WO2021017216A1 - High-frequency low-hysteresis manganese-zinc soft ferrite material and preparation method therefor - Google Patents
High-frequency low-hysteresis manganese-zinc soft ferrite material and preparation method therefor Download PDFInfo
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- WO2021017216A1 WO2021017216A1 PCT/CN2019/113527 CN2019113527W WO2021017216A1 WO 2021017216 A1 WO2021017216 A1 WO 2021017216A1 CN 2019113527 W CN2019113527 W CN 2019113527W WO 2021017216 A1 WO2021017216 A1 WO 2021017216A1
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
- H01F1/34—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials non-metallic substances, e.g. ferrites
- H01F1/36—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials non-metallic substances, e.g. ferrites in the form of particles
- H01F1/37—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials non-metallic substances, e.g. ferrites in the form of particles in a bonding agent
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
Definitions
- the invention relates to the technical field of magnetic materials, in particular to a high-frequency low-hysteresis manganese-zinc soft ferrite material and a preparation method thereof.
- Soft ferrite and magnetic components made of it are the core of various inductors, electronic transformers, chokes, suppressors and filters, and have been widely used in automatic control, automotive electronics, aerospace, household appliances, and computers , Ships, communication electronics, green energy, military equipment and other fields, covering all aspects of national economy, people's death and national defense. Soft ferrite devices mainly play the role of power transformation, anti-electromagnetic interference and signal processing in these fields.
- the initial permeability has a high-frequency transmission delay.
- the purpose of the present invention is to provide a high-frequency low-hysteresis manganese-zinc soft ferrite material and its preparation method in view of the defects and deficiencies of the prior art. It has good temperature stability, low hysteresis loss and initial permeability
- the application rate is high, which is beneficial to reduce waveform distortion during signal transmission, reduce transmission errors, extend transmission distance and solve high-frequency transmission delay problems, and meet the application requirements of current high-speed network broadband access technology.
- a high frequency low hysteresis manganese zinc soft ferrite material and a preparation method thereof which are composed of the following parts by weight of raw materials: anisotropic neodymium iron boron magnetic powder 60 ⁇ 90 parts, anisotropic samarium cobalt magnetic powder 5-40 parts, anisotropic strontium ferrite magnetic powder 0.5-15 parts, iron oxide 20-25 parts, bismuth oxide 15-25 parts, nickel oxide 12-17 parts, oxide Titanium 10-17 parts, silicon dioxide 11-17 parts, niobium oxide 4-7 parts, tantalum oxide 4-6 parts, graphene 13-19 parts, epoxy resin 8-11 parts, manganese oxide 3-5 parts, 2.5 to 3.5 parts of cobalt oxide, 12 to 14 parts of calcium carbonate, 2 to 3 parts of dispersant, 5 to 7 parts of binder, 1 to 2 parts of wetting agent, 13-17 parts of polyvinyl alcohol, hexadecyl three 0.5
- the particle size of the anisotropic neodymium iron boron magnetic powder is controlled within 30-240 ⁇ m.
- the particle size of the anisotropic samarium cobalt magnetic powder is less than 80 ⁇ m.
- the particle size of the anisotropic strontium ferrite magnetic powder is less than 10 ⁇ m.
- the preparation method includes powder preparation, bonding magnetic powder preparation, warm-pressing molding, primary demagnetization, cooling demolding, and secondary demagnetization and solidification steps.
- a given mold is used in the warm press forming process of the junction magnet, and each process is described as follows:
- Powder preparation Weigh anisotropic neodymium iron boron magnetic powder 60-90 with a particle size of 30-240 ⁇ m, anisotropic samarium cobalt magnetic powder 5-40 with a particle size of less than 80 ⁇ m, and anisotropic strontium with a particle size of less than 10 ⁇ m. Ferrite magnetic powder 0.5 ⁇ 15 are put into the blender and mixed evenly to obtain mixed magnetic powder;
- Preparation of bonded magnetic powder Weigh 100 parts by weight of the mixed magnetic powder and add 0.5-10 parts by weight of thermosetting resin and 0.01-3 parts by weight of zinc stearate, and continue to stir evenly at room temperature to 120°C to obtain a sticky Magnetic powder
- thermosetting resin is bisphenol A type epoxy resin, or phenolic type epoxy resin, or thermosetting phenolic resin;
- Warm pressure molding Put the prepared bonded magnetic powder into a mold, and perform warm pressure molding on the bonded magnetic powder under a positive magnetic field strength> 10.0KGs at 60-180°C. Control at 200 ⁇ 500MPa, control the holding time of warm press molding at 0.1 ⁇ 60s, and obtain bonded magnets in the mold after warm press molding;
- One-time demagnetization demagnetize the bonded magnet with a reverse magnetic field, and the reverse magnetic field strength is controlled at 1.0KGs ⁇ 20.0KGs;
- Cooling and demolding cooling the bonded magnet after one demagnetization, using air cooling or water cooling, after 5-10 seconds of air cooling or water cooling, eject the bonded magnet from the mold for demolding, demolding The time is controlled within 10 ⁇ 180s;
- Secondary demagnetization and solidification Put the demolded bonded magnet into an oscillating pulsed magnetic field for secondary demagnetization.
- the maximum peak value of the oscillating pulsed magnetic field is> 20.0KGs.
- the maximum surface magnetism is less than 50Gs, and then the bonded magnet after the secondary demagnetization is put into an oven and cured at 100-180°C for 0.5-2h to prepare the magnet.
- the present invention has the following beneficial effects: it has good temperature stability, low hysteresis loss, high initial permeability, and is beneficial to reduce waveform distortion in the signal transmission process, reduce transmission errors, and extend transmission. Distance and solve the problem of high-frequency transmission delay to meet the application requirements of current high-speed network broadband access technology.
- a high-frequency low-hysteresis manganese-zinc soft ferrite material and a preparation method thereof which are composed of the following parts by weight of raw materials: 60 parts of anisotropic neodymium iron boron magnetic powder, 5 parts of anisotropic samarium cobalt magnetic powder; Anisotropic strontium ferrite magnetic powder 0.5 parts, iron oxide 20 parts, bismuth oxide 15 parts, nickel oxide 12 parts, titanium oxide 10 parts, silicon dioxide 11 parts, niobium oxide 4 parts, tantalum oxide 4 parts, graphene 13 parts, 8 parts of epoxy resin, 3 parts of manganese oxide, 2.5 parts of cobalt oxide, 12 parts of calcium carbonate, 2 parts of dispersant, 5 parts of adhesive, 1 part of wetting agent, 0.5 part of cetyltrimethylammonium bromide , 0.1 part of polydimethylsiloxane, 0.6 part of magnesium stearate, 75 parts of water.
- the preparation method includes powder preparation, bonding magnetic powder preparation, warm-pressing molding, primary demagnetization, cooling demolding, and secondary demagnetization and solidification steps.
- a given mold is used in the warm press forming process of the junction magnet, and each process is described as follows:
- Powder preparation Weigh anisotropic neodymium iron boron magnetic powder 60-90 with a particle size of 30-240 ⁇ m, anisotropic samarium cobalt magnetic powder 5-40 with a particle size of less than 80 ⁇ m, and anisotropic strontium with a particle size of less than 10 ⁇ m. Ferrite magnetic powder 0.5 ⁇ 15 are put into the blender and mixed evenly to obtain mixed magnetic powder;
- Preparation of bonded magnetic powder Weigh 100 parts by weight of the mixed magnetic powder and add 0.5-10 parts by weight of thermosetting resin and 0.01-3 parts by weight of zinc stearate, and continue to stir evenly at room temperature to 120°C to obtain a sticky Magnetic powder
- thermosetting resin is bisphenol A type epoxy resin, or phenolic type epoxy resin, or thermosetting phenolic resin;
- Warm pressure molding Put the prepared bonded magnetic powder into a mold, and perform warm pressure molding on the bonded magnetic powder under a positive magnetic field strength> 10.0KGs at 60-180°C. Control at 200 ⁇ 500MPa, control the holding time of warm press molding at 0.1 ⁇ 60s, and obtain bonded magnets in the mold after warm press molding;
- One-time demagnetization demagnetize the bonded magnet with a reverse magnetic field, and the reverse magnetic field strength is controlled at 1.0KGs ⁇ 20.0KGs;
- Cooling and demolding cooling the bonded magnet after one demagnetization, using air cooling or water cooling, after 5-10 seconds of air cooling or water cooling, eject the bonded magnet from the mold for demolding, demolding The time is controlled within 10 ⁇ 180s;
- Secondary demagnetization and solidification Put the demolded bonded magnet into an oscillating pulsed magnetic field for secondary demagnetization.
- the maximum peak value of the oscillating pulsed magnetic field is> 20.0KGs.
- the maximum surface magnetism is less than 50Gs, and then the bonded magnet after the secondary demagnetization is put into an oven and cured at 100-180°C for 0.5-2h to prepare the magnet.
- this embodiment is composed of the following parts by weight of raw materials: 65 parts of anisotropic neodymium iron boron magnetic powder, 25 parts of anisotropic samarium cobalt magnetic powder; anisotropic strontium ferrite magnetic powder 5 Parts, iron oxide 25 parts, bismuth oxide 18 parts, nickel oxide 15 parts, titanium oxide 12 parts, silica 15 parts, niobium oxide 5 parts, tantalum oxide 5 parts, graphene 15 parts, epoxy resin 9 parts, oxide 4 parts of manganese, 3 parts of cobalt oxide, 13 parts of calcium carbonate, 2.5 parts of dispersant, 6 parts of binder, 2 parts of wetting agent, 0.6 part of cetyltrimethylammonium bromide, polydimethylsiloxane 0.2 parts of alkane, 0.7 parts of magnesium stearate, and 80 parts of water.
- this embodiment is composed of the following parts by weight of raw materials: 90 parts of anisotropic neodymium iron boron magnetic powder, 40 parts of anisotropic samarium cobalt magnetic powder; 15 parts of anisotropic strontium ferrite magnetic powder Parts, iron oxide 25 parts, bismuth oxide 25 parts, nickel oxide 17 parts, titanium oxide 12 parts, silicon dioxide 15 parts, niobium oxide 7 parts, tantalum oxide 6 parts, graphene 19 parts, epoxy resin 11 parts, oxide 5 parts manganese, 3.5 parts cobalt oxide, 14 parts calcium carbonate, 3 parts dispersant, 7 parts binder, 2 parts wetting agent, 0.7 parts cetyltrimethylammonium bromide, polydimethylsiloxane 0.3 parts of alkane, 0.8 parts of magnesium stearate, 85 parts of water.
- the present invention has the following beneficial effects: it has good temperature stability, low hysteresis loss, high initial permeability, and is beneficial to reduce waveform distortion in the signal transmission process, reduce transmission errors, and extend transmission. Distance and solve the problem of high-frequency transmission delay to meet the application requirements of current high-speed network broadband access technology.
Abstract
A high-frequency low-hysteresis manganese-zinc soft ferrite material and a preparation method therefor, which pertain to the technical field of magnetic materials. The material is composed of the following raw materials: an anisotropic neodymium iron boron magnetic powder, an anisotropic samarium cobalt magnetic powder, an anisotropic strontium ferrite powder, iron oxide, bismuth oxide, nickel oxide, titanium oxide, silicon dioxide, niobium oxide, tantalum oxide, graphene, an epoxy resin, manganese oxide, cobalt oxide, calcium carbonate, a dispersant, an adhesive, a wetter, polyvinyl alcohol, cetyltrimethylammonium bromide, polydimethylsiloxane, magnesium stearate, and water. The preparation can be accomplished by obtaining the above raw materials according to measured quantity ratios and performing processing according to the high-frequency low-hysteresis manganese-zinc soft ferrite material and the preparation method therefor. The present invention has the following beneficial effects: the material has good temperature stability, low hysteresis loss, and high initial magnetic permeability, and when applied, is conducive to reducing waveform distortion during signal transmission, reducing transmission errors, extending transmission distances, and resolving the high-frequency transmission delay problem.
Description
本发明涉及磁性材料技术领域，具体涉及一种高频低磁滞锰锌软磁铁氧体材料及其制备方法。The invention relates to the technical field of magnetic materials, in particular to a high-frequency low-hysteresis manganese-zinc soft ferrite material and a preparation method thereof.
软磁铁氧体及以其制成的磁性元件作为各种电感器、电子变压器、扼流圈、抑制器和滤波器的核心，已广泛应用于自动控制、汽车电子、航空航天、家用电器、计算机、船舶、通信电子、绿色能源、军用设备等领域，遍及国计民生和国防领域的各个方面，软磁铁氧体器件在这些领域中主要起功率变压、抗电磁干扰及信号处理等作用。Soft ferrite and magnetic components made of it are the core of various inductors, electronic transformers, chokes, suppressors and filters, and have been widely used in automatic control, automotive electronics, aerospace, household appliances, and computers , Ships, communication electronics, green energy, military equipment and other fields, covering all aspects of national economy, people's livelihood and national defense. Soft ferrite devices mainly play the role of power transformation, anti-electromagnetic interference and signal processing in these fields.
近年来，随着互联网的快速发展及全球经济信息化的进程加快，世界各地都掀起新的宽带网络的建设热潮。由于调制解调技术的提高、快速数字信号处理芯片生产技术的进步，出现了以快速数字信号处理技术和先进调制解调技术相结合的新的接入方式，如不对称数字用户环线技术、高速数字用户环线和电缆调制解调技术等。在这些宽带接入技术中，需要应用到大量宽带变压器来实现物理隔离、阻抗匹配、带通滤波等功能。In recent years, with the rapid development of the Internet and the accelerating process of global economic informatization, new broadband networks have been built up all over the world. Due to the improvement of modem technology and the advancement of fast digital signal processing chip production technology, new access methods combining fast digital signal processing technology and advanced modem technology have emerged, such as asymmetric digital subscriber loop technology, high-speed Digital subscriber loop and cable modem technology, etc. In these broadband access technologies, a large number of broadband transformers need to be applied to achieve functions such as physical isolation, impedance matching, and band-pass filtering.
通讯宽带变压器的核心器件——软磁铁氧体磁心在磁化场的作用下运行时，磁感应强度B和外加磁场H的非线性关系引发的信号失真现象直接导致谐波失真，继而引发信号传输过程中出现波形失真、传输错误、传输距离短等现象。另外，由于原始配方的不同，使得起始磁导率，出现高频传输延时现象。When the core component of the communication broadband transformer-the soft ferrite core is operating under the action of the magnetizing field, the signal distortion caused by the nonlinear relationship between the magnetic induction B and the external magnetic field H directly leads to harmonic distortion, which in turn leads to signal transmission. Phenomena such as waveform distortion, transmission error, and short transmission distance occur. In addition, due to the difference in the original formula, the initial permeability has a high-frequency transmission delay.
发明内容Summary of the invention
本发明的目的在于针对现有技术的缺陷和不足，提供一种高频低磁滞锰锌软磁铁氧体材料及其制备方法，它具有温度稳定性好，磁滞损耗小，起始磁导率高，在应用有利于降低在信号传输过程中波形失真、减少传输错误、 延长传输距离和解决高频传输延时问题，满足当前高速网络宽带接入技术的应用需求。The purpose of the present invention is to provide a high-frequency low-hysteresis manganese-zinc soft ferrite material and its preparation method in view of the defects and deficiencies of the prior art. It has good temperature stability, low hysteresis loss and initial permeability The application rate is high, which is beneficial to reduce waveform distortion during signal transmission, reduce transmission errors, extend transmission distance and solve high-frequency transmission delay problems, and meet the application requirements of current high-speed network broadband access technology.
为实现上述目的，本发明采用以下技术方案是：一种高频低磁滞锰锌软磁铁氧体材料及其制备方法，它由以下重量份数的原料组成：各向异性钕铁硼磁粉60～90份、各向异性钐钴磁粉5～40份、各向异性锶铁氧体磁粉0.5～15份、氧化铁20～25份、氧化铋15～25份、氧化镍12～17份、氧化钛10～17份、二氧化硅11～17份、氧化铌4～7份、氧化钽4～6份、石墨烯13～19份、环氧树脂8～11份、氧化锰3～5份、氧化钴2.5～3.5份、碳酸钙12～14份、分散剂2～3份、粘合剂5～7份、润湿剂1～2份、聚乙烯醇13-17份、十六烷基三甲基溴化铵0.5-0.7份，聚二甲基硅氧烷0.1-0.3份，硬脂酸镁0.6-0.8份，水75-85份。In order to achieve the above objective, the present invention adopts the following technical solutions: a high frequency low hysteresis manganese zinc soft ferrite material and a preparation method thereof, which are composed of the following parts by weight of raw materials: anisotropic neodymium iron boron magnetic powder 60 ～90 parts, anisotropic samarium cobalt magnetic powder 5-40 parts, anisotropic strontium ferrite magnetic powder 0.5-15 parts, iron oxide 20-25 parts, bismuth oxide 15-25 parts, nickel oxide 12-17 parts, oxide Titanium 10-17 parts, silicon dioxide 11-17 parts, niobium oxide 4-7 parts, tantalum oxide 4-6 parts, graphene 13-19 parts, epoxy resin 8-11 parts, manganese oxide 3-5 parts, 2.5 to 3.5 parts of cobalt oxide, 12 to 14 parts of calcium carbonate, 2 to 3 parts of dispersant, 5 to 7 parts of binder, 1 to 2 parts of wetting agent, 13-17 parts of polyvinyl alcohol, hexadecyl three 0.5-0.7 parts of methyl ammonium bromide, 0.1-0.3 parts of polydimethylsiloxane, 0.6-0.8 parts of magnesium stearate, 75-85 parts of water.
所述的各向异性钕铁硼磁粉的粒径控制在30～240μm。The particle size of the anisotropic neodymium iron boron magnetic powder is controlled within 30-240 μm.
所述的各向异性钐钴磁粉的粒径小于80μm。The particle size of the anisotropic samarium cobalt magnetic powder is less than 80 μm.
所述的各向异性锶铁氧体磁粉的粒径小于10μm。The particle size of the anisotropic strontium ferrite magnetic powder is less than 10 μm.
一种高频低磁滞锰锌软磁铁氧体材料及其制备方法，该制备方法包括配粉、粘结磁粉配制、温压成型、一次退磁、冷却脱模、二次退磁固化工序，其中粘结磁体温压成型工序中使用到给定模具，各工序分述如下：A high-frequency low-hysteresis manganese-zinc soft ferrite material and a preparation method thereof. The preparation method includes powder preparation, bonding magnetic powder preparation, warm-pressing molding, primary demagnetization, cooling demolding, and secondary demagnetization and solidification steps. A given mold is used in the warm press forming process of the junction magnet, and each process is described as follows:
配粉：按重量份分别称取粒径30～240μm的各向异性钕铁硼磁粉60～90、粒径小于80μm的各向异性钐钴磁粉5～40及粒径小于10μm的各向异性锶铁氧体磁粉0.5～15一同放入搅拌机中搅拌均匀并得到混合磁粉；Powder preparation: Weigh anisotropic neodymium iron boron magnetic powder 60-90 with a particle size of 30-240μm, anisotropic samarium cobalt magnetic powder 5-40 with a particle size of less than 80μm, and anisotropic strontium with a particle size of less than 10μm. Ferrite magnetic powder 0.5～15 are put into the blender and mixed evenly to obtain mixed magnetic powder;
粘结磁粉配制：称取所述混合磁粉100重量份并加入0.5～10重量份的热固性树脂和0.01～3重量份的硬脂酸锌，在室温～120℃的温度下继续搅拌均匀并得到粘结磁粉；Preparation of bonded magnetic powder: Weigh 100 parts by weight of the mixed magnetic powder and add 0.5-10 parts by weight of thermosetting resin and 0.01-3 parts by weight of zinc stearate, and continue to stir evenly at room temperature to 120°C to obtain a sticky Magnetic powder
上述热固性树脂是双酚A型环氧树脂，或是酚醛型环氧树脂，或是热固性酚醛树脂；The above-mentioned thermosetting resin is bisphenol A type epoxy resin, or phenolic type epoxy resin, or thermosetting phenolic resin;
温压成型：将配制好的所述粘结磁粉装入模具中，在正向磁场强度＞10.0KGs下并在60～180℃内对所述粘结磁粉进行温压成型，温压成型的压力 控制在200～500MPa，温压成型的保压时间控制在0.1～60s，温压成型后得到模具中的粘结磁体；Warm pressure molding: Put the prepared bonded magnetic powder into a mold, and perform warm pressure molding on the bonded magnetic powder under a positive magnetic field strength> 10.0KGs at 60-180°C. Control at 200～500MPa, control the holding time of warm press molding at 0.1～60s, and obtain bonded magnets in the mold after warm press molding;
一次退磁：对所述粘结磁体进行反向磁场退磁，所述反向磁场强度控制在1.0KGs～20.0KGs；One-time demagnetization: demagnetize the bonded magnet with a reverse magnetic field, and the reverse magnetic field strength is controlled at 1.0KGs～20.0KGs;
冷却脱模：对一次退磁后的所述粘结磁体进行冷却，冷却采用风冷或是水冷，待风冷或是水冷5～10s后将所述粘结磁体顶出模具进行脱模，脱模时间控制在10～180s内；Cooling and demolding: cooling the bonded magnet after one demagnetization, using air cooling or water cooling, after 5-10 seconds of air cooling or water cooling, eject the bonded magnet from the mold for demolding, demolding The time is controlled within 10～180s;
二次退磁固化：将脱模后的所述粘结磁体放入振荡脉冲磁场中进行二次退磁，所述振荡脉冲磁场的强度最大峰值＞20.0KGs，要求二次退磁后所述粘结磁体的最大表磁＜50Gs，然后将二次退磁后的所述粘结磁体放入烘箱中，并在100～180℃内固化0.5～2h后即制备出磁体。Secondary demagnetization and solidification: Put the demolded bonded magnet into an oscillating pulsed magnetic field for secondary demagnetization. The maximum peak value of the oscillating pulsed magnetic field is> 20.0KGs. The maximum surface magnetism is less than 50Gs, and then the bonded magnet after the secondary demagnetization is put into an oven and cured at 100-180°C for 0.5-2h to prepare the magnet.
采用上述技术方案后，本发明有益效果为：它具有温度稳定性好，磁滞损耗小，起始磁导率高，在应用有利于降低在信号传输过程中波形失真、减少传输错误、延长传输距离和解决高频传输延时问题，满足当前高速网络宽带接入技术的应用需求。After adopting the above technical solution, the present invention has the following beneficial effects: it has good temperature stability, low hysteresis loss, high initial permeability, and is beneficial to reduce waveform distortion in the signal transmission process, reduce transmission errors, and extend transmission. Distance and solve the problem of high-frequency transmission delay to meet the application requirements of current high-speed network broadband access technology.
实施例1Example 1
一种高频低磁滞锰锌软磁铁氧体材料及其制备方法，它由以下重量份数的原料组成：各向异性钕铁硼磁粉60份、各向异性钐钴磁粉5份；各向异性锶铁氧体磁粉0.5份、氧化铁20份、氧化铋15份、氧化镍12份、氧化钛10份、二氧化硅11份、氧化铌4份、氧化钽4份、石墨烯13份、环氧树脂8份、氧化锰3份、氧化钴2.5份、碳酸钙12份、分散剂2份、粘合剂5份、润湿剂1份、十六烷基三甲基溴化铵0.5份、聚二甲基硅氧烷0.1份、硬脂酸镁0.6份、水75份。A high-frequency low-hysteresis manganese-zinc soft ferrite material and a preparation method thereof, which are composed of the following parts by weight of raw materials: 60 parts of anisotropic neodymium iron boron magnetic powder, 5 parts of anisotropic samarium cobalt magnetic powder; Anisotropic strontium ferrite magnetic powder 0.5 parts, iron oxide 20 parts, bismuth oxide 15 parts, nickel oxide 12 parts, titanium oxide 10 parts, silicon dioxide 11 parts, niobium oxide 4 parts, tantalum oxide 4 parts, graphene 13 parts, 8 parts of epoxy resin, 3 parts of manganese oxide, 2.5 parts of cobalt oxide, 12 parts of calcium carbonate, 2 parts of dispersant, 5 parts of adhesive, 1 part of wetting agent, 0.5 part of cetyltrimethylammonium bromide , 0.1 part of polydimethylsiloxane, 0.6 part of magnesium stearate, 75 parts of water.
一种高频低磁滞锰锌软磁铁氧体材料及其制备方法，该制备方法包括配粉、粘结磁粉配制、温压成型、一次退磁、冷却脱模、二次退磁固化工序，其中粘结磁体温压成型工序中使用到给定模具，各工序分述如下：A high-frequency low-hysteresis manganese-zinc soft ferrite material and a preparation method thereof. The preparation method includes powder preparation, bonding magnetic powder preparation, warm-pressing molding, primary demagnetization, cooling demolding, and secondary demagnetization and solidification steps. A given mold is used in the warm press forming process of the junction magnet, and each process is described as follows:
配粉：按重量份分别称取粒径30～240μm的各向异性钕铁硼磁粉60～90、粒径小于80μm的各向异性钐钴磁粉5～40及粒径小于10μm的各向异性锶铁氧体磁粉0.5～15一同放入搅拌机中搅拌均匀并得到混合磁粉；Powder preparation: Weigh anisotropic neodymium iron boron magnetic powder 60-90 with a particle size of 30-240μm, anisotropic samarium cobalt magnetic powder 5-40 with a particle size of less than 80μm, and anisotropic strontium with a particle size of less than 10μm. Ferrite magnetic powder 0.5～15 are put into the blender and mixed evenly to obtain mixed magnetic powder;
粘结磁粉配制：称取所述混合磁粉100重量份并加入0.5～10重量份的热固性树脂和0.01～3重量份的硬脂酸锌，在室温～120℃的温度下继续搅拌均匀并得到粘结磁粉；Preparation of bonded magnetic powder: Weigh 100 parts by weight of the mixed magnetic powder and add 0.5-10 parts by weight of thermosetting resin and 0.01-3 parts by weight of zinc stearate, and continue to stir evenly at room temperature to 120°C to obtain a sticky Magnetic powder
上述热固性树脂是双酚A型环氧树脂，或是酚醛型环氧树脂，或是热固性酚醛树脂；The above-mentioned thermosetting resin is bisphenol A type epoxy resin, or phenolic type epoxy resin, or thermosetting phenolic resin;
温压成型：将配制好的所述粘结磁粉装入模具中，在正向磁场强度＞10.0KGs下并在60～180℃内对所述粘结磁粉进行温压成型，温压成型的压力控制在200～500MPa，温压成型的保压时间控制在0.1～60s，温压成型后得到模具中的粘结磁体；Warm pressure molding: Put the prepared bonded magnetic powder into a mold, and perform warm pressure molding on the bonded magnetic powder under a positive magnetic field strength> 10.0KGs at 60-180°C. Control at 200～500MPa, control the holding time of warm press molding at 0.1～60s, and obtain bonded magnets in the mold after warm press molding;
一次退磁：对所述粘结磁体进行反向磁场退磁，所述反向磁场强度控制在1.0KGs～20.0KGs；One-time demagnetization: demagnetize the bonded magnet with a reverse magnetic field, and the reverse magnetic field strength is controlled at 1.0KGs～20.0KGs;
冷却脱模：对一次退磁后的所述粘结磁体进行冷却，冷却采用风冷或是水冷，待风冷或是水冷5～10s后将所述粘结磁体顶出模具进行脱模，脱模时间控制在10～180s内；Cooling and demolding: cooling the bonded magnet after one demagnetization, using air cooling or water cooling, after 5-10 seconds of air cooling or water cooling, eject the bonded magnet from the mold for demolding, demolding The time is controlled within 10～180s;
二次退磁固化：将脱模后的所述粘结磁体放入振荡脉冲磁场中进行二次退磁，所述振荡脉冲磁场的强度最大峰值＞20.0KGs，要求二次退磁后所述粘结磁体的最大表磁＜50Gs，然后将二次退磁后的所述粘结磁体放入烘箱中，并在100～180℃内固化0.5～2h后即制备出磁体。Secondary demagnetization and solidification: Put the demolded bonded magnet into an oscillating pulsed magnetic field for secondary demagnetization. The maximum peak value of the oscillating pulsed magnetic field is> 20.0KGs. The maximum surface magnetism is less than 50Gs, and then the bonded magnet after the secondary demagnetization is put into an oven and cured at 100-180°C for 0.5-2h to prepare the magnet.
实施例2Example 2
本实施例与实施例1的不同点在于：它由以下重量份数的原料组成：各向异性钕铁硼磁粉65份、各向异性钐钴磁粉25份；各向异性锶铁氧体磁粉5份、氧化铁25份、氧化铋18份、氧化镍15份、氧化钛12份、二氧化硅15份、氧化铌5份、氧化钽5份、石墨烯15份、环氧树脂9份、氧化锰4份、氧化钴3份、碳酸钙13份、分散剂2.5份、粘合剂6份、润湿剂2份、十六 烷基三甲基溴化铵0.6份、聚二甲基硅氧烷0.2份、硬脂酸镁0.7份、水80份。The difference between this embodiment and embodiment 1 is that it is composed of the following parts by weight of raw materials: 65 parts of anisotropic neodymium iron boron magnetic powder, 25 parts of anisotropic samarium cobalt magnetic powder; anisotropic strontium ferrite magnetic powder 5 Parts, iron oxide 25 parts, bismuth oxide 18 parts, nickel oxide 15 parts, titanium oxide 12 parts, silica 15 parts, niobium oxide 5 parts, tantalum oxide 5 parts, graphene 15 parts, epoxy resin 9 parts, oxide 4 parts of manganese, 3 parts of cobalt oxide, 13 parts of calcium carbonate, 2.5 parts of dispersant, 6 parts of binder, 2 parts of wetting agent, 0.6 part of cetyltrimethylammonium bromide, polydimethylsiloxane 0.2 parts of alkane, 0.7 parts of magnesium stearate, and 80 parts of water.
实施例3Example 3
本实施例与实施例1的不同点在于：它由以下重量份数的原料组成：各向异性钕铁硼磁粉90份、各向异性钐钴磁粉40份；各向异性锶铁氧体磁粉15份、氧化铁25份、氧化铋25份、氧化镍17份、氧化钛12份、二氧化硅15份、氧化铌7份、氧化钽6份、石墨烯19份、环氧树脂11份、氧化锰5份、氧化钴3.5份、碳酸钙14份、分散剂3份、粘合剂7份、润湿剂2份、十六烷基三甲基溴化铵0.7份，聚二甲基硅氧烷0.3份，硬脂酸镁0.8份，水85份。The difference between this embodiment and embodiment 1 is that it is composed of the following parts by weight of raw materials: 90 parts of anisotropic neodymium iron boron magnetic powder, 40 parts of anisotropic samarium cobalt magnetic powder; 15 parts of anisotropic strontium ferrite magnetic powder Parts, iron oxide 25 parts, bismuth oxide 25 parts, nickel oxide 17 parts, titanium oxide 12 parts, silicon dioxide 15 parts, niobium oxide 7 parts, tantalum oxide 6 parts, graphene 19 parts, epoxy resin 11 parts, oxide 5 parts manganese, 3.5 parts cobalt oxide, 14 parts calcium carbonate, 3 parts dispersant, 7 parts binder, 2 parts wetting agent, 0.7 parts cetyltrimethylammonium bromide, polydimethylsiloxane 0.3 parts of alkane, 0.8 parts of magnesium stearate, 85 parts of water.
采用上述技术方案后，本发明有益效果为：它具有温度稳定性好，磁滞损耗小，起始磁导率高，在应用有利于降低在信号传输过程中波形失真、减少传输错误、延长传输距离和解决高频传输延时问题，满足当前高速网络宽带接入技术的应用需求。After adopting the above technical solution, the present invention has the following beneficial effects: it has good temperature stability, low hysteresis loss, high initial permeability, and is beneficial to reduce waveform distortion in the signal transmission process, reduce transmission errors, and extend transmission. Distance and solve the problem of high-frequency transmission delay to meet the application requirements of current high-speed network broadband access technology.
以上所述，仅用以说明本发明的技术方案而非限制，本领域普通技术人员对本发明的技术方案所做的其它修改或者等同替换，只要不脱离本发明技术方案的精神和范围，均应涵盖在本发明的权利要求范围当中。The above descriptions are only used to illustrate the technical solutions of the present invention and not to limit them. Other modifications or equivalent substitutions made by those of ordinary skill in the art to the technical solutions of the present invention shall be applicable as long as they do not depart from the spirit and scope of the technical solutions of the present invention. Covered in the scope of the claims of the present invention.
Claims (8)
- 一种高频低磁滞锰锌软磁铁氧体材料，其特征在于它由以下重量份数的原料组成：各向异性钕铁硼磁粉60～90份、各向异性钐钴磁粉5～40份、各向异性锶铁氧体磁粉0.5～15份、氧化铁20～25份、氧化铋15～25份、氧化镍12～17份、氧化钛10～17份、二氧化硅11～17份、氧化铌4～7份、氧化钽4～6份、石墨烯13～19份、环氧树脂8～11份、氧化锰3～5份、氧化钴2.5～3.5份、碳酸钙12～14份、分散剂2～3份、粘合剂5～7份、润湿剂1～2份、聚乙烯醇13-17份、十六烷基三甲基溴化铵0.5-0.7份，聚二甲基硅氧烷0.1-0.3份，硬脂酸镁0.6-0.8份，水75-85份。A high-frequency low-hysteresis manganese-zinc soft ferrite material, characterized in that it is composed of the following parts by weight: 60 to 90 parts of anisotropic neodymium iron boron magnetic powder, and 5 to 40 parts of anisotropic samarium cobalt magnetic powder , Anisotropic strontium ferrite powder 0.5-15 parts, iron oxide 20-25 parts, bismuth oxide 15-25 parts, nickel oxide 12-17 parts, titanium oxide 10-17 parts, silicon dioxide 11-17 parts, 4 to 7 parts of niobium oxide, 4 to 6 parts of tantalum oxide, 13 to 19 parts of graphene, 8 to 11 parts of epoxy resin, 3 to 5 parts of manganese oxide, 2.5 to 3.5 parts of cobalt oxide, 12 to 14 parts of calcium carbonate, 2～3 parts of dispersant, 5～7 parts of adhesive, 1～2 parts of wetting agent, 13-17 parts of polyvinyl alcohol, 0.5-0.7 parts of cetyltrimethylammonium bromide, polydimethyl 0.1-0.3 parts of siloxane, 0.6-0.8 parts of magnesium stearate, 75-85 parts of water.
- 一种高频低磁滞锰锌软磁铁氧体材料及其制备方法，该制备方法包括配粉、粘结磁粉配制、温压成型、一次退磁、冷却脱模、二次退磁固化工序，其中粘结磁体温压成型工序中使用到给定模具，各工序分述如下：配粉：按重量份分别称取粒径30～240μm的各向异性钕铁硼磁粉60～90、粒径小于80μm的各向异性钐钴磁粉5～40及粒径小于10μm的各向异性锶铁氧体磁粉0.5～15一同放入搅拌机中搅拌均匀并得到混合磁粉；粘结磁粉配制：称取所述混合磁粉100重量份并加入0.5～10重量份的热固性树脂和0.01～3重量份的硬脂酸锌，在室温～120℃的温度下继续搅拌均匀并得到粘结磁粉；上述热固性树脂是双酚A型环氧树脂，或是酚醛型环氧树脂，或是热固性酚醛树脂；温压成型：将配制好的所述粘结磁粉装入模具中，在正向磁场强度＞10.0KGs下并在60～180℃内对所述粘结磁粉进行温压成型，温压成型的压力控制在200～500MPa，温压成型的保压时间控制在0.1～60s，温压成型后得到模具中的粘结磁体；一次退磁：对所述粘结磁体进行反向磁场退磁，所述反向磁场强度控制在1.0KGs～20.0KGs；冷却脱模：对一次退磁后的所述粘结磁体进行冷却，冷却采用风冷或是水冷，待风冷或是水冷5～10s后将所述粘结磁体顶出模具进行脱模，脱模时间控制在10～180s内；二次退磁固化：将脱模后的所述粘结磁体放入振荡脉冲磁场中进行二次退磁，所述振荡脉冲磁 场的强度最大峰值＞20.0KGs，要求二次退磁后所述粘结磁体的最大表磁＜50Gs，然后将二次退磁后的所述粘结磁体放入烘箱中，并在100～180℃内固化0.5～2h后即制备出磁体。A high-frequency low-hysteresis manganese-zinc soft ferrite material and a preparation method thereof. The preparation method includes powder preparation, bonding magnetic powder preparation, warm-pressing molding, primary demagnetization, cooling demolding, and secondary demagnetization and solidification steps. A given mold is used in the warm press forming process of the junction magnet, and each process is described as follows: Powder preparation: Weigh the anisotropic neodymium iron boron magnetic powder 60-90 with a particle size of 30-240μm in parts by weight and a particle size less than 80μm Anisotropic samarium cobalt magnetic powder 5～40 and anisotropic strontium ferrite magnetic powder 0.5～15 with a particle size of less than 10μm are put into a mixer and mixed evenly to obtain a mixed magnetic powder; preparation of bonded magnetic powder: weigh the mixed magnetic powder 100 Add 0.5-10 parts by weight of thermosetting resin and 0.01-3 parts by weight of zinc stearate, and continue stirring at room temperature to 120°C to obtain bonded magnetic powder; the thermosetting resin is a bisphenol A ring Oxygen resin, or phenolic type epoxy resin, or thermosetting phenolic resin; warm press molding: put the prepared bonded magnetic powder into a mold, and at a positive magnetic field strength> 10.0KGs and at 60～180℃ The bonded magnetic powder is subjected to warm press molding, the pressure of the warm press molding is controlled at 200-500MPa, and the holding time of the warm press molding is controlled at 0.1-60s. After the warm press molding, the bonded magnet in the mold is obtained; one demagnetization : Demagnetize the bonded magnet with reverse magnetic field, the strength of the reverse magnetic field is controlled within 1.0KGs～20.0KGs; cooling and demolding: cool the bonded magnet after one demagnetization, and the cooling adopts air cooling or Water cooling, after air cooling or water cooling for 5-10s, the bonded magnet is ejected from the mold for demolding, and the demolding time is controlled within 10 to 180s; secondary demagnetization curing: the bonded magnet after demolding Put it into an oscillating pulsed magnetic field for secondary demagnetization. The maximum peak strength of the oscillating pulsed magnetic field is greater than 20.0KGs, and the maximum surface magnetization of the bonded magnet after the secondary demagnetization is required to be less than 50Gs. The bonded magnet is placed in an oven and cured at 100-180°C for 0.5-2h to prepare the magnet.
- 根据权利要求1所述的一种高频低磁滞锰锌软磁铁氧体材料，由以下重量份数的原料组成：各向异性钕铁硼磁粉60份、各向异性钐钴磁粉5份；各向异性锶铁氧体磁粉0.5份、氧化铁20份、氧化铋15份、氧化镍12份、氧化钛10份、二氧化硅11份、氧化铌4份、氧化钽4份、石墨烯13份、环氧树脂8份、氧化锰3份、氧化钴2.5份、碳酸钙12份、分散剂2份、粘合剂5份、润湿剂1份、十六烷基三甲基溴化铵0.5份、聚二甲基硅氧烷0.1份、硬脂酸镁0.6份、水75份。A high-frequency low-hysteresis manganese-zinc soft ferrite material according to claim 1, consisting of the following parts by weight of raw materials: 60 parts of anisotropic neodymium iron boron magnetic powder and 5 parts of anisotropic samarium cobalt magnetic powder; Anisotropic strontium ferrite magnetic powder 0.5 parts, iron oxide 20 parts, bismuth oxide 15 parts, nickel oxide 12 parts, titanium oxide 10 parts, silicon dioxide 11 parts, niobium oxide 4 parts, tantalum oxide 4 parts, graphene 13 Parts, 8 parts epoxy resin, 3 parts manganese oxide, 2.5 parts cobalt oxide, 12 parts calcium carbonate, 2 parts dispersant, 5 parts adhesive, 1 part wetting agent, cetyltrimethylammonium bromide 0.5 part, 0.1 part of polydimethylsiloxane, 0.6 part of magnesium stearate, 75 parts of water.
- 根据权利要求1所述的一种高频低磁滞锰锌软磁铁氧体材料，由以下重量份数的原料组成：各向异性钕铁硼磁粉65份、各向异性钐钴磁粉25份；各向异性锶铁氧体磁粉5份、氧化铁25份、氧化铋18份、氧化镍15份、氧化钛12份、二氧化硅15份、氧化铌5份、氧化钽5份、石墨烯15份、环氧树脂9份、氧化锰4份、氧化钴3份、碳酸钙13份、分散剂2.5份、粘合剂6份、润湿剂2份、十六烷基三甲基溴化铵0.6份、聚二甲基硅氧烷0.2份、硬脂酸镁0.7份、水80份。A high-frequency low-hysteresis manganese-zinc soft ferrite material according to claim 1, comprising the following parts by weight of raw materials: 65 parts of anisotropic neodymium iron boron magnetic powder and 25 parts of anisotropic samarium cobalt magnetic powder; 5 parts of anisotropic strontium ferrite powder, 25 parts of iron oxide, 18 parts of bismuth oxide, 15 parts of nickel oxide, 12 parts of titanium oxide, 15 parts of silicon dioxide, 5 parts of niobium oxide, 5 parts of tantalum oxide, 15 parts of graphene Parts, 9 parts of epoxy resin, 4 parts of manganese oxide, 3 parts of cobalt oxide, 13 parts of calcium carbonate, 2.5 parts of dispersant, 6 parts of adhesive, 2 parts of wetting agent, cetyltrimethylammonium bromide 0.6 parts, 0.2 parts of polydimethylsiloxane, 0.7 parts of magnesium stearate, and 80 parts of water.
- 根据权利要求1所述的一种高频低磁滞锰锌软磁铁氧体材料，由以下重量份数的原料组成：各向异性钕铁硼磁粉90份、各向异性钐钴磁粉40份；各向异性锶铁氧体磁粉15份、氧化铁25份、氧化铋25份、氧化镍17份、氧化钛12份、二氧化硅15份、氧化铌7份、氧化钽6份、石墨烯19份、环氧树脂11份、氧化锰5份、氧化钴3.5份、碳酸钙14份、分散剂3份、粘合剂7份、润湿剂2份、十六烷基三甲基溴化铵0.7份，聚二甲基硅氧烷0.3份，硬脂酸镁0.8份，水85份。A high-frequency low-hysteresis manganese-zinc soft ferrite material according to claim 1, which is composed of the following parts by weight of raw materials: 90 parts of anisotropic neodymium iron boron magnetic powder and 40 parts of anisotropic samarium cobalt magnetic powder; 15 parts of anisotropic strontium ferrite magnetic powder, 25 parts of iron oxide, 25 parts of bismuth oxide, 17 parts of nickel oxide, 12 parts of titanium oxide, 15 parts of silicon dioxide, 7 parts of niobium oxide, 6 parts of tantalum oxide, 19 parts of graphene Parts, 11 parts of epoxy resin, 5 parts of manganese oxide, 3.5 parts of cobalt oxide, 14 parts of calcium carbonate, 3 parts of dispersant, 7 parts of adhesive, 2 parts of wetting agent, cetyltrimethylammonium bromide 0.7 parts, 0.3 parts of polydimethylsiloxane, 0.8 parts of magnesium stearate, 85 parts of water.
- 根据权利要求2所述的一种永磁铁氧体磁环磁粉的制备方法，其特征在于：所述的各向异性钕铁硼磁粉的粒径控制在30～240μm。The method for preparing permanent ferrite magnetic ring magnetic powder according to claim 2, wherein the particle size of the anisotropic neodymium iron boron magnetic powder is controlled to be 30-240 μm.
- 根据权利要求2所述的一种永磁铁氧体磁环磁粉的制备方法，其特征 在于：所述的各向异性钐钴磁粉的粒径小于80μm。The method for preparing permanent ferrite magnetic ring magnetic powder according to claim 2, wherein the particle size of the anisotropic samarium cobalt magnetic powder is less than 80 m.
- 根据权利要求2所述的一种永磁铁氧体磁环磁粉的制备方法，其特征在于：所述的各向异性锶铁氧体磁粉的粒径小于10μm。The method for preparing permanent ferrite magnetic ring magnetic powder according to claim 2, wherein the particle size of the anisotropic strontium ferrite magnetic powder is less than 10 μm.
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| JP2007194402A (en) * | 2006-01-19 | 2007-08-02 | Millenium Gate Technology Co Ltd | Magnetic multilayer nanoparticle, its manufacturing method, and magnetic material using the same |
| CN104616853A (en) * | 2015-01-29 | 2015-05-13 | 厦门双瑞高磁科技有限公司 | Formula and preparation method for forming bonded magnet with three types of anisotropic magnet powder |
| CN107151137A (en) * | 2017-05-23 | 2017-09-12 | 安徽省东方磁磁铁制造有限公司 | A kind of Mn-Zn soft magnetic ferrite and preparation method thereof |
| CN109748579A (en) * | 2019-02-26 | 2019-05-14 | 南通华兴磁性材料有限公司 | The preparation method of high impedance high magnetic characteristics nickel-manganese Zinc ferrite material |
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- 2019-10-28 WO PCT/CN2019/113527 patent/WO2021017216A1/en active Application Filing
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2007194402A (en) * | 2006-01-19 | 2007-08-02 | Millenium Gate Technology Co Ltd | Magnetic multilayer nanoparticle, its manufacturing method, and magnetic material using the same |
| CN104616853A (en) * | 2015-01-29 | 2015-05-13 | 厦门双瑞高磁科技有限公司 | Formula and preparation method for forming bonded magnet with three types of anisotropic magnet powder |
| CN107151137A (en) * | 2017-05-23 | 2017-09-12 | 安徽省东方磁磁铁制造有限公司 | A kind of Mn-Zn soft magnetic ferrite and preparation method thereof |
| CN109748579A (en) * | 2019-02-26 | 2019-05-14 | 南通华兴磁性材料有限公司 | The preparation method of high impedance high magnetic characteristics nickel-manganese Zinc ferrite material |
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