.5mm* ⁇ 7.5mm*7mm;
  • Step 6 Sintering: the sintering temperature is 1120°C, the holding time is 6h, and the equilibrium oxygen content is 1.6%;
  • Step 7 Annealing: raise the temperature to 700° C. at a certain rate under vacuum conditions, keep it for 2 hours, and then gradually lower it to room temperature at a certain rate.
  • a manganese-zinc soft magnetic ferrite material is composed of a main component and an auxiliary component.
  • the preparation method is as follows:
  • Step 1 Ingredients: Fe 2 O 3 : 74.3wt%, ZnO: 1.8wt%, the rest is Mn 3 O 4 ingredients, and then mixed by wet ball milling, the mixing time is 15min;
  • Step 2 Pre-burning: pre-burn the mixture obtained in step 1 after drying, the pre-burning temperature is 900°C, and the heating rate is 5°C/min;
  • Step 3 Sanding: vibrating the obtained calcined material, then adding auxiliary components: CaCO 3 : 600ppm, ZrO 2 : 200ppm, TiO 2 : 800ppm, Co 2 O 3 : 1800ppm, CuO: 50-200ppm, sanding for 70min ;
  • Step 4 Granulation: according to the total weight of the powder obtained after grinding, add 15wt% polyvinyl alcohol, grind and sieve into particles of a certain size;
  • Step 5 Press molding: press into a circular green body with a size of ⁇ 12.5mm* ⁇ 7.5mm*7mm;
  • Step 6 Sintering: the sintering temperature is 1120°C, the holding time is 6h, and the equilibrium oxygen content is 1.6%;
  • Step 7 Annealing: raise the temperature to 700° C. at a certain rate under vacuum conditions, keep it for 2 hours, and then gradually lower it to room temperature at a certain rate.
  • Comparative Example 4 A manganese-zinc soft magnetic ferrite material is composed of a main component and an auxiliary component.
  • the preparation method is as follows:
  • Step 1 Ingredients: Fe 2 O 3 : 74.6wt%, ZnO: 3.4wt%, MoO 3 : 0.04wt% and the rest of Mn 3 O 4 ingredients, and then mixed by wet ball milling, the mixing time is 15min;
  • Step 2 Pre-burning: pre-burn the mixture obtained in step 1 after drying, the pre-burning temperature is 900°C, and the heating rate is 5°C/min;
  • Step 3 Sanding: vibrating the obtained calcined material, then adding auxiliary components: CaCO 3 : 600ppm, ZrO 2 : 200ppm, TiO 2 : 800ppm, Co 2 O 3 : 1800ppm, CuO: 50-200ppm, sanding for 70min ;
  • Step 4 Granulation: according to the total weight of the powder obtained after grinding, add 15wt% polyvinyl alcohol, grind and sieve into particles of a certain size;
  • Step 5 Press forming: press into a circular green body with a size of ⁇ 12.5mm* ⁇ 7.5mm*7mm, and a density of 3.2g/cm 3 ;
  • Step 6 Sintering: the sintering temperature is 1120° C., the holding time is 6 hours, and the equilibrium oxygen content is 1.6%.
  • Examples 1, 2 and 3 obtain the best magnetic properties according to the manufacturing method of the present invention. Comparing the comparative example 1 with the embodiment, or comparing the comparative example 2 with the comparative example 4, it can be obtained that after the annealing process, the magnetic permeability is obviously increased and the loss is also reduced. Comparing Comparative Example 2 with Examples shows that when the main formula Zn content is low, the high frequency loss is significantly reduced. Comparing Comparative Example 3 with Examples shows that when MoO3 is added to the main formula, the magnetic permeability increases and the high-frequency loss decreases.

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Abstract

The present invention pertains to the technical field of magnetic materials, and an ultra-high-frequency high-permeability low-loss manganese-zinc soft magnetic ferrite and a preparation method are disclosed. The material of the present invention includes primary components and auxiliary components, the primary components comprising Fe2O3, ZnO, MoO3, and Mn3O4, and the auxiliary components comprise CaCO3, ZrO2, TiO2, Co2O3, and CuO. In the present invention, by means of suitable primary components and doping materials and the use of a low-Zn main formula, the ZnO content is 0-3.0 wt%, which increases a cut-off frequency; doping the primary formula with the low-melting point material MoO3 reduces the sintering temperature; annealing at 600-900°C increases magnetic permeability. By means of the above method, a manganese zinc soft ferrite material with ultra-high frequency, high permeability and low loss under the conditions of 6MHz, 30mT, 8MHz, 10mT, and 25°C and 40°C is successfully produced.

Description

一种超高频高磁导率低损耗锰锌软磁铁氧体及制备方法A kind of ultra-high frequency high magnetic permeability low loss manganese zinc soft magnetic ferrite and its preparation method 技术领域technical field
本发明涉及超高频高磁导率低损耗锰锌软磁铁氧体及制备方法，属于磁性材料技术领域。The invention relates to an ultra-high frequency, high magnetic permeability, low loss manganese zinc soft magnetic ferrite and a preparation method, belonging to the technical field of magnetic materials.
背景技术Background technique
随着微电子技术的发展，传统Si和GaAs半导体器件性能已经接近其材料本身决定的理论极限。而以碳化硅(SiC)和氮化镓(GaN)为代表的第三代半导体即宽禁带半导体材料，由于具有宽带隙、高饱和漂移速度、高临界击穿电场等突出优点，成为制作大功率、高频及抗辐照电子器件的理想替代材料。当前高频变压器的工作频率已高于1MHz，随着科技的发展，未来发展趋势为5MHz之上。目前常见的使用频率在5MHz以上的材料是NiZn铁氧体，但是其成本较MnZn铁氧体高很多。因此为了满足磁性器件对高频的要求，并进一步节省成本，拟开发6MHz～8MHz频段的超高频低损耗、高磁导率、高直流偏置能力的新一代高性能软磁材料。With the development of microelectronics technology, the performance of traditional Si and GaAs semiconductor devices has approached the theoretical limit determined by their materials themselves. The third-generation semiconductors represented by silicon carbide (SiC) and gallium nitride (GaN), that is, wide-bandgap semiconductor materials, have become a large It is an ideal substitute material for power, high-frequency and radiation-resistant electronic devices. At present, the operating frequency of high-frequency transformers is higher than 1MHz. With the development of science and technology, the future development trend will be above 5MHz. At present, NiZn ferrite is a commonly used material with a frequency above 5MHz, but its cost is much higher than that of MnZn ferrite. Therefore, in order to meet the high-frequency requirements of magnetic devices and further save costs, it is planned to develop a new generation of high-performance soft magnetic materials with ultra-high frequency, low loss, high magnetic permeability, and high DC bias capability in the 6MHz to 8MHz frequency band.
授权公告号为CN106830913B的中国专利公开了一种高频高饱和磁通密度低损耗MnZn铁氧体的制作方法，其配方和工艺与本发明相差大，且没有涉及磁导率且适用频率没有突破6MHz。公布号为CN112759379A的中国专利公开了一种降低高频MnZn铁氧体烧结磁芯损耗的回火工艺，该工艺在氮气的氛围中将磁芯在Tc±150℃的温度下处理后，虽然损耗得到改善，但没有说明其他磁性能的变化情况。与本发明退火的方式有很大差别，本发明不仅可以改善损耗还可以提高磁导率，使磁芯在超高频下磁导率没有发生恶化。The Chinese patent with the authorized announcement number CN106830913B discloses a method for making MnZn ferrite with high frequency, high saturation magnetic flux density and low loss. 6MHz. The Chinese patent with the publication number CN112759379A discloses a tempering process for reducing the loss of high-frequency MnZn ferrite sintered magnetic core. improved, but did not account for changes in other magnetic properties. It is very different from the annealing method of the present invention, and the present invention can not only improve the loss but also increase the magnetic permeability, so that the magnetic permeability of the magnetic core does not deteriorate under ultra-high frequency.
发明内容Contents of the invention
为解决以上问题，本发明提供一种超高频高磁导率锰锌软磁铁氧体及制备方法。本发明通过合适的主成分与掺杂，采用低Zn主配方，提高材料截止频率，使其在6～8MHz频率特性下具有较低损耗。在主配方中掺杂低熔点物质MoO 3，起到助溶、降低烧结温度和加快反应速度等作用，减小晶粒尺寸，降低高频损耗。由于低Zn配方和助溶剂的掺杂，使材料的 磁导率减小，为了进一步降低损耗和提高磁导率，将其在600～900℃进行退火处理。通过退火，不仅可以消除磁芯内应力，提高磁导率，还可以使液相分布更加均匀，提高电阻率，降低损耗。最终获得一种超高频高磁导率锰锌软磁铁氧体。 In order to solve the above problems, the present invention provides a manganese-zinc soft magnetic ferrite with ultra-high frequency and high magnetic permeability and a preparation method. The invention adopts suitable main components and doping, adopts low Zn main formula, improves the material cut-off frequency, and makes it have lower loss under the frequency characteristic of 6-8MHz. Doping the low-melting-point material MoO 3 in the main formula can help dissolve, reduce the sintering temperature and accelerate the reaction speed, reduce the grain size and reduce the high-frequency loss. Due to the low Zn formula and the doping of co-solvent, the magnetic permeability of the material is reduced. In order to further reduce the loss and increase the magnetic permeability, it is annealed at 600-900°C. Annealing can not only eliminate the internal stress of the magnetic core and increase the magnetic permeability, but also make the liquid phase distribution more uniform, increase the resistivity and reduce the loss. Finally, a manganese-zinc soft ferrite with ultra-high frequency and high magnetic permeability is obtained.
为实现上述目的，本发明采用的具体技术方案如下：In order to achieve the above object, the concrete technical scheme that the present invention adopts is as follows:
步骤1：配料：按照比例称重Fe 2O 3：73.5～76.5wt％，ZnO：0～3.0wt％，MoO 3：0.01～0.04wt％，其余为Mn 3O 4，然后进行湿法砂磨混合，混合时间为10～20min； Step 1: Ingredients: Weigh Fe2O3 according to the proportion: 73.5~76.5wt%, ZnO: 0 ~ 3.0wt%, MoO3 : 0.01~ 0.04wt %, the rest is Mn3O4 , and then carry out wet sanding Mixing, the mixing time is 10-20min;
步骤2：预烧：对步骤1中所得混合料烘干后进行预烧，在空气中进行预烧，预烧温度为800～1000℃，升温速率为3～5℃/min；Step 2: Pre-burning: Pre-burning the mixture obtained in step 1 after drying, and pre-burning in the air, the pre-burning temperature is 800-1000°C, and the heating rate is 3-5°C/min;
步骤3：砂磨：对步骤2所得预烧料振磨，然后按照比例加入辅助成分：CaCO 3：400～600ppm、ZrO 2：100～300ppm、TiO 2：500～800ppm、Co 2O 3：1500～4000ppm、CuO:50～200ppm，砂磨且砂磨时间是30～90min； Step 3: Sanding: vibrate and grind the calcined material obtained in Step 2, and then add auxiliary components according to the proportion: CaCO 3 : 400-600ppm, ZrO 2 : 100-300ppm, TiO 2 : 500-800ppm, Co 2 O 3 : 1500 ～4000ppm, CuO: 50～200ppm, sanding and sanding time is 30～90min;
步骤4：造粒：根据研磨后得到粉料总重量，加入15wt％聚乙烯醇，研磨过筛成一定尺寸的颗粒，对砂磨后的料浆烘干并造粒；Step 4: Granulation: According to the total weight of the powder obtained after grinding, add 15wt% polyvinyl alcohol, grind and sieve into particles of a certain size, dry and granulate the slurry after sanding;
步骤5：压制成型：压制成尺寸为Φ12.5mm*Φ7.5mm*7mm环形生坯；Step 5: Press molding: press into a circular green body with a size of Φ12.5mm*Φ7.5mm*7mm;
步骤6：烧结，烧结温度为1000～1200℃，保温时间为4～8h，平衡氧含量为1.5～3.0％；Step 6: sintering, the sintering temperature is 1000-1200°C, the holding time is 4-8 hours, and the equilibrium oxygen content is 1.5-3.0%;
步骤7：退火，对烧成产品在真空条件下做退火处理。升温过程中先以3～5℃/min升温至250～400℃，保温30～60min，然后以1～3℃升温至600～900℃，保温2～4h，然后逐渐降温，且降温速率开始以1～3℃/min降至300～500℃，然后以5～8℃降至室温。Step 7: annealing, annealing the fired product under vacuum condition. During the heating process, first raise the temperature to 250-400°C at 3-5°C/min, keep it warm for 30-60min, then raise the temperature at 1-3°C to 600-900°C, keep it warm for 2-4h, and then gradually cool down, and the cooling rate starts at 1-3°C/min to 300-500°C, and then to room temperature at 5-8°C.
进一步优选的，一种超高频高磁导率低损耗锰锌铁氧体的主成分包括Fe 2O 3：74.0～75.5wt％，ZnO：1.4～3.0wt％，MoO 3：0.03～0.04wt％，其余为Mn 3O 4；辅助成分：CaCO 3：400～600ppm、ZrO 2：100～300ppm、TiO 2：500～800ppm、Co 2O 3：1500～2000ppm、CuO:50～200ppm。 Further preferably, the main components of an ultra-high-frequency high-permeability low-loss manganese-zinc ferrite include Fe 2 O 3 : 74.0-75.5wt%, ZnO: 1.4-3.0wt%, MoO 3 : 0.03-0.04wt% %, the rest is Mn 3 O 4 ; auxiliary components: CaCO 3 : 400-600ppm, ZrO 2 : 100-300ppm, TiO 2 : 500-800ppm, Co 2 O 3 : 1500-2000ppm, CuO: 50-200ppm.
进一步优选的，步骤6中的烧结温度为1050～1150℃，烧结后的晶粒尺寸为2～4μm。Further preferably, the sintering temperature in step 6 is 1050-1150° C., and the grain size after sintering is 2-4 μm.
与现有技术相比，本发明的有益效果为：Compared with prior art, the beneficial effect of the present invention is:
本发明的锰锌软磁铁氧体，在6～8MHz频率特性下具有较低损耗和高磁导率，达到技术性能、指标和参数如下：The manganese-zinc soft magnetic ferrite of the present invention has lower loss and high magnetic permeability under the frequency characteristics of 6-8 MHz, and the technical performance, index and parameters are as follows:
(1)初始磁导率μi≥850(T＝25℃，B<0.25mT)；(1) Initial magnetic permeability μi≥850 (T=25℃, B<0.25mT);
(2)磁损耗Pcv≤1150kW/m 3(T＝25℃，f＝6MHz，B＝30mT)；Pcv≤1250kW/m 3(T＝40℃，f＝6MHz，B＝30mT)；Pcv≤600kW/m 3(T＝25℃，f＝8MHz，B＝10mT)；Pcv≤730kW/m 3(T＝40℃，f＝8MHz，B＝10mT)； (2) Magnetic loss Pcv≤1150kW/m 3 (T=25℃, f=6MHz, B=30mT); Pcv≤1250kW/m 3 (T=40℃, f=6MHz, B=30mT); Pcv≤600kW /m 3 (T=25°C, f=8MHz, B=10mT); Pcv≤730kW/m 3 (T=40°C, f=8MHz, B=10mT);
(3)饱和磁感应强度Bs≥530mT(25℃，H＝1194A/m)；Bs≥440mT(100℃，H＝1194A/m)；(3) Saturation magnetic induction Bs≥530mT (25°C, H=1194A/m); Bs≥440mT (100°C, H=1194A/m);
本发明的超高频高磁导率低损耗锰锌软磁铁氧体不仅可以取代部分NiZn铁氧体，满足磁性器件对超高频的使用要求，大幅度降低材料成本，还有助于减小器件体积和绕线匝数，减小线损和降低温升，可广泛适用于小型化器件中，为将来器件更加小型化做好材料储备。The ultra-high-frequency high-permeability low-loss manganese-zinc soft magnetic ferrite of the present invention can not only replace part of NiZn ferrite, meet the requirements of magnetic devices for ultra-high frequencies, greatly reduce material costs, but also help reduce The size of the device and the number of winding turns reduce the line loss and temperature rise, and can be widely used in miniaturized devices, making a good material reserve for future device miniaturization.
具体实施方式Detailed ways
下面通过具体的实施案例，对本发明所制备的超高频高磁导率低损耗锰锌软磁铁氧体材料及制备工艺进一步具体说明。根据以下制备方法制备出实施例1和实施例2两种MnZn软磁铁氧体材料以及比较例1、比较例2、比较例3、比较例4四种MnZn软磁铁氧体材料。The ultra-high frequency high magnetic permeability low loss manganese zinc soft ferrite material prepared by the present invention and the preparation process are further specifically described below through specific implementation cases. Two MnZn soft ferrite materials of Example 1 and Example 2 and four MnZn soft ferrite materials of Comparative Example 1, Comparative Example 2, Comparative Example 3 and Comparative Example 4 were prepared according to the following preparation methods.
实施例1：一种超高频高磁导率低损耗锰锌软磁铁氧体，由主成分和辅助成分组成，制备方法如下：Embodiment 1: A manganese-zinc soft magnetic ferrite with high magnetic permeability and low loss at ultra-high frequency is composed of a main component and an auxiliary component. The preparation method is as follows:
步骤1：配料：Fe 2O 3：74.3wt％，ZnO：1.8wt％，MoO 3：0.04wt％和其余的Mn 3O 4配料，然后进行湿法球磨混合，混合时间为15min； Step 1: Ingredients: Fe 2 O 3 : 74.3wt%, ZnO: 1.8wt%, MoO 3 : 0.04wt% and the rest of Mn 3 O 4 ingredients, and then mixed by wet ball milling, the mixing time is 15min;
步骤2：预烧：对步骤1中所得混合料烘干后在进行预烧，预烧温度为900℃，升温速率为5℃/min；Step 2: Pre-burning: pre-burn the mixture obtained in step 1 after drying, the pre-burning temperature is 900°C, and the heating rate is 5°C/min;
步骤3：砂磨：对所得预烧料振磨，然后加入辅助成分：CaCO 3：600ppm、ZrO 2：200ppm、TiO 2：800ppm、Co 2O 3：1800ppm、CuO:50～200ppm，砂磨70min； Step 3: Sanding: vibrating the obtained calcined material, then adding auxiliary components: CaCO 3 : 600ppm, ZrO 2 : 200ppm, TiO 2 : 800ppm, Co 2 O 3 : 1800ppm, CuO: 50-200ppm, sanding for 70min ;
步骤4：造粒：根据研磨后得到粉料总重量，加入15wt％聚乙烯醇，研磨过筛成一定尺寸的颗粒；Step 4: Granulation: according to the total weight of the powder obtained after grinding, add 15wt% polyvinyl alcohol, grind and sieve into particles of a certain size;
步骤5：压制成型：压制成尺寸为Φ12.5mm*Φ7.5mm*7mm环形生坯；Step 5: Press molding: press into a circular green body with a size of Φ12.5mm*Φ7.5mm*7mm;
步骤6：烧结：烧结温度为1120℃，保温时间为6h，平衡氧含量为1.6％；Step 6: Sintering: the sintering temperature is 1120°C, the holding time is 6h, and the equilibrium oxygen content is 1.6%;
步骤7：退火：在真空条件下以一定升温速率升至700℃，保温2h，然后逐渐以一定速率降至室温。Step 7: Annealing: raise the temperature to 700° C. at a certain rate under vacuum conditions, keep it for 2 hours, and then gradually lower it to room temperature at a certain rate.
实施例2：一种超高频高磁导率低损耗锰锌软磁铁氧体材料，由主成分和辅助成分组成，制备方法如下：Embodiment 2: A manganese-zinc soft magnetic ferrite material with high magnetic permeability and low loss at ultra-high frequency, which is composed of main components and auxiliary components, and the preparation method is as follows:
步骤1：配料：Fe 2O 3：74.8wt％，ZnO：2.4wt％，MoO 3：0.04wt％和其余的Mn 3O 4配料，然后进行湿法球磨混合，混合时间为15min； Step 1: Ingredients: Fe 2 O 3 : 74.8wt%, ZnO: 2.4wt%, MoO 3 : 0.04wt% and the rest of Mn 3 O 4 ingredients, and then mixed by wet ball milling, the mixing time is 15min;
步骤2：预烧：对步骤1中所得混合料烘干后在进行预烧，预烧温度为900℃，升温速率为5℃/min；Step 2: Pre-burning: pre-burn the mixture obtained in step 1 after drying, the pre-burning temperature is 900°C, and the heating rate is 5°C/min;
步骤3：砂磨：对所得预烧料振磨，然后加入辅助成分：CaCO 3：600ppm、ZrO 2：200ppm、TiO 2：800ppm、Co 2O 3：1800ppm、CuO:80ppm，砂磨70min； Step 3: sanding: vibrating the obtained calcined material, then adding auxiliary components: CaCO 3 : 600ppm, ZrO 2 : 200ppm, TiO 2 : 800ppm, Co 2 O 3 : 1800ppm, CuO: 80ppm, sanding for 70min;
步骤4：造粒：根据研磨后得到粉料总重量，加入15wt％聚乙烯醇，研磨过筛成一定尺寸的颗粒；Step 4: Granulation: according to the total weight of the powder obtained after grinding, add 15wt% polyvinyl alcohol, grind and sieve into particles of a certain size;
步骤5：压制成型：压制成尺寸为Φ12.5mm*Φ7.5mm*7mm环形生坯；Step 5: Press molding: press into a circular green body with a size of Φ12.5mm*Φ7.5mm*7mm;
步骤6：烧结：烧结温度为1120℃，保温时间为6h，平衡氧含量为1.6％；Step 6: Sintering: the sintering temperature is 1120°C, the holding time is 6h, and the equilibrium oxygen content is 1.6%;
步骤7：退火：在真空条件下以一定升温速率升至700℃，保温2h，然后逐渐以一定速率降至室温。Step 7: Annealing: raise the temperature to 700° C. at a certain rate under vacuum conditions, keep it for 2 hours, and then gradually lower it to room temperature at a certain rate.
实施例3：一种超高频高磁导率低损耗锰锌软磁铁氧体材料，由主成分和辅助成分组成，制备方法如下：Embodiment 3: An ultra-high frequency high magnetic permeability low loss manganese zinc soft magnetic ferrite material is composed of main components and auxiliary components. The preparation method is as follows:
步骤1：配料：Fe 2O 3：75.2wt％，ZnO：2.8wt％，MoO 3：0.03wt％和其余的Mn 3O 4配料，然 后进行湿法球磨混合，混合时间为15min； Step 1: Ingredients: Fe 2 O 3 : 75.2wt%, ZnO: 2.8wt%, MoO 3 : 0.03wt% and the rest of Mn 3 O 4 ingredients, and then mixed by wet ball milling, the mixing time is 15min;
步骤2：预烧：对步骤1中所得混合料烘干后在进行预烧，预烧温度为900℃，升温速率为5℃/min；Step 2: Pre-burning: pre-burn the mixture obtained in step 1 after drying, the pre-burning temperature is 900°C, and the heating rate is 5°C/min;
步骤3：砂磨：对所得预烧料振磨，然后加入辅助成分：CaCO 3：600ppm、ZrO 2：200ppm、TiO 2：800ppm、Co 2O 3：1800ppm、CuO:80ppm，砂磨70min。 Step 3: Sanding: vibrating the obtained calcined material, then adding auxiliary components: CaCO 3 : 600ppm, ZrO 2 : 200ppm, TiO 2 : 800ppm, Co 2 O 3 : 1800ppm, CuO: 80ppm, and sanding for 70min.
步骤4：造粒：根据研磨后得到粉料总重量，加入15wt％聚乙烯醇，研磨过筛成一定尺寸的颗粒；Step 4: Granulation: according to the total weight of the powder obtained after grinding, add 15wt% polyvinyl alcohol, grind and sieve into particles of a certain size;
步骤5：压制成型：压制成尺寸为Φ12.5mm*Φ7.5mm*7mm环形生坯；Step 5: Press molding: press into a circular green body with a size of Φ12.5mm*Φ7.5mm*7mm;
步骤6：烧结：烧结温度为1120℃，保温时间为6h，平衡氧含量为1.6％；Step 6: Sintering: the sintering temperature is 1120°C, the holding time is 6h, and the equilibrium oxygen content is 1.6%;
步骤7：退火：在真空条件下以一定升温速率升至800℃，保温2h，然后逐渐以一定速率降至室温。Step 7: Annealing: raise the temperature to 800° C. at a certain rate under vacuum conditions, keep it for 2 hours, and then gradually lower it to room temperature at a certain rate.
比较例1：一种锰锌软磁铁氧体材料，由主成分和辅助成分组成，制备方法如下：Comparative Example 1: A manganese-zinc soft magnetic ferrite material is composed of a main component and an auxiliary component. The preparation method is as follows:
步骤1：配料：Fe 2O 3：74.3wt％，ZnO：2.2wt％，MoO 3：0.04wt％和其余的Mn 3O 4配料，然后进行湿法球磨混合，混合时间为15min； Step 1: Ingredients: Fe 2 O 3 : 74.3wt%, ZnO: 2.2wt%, MoO 3 : 0.04wt% and the rest of Mn 3 O 4 ingredients, and then mixed by wet ball milling, the mixing time is 15min;
步骤2：预烧：对步骤1中所得混合料烘干后在进行预烧，预烧温度为900℃，升温速率为5℃/min；Step 2: Pre-burning: pre-burn the mixture obtained in step 1 after drying, the pre-burning temperature is 900°C, and the heating rate is 5°C/min;
步骤3：砂磨：对所得预烧料振磨，然后加入辅助成分：CaCO 3：600ppm、ZrO 2：200ppm、TiO 2：800ppm、Co 2O 3：1800ppm、CuO:50～200ppm，砂磨70min； Step 3: Sanding: vibrating the obtained calcined material, then adding auxiliary components: CaCO 3 : 600ppm, ZrO 2 : 200ppm, TiO 2 : 800ppm, Co 2 O 3 : 1800ppm, CuO: 50-200ppm, sanding for 70min ;
步骤4：造粒：根据研磨后得到粉料总重量，加入15wt％聚乙烯醇，研磨过筛成一定尺寸的颗粒；Step 4: Granulation: according to the total weight of the powder obtained after grinding, add 15wt% polyvinyl alcohol, grind and sieve into particles of a certain size;
步骤5：压制成型：压制成尺寸为Φ12.5mm*Φ7.5mm*7mm环形生坯；Step 5: Press molding: press into a circular green body with a size of Φ12.5mm*Φ7.5mm*7mm;
步骤6：烧结：烧结温度为1120℃，保温时间为6h，平衡氧含量为1.6％。Step 6: Sintering: the sintering temperature is 1120° C., the holding time is 6 hours, and the equilibrium oxygen content is 1.6%.
比较例2：一种锰锌软磁铁氧体材料，由主成分和辅助成分组成，制备方法如下：Comparative Example 2: A manganese-zinc soft magnetic ferrite material is composed of a main component and an auxiliary component. The preparation method is as follows:
步骤1：配料：Fe 2O 3：74.6wt％，ZnO：3.4wt％，MoO 3：0.04wt％和其余的Mn 3O 4配料，然后进行湿法球磨混合，混合时间为15min； Step 1: Ingredients: Fe 2 O 3 : 74.6wt%, ZnO: 3.4wt%, MoO 3 : 0.04wt% and the rest of Mn 3 O 4 ingredients, and then mixed by wet ball milling, the mixing time is 15min;
步骤2：预烧：对步骤1中所得混合料烘干后在进行预烧，预烧温度为900℃，升温速率为5℃/min；Step 2: Pre-burning: pre-burn the mixture obtained in step 1 after drying, the pre-burning temperature is 900°C, and the heating rate is 5°C/min;
步骤3：砂磨：对所得预烧料振磨，然后加入辅助成分：CaCO 3：600ppm、ZrO 2：200ppm、TiO 2：800ppm、Co 2O 3：1800ppm、CuO:50～200ppm，砂磨70min； Step 3: Sanding: vibrating the obtained calcined material, then adding auxiliary components: CaCO 3 : 600ppm, ZrO 2 : 200ppm, TiO 2 : 800ppm, Co 2 O 3 : 1800ppm, CuO: 50-200ppm, sanding for 70min ;
步骤4：造粒：根据研磨后得到粉料总重量，加入15wt％聚乙烯醇，研磨过筛成一定尺寸的颗粒；Step 4: Granulation: according to the total weight of the powder obtained after grinding, add 15wt% polyvinyl alcohol, grind and sieve into particles of a certain size;
步骤5：压制成型：压制成尺寸为Φ12.5mm*Φ7.5mm*7mm环形生坯；Step 5: Press molding: press into a circular green body with a size of Φ12.5mm*Φ7.5mm*7mm;
步骤6：烧结：烧结温度为1120℃，保温时间为6h，平衡氧含量为1.6％；Step 6: Sintering: the sintering temperature is 1120°C, the holding time is 6h, and the equilibrium oxygen content is 1.6%;
步骤7：退火：在真空条件下以一定升温速率升至700℃，保温2h，然后逐渐以一定速率降至室温。Step 7: Annealing: raise the temperature to 700° C. at a certain rate under vacuum conditions, keep it for 2 hours, and then gradually lower it to room temperature at a certain rate.
比较例3：一种锰锌软磁铁氧体材料，由主成分和辅助成分组成，制备方法如下：Comparative Example 3: A manganese-zinc soft magnetic ferrite material is composed of a main component and an auxiliary component. The preparation method is as follows:
步骤1：配料：Fe 2O 3：74.3wt％，ZnO：1.8wt％，其余为Mn 3O 4配料，然后进行湿法球磨混合，混合时间为15min； Step 1: Ingredients: Fe 2 O 3 : 74.3wt%, ZnO: 1.8wt%, the rest is Mn 3 O 4 ingredients, and then mixed by wet ball milling, the mixing time is 15min;
步骤2：预烧：对步骤1中所得混合料烘干后在进行预烧，预烧温度为900℃，升温速率为5℃/min；Step 2: Pre-burning: pre-burn the mixture obtained in step 1 after drying, the pre-burning temperature is 900°C, and the heating rate is 5°C/min;
步骤3：砂磨：对所得预烧料振磨，然后加入辅助成分：CaCO 3：600ppm、ZrO 2：200ppm、TiO 2：800ppm、Co 2O 3：1800ppm、CuO:50～200ppm，砂磨70min； Step 3: Sanding: vibrating the obtained calcined material, then adding auxiliary components: CaCO 3 : 600ppm, ZrO 2 : 200ppm, TiO 2 : 800ppm, Co 2 O 3 : 1800ppm, CuO: 50-200ppm, sanding for 70min ;
步骤4：造粒：根据研磨后得到粉料总重量，加入15wt％聚乙烯醇，研磨过筛成一定尺寸的颗粒；Step 4: Granulation: according to the total weight of the powder obtained after grinding, add 15wt% polyvinyl alcohol, grind and sieve into particles of a certain size;
步骤5：压制成型：压制成尺寸为Φ12.5mm*Φ7.5mm*7mm环形生坯；Step 5: Press molding: press into a circular green body with a size of Φ12.5mm*Φ7.5mm*7mm;
步骤6：烧结：烧结温度为1120℃，保温时间为6h，平衡氧含量为1.6％；Step 6: Sintering: the sintering temperature is 1120°C, the holding time is 6h, and the equilibrium oxygen content is 1.6%;
步骤7：退火：在真空条件下以一定升温速率升至700℃，保温2h，然后逐渐以一定速率降至室温。Step 7: Annealing: raise the temperature to 700° C. at a certain rate under vacuum conditions, keep it for 2 hours, and then gradually lower it to room temperature at a certain rate.
比较例4：一种锰锌软磁铁氧体材料，由主成分和辅助成分组成，制备方法如下：Comparative Example 4: A manganese-zinc soft magnetic ferrite material is composed of a main component and an auxiliary component. The preparation method is as follows:
步骤1：配料：Fe 2O 3：74.6wt％，ZnO：3.4wt％，MoO 3：0.04wt％和其余的Mn 3O 4配料，然后进行湿法球磨混合，混合时间为15min； Step 1: Ingredients: Fe 2 O 3 : 74.6wt%, ZnO: 3.4wt%, MoO 3 : 0.04wt% and the rest of Mn 3 O 4 ingredients, and then mixed by wet ball milling, the mixing time is 15min;
步骤2：预烧：对步骤1中所得混合料烘干后在进行预烧，预烧温度为900℃，升温速率为5℃/min；Step 2: Pre-burning: pre-burn the mixture obtained in step 1 after drying, the pre-burning temperature is 900°C, and the heating rate is 5°C/min;
步骤3：砂磨：对所得预烧料振磨，然后加入辅助成分：CaCO 3：600ppm、ZrO 2：200ppm、TiO 2：800ppm、Co 2O 3：1800ppm、CuO:50～200ppm，砂磨70min； Step 3: Sanding: vibrating the obtained calcined material, then adding auxiliary components: CaCO 3 : 600ppm, ZrO 2 : 200ppm, TiO 2 : 800ppm, Co 2 O 3 : 1800ppm, CuO: 50-200ppm, sanding for 70min ;
步骤4：造粒：根据研磨后得到粉料总重量，加入15wt％聚乙烯醇，研磨过筛成一定尺寸的颗粒；Step 4: Granulation: according to the total weight of the powder obtained after grinding, add 15wt% polyvinyl alcohol, grind and sieve into particles of a certain size;
步骤5：压制成型：压制成尺寸为Φ12.5mm*Φ7.5mm*7mm环形生坯，密度为3.2g/cm 3； Step 5: Press forming: press into a circular green body with a size of Φ12.5mm*Φ7.5mm*7mm, and a density of 3.2g/cm 3 ;
步骤6：烧结：烧结温度为1120℃，保温时间为6h，平衡氧含量为1.6％。Step 6: Sintering: the sintering temperature is 1120° C., the holding time is 6 hours, and the equilibrium oxygen content is 1.6%.
实施例与比较例测试磁性能如下表：Embodiment and comparative example test magnetic properties are as follows table:
Figure PCTCN2021134490-appb-000001
Figure PCTCN2021134490-appb-000001
从表中可以得到：实施例1、2和3根据本发明的制作方式，得到最佳磁性能。将比较例1 和实施例进行对比，或者将比较例2和比较例4进行对比，均可以得到经过退火工艺处理，磁导率明显升高，损耗也有所降低。将比较例2和实施例对比表明，当主配方Zn含量较低时，高频损耗明显降低。将比较例3和实施例比较表明，当主配方添加MoO 3时，磁导率升高，高频损耗降低。 It can be obtained from the table: Examples 1, 2 and 3 obtain the best magnetic properties according to the manufacturing method of the present invention. Comparing the comparative example 1 with the embodiment, or comparing the comparative example 2 with the comparative example 4, it can be obtained that after the annealing process, the magnetic permeability is obviously increased and the loss is also reduced. Comparing Comparative Example 2 with Examples shows that when the main formula Zn content is low, the high frequency loss is significantly reduced. Comparing Comparative Example 3 with Examples shows that when MoO3 is added to the main formula, the magnetic permeability increases and the high-frequency loss decreases.

Claims (4)

  1. 一种超高频高磁导率低损耗锰锌软磁铁氧体，其特征在于，所述超高频高磁导率低损耗锰锌软磁铁氧体材料包含主成分和辅助成分，其中，所述主成分包括Fe 2O 3：73.5～76.5wt％，ZnO：0～3.0wt％，MoO 3：0.01～0.04wt％，其余为Mn 3O 4，按主成分总重量计，所述辅助成分包括：CaCO 3：400～600ppm、ZrO 2：100～300ppm、TiO 2：500～800ppm、Co 2O 3：1500～4000ppm、CuO:50～200ppm， An ultra-high-frequency high-permeability low-loss manganese-zinc soft magnetic ferrite is characterized in that the ultra-high-frequency high-permeability low-loss manganese-zinc soft magnetic ferrite material includes a main component and an auxiliary component, wherein the The main components include Fe 2 O 3 : 73.5-76.5 wt%, ZnO: 0-3.0 wt%, MoO 3 : 0.01-0.04 wt%, and the rest is Mn 3 O 4 , based on the total weight of the main components, the auxiliary components Including: CaCO 3 : 400-600ppm, ZrO 2 : 100-300ppm, TiO 2 : 500-800ppm, Co 2 O 3 : 1500-4000ppm, CuO: 50-200ppm,
    一种超高频高磁导率低损耗锰锌软磁铁氧体的制备方法包括以下步骤：A preparation method of ultra-high-frequency high-permeability low-loss manganese-zinc soft magnetic ferrite comprises the following steps:
    步骤1：配料：按照比例称重Fe 2O 3、ZnO、MoO 3、Mn 3O 4，然后进行湿法砂磨混合，混合时间为10～20min； Step 1: Ingredients: Weigh Fe 2 O 3 , ZnO, MoO 3 , Mn 3 O 4 according to the proportion, then carry out wet sanding and mixing, and the mixing time is 10-20 minutes;
    步骤2：预烧：对步骤1中所得混合料烘干后进行预烧，在空气中进行预烧，预烧温度为800～1000℃，升温速率为3～5℃/min；Step 2: Pre-burning: Pre-burning the mixture obtained in step 1 after drying, and pre-burning in the air, the pre-burning temperature is 800-1000°C, and the heating rate is 3-5°C/min;
    步骤3：砂磨：对步骤2所得预烧料振磨，然后按照比例加入辅助成分：CaCO 3、ZrO 2、TiO 2、Co 2O 3、CuO，砂磨且砂磨时间是30～90min； Step 3: Sanding: vibrate and grind the calcined material obtained in Step 2, and then add auxiliary components according to the proportion: CaCO 3 , ZrO 2 , TiO 2 , Co 2 O 3 , CuO, sanding and the sanding time is 30-90 minutes;
    步骤4：造粒：对砂磨后的料浆烘干并造粒；Step 4: Granulating: drying and granulating the slurry after sanding;
    步骤5：压制成型：压制成尺寸为Φ12.5mm*Φ7.5mm*7mm环形生坯；Step 5: Press molding: press into a circular green body with a size of Φ12.5mm*Φ7.5mm*7mm;
    步骤6：烧结，烧结温度为1000～1200℃，保温时间为4～8h，平衡氧含量为1.5～3.0％；Step 6: sintering, the sintering temperature is 1000-1200°C, the holding time is 4-8 hours, and the equilibrium oxygen content is 1.5-3.0%;
    步骤7：退火，对烧成产品在真空条件下做退火处理，是在真空条件下升温至600～900℃，保温2～4h。Step 7: annealing, the annealing treatment is performed on the fired product under vacuum condition, and the temperature is raised to 600-900° C. under vacuum condition, and the temperature is kept for 2-4 hours.
  2. 根据权利要求1所述超高频高磁导率低损耗锰锌软磁铁氧体，其特征在于，所述主成分包括Fe 2O 3：74.0～75.5wt％，ZnO：1.4～3.0wt％，MoO 3：0.03～0.04wt％，其余为Mn 3O 4；辅助成分：CaCO 3：400～600ppm、ZrO 2：100～300ppm、TiO 2：500～800ppm、Co 2O 3：1500～2000ppm、CuO:50～200ppm。 According to the ultra-high frequency high magnetic permeability and low loss manganese zinc soft magnetic ferrite according to claim 1, it is characterized in that the main components include Fe2O3 : 74.0-75.5wt%, ZnO: 1.4-3.0wt%, MoO 3 : 0.03～0.04wt%, the rest is Mn 3 O 4 ; auxiliary components: CaCO 3 : 400～600ppm, ZrO 2 : 100～300ppm, TiO 2 : 500～800ppm, Co 2 O 3 : 1500～2000ppm, CuO :50～200ppm.
  3. 根据权利要求1-2任一所述超高频高磁导率低损耗锰锌软磁铁氧体，其特征在于，所述步骤6中的烧结温度为1050～1150℃，烧结后的晶粒尺寸为2～4μm。According to any one of claims 1-2, the ultra-high-frequency high-permeability low-loss manganese-zinc soft magnetic ferrite is characterized in that the sintering temperature in the step 6 is 1050-1150°C, and the grain size after sintering 2 to 4 μm.
  4. 根据权利要求1-2任一所述超高频高磁导率低损耗锰锌软磁铁氧体，其特征在于，所述步骤7中，退火处理过程中，先以3～5℃/min升温至250～400℃，保温30～60min，然后以1～3℃/min升温至600～900℃，保温2～4h，然后以1～3℃/min降温至300～500℃，最后以5～8℃/min降温至室温。According to any one of claims 1-2, the ultra-high frequency, high magnetic permeability and low loss manganese zinc soft magnetic ferrite is characterized in that, in the step 7, during the annealing process, the temperature is first raised at 3-5°C/min to 250-400°C, keep warm for 30-60min, then raise the temperature to 600-900°C at 1-3°C/min, keep warm for 2-4h, then cool down to 300-500°C at 1-3°C/min, and finally at 5-3°C Cool down to room temperature at 8°C/min.
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