CN106531388A - Composite magnetic powder and preparation method therefor - Google Patents
Composite magnetic powder and preparation method therefor Download PDFInfo
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- 239000006247 magnetic powder Substances 0.000 title claims abstract description 123
- 239000002131 composite material Substances 0.000 title claims abstract description 74
- 238000002360 preparation method Methods 0.000 title claims abstract description 37
- 229910000702 sendust Inorganic materials 0.000 claims abstract description 79
- 239000000843 powder Substances 0.000 claims abstract description 52
- 229910000859 α-Fe Inorganic materials 0.000 claims abstract description 47
- 238000000034 method Methods 0.000 claims abstract description 37
- 239000012634 fragment Substances 0.000 claims abstract description 25
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- 239000002245 particle Substances 0.000 claims description 8
- 238000007578 melt-quenching technique Methods 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 6
- 239000000463 material Substances 0.000 claims description 5
- 238000003701 mechanical milling Methods 0.000 claims 1
- 229910000838 Al alloy Inorganic materials 0.000 abstract description 27
- 238000012360 testing method Methods 0.000 abstract description 16
- -1 iron-silicon-aluminum Chemical compound 0.000 abstract description 9
- 238000010791 quenching Methods 0.000 abstract description 3
- 230000000171 quenching effect Effects 0.000 abstract description 3
- 239000000696 magnetic material Substances 0.000 abstract description 2
- 239000000155 melt Substances 0.000 abstract description 2
- 238000002474 experimental method Methods 0.000 abstract 1
- 238000009987 spinning Methods 0.000 abstract 1
- 230000035699 permeability Effects 0.000 description 39
- 229910001289 Manganese-zinc ferrite Inorganic materials 0.000 description 21
- JIYIUPFAJUGHNL-UHFFFAOYSA-N [O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[Mn++].[Mn++].[Mn++].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Zn++].[Zn++] Chemical group [O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[Mn++].[Mn++].[Mn++].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Zn++].[Zn++] JIYIUPFAJUGHNL-UHFFFAOYSA-N 0.000 description 21
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 18
- 229910052782 aluminium Inorganic materials 0.000 description 17
- 230000008569 process Effects 0.000 description 16
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 13
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- 238000000576 coating method Methods 0.000 description 6
- 238000009413 insulation Methods 0.000 description 6
- HQKMJHAJHXVSDF-UHFFFAOYSA-L magnesium stearate Chemical group [Mg+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O HQKMJHAJHXVSDF-UHFFFAOYSA-L 0.000 description 6
- 239000010935 stainless steel Substances 0.000 description 6
- 229910001220 stainless steel Inorganic materials 0.000 description 6
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 5
- 229910052802 copper Inorganic materials 0.000 description 5
- 239000010949 copper Substances 0.000 description 5
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- 150000002696 manganese Chemical class 0.000 description 4
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- 239000007864 aqueous solution Substances 0.000 description 2
- 239000002585 base Substances 0.000 description 2
- 238000000975 co-precipitation Methods 0.000 description 2
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- 238000010438 heat treatment Methods 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 229910052748 manganese Inorganic materials 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 238000000197 pyrolysis Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
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- 238000005253 cladding Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
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Classifications
-
- 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
- H01F1/33—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 mixtures of metallic and non-metallic particles; metallic particles having oxide skin
-
- 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
- H01F41/0206—Manufacturing of magnetic cores by mechanical means
- H01F41/0246—Manufacturing of magnetic circuits by moulding or by pressing powder
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- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Dispersion Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Soft Magnetic Materials (AREA)
Abstract
Description
技术领域technical field
本发明属于磁性材料制备领域,尤其涉及一种复合磁粉及复合磁粉芯的制备方法。The invention belongs to the field of magnetic material preparation, and in particular relates to a preparation method of composite magnetic powder and composite magnetic powder core.
背景技术Background technique
铁硅铝软磁合金,又称为Sendust合金,其化学组成为5.4wt.%Al,9.6Sendust soft magnetic alloy, also known as Sendust alloy, has a chemical composition of 5.4wt.% Al, 9.6
wt.%Si,其余为Fe(85wt.%)。铁硅铝合金非常脆,很容易破碎成粉,一般制备成磁粉芯使用。wt.% Si, the rest is Fe (85wt.%). Sensil is very brittle and is easily broken into powder. It is generally prepared as a magnetic powder core for use.
与铁硅芯及铁粉芯相比,铁硅铝磁粉芯高频损耗更低,而且具有较高的饱和磁感应强度和磁导率,价格低廉,有利于实现小型化。此外,铁硅铝合金的磁致伸缩系数λs接近于零,有利于消除滤波电感器工作时产生的听觉频率噪声。由于具有低损耗、低成本等特点,以及其他磁粉芯无可比拟的综合性能,铁硅铝磁粉芯已快速发展起来,在输出电感、线路滤波器、功率因素校正器等器件中得到了广泛的应用。Compared with iron-silicon cores and iron powder cores, sendust magnetic powder cores have lower high-frequency loss, and have higher saturation magnetic induction and magnetic permeability, and are inexpensive, which is conducive to miniaturization. In addition, the magnetostriction coefficient λ s of sendust is close to zero, which is beneficial to eliminate the auditory frequency noise generated when the filter inductor is working. Due to the characteristics of low loss, low cost, etc., and the incomparable comprehensive performance of other magnetic powder cores, sendust magnetic powder cores have developed rapidly, and have been widely used in devices such as output inductors, line filters, and power factor correctors. application.
早期的铁硅铝磁粉芯工作频率比较低,只要求高的磁导率而对损耗要求并不高。随着铁硅铝磁粉芯的使用工作频率越来越高,高频损耗大,如何在保证磁粉芯高磁导率的情况下,降低磁芯高频损耗成为突出问题。因此研究磁粉芯磁导率和磁芯损耗的影响因素就显得尤为重要。国内外关于金属磁粉芯的研究主要是通过提高磁粉性能、选择合适的绝缘剂及磁粉粒度、调整压制参数等方法来改善磁粉芯的磁性能。随着研究的深入,考虑从工艺方面进行改进,如成型压力、绝缘包覆工艺和热处理对磁粉芯的磁导率和损耗的影响越来越受到关注。铁硅铝磁粉芯生产过程中最关键工序之一就是粉末的绝缘包覆工艺。通过绝缘包覆,可阻隔磁粉之间的电接触,从而可以增大磁粉的电阻率,降低高频损耗。The early sendust magnetic powder cores had a relatively low operating frequency and only required high magnetic permeability but not high requirements for loss. With the use of sendust magnetic powder cores, the operating frequency is getting higher and higher, and the high-frequency loss is large. How to reduce the high-frequency loss of the magnetic core while ensuring the high magnetic permeability of the magnetic powder core has become a prominent problem. Therefore, it is particularly important to study the influencing factors of magnetic powder core permeability and core loss. The research on metal magnetic powder cores at home and abroad is mainly to improve the magnetic properties of magnetic powder cores by improving the performance of magnetic powder, selecting appropriate insulating agents and particle size of magnetic powder, and adjusting pressing parameters. With the deepening of the research, considering the improvement of the process, such as the impact of molding pressure, insulation coating process and heat treatment on the magnetic permeability and loss of the magnetic powder core, more and more attention has been paid. One of the most critical processes in the production process of sendust magnetic powder cores is the powder insulation coating process. The electrical contact between the magnetic powders can be blocked by insulating coating, so that the resistivity of the magnetic powders can be increased and the high-frequency loss can be reduced.
目前国内外常用的铁硅铝磁粉芯制备方法采用的绝缘包覆工艺,使用的非磁性绝缘层稀释了磁性,导致磁导率低;绝缘层不稳定(高温分解)且强度低(磁粉芯压制成型过程中包覆层容易被压破)导致高频损耗高。此外,目前常用的铁硅铝磁粉扁平度不够好,不利于进一步提高磁导率及降低高频损耗。At present, the commonly used sendust magnetic powder core preparation method at home and abroad adopts the insulation coating process, and the non-magnetic insulating layer used dilutes the magnetism, resulting in low magnetic permeability; the insulating layer is unstable (pyrolysis) and low in strength (magnetic powder core pressing The cladding layer is easily crushed during the molding process) resulting in high high-frequency loss. In addition, the currently commonly used sendust magnetic powder is not flat enough, which is not conducive to further improving the magnetic permeability and reducing high-frequency loss.
发明内容Contents of the invention
有鉴于此,本发明的目的在于提供一种复合磁粉及复合磁粉芯的制备方法,由本发明提供的方法制得的磁粉芯具有较高的磁导率和较低的高频损耗。In view of this, the object of the present invention is to provide a method for preparing composite magnetic powder and composite magnetic powder core. The magnetic powder core prepared by the method provided by the present invention has higher magnetic permeability and lower high-frequency loss.
本发明提供了一种复合磁粉的制备方法,包括以下步骤:The invention provides a kind of preparation method of composite magnetic powder, comprises the following steps:
a)、采用熔体快淬法制备铁硅铝合金薄带;制备过程中,甩带时施加定向磁场;将制得的铁硅铝合金薄带进行破碎,得到铁硅铝合金碎片;a) Using a melt quenching method to prepare sendust aluminum alloy strips; during the preparation process, applying a directional magnetic field when the strips are thrown; breaking the prepared sendust aluminum alloy thin strips to obtain sendust aluminum alloy fragments;
b)、将所述铁硅铝合金碎片与铁氧体粉末混合球磨,得到复合磁粉。b) Mixing and ball milling the sendust powder and ferrite powder to obtain composite magnetic powder.
优选的,所述定向磁场的磁场强度为500~2000Oe。Preferably, the magnetic field strength of the orientation magnetic field is 500-2000 Oe.
优选的,甩带过程中一直施加定向磁场。Preferably, a directional magnetic field is applied all the time during the belt throwing process.
优选的,所述铁硅铝合金薄带的厚度为5~50μm。Preferably, the thickness of the sendust aluminum strip is 5-50 μm.
优选的,所述铁氧体粉末的粒径为10nm~2μm。Preferably, the particle diameter of the ferrite powder is 10 nm˜2 μm.
优选的,所述铁硅铝合金碎片与铁氧体粉末的质量比为100:(2~20)。Preferably, the mass ratio of the sendust pieces to the ferrite powder is 100:(2-20).
优选的,所述球磨过程中的球料质量比为(10~15):1。Preferably, the ball-to-material mass ratio in the ball milling process is (10-15):1.
优选的,所述球磨采用的磨球直径为3~15mm。Preferably, the diameter of the balls used in the ball mill is 3-15 mm.
本发明提供了一种复合磁粉芯的制备方法,包括以下步骤:The invention provides a preparation method of a composite magnetic powder core, comprising the following steps:
粘结剂、润滑剂和按照上述技术方案所述方法制备得到的复合磁粉依次进行混合和压制,得到复合磁粉芯。The binder, the lubricant, and the composite magnetic powder prepared according to the method described in the above technical solution are mixed and pressed in sequence to obtain a composite magnetic powder core.
优选的,所述压制的压力为1500~2000MPa;所述压制的时间为3~8min。Preferably, the pressing pressure is 1500-2000 MPa; the pressing time is 3-8 minutes.
与现有技术相比,本发明提供了一种复合磁粉及复合磁粉芯的制备方法,本发明提供的复合磁粉芯的制备方法包括以下步骤:a)、采用熔体快淬法制备铁硅铝合金薄带;制备过程中,甩带时施加定向磁场;将制得的铁硅铝合金薄带进行破碎,得到铁硅铝合金碎片;b)、将所述铁硅铝合金碎片与铁氧体粉末混合球磨,得到复合磁粉;c)、将粘结剂、润滑剂和所述复合磁粉依次进行混合和压制,得到复合磁粉芯。本发明首先在制备铁硅铝合金薄带时的甩带过程中施加定向磁场,通过这种方式提高了铁硅铝合金薄带的饱和磁化强度和磁导率。之后将破碎得到铁硅铝合金碎片与铁氧体粉末球磨,借助于球磨时碾压作用,使铁氧体粉末均匀嵌入在铁硅铝合金碎片表面,形成铁氧体绝缘包覆层。本发明通过球磨的方式混合铁氧体粉末和铁硅铝合金碎片,不但能够使铁氧体均匀、牢固的包覆在铁硅铝合金碎片表面,而且在铁氧体粉末的用量较低的情况下就能够实现铁氧体粉末对铁硅铝合金表面的完全包覆,降低了铁氧体的引入对于磁粉磁导率的影响,使磁粉的磁导率维持在较高水平,同时球磨还可以进一步实现磁粉的扁平化,从而进一步提高磁粉的磁导率和降低由其制成的磁粉芯的高频损耗。由本发明提供的复合磁粉制成的磁粉芯具有高的磁导率和低的高频损耗,应用前景广阔,不仅可用于电讯、雷达,还可应用于吸波及电磁屏蔽领域。实验结果表明,由本发明提供的方法制成的磁粉芯在100kHz的测试频率下的有效磁导率高于40,在100kHz,Bm=300mT测试条件下的损耗低于83W/kg。Compared with the prior art, the present invention provides a preparation method of composite magnetic powder and composite magnetic powder core, the preparation method of the composite magnetic powder core provided by the present invention comprises the following steps: a) preparing sendust by melt rapid quenching Alloy thin strip; during the preparation process, a directional magnetic field is applied when the strip is thrown; the prepared sendust aluminum strip is broken to obtain sendust aluminum fragments; b) combining the sendust aluminum alloy fragments with ferrite The powders are mixed and ball milled to obtain a composite magnetic powder; c) sequentially mixing and pressing a binder, a lubricant and the composite magnetic powder to obtain a composite magnetic powder core. In the present invention, a directional magnetic field is firstly applied during the belt throwing process when preparing the sendust aluminum strip, and in this way the saturation magnetization and magnetic permeability of the sendust aluminum strip are improved. Afterwards, the crushed sendust aluminum alloy fragments are ball milled with ferrite powder, and the ferrite powder is evenly embedded on the surface of the sendust aluminum alloy fragments by means of the rolling action during ball milling to form a ferrite insulating coating layer. The present invention mixes ferrite powder and sendust fragments by ball milling, which not only enables ferrite to coat the surface of sendust fragments evenly and firmly, but also makes the ferrite powder less ferrite powder The ferrite powder can completely cover the surface of the sendust, which reduces the influence of the introduction of ferrite on the magnetic permeability of the magnetic powder, and maintains the magnetic permeability of the magnetic powder at a high level. At the same time, ball milling can also Further realize the flattening of the magnetic powder, thereby further improving the magnetic permeability of the magnetic powder and reducing the high-frequency loss of the magnetic powder core made of it. The magnetic powder core made of the composite magnetic powder provided by the invention has high magnetic permeability and low high-frequency loss, and has broad application prospects. It can be used not only in telecommunications and radar, but also in the fields of wave absorption and electromagnetic shielding. Experimental results show that the effective magnetic permeability of the magnetic powder core made by the method provided by the invention is higher than 40 at the test frequency of 100kHz, and the loss is lower than 83W/kg under the test condition of 100kHz and Bm=300mT.
附图说明Description of drawings
为了更清楚地说明本发明实施例或现有技术中的技术方案,下面将对实施例或现有技术描述中所需要使用的附图作简单地介绍,显而易见地,下面描述中的附图仅仅是本发明的实施例,对于本领域普通技术人员来讲,在不付出创造性劳动的前提下,还可以根据提供的附图获得其他的附图。In order to more clearly illustrate the technical solutions in the embodiments of the present invention or the prior art, the following will briefly introduce the drawings that need to be used in the description of the embodiments or the prior art. Obviously, the accompanying drawings in the following description are only It is an embodiment of the present invention, and those skilled in the art can also obtain other drawings according to the provided drawings without creative work.
图1是本发明实施例6提供的不同配比的复合磁粉芯的有效磁导率;Fig. 1 is the effective magnetic permeability of the composite magnetic powder core of different proportioning provided by embodiment 6 of the present invention;
图2是本发明实施例6提供的不同配比的复合磁粉芯的损耗;Fig. 2 is the loss of the composite magnetic powder core of different proportioning provided by embodiment 6 of the present invention;
图3是本发明实施例12提供的不同退火温度的复合磁粉芯的有效磁导率;Fig. 3 is the effective magnetic permeability of the composite magnetic powder core with different annealing temperatures provided by Embodiment 12 of the present invention;
图4是本发明实施例12提供的不同退火温度的复合磁粉芯的损耗。Fig. 4 shows the losses of the composite magnetic powder cores provided by Example 12 of the present invention with different annealing temperatures.
具体实施方式detailed description
下面对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例仅仅是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。The following clearly and completely describes the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only some of the embodiments of the present invention, but not all of them. Based on the embodiments of the present invention, all other embodiments obtained by persons of ordinary skill in the art without making creative efforts belong to the protection scope of the present invention.
本发明提供了一种复合磁粉的制备方法,包括以下步骤:The invention provides a kind of preparation method of composite magnetic powder, comprises the following steps:
a)、采用熔体快淬法制备铁硅铝合金薄带;制备过程中,甩带时施加定向磁场;将制得的铁硅铝合金薄带进行破碎,得到铁硅铝合金碎片;a) Using a melt quenching method to prepare sendust aluminum alloy strips; during the preparation process, applying a directional magnetic field when the strips are thrown; breaking the prepared sendust aluminum alloy thin strips to obtain sendust aluminum alloy fragments;
b)、将所述铁硅铝合金碎片与铁氧体粉末混合球磨,得到复合磁粉。b) Mixing and ball milling the sendust powder and ferrite powder to obtain composite magnetic powder.
在本发明提供的制备方法中,首先制备铁硅铝合金薄带。本发明采用熔体快淬法制备铁硅铝合金薄带,在甩带过程中一直施加定向磁场。在本发明中,所述定向磁场的磁场强度优选为500~2000Oe,更优选为1000~1200Oe。在本发明中,甩带过程中,可通过调整铜辊转速来控制薄带的厚度,铜辊转速越快,厚度越薄,铜辊转速优选为30~80m/s。本发明对制备铁硅铝合金薄带的设备没有特别限定,优选为本领域技术人员熟知的感应式熔体快淬设备。制备完毕后,得到铁硅铝合金薄带。在本发明中,所述铁硅铝合金薄带由Si、Al和Fe组成,其中,Si在合金薄带中的含量优选为9.3~9.7wt%,更优选为9.6wt%;Al的在合金薄带中的含量优选为5.2~5.6wt%,更优选为5.4wt%;余量为Fe。在本发明中,所述铁硅铝合金薄带的厚度优选为5~50μm,更优选为5~30μm,最优选为5~15μm。得到铁硅铝合金薄带后,将制得的铁硅铝合金薄带进行破碎,得到铁硅铝合金碎片。In the preparation method provided by the present invention, sendust aluminum strips are firstly prepared. The invention adopts the melt rapid quenching method to prepare the iron-silicon-aluminum alloy thin strip, and always applies a directional magnetic field during the strip throwing process. In the present invention, the magnetic field strength of the orientation magnetic field is preferably 500-2000 Oe, more preferably 1000-1200 Oe. In the present invention, during the stripping process, the thickness of the thin strip can be controlled by adjusting the copper roll speed, the faster the copper roll speed, the thinner the thickness, and the copper roll speed is preferably 30-80m/s. The present invention has no particular limitation on the equipment for preparing the sendust thin strip, and is preferably an induction melt quenching equipment well known to those skilled in the art. After the preparation is completed, the sendust aluminum strip is obtained. In the present invention, the sendust aluminum strip is composed of Si, Al and Fe, wherein the content of Si in the alloy strip is preferably 9.3-9.7wt%, more preferably 9.6wt%; The content in the ribbon is preferably 5.2-5.6 wt%, more preferably 5.4 wt%; the balance is Fe. In the present invention, the thickness of the sendust aluminum strip is preferably 5-50 μm, more preferably 5-30 μm, and most preferably 5-15 μm. After the sendust aluminum strip is obtained, the prepared sendust aluminum strip is crushed to obtain sendust aluminum alloy fragments.
得到铁硅铝合金碎片后,将所述铁硅铝合金碎片与铁氧体粉末混合球磨。其中,铁氧体粉末优选为锰锌铁氧体粉末,其化学通式为MnxZn1-xFe2O4,0<x<1。在本发明提供的一个实施例中,所述锰锌铁氧体粉末的化学通式为Mn0.4Zn0.6Fe2O4。在本发明中,所述铁氧体粉末的粒径优选为10nm~2μm。本发明对所述铁氧体粉末的来源没有特别限定,可采用化学共沉法制备得到,以锰锌铁氧体粉末为例,可以按照以下方法制备得到:After the sendust shards are obtained, the sendust shards are mixed with ferrite powder for ball milling. Among them, the ferrite powder is preferably manganese zinc ferrite powder, whose general chemical formula is Mn x Zn 1-x Fe 2 O 4 , 0<x<1. In an embodiment provided by the present invention, the general chemical formula of the manganese zinc ferrite powder is Mn 0.4 Zn 0.6 Fe 2 O 4 . In the present invention, the particle size of the ferrite powder is preferably 10 nm to 2 μm. In the present invention, the source of the ferrite powder is not particularly limited, and it can be prepared by chemical co-precipitation. Taking manganese-zinc ferrite powder as an example, it can be prepared according to the following method:
(1)、铁盐、锌盐、锰盐和水混合,得到混合盐溶液;(1), iron salt, zinc salt, manganese salt and water are mixed, obtain mixed salt solution;
(2)、用可溶性碱调节所述混合盐溶液的pH值,进行反应,得到锰锌铁氧体前驱体;(2), adjust the pH value of described mixed salt solution with soluble alkali, carry out reaction, obtain manganese zinc ferrite precursor;
(3)、所述锰锌铁氧体前驱体进行焙烧,得到锰锌铁氧体粉末。(3) The manganese zinc ferrite precursor is calcined to obtain manganese zinc ferrite powder.
在本发明提供的上述制备锰锌铁氧体粉末的方法中,首先将铁盐、锌盐、锰盐和水混合,其中,所述铁盐为铁的可溶盐或其水合物,包括但不限于FeCl3、Fe(NO3)3和Fe2(SO4)3中的一种或多种;所述锌盐为锌的可溶盐或其水合物,包括但不限于ZnCl2、Zn(NO3)2和ZnSO4中的一种或多种;所述锰盐为锰的可溶盐或其水合物,包括但不限于MnCl2、MnCl2·4H2O、Mn(NO3)2和MnSO4中的一种或多种。铁盐、锌盐和锰盐在水中完全溶解后,得到混合盐溶液。In the above-mentioned method for preparing manganese-zinc ferrite powder provided by the present invention, first mix iron salt, zinc salt, manganese salt and water, wherein, the iron salt is a soluble salt of iron or a hydrate thereof, including but Not limited to one or more of FeCl 3 , Fe(NO 3 ) 3 and Fe 2 (SO 4 ) 3 ; the zinc salt is a soluble salt of zinc or a hydrate thereof, including but not limited to ZnCl 2 , Zn One or more of (NO 3 ) 2 and ZnSO 4 ; the manganese salt is a soluble salt of manganese or a hydrate thereof, including but not limited to MnCl 2 , MnCl 2 ·4H 2 O, Mn(NO 3 ) 2 and one or more of MnSO 4 . After the iron salt, zinc salt and manganese salt are completely dissolved in water, a mixed salt solution is obtained.
得到混合盐溶液后,用可溶性碱调节所述混合盐溶液的pH值至碱性。其中,所述可溶性碱优选为NaOH或其水溶液,所述NaOH水溶液的浓度优选为1~2mol/L。在本发明中,优选调节所述混合盐溶液的pH值至9~13,更优选为10~11。在本发明中,优选现将所述混合液溶液的温度加热至50~90℃,更优选为70~80℃后再调节其pH值。pH调节完毕后,混合盐溶液中的各离子之间发生反应,得到固体沉淀物,所述固体沉淀物即为锰锌铁氧体前驱体。在本发明中,所述反应的时间优选为10~60min,更优选为30~40min。After the mixed salt solution is obtained, the pH value of the mixed salt solution is adjusted to alkaline with a soluble base. Wherein, the soluble base is preferably NaOH or its aqueous solution, and the concentration of the NaOH aqueous solution is preferably 1-2 mol/L. In the present invention, the pH value of the mixed salt solution is preferably adjusted to 9-13, more preferably 10-11. In the present invention, it is preferred to adjust the pH value of the mixed liquid solution after heating it to 50-90°C, more preferably 70-80°C. After the pH is adjusted, the ions in the mixed salt solution react to obtain a solid precipitate, which is the precursor of manganese zinc ferrite. In the present invention, the reaction time is preferably 10-60 min, more preferably 30-40 min.
得到锰锌铁氧体前驱体后,对所述锰锌铁氧体前驱体进行焙烧。其中,所述焙烧的温度优选为800~900℃,更优选为850~870℃;所述焙烧的时间优选为1~5h,更优选为2~3h。焙烧结束后,得到锰锌铁氧体粉末。在本发明中,所述锰锌铁氧体前驱体优选在进行焙烧之前,先进行洗涤和干燥。所述干燥的温度优选为90~100℃;所述干燥的时间优选为1~2h。After the manganese zinc ferrite precursor is obtained, the manganese zinc ferrite precursor is calcined. Wherein, the temperature of the calcination is preferably 800-900° C., more preferably 850-870° C.; the calcination time is preferably 1-5 hours, more preferably 2-3 hours. After calcination, manganese zinc ferrite powder is obtained. In the present invention, the manganese zinc ferrite precursor is preferably washed and dried before being fired. The drying temperature is preferably 90-100° C.; the drying time is preferably 1-2 hours.
在本发明中,铁氧体粉末与铁硅铝合金碎片进行球磨的过程中,所述铁硅铝合金碎片与铁氧体粉末的质量比优选为10:(2~20),更优选为100:2、100:4、100:6、100:10或100:20。在本发明中,所述球磨过程中的球料质量比优选为(10~15):1,更优选为(12~13):1。在本发明中,所述球磨采用的磨球优选为钢球;所述钢球直径优选为3~15mm,更优选为5~10mm;在本发明提供的一个实施例中,所述磨球包括直径为5mm的钢球和直径为10mm的钢球,直径为5mm的钢球和直径为10mm的钢球的个数比优选为(3~10):1,更优选为5:1。在本发明中,所述球磨的转速优选为30~80rpm,更优选为50~60rpm;所述球磨的时间优选为20~60h,更优选为30~40h。球磨结束后,得到复合磁粉。In the present invention, during the ball milling process of ferrite powder and sendust shards, the mass ratio of the sendust shards to ferrite powder is preferably 10:(2-20), more preferably 100 :2, 100:4, 100:6, 100:10, or 100:20. In the present invention, the ball-to-material mass ratio in the ball milling process is preferably (10-15):1, more preferably (12-13):1. In the present invention, the grinding balls used in the ball mill are preferably steel balls; the diameter of the steel balls is preferably 3-15 mm, more preferably 5-10 mm; in an embodiment provided by the present invention, the grinding balls include Steel balls with a diameter of 5 mm and steel balls with a diameter of 10 mm, the number ratio of the steel balls with a diameter of 5 mm to the steel balls with a diameter of 10 mm is preferably (3-10):1, more preferably 5:1. In the present invention, the rotational speed of the ball mill is preferably 30-80 rpm, more preferably 50-60 rpm; the time of the ball mill is preferably 20-60 h, more preferably 30-40 h. After ball milling, composite magnetic powder is obtained.
本发明首先在制备铁硅铝合金薄带时的甩带过程中施加定向磁场,通过这种方式能够提高铁硅铝合金薄带的饱和磁化强度和磁导率。之后将破碎的铁硅铝合金薄带与铁氧体粉末球磨,借助于球磨时碾压作用,使铁氧体粉末均匀嵌入在铁硅铝合金碎片表面,形成铁氧体绝缘包覆层。本发明通过球磨的方式混合铁氧体粉末和铁硅铝合金碎片不但能够使铁氧体均匀、牢固的包覆在铁硅铝合金碎片表面,而且在铁氧体粉末的用量较低的情况下就能够实现铁氧体粉末对铁硅铝合金表面的完全包覆,降低了铁氧体的引入对于磁粉磁导率的影响,使磁粉的磁导率维持在较高水平,同时球磨还可以实现磁粉的扁平化,从而进一步提高磁粉的磁导率和降低由其制成的磁粉芯的高频损耗。以本发明提供的方法制备的复合磁粉为原料制成的磁粉芯具有高的磁导率和低的高频损耗,应用前景广阔,不仅可用于电讯、雷达,还可应用于吸波及电磁屏蔽领域。实验结果表明,以本发明提供的方法制得的复合磁粉为原料制成的复合磁粉芯在100kHz的测试频率下的有效磁导率高于40,在100kHz,Bm=300mT测试条件下的损耗低于83W/kg。In the present invention, a directional magnetic field is firstly applied during the spin-off process when preparing the sendust aluminum strip, and in this way the saturation magnetization and magnetic permeability of the sendust aluminum strip can be improved. Afterwards, the broken sendust aluminum strip is ball-milled with ferrite powder, and the ferrite powder is evenly embedded on the surface of the sendust aluminum fragment by means of rolling during ball milling to form a ferrite insulating coating layer. The present invention mixes ferrite powder and sendust shards by means of ball milling, not only can ferrite be evenly and firmly coated on the surface of sendust shards, but also when the amount of ferrite powder is low It can realize the complete coating of the surface of sendust aluminum alloy by ferrite powder, reduce the influence of the introduction of ferrite on the magnetic permeability of magnetic powder, and maintain the magnetic permeability of magnetic powder at a high level. At the same time, ball milling can also achieve The flattening of the magnetic powder further improves the magnetic permeability of the magnetic powder and reduces the high-frequency loss of the magnetic powder core made of it. The magnetic powder core made of the composite magnetic powder prepared by the method provided by the present invention has high magnetic permeability and low high-frequency loss, and has broad application prospects. It can be used not only in telecommunications and radar, but also in the fields of wave absorption and electromagnetic shielding . Experimental result shows, with the composite magnetic powder that the method provided by the present invention makes is that the effective magnetic permeability of the composite magnetic powder core that raw material is made is higher than 40 at the test frequency of 100kHz, at 100kHz, the loss under Bm=300mT test condition is low At 83W/kg.
本发明还提供了一种按照上述方法制备得到的复合磁粉,该复合磁粉包括铁硅铝合金磁粉和包覆在所述铁硅铝磁粉表面的铁氧体粉末,该复合磁粉呈扁平状,具有较高的磁导率、较高的饱和磁化强度和较低的高频损耗,应用前景广阔。The present invention also provides a composite magnetic powder prepared according to the above-mentioned method. The composite magnetic powder includes sendust magnetic powder and ferrite powder coated on the surface of the sendust magnetic powder. The composite magnetic powder is flat and has Higher permeability, higher saturation magnetization and lower high-frequency loss, broad application prospects.
本发明还提供了一种复合磁粉芯的制备方法,包括以下步骤:The present invention also provides a preparation method of a composite magnetic powder core, comprising the following steps:
粘结剂、润滑剂和按照上述技术方案所述方法制备得到的复合磁粉依次进行混合和压制,得到复合磁粉芯。The binder, the lubricant, and the composite magnetic powder prepared according to the method described in the above technical solution are mixed and pressed in sequence to obtain a composite magnetic powder core.
在本发明提供的复合磁粉芯的制备方法中,首先将粘结剂、润滑剂和所述复合磁粉进行混合。其中,所述粘结剂优选为环氧树脂;所述粘结剂和复合磁粉的质量比优选为(1~2):100,更优选为1.5:100。所述润滑剂优选为硬脂酸镁;所述润滑剂和复合磁粉的质量比优选为(0.5~2):100,更优选为(1~1.5):100。混合完毕后,进行压制。其中,所述压制的压力优选为1500~2000MPa,更优选为1700~1800MPa;所述压制的时间优选为3~8min。压制完毕后,得到复合磁粉芯。在本发明中,优选对得到的复合磁粉芯进行退火处理,以消除其内部应力,提高磁导率。其中,所述退火处理的温度优选为600~700℃,更优选为650~690℃;所述退火处理的保温时间优选为1~2h。In the preparation method of the composite magnetic powder core provided by the present invention, firstly, the binder, the lubricant and the composite magnetic powder are mixed. Wherein, the binder is preferably epoxy resin; the mass ratio of the binder to the composite magnetic powder is preferably (1-2):100, more preferably 1.5:100. The lubricant is preferably magnesium stearate; the mass ratio of the lubricant to the composite magnetic powder is preferably (0.5-2):100, more preferably (1-1.5):100. After mixing, press. Wherein, the pressing pressure is preferably 1500-2000 MPa, more preferably 1700-1800 MPa; the pressing time is preferably 3-8 minutes. After pressing, a composite magnetic powder core is obtained. In the present invention, it is preferable to anneal the obtained composite magnetic powder core to eliminate its internal stress and increase the magnetic permeability. Wherein, the temperature of the annealing treatment is preferably 600-700° C., more preferably 650-690° C.; the holding time of the annealing treatment is preferably 1-2 hours.
采用本发明提供的方法制得的复合磁粉芯具有高的磁导率和低的高频损耗,应用前景广阔,不仅可用于电讯、雷达,还可应用于吸波及电磁屏蔽领域。实验结果表明,本发明提供的的复合磁粉芯在100kHz的测试频率下的有效磁导率高于40,在100kHz,Bm=300mT测试条件下的损耗低于83W/kg。The composite magnetic powder core prepared by the method provided by the invention has high magnetic permeability and low high-frequency loss, and has broad application prospects. It can be used not only in telecommunications and radar, but also in the fields of wave absorption and electromagnetic shielding. Experimental results show that the effective magnetic permeability of the composite magnetic powder core provided by the present invention is higher than 40 at a test frequency of 100 kHz, and the loss is lower than 83 W/kg under test conditions of 100 kHz and Bm=300mT.
综合评价本发明提供的技术方案,其具有以下优点:Comprehensive evaluation technical scheme that the present invention provides, it has the following advantages:
1)采用感应式熔体快淬设备制取铁硅铝合金薄带,甩带过程中施加定向磁场,使易轴沿外磁场取向,提高了制得的铁硅铝合金薄带的饱和磁化强度和磁导率;1) The induction-type melt quenching equipment is used to prepare the sendust aluminum alloy thin strip, and a directional magnetic field is applied during the stripping process to make the easy axis oriented along the external magnetic field, which improves the saturation magnetization of the prepared sendust aluminum alloy thin strip and magnetic permeability;
2)、采用球磨的方式混合铁氧体粉末和铁硅铝合金碎片,借助于球磨时碾压作用,使铁氧体粉末均匀嵌入在铁硅铝合金碎片表面,形成均匀、牢固的铁氧体绝缘包覆层;避免了铁硅铝磁粉在绝缘包覆过程中易出现的绝缘层不稳定(高温分解)、强度低(压制成型过程中包覆层容易被压破)、不连续及厚度难以控制等问题;2) Mix ferrite powder and sendust debris by ball milling, and use the rolling action of ball milling to embed ferrite powder evenly on the surface of sendust debris to form uniform and firm ferrite Insulation coating layer; avoids the instability of the insulation layer (pyrolysis), low strength (the coating layer is easily crushed during the pressing molding process), discontinuity and difficulty in the thickness of the sendust magnetic powder during the insulation coating process. issues of control;
3)、采用球磨的方式混合铁氧体粉末和铁硅铝合金碎片,可在铁氧体粉末的用量较低的情况下就能够实现铁氧体粉末对铁硅铝合金表面的完全包覆,降低了铁氧体的引入对于磁粉磁导率的影响,使磁粉的磁导率维持在较高水平,为获得高磁导率的磁粉芯提供了技术保障;3) Mixing ferrite powder and sendust fragments by ball milling can completely cover the surface of sendust with ferrite powder when the amount of ferrite powder is low. Reduce the influence of the introduction of ferrite on the magnetic permeability of magnetic powder, maintain the magnetic permeability of magnetic powder at a high level, and provide technical support for obtaining magnetic powder cores with high magnetic permeability;
4)、通过对铁硅铝合金碎片进行球磨,可得到扁平化磁粉,从而进一步提高磁粉的磁导率和降低由其制成的磁粉芯的高频损耗;4) Flattened magnetic powder can be obtained by ball milling the sendust aluminum alloy fragments, thereby further improving the magnetic permeability of the magnetic powder and reducing the high-frequency loss of the magnetic powder core made of it;
5)、优选采用化学共沉淀法制备铁氧体粉末,反应速度快,产率高;5), it is preferable to adopt chemical co-precipitation method to prepare ferrite powder, which has fast reaction speed and high yield;
6)、优选对压制得到的复合磁粉芯进行退火处理,以消除磁粉芯的内应力,进一步提高磁粉芯的磁导率。6) Preferably, the composite magnetic powder core obtained by pressing is annealed to eliminate the internal stress of the magnetic powder core and further increase the magnetic permeability of the magnetic powder core.
为更清楚起见,下面通过以下实施例进行详细说明。For more clarity, detailed description is given below through the following examples.
实施例1Example 1
(1)在感应式熔体快淬设备中制备厚度为5~15μm的标准成分铁硅铝合金带(5.4wt%Al,9.6wt%Si,其余Fe),制备合金带的过程中,甩带时的铜辊转速为60m/s,甩带过程中一直施加1000Oe的定向磁场。得到铁硅铝合金带后,在不锈钢罐中进行破碎,得到铁硅铝合金碎片。(1) In the induction type melt quenching equipment, prepare a standard composition iron-silicon-aluminum alloy strip (5.4wt% Al, 9.6wt% Si, the rest Fe) with a thickness of 5-15 μm. During the preparation of the alloy strip, the strip The rotational speed of the copper roller is 60m/s, and a directional magnetic field of 1000Oe is always applied during the belt throwing process. After the sendust strip is obtained, it is crushed in a stainless steel tank to obtain sendust fragments.
(2)以FeCl3、ZnCl2及MnCl2·4H2O为原料,按Mn0.4Zn0.6Fe2O4中Fe3+、Zn2+、Mn2+的摩尔比n[Fe3+]:n[Zn2+]:n[Mn2+]=10:3:2分别称量需要的原料,加入适量去离子水,不断搅拌使原料颗粒溶解完全,得到Fe-Zn-Mn混合盐溶液,加热到80℃,同时滴入浓度为2mol/L的NaOH溶液,不断搅拌,调节溶液的pH值为10,反应30min,合成锰锌铁氧体前驱体;反应结束后用去离子水洗涤铁氧体前驱体数次,置于干燥箱中在100℃下干燥1h。将干燥后的铁养体前驱体置于马弗炉中在850℃焙烧2h,得到粒径为10nm~2μm的锰锌铁氧体粉末。(2) Using FeCl 3 , ZnCl 2 and MnCl 2 4H 2 O as raw materials, according to the molar ratio n[Fe 3+ ] of Fe 3+ , Zn 2+ , and Mn 2+ in Mn 0.4 Zn 0.6 Fe 2 O 4 : n[Zn 2+ ]:n[Mn 2+ ]=10:3:2 Weigh the required raw materials respectively, add an appropriate amount of deionized water, and stir continuously to completely dissolve the raw material particles to obtain Fe-Zn-Mn mixed salt solution, Heat to 80°C, drop NaOH solution with a concentration of 2mol/L at the same time, keep stirring, adjust the pH value of the solution to 10, and react for 30 minutes to synthesize the precursor of manganese zinc ferrite; after the reaction, wash the ferrite with deionized water The body precursor was dried several times in a drying oven at 100 °C for 1 h. The dried ferrotrophic precursor is placed in a muffle furnace and calcined at 850° C. for 2 hours to obtain MnZn ferrite powder with a particle size of 10 nm˜2 μm.
(3)将铁硅铝合金碎片置于球磨机的不锈钢球磨罐中,按锰锌铁氧体粉末与铁硅铝合金碎片的质量比为2%,将相应质量的锰锌铁氧体粉末放入不锈钢球磨罐中与铁硅铝合金碎片进行球磨;球磨采用的磨球为直径10mm和5mm的钢球,大球与小球的个数比为1:5;球磨时的球料质量比为12:1,球磨机转速为50rpm,球磨30h后,得到铁硅铝/铁氧体复合磁粉。(3) Put the sendust aluminum alloy fragments in the stainless steel ball milling tank of the ball mill, and the mass ratio of the manganese zinc ferrite powder to the sendust aluminum alloy fragments is 2%, put the manganese zinc ferrite powder of corresponding quality into The stainless steel ball milling tank is used for ball milling with FeSiAl alloy fragments; the balls used for ball milling are steel balls with diameters of 10mm and 5mm, and the number ratio of large balls to small balls is 1:5; the mass ratio of balls to materials during ball milling is 12 : 1, the rotating speed of the ball mill is 50rpm, after ball milling for 30 hours, sendust/ferrite composite magnetic powder is obtained.
(4)在得到的复合磁粉中添加复合磁粉质量1.5wt%的环氧树脂和复合磁粉质量1wt.%的硬脂酸镁,之后在1800Mpa下冷压5min,得到复合磁粉芯坯料。(4) Add 1.5wt% epoxy resin and 1wt.% magnesium stearate to the obtained composite magnetic powder, and then cold press at 1800Mpa for 5min to obtain a composite magnetic powder core blank.
(5)将复合磁粉芯坯料在600℃于氮气中退火2h,得到复合磁粉芯制品。(5) Anneal the composite magnetic powder core blank at 600° C. for 2 hours in nitrogen to obtain a composite magnetic powder core product.
实施例2~5Embodiment 2-5
参见实施例1的制备方法,依次调整锰锌铁氧体粉末与铁硅铝合金碎片的质量比为4%、6%、10%、20%,制备得到复合磁粉芯制品。Referring to the preparation method of Example 1, the mass ratios of manganese-zinc-ferrite powder and sendust-aluminum fragments were sequentially adjusted to 4%, 6%, 10%, and 20%, to prepare composite magnetic powder core products.
对比例1Comparative example 1
参见实施例1的制备方法,调整锰锌铁氧体粉末与铁硅铝合金碎片的质量比为0,制备得到复合磁粉芯制品。Referring to the preparation method of Example 1, adjust the mass ratio of manganese zinc ferrite powder and sendust aluminum alloy fragments to 0 to prepare a composite magnetic powder core product.
实施例6Example 6
在100kHz的测试频率下分别测试实施例1~5和对比例1制得的复合磁粉芯制品的有效磁导率,结果如图1所示,图1是本发明实施例6提供的不同配比的复合磁粉芯的有效磁导率,通过图1可以看出,采用实施例1~5提供的方法制得的磁粉芯的有效磁导率高于40。Under the test frequency of 100kHz, test the effective magnetic permeability of the composite magnetic powder core products that embodiment 1~5 and comparative example 1 make respectively, the result is as shown in Figure 1, and Figure 1 is the different proportioning provided by Example 6 of the present invention The effective magnetic permeability of the composite magnetic powder core can be seen from Figure 1 that the effective magnetic permeability of the magnetic powder core prepared by the method provided in Examples 1-5 is higher than 40.
在100kHz,Bm=300mT测试条件下分别测试实施例1~5和对比例1制得的复合磁粉芯制品的的损耗(Core loss),结果如图2所示,图2是本发明实施例6提供的不同配比的复合磁粉芯的损耗,通过图2可以看出,采用实施例1~5提供的方法制得的磁粉芯的损耗低于83W/kg。At 100kHz, the loss (Core loss) of the composite magnetic powder core product that embodiment 1~5 and comparative example 1 make are tested respectively under the test condition of Bm=300mT, and result is as shown in Figure 2, and Figure 2 is embodiment 6 of the present invention The losses of the composite magnetic powder cores provided with different proportions can be seen from FIG. 2 , the losses of the magnetic powder cores prepared by the method provided in Examples 1-5 are lower than 83W/kg.
实施例7Example 7
(1)在感应式熔体快淬设备中制备厚度为5~15μm的标准成分铁硅铝合金带(5.4wt%Al,9.6wt%Si,其余Fe),制备合金带的过程中,甩带时的铜辊转速为60m/s,甩带过程中一直施加1000Oe的定向磁场。得到铁硅铝合金带后,在不锈钢罐中进行破碎,得到铁硅铝合金碎片。(1) In the induction type melt quenching equipment, prepare a standard composition iron-silicon-aluminum alloy strip (5.4wt% Al, 9.6wt% Si, the rest Fe) with a thickness of 5-15 μm. During the preparation of the alloy strip, the strip The rotational speed of the copper roller is 60m/s, and a directional magnetic field of 1000Oe is always applied during the belt throwing process. After the sendust strip is obtained, it is crushed in a stainless steel tank to obtain sendust fragments.
(2)以FeCl3、ZnCl2及MnCl2·4H2O为原料,按Mn0.4Zn0.6Fe2O4中Fe3+、Zn2+、Mn2+的摩尔比n[Fe3+]:n[Zn2+]:n[Mn2+]=10:3:2分别称量需要的原料,加入适量去离子水,不断搅拌使原料颗粒溶解完全,得到Fe-Zn-Mn混合盐溶液,加热到80℃,同时滴入浓度为2mol/L的NaOH溶液,不断搅拌,调节溶液的pH值为10,反应30min,合成锰锌铁氧体前驱体;反应结束后用去离子水洗涤铁氧体前驱体数次,置于干燥箱中在100℃下干燥1h。将干燥后的铁养体前驱体置于马弗炉中在850℃焙烧2h,得到粒径为10nm~2μm的锰锌铁氧体粉末。(2) Using FeCl 3 , ZnCl 2 and MnCl 2 4H 2 O as raw materials, according to the molar ratio n[Fe 3+ ] of Fe 3+ , Zn 2+ , and Mn 2+ in Mn 0.4 Zn 0.6 Fe 2 O 4 : n[Zn 2+ ]:n[Mn 2+ ]=10:3:2 Weigh the required raw materials respectively, add an appropriate amount of deionized water, and stir continuously to completely dissolve the raw material particles to obtain Fe-Zn-Mn mixed salt solution, Heat to 80°C, drop NaOH solution with a concentration of 2mol/L at the same time, keep stirring, adjust the pH value of the solution to 10, and react for 30 minutes to synthesize the precursor of manganese zinc ferrite; after the reaction, wash the ferrite with deionized water The body precursor was dried several times in a drying oven at 100 °C for 1 h. The dried ferrotrophic precursor is placed in a muffle furnace and calcined at 850° C. for 2 hours to obtain MnZn ferrite powder with a particle size of 10 nm˜2 μm.
(3)将铁硅铝合金碎片置于球磨机的不锈钢球磨罐中,按锰锌铁氧体粉末与铁硅铝合金碎片的质量比为6%,将相应质量的锰锌铁氧体粉末放入不锈钢球磨罐中与铁硅铝合金碎片进行球磨;球磨采用的磨球为直径10mm和5mm的钢球,大球与小球的个数比为1:5;球磨时的球料质量比为12:1,球磨机转速为50rpm,球磨30h,球磨结束后,得到铁硅铝/铁氧体复合磁粉。(3) Put the sendust aluminum alloy fragments in the stainless steel ball milling tank of the ball mill, and the mass ratio of the manganese zinc ferrite powder to the sendust aluminum alloy fragments is 6%, put the manganese zinc ferrite powder of the corresponding quality into The stainless steel ball milling tank is used for ball milling with FeSiAl alloy fragments; the balls used for ball milling are steel balls with diameters of 10mm and 5mm, and the number ratio of large balls to small balls is 1:5; the mass ratio of balls to materials during ball milling is 12 : 1, the rotating speed of the ball mill is 50rpm, the ball mill is 30h, and after the ball mill is finished, sendust/ferrite composite magnetic powder is obtained.
(4)在得到的复合磁粉中添加复合磁粉质量1.5wt%的环氧树脂和复合磁粉质量1wt.%的硬脂酸镁,之后在1800Mpa下冷压5min,得到复合磁粉芯坯料。(4) Add 1.5wt% epoxy resin and 1wt.% magnesium stearate to the obtained composite magnetic powder, and then cold press at 1800Mpa for 5min to obtain a composite magnetic powder core blank.
(5)将复合磁粉芯坯料在600℃于氮气中退火1h,得到复合磁粉芯制品。(5) Anneal the composite magnetic powder core blank at 600° C. for 1 h in nitrogen to obtain a composite magnetic powder core product.
实施例8~11Embodiment 8~11
参见实施例7的制备方法,依次调整复合磁粉芯坯料退火的温度为630℃、660℃、690℃、720℃,制备得到复合磁粉芯制品。Referring to the preparation method in Example 7, the annealing temperature of the composite magnetic powder core blank was sequentially adjusted to 630° C., 660° C., 690° C., and 720° C. to prepare a composite magnetic powder core product.
实施例12Example 12
在100kHz的测试频率下分别测试实施例7~11制得的复合磁粉芯制品的有效磁导率,结果如图3所示,图3是本发明实施例12提供的不同退火温度的复合磁粉芯的有效磁导率,通过图3可以看出,采用实施例7~11提供的方法制得的磁粉芯的有效磁导率高于60。Under the test frequency of 100kHz, test the effective magnetic permeability of the composite magnetic powder core products that embodiment 7~11 makes respectively, the result is as shown in Figure 3, and Figure 3 is the composite magnetic powder core of the different annealing temperature that embodiment 12 of the present invention provides It can be seen from FIG. 3 that the effective magnetic permeability of the magnetic powder core prepared by the method provided in Examples 7-11 is higher than 60.
在100kHz,Bm=300mT测试条件下分别测试实施例7~11制得的复合磁粉芯制品的的损耗(Core loss),结果如图4所示,图4是本发明实施例12提供的不同退火温度的复合磁粉芯的损耗,通过图4可以看出,采用实施例7~11提供的方法制得的磁粉芯的损耗低于68W/kg。At 100kHz, the loss (Core loss) of the composite magnetic powder core product that embodiment 7~11 makes is tested respectively under the test condition of Bm=300mT, and the result is as shown in Figure 4, and Figure 4 is the different annealing that embodiment 12 of the present invention provides The loss of the composite magnetic powder core according to the temperature can be seen from Figure 4, the loss of the magnetic powder core prepared by the method provided in Examples 7-11 is lower than 68W/kg.
对比例2Comparative example 2
参见实施例1的制备方法,只是在甩带过程中没有施加定向磁场,锰锌铁氧体粉末与铁硅铝合金碎片的质量比为6%,制备得到复合磁粉芯制品,在690℃于氮气中退火1h后,检测有效磁导率及损耗。在100kHz的测试频率下有效磁导率仅为51.2。在100kHz,Bm=300mT测试条件下损耗为71W/kg。Refer to the preparation method of Example 1, except that no directional magnetic field is applied during the stripping process, the mass ratio of manganese-zinc-ferrite powder to sendust aluminum alloy fragments is 6%, and a composite magnetic powder core product is prepared. After medium annealing for 1 hour, detect the effective permeability and loss. The effective permeability is only 51.2 at the test frequency of 100kHz. Under the test conditions of 100kHz and Bm=300mT, the loss is 71W/kg.
以上所述仅是本发明的优选实施方式,应当指出,对于本技术领域的普通技术人员来说,在不脱离本发明原理的前提下,还可以做出若干改进和润饰,这些改进和润饰也应视为本发明的保护范围。The above is only a preferred embodiment of the present invention, it should be pointed out that, for those of ordinary skill in the art, without departing from the principle of the present invention, some improvements and modifications can also be made, and these improvements and modifications can also be made. It should be regarded as the protection scope of the present invention.
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