CN107393672B - Iron-nickel-based nanocrystalline magnetic core and preparation method thereof - Google Patents
Iron-nickel-based nanocrystalline magnetic core and preparation method thereof Download PDFInfo
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- UGKDIUIOSMUOAW-UHFFFAOYSA-N iron nickel Chemical compound [Fe].[Ni] UGKDIUIOSMUOAW-UHFFFAOYSA-N 0.000 title claims abstract description 96
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- 229910052796 boron Inorganic materials 0.000 claims abstract description 11
- 229910052802 copper Inorganic materials 0.000 claims abstract description 11
- 229910052758 niobium Inorganic materials 0.000 claims abstract description 11
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 11
- 229910001030 Iron–nickel alloy Inorganic materials 0.000 claims abstract description 8
- 238000000137 annealing Methods 0.000 claims description 44
- 238000010438 heat treatment Methods 0.000 claims description 38
- 238000000034 method Methods 0.000 claims description 36
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- 229910045601 alloy Inorganic materials 0.000 claims description 24
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- 238000010791 quenching Methods 0.000 claims description 20
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- 239000007789 gas Substances 0.000 claims description 15
- 238000007598 dipping method Methods 0.000 claims description 13
- 239000002994 raw material Substances 0.000 claims description 13
- 229910052757 nitrogen Inorganic materials 0.000 claims description 10
- 229910052739 hydrogen Inorganic materials 0.000 claims description 9
- 239000001257 hydrogen Substances 0.000 claims description 9
- 238000003723 Smelting Methods 0.000 claims description 8
- 229910052804 chromium Inorganic materials 0.000 claims description 8
- 229910052732 germanium Inorganic materials 0.000 claims description 8
- 229910052750 molybdenum Inorganic materials 0.000 claims description 8
- 230000000171 quenching effect Effects 0.000 claims description 8
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- 229910052720 vanadium Inorganic materials 0.000 claims description 7
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 6
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- 230000035699 permeability Effects 0.000 abstract description 20
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- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 abstract description 12
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- 229910052742 iron Inorganic materials 0.000 description 6
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- 229910052759 nickel Inorganic materials 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
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- 229910052782 aluminium Inorganic materials 0.000 description 1
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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
- H01F1/14—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 metals or alloys
- H01F1/147—Alloys characterised by their composition
- H01F1/14708—Fe-Ni based alloys
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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
- H01F41/0206—Manufacturing of magnetic cores by mechanical means
- H01F41/0213—Manufacturing of magnetic circuits made from strip(s) or ribbon(s)
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Abstract
本发明涉及高频逆变电源技术领域，具体涉及一种铁镍基纳米晶磁芯及其制备方法，所述铁镍基纳米晶磁芯由铁镍合金制成，所述铁镍基纳米晶带材包括如下重量百分比的元素：Ni：15%‑25%、Si：10%‑12%、B：3%‑5%、Nb：2%‑4%、Cu：0.3%‑0.5%、Co：4%‑8%，余量为Fe。本发明的铁镍基纳米晶磁芯具有稳定的磁导率和直流偏置能力，还具有高饱和磁感应强度、低损耗值、低矫顽力、耐高温等优点，综合性能优良。The invention relates to the technical field of high-frequency inverter power supplies, in particular to an iron-nickel-based nanocrystalline magnetic core and a preparation method thereof, wherein the iron-nickel-based nanocrystalline magnetic core is made of an iron-nickel alloy, and the iron-nickel-based nanocrystalline The strip includes the following elements by weight: Ni: 15%-25%, Si: 10%-12%, B: 3%-5%, Nb: 2%-4%, Cu: 0.3%-0.5%, Co : 4%-8%, the balance is Fe. The iron-nickel-based nanocrystalline magnetic core of the invention has stable magnetic permeability and DC bias capability, and also has the advantages of high saturation magnetic induction intensity, low loss value, low coercive force, high temperature resistance, etc., and excellent comprehensive performance.
Description
技术领域technical field
本发明涉及高频逆变电源技术领域，具体涉及一种铁镍基纳米晶磁芯及其制备方法。The invention relates to the technical field of high-frequency inverter power supplies, in particular to an iron-nickel-based nanocrystalline magnetic core and a preparation method thereof.
背景技术Background technique
软磁材料是具有低矫顽力和高磁导率的磁性材料，软磁材料易于磁化，也易于退磁，所以被广泛应用于电工设备和电子设备中。其中，铁基非晶合金作为目前常用的一种铁芯软磁材料，主要由Fe元素和Si、B类金属元素所构成，它具有高饱和磁感应强度、高磁导率与低铁芯损耗等特点，可广泛应用于配电变压器、大功率开关电源、脉冲变压器、磁放大器、中频变压器及逆变器铁芯。Soft magnetic materials are magnetic materials with low coercivity and high permeability. Soft magnetic materials are easy to magnetize and easy to demagnetize, so they are widely used in electrical and electronic equipment. Among them, iron-based amorphous alloy, as a commonly used iron core soft magnetic material, is mainly composed of Fe element and Si and B metal elements. It has high saturation magnetic induction intensity, high magnetic permeability and low iron core loss, etc. It can be widely used in distribution transformers, high-power switching power supplies, pulse transformers, magnetic amplifiers, intermediate frequency transformers and inverter cores.
申请号为CN103258612A的专利申请文件中公开了一种低导磁磁芯及其制造方法与用途，该磁芯材质是铁基非晶态，磁导率在500～5000之间，矫顽力磁场强度的值小于10Am-1，磁芯材质制备时的退火温度为350℃～500℃，退火时间在2h以内。由于铁基非晶态材料的磁芯磁致伸缩系数较高，同时由于制备时的退火温度较低，退火时间较短，从而使去应力热处理不够充分，进而导致应力没有完全消除，影响了恒导磁的磁导率的线性度；另外，由于该磁芯的磁导率较低，而且软磁特性如矫顽力较高，铁芯损耗较大，不适用于高频和高电感的使用环境中。The patent application document with the application number CN103258612A discloses a low magnetic permeability magnetic core and its manufacturing method and application. The value of the strength is less than 10Am -1 , the annealing temperature during the preparation of the magnetic core material is 350°C to 500°C, and the annealing time is within 2 hours. Due to the high magnetostriction coefficient of the magnetic core of the iron-based amorphous material, and the low annealing temperature and short annealing time during preparation, the stress relief heat treatment is not sufficient, and the stress is not completely eliminated, which affects the constant The linearity of the magnetic permeability of the magnetic permeability; in addition, due to the low permeability of the magnetic core, and the soft magnetic properties such as high coercivity, the core loss is large, and it is not suitable for the use of high frequency and high inductance Environment.
随着新兴电子产业发展，对软磁材料提出了更多更高的要求，例如光伏、风电、变频拖动等逆变电源的进展，对电磁兼容的关键元器件电感提出了具有高电感量、高抗饱和性能、优异的MHz级的频率特性等要求，因此在铁基非晶态材料的基础上，铁基纳米晶合金应运而生。该类合金以铁元素为主，同时加入少量的Nb、Cu、Si、B等元素。上述元素构成的合金经快速凝固工艺会首先形成一种非晶态材料，该非晶态材料再经过晶化热处理后可获得直径为10～20nm的纳米晶粒主相,同时还保留少量的非晶残留相，总体简称为纳米晶材料。纳米晶材料具有高饱和磁感应强度、高初始磁导率和低矫顽力等综合磁性能，纳米晶材料制成的磁芯在高频、高磁感下具有很低的铁芯损耗，并且具有极小的磁致伸缩系数以及极强的感生各向异性常数Ku，在经过纵向或横向磁场处理后，可得到高剩余磁感应强度值或低剩余磁感应强度值的磁芯，可广泛的适用不同的频率范围内。纳米晶磁芯广泛应用于大功率开关电源、逆变电源、磁放大器、高频变压器、高频变换器、高频扼流圈铁芯、电流互感器铁芯、漏电保护开关和共模电感铁芯中。With the development of the emerging electronic industry, more and higher requirements have been put forward for soft magnetic materials, such as the progress of photovoltaic, wind power, variable frequency drive and other inverter power supplies. High anti-saturation performance, excellent frequency characteristics of MHz level and other requirements, so on the basis of iron-based amorphous materials, iron-based nanocrystalline alloys came into being. This type of alloy is mainly composed of iron element, and a small amount of Nb, Cu, Si, B and other elements are added at the same time. The alloy composed of the above elements will firstly form an amorphous material through a rapid solidification process, and the amorphous material will be subjected to crystallization and heat treatment to obtain a nano-grain main phase with a diameter of 10-20 nm, while retaining a small amount of amorphous material. The crystalline residual phase is generally referred to as nanocrystalline material. Nanocrystalline materials have comprehensive magnetic properties such as high saturation magnetic induction, high initial permeability and low coercivity. The magnetic core made of nanocrystalline materials has very low core loss at high frequency and high magnetic induction, and has The extremely small magnetostriction coefficient and the extremely strong induced anisotropy constant Ku can obtain a magnetic core with a high residual magnetic induction intensity value or a low residual magnetic induction intensity value after being treated with a longitudinal or transverse magnetic field, which can be widely used in different within the frequency range. Nanocrystalline magnetic cores are widely used in high-power switching power supplies, inverter power supplies, magnetic amplifiers, high-frequency transformers, high-frequency converters, high-frequency choke coil cores, current transformer cores, leakage protection switches and common mode inductors. in the core.
现有的磁芯产品主要有铁芯、铁硅铝磁芯、铁镍磁芯、MPP磁芯等。常规的铁镍磁芯在1MHz 的频率范围内具有极佳的频率特性，并且损耗较低,具有最高的直流偏置能力，产品性能好。但是铁镍磁芯中还有50%的镍，价格高昂，生产成本高。The existing magnetic core products mainly include iron core, iron silicon aluminum magnetic core, iron nickel magnetic core, MPP magnetic core and so on. Conventional iron-nickel cores have excellent frequency characteristics in the frequency range of 1MHz, and have low loss, the highest DC bias capability, and good product performance. However, there is still 50% nickel in the iron-nickel core, which is expensive and expensive to produce.
发明内容SUMMARY OF THE INVENTION
为了克服现有技术中存在的缺点和不足，本发明的目的在于提供一种铁镍基纳米晶磁芯，该铁镍基纳米晶磁芯具有稳定的磁导率和直流偏置能力，还具有高饱和磁感应强度、低损耗值、低矫顽力、耐高温等优点，综合性能优良。In order to overcome the shortcomings and deficiencies in the prior art, the purpose of the present invention is to provide an iron-nickel-based nanocrystalline magnetic core, the iron-nickel-based nanocrystalline magnetic core has stable magnetic permeability and DC bias capability, and also has High saturation magnetic induction, low loss value, low coercivity, high temperature resistance and other advantages, excellent comprehensive performance.
本发明的另一目的在于提供一种铁镍基纳米晶磁芯的制备方法，该制备方法工艺简单，操作控制方便，质量稳定，生产效率高，生产成本低，可大规模工业化生产。Another object of the present invention is to provide a preparation method of an iron-nickel-based nanocrystalline magnetic core, which is simple in process, convenient in operation and control, stable in quality, high in production efficiency, low in production cost, and capable of large-scale industrial production.
本发明的目的通过下述技术方案实现：一种铁镍基纳米晶磁芯，所述铁镍基纳米晶磁芯由铁镍合金制成，所述铁镍基纳米晶带材包括如下重量百分比的元素：Ni：15%-25%、Si：10%-12%、B：3%-5%、Nb：2%-4%、Cu：0.3%-0.5%、Co：4%-8%，余量为Fe。The purpose of the present invention is achieved through the following technical solutions: an iron-nickel-based nanocrystalline magnetic core, the iron-nickel-based nanocrystalline magnetic core is made of an iron-nickel alloy, and the iron-nickel-based nanocrystalline tape includes the following weight percentages Elements: Ni: 15%-25%, Si: 10%-12%, B: 3%-5%, Nb: 2%-4%, Cu: 0.3%-0.5%, Co: 4%-8% , the remainder is Fe.
非晶形成元素Si、B，铁基纳米晶软磁合金一般都是在非晶态合金基础上，通过合适的晶化退火使其形成纳米晶材料，因而非晶化元素是基本组成元素，特别是B元素，其原子半径较小，外层电子多，非常有利于形成非晶态合金，Si也是重要的非晶化元素，在本发明中，含Si量高于18at％将使合金的饱和磁化强度降低，而含Si量低于7at％则不易形成非晶态，同时，Si元素还是α-Fe(Si)纳米晶相的构成元素；Amorphous forming elements Si, B, and iron-based nanocrystalline soft magnetic alloys are generally based on amorphous alloys, through appropriate crystallization annealing to form nanocrystalline materials, so amorphizing elements are the basic constituent elements, especially It is B element, which has a small atomic radius and many outer electrons, which is very beneficial to the formation of amorphous alloys. Si is also an important amorphization element. In the present invention, the content of Si higher than 18at% will make the alloy saturated The magnetization decreases, and the Si content is less than 7at%, it is difficult to form an amorphous state, and at the same time, Si element is also a constituent element of α-Fe(Si) nanocrystalline phase;
纳米晶形成元素Cu、Nb，晶化时Cu首先与Fe分离，形成该金属元素的富集区，为纳米晶化起形核作用，Nb元素扩散缓慢，主要作用是阻碍α-Fe晶粒的长大，从而保证晶粒尺寸在纳米量级，Cu、Nb含量的控制对于保持磁芯的微观组织结构非常重要。Nanocrystal forming elements Cu and Nb. During crystallization, Cu is first separated from Fe to form the enrichment area of this metal element, which plays a role in nucleation for nanocrystallization. To ensure that the grain size is in the nanometer scale, the control of Cu and Nb content is very important to maintain the microstructure of the magnetic core.
加入 Cu 元素可以在随后的非晶晶化初始阶段形成高密度 α 相结晶晶核，以作为纳米尺寸结晶的生长中心。The addition of Cu element can form high-density α-phase crystal nuclei in the subsequent initial stage of amorphization as the growth center of nano-sized crystals.
本发明的铁镍基纳米晶磁芯在传统的铁基纳米晶磁芯的配方上作出了改良，增加了适当比例的金属镍，制备出的纳米晶磁芯具有更佳的韧性、耐温性和导磁率。The iron-nickel-based nanocrystalline magnetic core of the present invention is improved on the formula of the traditional iron-based nanocrystalline magnetic core, and an appropriate proportion of metal nickel is added, and the prepared nanocrystalline magnetic core has better toughness and temperature resistance. and magnetic permeability.
本发明的铁镍基纳米晶磁芯中用Co元素代替部分Fe，可以明显提高磁芯的高温、高频特性和品质因数，磁芯的居里温度、磁化强度比Co置换Fe前明显提高。In the iron-nickel-based nanocrystalline magnetic core of the present invention, Co element is used to replace part of Fe, which can obviously improve the high temperature, high frequency characteristics and quality factor of the magnetic core, and the Curie temperature and magnetization of the magnetic core are significantly higher than those before Co replaces Fe.
本发明的铁镍基纳米晶磁芯采用Al、Ni部分取代磁芯中的贵金属Nb，添加Nb有利于提高磁芯的饱和磁感强度，添加Al有利于矫顽力的降低，同时可以明显降低磁芯的生产成本。The iron-nickel-based nanocrystalline magnetic core of the present invention adopts Al and Ni to partially replace the precious metal Nb in the magnetic core. The addition of Nb is beneficial to improve the saturation magnetic induction intensity of the magnetic core, and the addition of Al is beneficial to the reduction of the coercive force, and at the same time, it can be significantly reduced The production cost of the magnetic core.
本发明的铁镍基纳米晶带材通过采用上述元素，并严格控制各原料的重量百分比，制得的铁镍基纳米晶磁芯具有稳定的磁导率和直流偏置能力，还具有高饱和磁感应强度、低损耗值、低矫顽力、耐高温等优点，综合性能优良。The iron-nickel-based nanocrystalline tape of the present invention adopts the above elements and strictly controls the weight percentage of each raw material, so that the prepared iron-nickel-based nanocrystalline magnetic core has stable magnetic permeability and DC bias capability, and also has high saturation Magnetic induction intensity, low loss value, low coercivity, high temperature resistance and other advantages, excellent comprehensive performance.
优选的，所述铁镍基纳米晶带材还包括Ga：0.4%-0.8%、V：0.1%-0.5%和Ti：0.2%-0.6%。Preferably, the iron-nickel-based nanocrystalline ribbon further comprises Ga: 0.4%-0.8%, V: 0.1%-0.5% and Ti: 0.2%-0.6%.
本发明的铁镍基纳米晶带材通过增加Ga、V和Ti元素，并严格控制各原料的重量百分比，可以提高合金的第一次晶化温度，从而降低了两次晶化温度间的差距。The iron-nickel-based nanocrystalline ribbon of the present invention can increase the first crystallization temperature of the alloy by increasing the elements of Ga, V and Ti, and strictly controlling the weight percentage of each raw material, thereby reducing the gap between the two crystallization temperatures. .
优选的，所述铁镍基纳米晶带材还包括Mn：1%-3%、Cr：0.5%-1.5%和Mo：0.8%-1.2%。Preferably, the iron-nickel-based nanocrystalline ribbon further comprises Mn: 1%-3%, Cr: 0.5%-1.5% and Mo: 0.8%-1.2%.
本发明的铁镍基纳米晶带材通过增加Mn、Cr和Mo元素，并严格控制各原料的重量百分比，可以使材料形成较强的退火感生各向异性常数，在横磁退火过程中形成可控调节的横向磁各向异性，以达到线性磁导率和抗饱和的特性。The iron-nickel-based nanocrystalline ribbon of the present invention can form a strong annealing-induced anisotropy constant by increasing the elements of Mn, Cr and Mo and strictly controlling the weight percentage of each raw material, which is formed during the transverse magnetic annealing process. Controllable tunable transverse magnetic anisotropy to achieve linear permeability and anti-saturation properties.
优选的，所述铁镍基纳米晶带材还包括C：1.2%-1.4%、Ge：0.01%-0.05%和P：0.001%-0.005%。Preferably, the iron-nickel-based nanocrystalline ribbon further comprises C: 1.2%-1.4%, Ge: 0.01%-0.05% and P: 0.001%-0.005%.
本发明的铁镍基纳米晶带材通过增加C、Ge和P元素，并严格控制各原料的重量百分比，可以提高合金的第一次晶化温度，从而降低了两次晶化温度间的差距。The iron-nickel-based nanocrystalline ribbon of the present invention can increase the first crystallization temperature of the alloy by increasing C, Ge and P elements and strictly controlling the weight percentage of each raw material, thereby reducing the gap between the two crystallization temperatures .
优选的，所述铁镍基纳米晶带材还包括Vb：1.4%-1.8%、Ta：0.3%-0.7%和W：0.04%-0.08%。Preferably, the iron-nickel-based nanocrystalline ribbon further comprises Vb: 1.4%-1.8%, Ta: 0.3%-0.7% and W: 0.04%-0.08%.
本发明的铁镍基纳米晶带材通过增加Vb、Ta和W元素，并严格控制各原料的重量百分比，可以阻止纳米晶晶粒长大，维持并最终形成纳米级的晶体尺寸结构。The iron-nickel-based nanocrystalline ribbon of the present invention can prevent the growth of nanocrystalline grains by increasing the elements of Vb, Ta and W and strictly controlling the weight percentage of each raw material, and maintain and finally form a nanoscale crystal size structure.
一种铁镍基纳米晶磁芯的制备方法，包括如下步骤：A preparation method of an iron-nickel-based nanocrystalline magnetic core, comprising the following steps:
（1）将上述组分的铁镍基纳米晶带材原料进行冶炼，得到合金熔体；(1) smelting the iron-nickel-based nanocrystalline ribbon raw materials of the above components to obtain an alloy melt;
（2）采用单辊急冷法将合金熔体进行喷制，得到铁镍基纳米晶带材；(2) The alloy melt is sprayed by a single-roller quenching method to obtain an iron-nickel-based nanocrystalline strip;
（3）将铁镍基纳米晶带材卷绕成环形纳米晶磁芯；(3) Winding the iron-nickel-based nanocrystalline ribbon into a ring-shaped nanocrystalline magnetic core;
（4）将纳米晶磁芯放入真空退火炉内进行热处理；(4) Put the nanocrystalline magnetic core into the vacuum annealing furnace for heat treatment;
（5）将热处理后的纳米晶磁芯放入真空退火炉内再次进行热处理。(5) Put the heat-treated nanocrystalline magnetic core into a vacuum annealing furnace for heat treatment again.
优选的，所述步骤（3）中，铁镍基纳米晶带材的厚度为15-25μm，宽度为20-30mm。本发明通过严格控制铁镍基纳米晶带材的厚度和宽度，使得铁镍基纳米晶磁芯在保持良好的电感量、较高的品质因数的同时，降低了产品的损耗值，提高了直流偏置能力。Preferably, in the step (3), the iron-nickel-based nanocrystalline tape has a thickness of 15-25 μm and a width of 20-30 mm. The invention strictly controls the thickness and width of the iron-nickel-based nanocrystalline strip, so that the iron-nickel-based nanocrystalline magnetic core maintains good inductance and high quality factor, reduces the loss value of the product, and improves the direct current. Biasing capability.
优选的，所述步骤（4）和所述步骤（5）中，热处理的步骤为：Preferably, in the step (4) and the step (5), the step of heat treatment is:
a) 经过110-130min把炉内温度从室温升温至640-660K；a) After 110-130min, the temperature in the furnace is raised from room temperature to 640-660K;
b) 在643-663K保温15-25min后，用32-40min升温至750-770K；b) After keeping the temperature at 643-663K for 15-25min, use 32-40min to heat up to 750-770K;
c) 在753-773K保温35-45min后，用11-15min升温至790-810K；c) After keeping the temperature at 753-773K for 35-45min, use 11-15min to heat up to 790-810K;
d) 在793-813K保温55-65min后，用10-14min升温至825-845K；d) After 793-813K heat preservation for 55-65min, use 10-14min to heat up to 825-845K;
e) 在828-848K保温35-45min后，退出炉罩强风把炉体温度急冷至340-360K，打开炉门把纳米晶磁芯取出；e) After keeping the temperature at 828-848K for 35-45min, exit the furnace hood with strong wind to quench the furnace body temperature to 340-360K, open the furnace door and take out the nanocrystalline magnetic core;
f) 把从炉内取出的纳米晶磁芯放在冷却架上再强风急冷至常温。f) Put the nanocrystalline magnetic core taken out from the furnace on the cooling rack and then quench it with strong wind to room temperature.
本发明的退火工艺用常规格退火炉把所要热处理的纳米晶磁芯通过两次相同热处理工艺以达到横磁炉降低纳米晶磁芯Ｂr的电性要求，简化了热处理工艺，工艺简单，减少了生产设备投入，还可以节省电力成本25%以上，生产成本低。通过本发明的退火工艺制得的纳米晶磁芯具有稳定的磁导率和直流偏置能力，还具有高饱和磁感应强度、低损耗值、低矫顽力、耐高温等优点，综合性能优良。The annealing process of the invention uses a conventional lattice annealing furnace to pass the nanocrystalline magnetic core to be heat-treated twice through the same heat treatment process to meet the electrical requirements of the transverse magnetic furnace to reduce the Br of the nanocrystalline magnetic core, which simplifies the heat treatment process, the process is simple, and the Investment in production equipment can also save more than 25% of electricity costs, and production costs are low. The nanocrystalline magnetic core prepared by the annealing process of the invention has stable magnetic permeability and DC bias capability, and also has the advantages of high saturation magnetic induction intensity, low loss value, low coercive force, high temperature resistance, etc., and excellent comprehensive performance.
优选的，所述步骤（4）和所述步骤（5）中，真空退火炉内的真空度小于-0.1Mpa，真空退火炉内充有混合气体，混合气体由体积百分比为10%-20%的氢气和体积百分比为80%-90%的氮气组成。Preferably, in the step (4) and the step (5), the vacuum degree in the vacuum annealing furnace is less than -0.1Mpa, the vacuum annealing furnace is filled with mixed gas, and the mixed gas is 10%-20% by volume The composition of hydrogen and nitrogen is 80%-90% by volume.
本发明通过严格控制真空退火炉内的真空度，并在真空退火炉内充入氮氢混合气体，可以提高纳米晶磁芯的磁导率。注入氮气后，氮气主要起到均匀温度的作用，氮气就是热量的传导介质，使炉内磁芯均匀的受热，从而使磁芯的温度均匀、平衡，纳米晶磁芯的磁导率与在退火炉气氛有关 ,退火炉的气氛不同时，磁导率有一定的差异；经过试验得出以下结论，磁芯的磁导率变化规律是：退火炉内的抽真空之后比没有抽真空之前好；抽真空再充入氮氢混合气体，比只抽真空要好。The invention can improve the magnetic permeability of the nanocrystalline magnetic core by strictly controlling the vacuum degree in the vacuum annealing furnace and filling the nitrogen-hydrogen mixed gas in the vacuum annealing furnace. After the nitrogen is injected, nitrogen mainly plays the role of uniform temperature. Nitrogen is the heat conduction medium, so that the magnetic core in the furnace is evenly heated, so that the temperature of the magnetic core is uniform and balanced. The atmosphere of the furnace is related. When the atmosphere of the annealing furnace is different, the magnetic permeability has a certain difference; after the experiment, the following conclusions are drawn, the change rule of the magnetic permeability of the magnetic core is: after the vacuum in the annealing furnace is better than before the vacuum; Vacuuming and then filling with nitrogen-hydrogen mixture is better than vacuuming only.
优选的，所述步骤（5）之后还包括步骤（6）将再次进行热处理后的纳米晶磁芯进行浸胶固化处理。Preferably, the step (5) further includes a step (6) of dipping and curing the nanocrystalline magnetic core after the heat treatment again.
所述步骤（6）中，浸胶固化处理包括如下步骤：In the step (6), the dipping and curing treatment includes the following steps:
A、将纳米晶磁芯在60-70℃温度下进行预热；A. Preheat the nanocrystalline magnetic core at a temperature of 60-70 °C;
B、采用环氧树脂胶漆作为固化剂，将环氧树脂胶漆在水浴60-70℃环境下加热；并用稀释剂以胶漆与稀释剂的比例为0.8-1.2:1来配兑稀释，稀释后的胶漆在60-70℃下保温40-80min；B. Using epoxy resin glue paint as curing agent, heat the epoxy resin glue paint in a water bath at 60-70 ℃; and use thinner to mix and dilute it with a ratio of glue paint and thinner of 0.8-1.2:1, The diluted glue paint is kept at 60-70℃ for 40-80min;
C、将预热后的纳米晶磁芯浸于配兑后的热胶漆中，采用真空含浸的方式，含浸30-50min，真空度为0.6-0.8Mpa；C. Immerse the preheated nanocrystalline magnetic core in the mixed hot glue paint, and use the method of vacuum impregnation for 30-50min, and the vacuum degree is 0.6-0.8Mpa;
D、将含浸后的纳米晶磁芯采用三段保温法固化，第一段温度60-80℃，保温40-80min；第二段温度100-120℃，保温80-120min；第三段温度140-160℃，保温80-120min；自然冷却。D. The impregnated nanocrystalline magnetic core is cured by three-stage heat preservation method. The temperature of the first stage is 60-80°C, and the temperature is kept for 40-80min; the temperature of the second stage is 100-120°C, and the temperature is kept for 80-120min; -160℃, heat preservation for 80-120min; natural cooling.
为解决纳米晶磁芯的固化方式问题，该方法的固化步骤采用了高粘接强度、低应力胶水固化成型，即环氧树脂胶漆。含浸前先预热胶漆和纳米晶磁芯，使得两者的温度均保持在60-70℃，当环氧树脂胶漆在70℃左右时，活性增加，粘度会下降，这样就可以保证在淋胶时，多余的胶漆能通过自身的重力作用流出纳米晶磁芯的内部，保证了纳米晶磁芯的表面干净，不影响磁芯后续的切割精度。其次，为进一步地改善胶漆的粘度和加热后的流动性，采用丙酮为稀释剂吗，胶漆与稀释剂以0.8-1.2:1的比例配兑。并且含浸后采用三段保温法固化，使配兑的胶漆在高温的情况下在纳米晶磁芯表面形成密封膜，保证胶漆存留在纳米晶磁芯内部，解决了现有常规方式的油漆渗漏及强度低等问题，同时胶漆的高强度和低应力对最终切割的不破损和镜面要求起到助力作用。In order to solve the problem of the curing method of the nanocrystalline magnetic core, the curing step of the method adopts high bonding strength, low stress glue curing and molding, that is, epoxy resin glue. Before impregnation, preheat the glue paint and the nanocrystalline magnetic core, so that the temperature of both is kept at 60-70℃. When the epoxy resin glue paint is about 70℃, the activity increases and the viscosity decreases. When the glue is poured, the excess glue paint can flow out of the inside of the nanocrystalline magnetic core through its own gravity, which ensures that the surface of the nanocrystalline magnetic core is clean and does not affect the subsequent cutting accuracy of the magnetic core. Secondly, in order to further improve the viscosity of the glue paint and the fluidity after heating, acetone is used as the thinner, and the glue paint and the thinner are mixed in a ratio of 0.8-1.2:1. And after the impregnation, the three-stage heat preservation method is used to cure, so that the mixed glue paint forms a sealing film on the surface of the nanocrystalline magnetic core under high temperature, so as to ensure that the glue paint remains inside the nanocrystalline magnetic core, which solves the problem of the existing conventional paint. The problems of leakage and low strength, and the high strength and low stress of the glue paint help the final cutting without damage and mirror surface requirements.
本发明的有益效果在于：本发明的铁镍基纳米晶磁芯具有稳定的磁导率和直流偏置能力，还具有高饱和磁感应强度、低损耗值、低矫顽力、耐高温等优点，综合性能优良。The beneficial effects of the present invention are: the iron-nickel-based nanocrystalline magnetic core of the present invention has stable magnetic permeability and DC bias capability, and also has the advantages of high saturation magnetic induction intensity, low loss value, low coercivity, high temperature resistance, and the like, Excellent overall performance.
本发明的制备方法工艺简单，操作控制方便，质量稳定，生产效率高，生产成本低，可大规模工业化生产。The preparation method of the invention has the advantages of simple process, convenient operation and control, stable quality, high production efficiency and low production cost, and can be industrialized on a large scale.
具体实施方式Detailed ways
为了便于本领域技术人员的理解，下面结合实施例对本发明作进一步的说明，实施方式提及的内容并非对本发明的限定。In order to facilitate the understanding of those skilled in the art, the present invention will be further described below with reference to the examples, and the contents mentioned in the embodiments are not intended to limit the present invention.
实施例1Example 1
一种铁镍基纳米晶磁芯，所述铁镍基纳米晶磁芯由铁镍合金制成，所述铁镍基纳米晶带材包括如下重量百分比的元素：Ni：15%、Si：10%、B：3%、Nb：2%、Cu：0.3%、Co：4%，余量为Fe。An iron-nickel-based nanocrystalline magnetic core, the iron-nickel-based nanocrystalline magnetic core is made of an iron-nickel alloy, and the iron-nickel-based nanocrystalline strip includes the following elements by weight: Ni: 15%, Si: 10% %, B: 3%, Nb: 2%, Cu: 0.3%, Co: 4%, and the balance is Fe.
所述铁镍基纳米晶带材还包括Ga：0.4%、V：0.1%、Ti：0.2、Mn：1%、Cr：0.5%、Mo：0.8%、C：1.2%、Ge：0.01%、P：0.001%、Vb：1.4%、Ta：0.3%和W：0.04%。The iron-nickel-based nanocrystalline ribbon further includes Ga: 0.4%, V: 0.1%, Ti: 0.2, Mn: 1%, Cr: 0.5%, Mo: 0.8%, C: 1.2%, Ge: 0.01%, P: 0.001%, Vb: 1.4%, Ta: 0.3% and W: 0.04%.
一种铁镍基纳米晶磁芯的制备方法，包括如下步骤：A preparation method of an iron-nickel-based nanocrystalline magnetic core, comprising the following steps:
（1）将上述组分的铁镍基纳米晶带材原料进行冶炼，得到合金熔体；(1) smelting the iron-nickel-based nanocrystalline ribbon raw materials of the above components to obtain an alloy melt;
（2）采用单辊急冷法将合金熔体进行喷制，得到铁镍基纳米晶带材；(2) The alloy melt is sprayed by a single-roller quenching method to obtain an iron-nickel-based nanocrystalline strip;
（3）将铁镍基纳米晶带材卷绕成环形纳米晶磁芯；(3) Winding the iron-nickel-based nanocrystalline ribbon into a ring-shaped nanocrystalline magnetic core;
（4）将纳米晶磁芯放入真空退火炉内进行热处理；(4) Put the nanocrystalline magnetic core into the vacuum annealing furnace for heat treatment;
（5）将热处理后的纳米晶磁芯放入真空退火炉内再次进行热处理。(5) Put the heat-treated nanocrystalline magnetic core into a vacuum annealing furnace for heat treatment again.
所述步骤（3）中，铁镍基纳米晶带材的厚度为15μm，宽度为20mm。In the step (3), the thickness of the iron-nickel-based nanocrystalline tape is 15 μm and the width is 20 mm.
所述步骤（4）和所述步骤（5）中，热处理的步骤为：In the step (4) and the step (5), the steps of heat treatment are:
a) 经过110min把炉内温度从室温升温至640K；a) After 110min, the temperature in the furnace is raised from room temperature to 640K;
b) 在643K保温15min后，用32min升温至750K；b) After holding at 643K for 15min, heat up to 750K in 32min;
c) 在753K保温35min后，用11min升温至790K；c) After being kept at 753K for 35min, the temperature was raised to 790K in 11min;
d) 在793K保温55min后，用10min升温至825K；d) After being kept at 793K for 55min, heat up to 825K in 10min;
e) 在828K保温35min后，退出炉罩强风把炉体温度急冷至340K，打开炉门把纳米晶磁芯取出；e) After holding at 828K for 35min, exit the furnace hood with strong wind to quench the furnace temperature to 340K, open the furnace door and take out the nanocrystalline magnetic core;
f) 把从炉内取出的纳米晶磁芯放在冷却架上再强风急冷至常温。f) Put the nanocrystalline magnetic core taken out from the furnace on the cooling rack and then quench it with strong wind to room temperature.
所述步骤（4）和所述步骤（5）中，真空退火炉内的真空度小于-0.1Mpa，真空退火炉内充有混合气体，混合气体由体积百分比为10%的氢气和体积百分比为90%的氮气组成。In the step (4) and the step (5), the vacuum degree in the vacuum annealing furnace is less than -0.1Mpa, the vacuum annealing furnace is filled with mixed gas, and the mixed gas is composed of 10% hydrogen by volume and 10% by volume. 90% nitrogen composition.
所述步骤（5）之后还包括步骤（6）将再次进行热处理后的纳米晶磁芯进行浸胶固化处理。After the step (5), it further includes a step (6) of dipping and curing the nanocrystalline magnetic core after the heat treatment again.
所述步骤（6）中，浸胶固化处理包括如下步骤：In the step (6), the dipping and curing treatment includes the following steps:
A、将纳米晶磁芯在60℃温度下进行预热；A. Preheat the nanocrystalline core at 60℃;
B、采用环氧树脂胶漆作为固化剂，将环氧树脂胶漆在水浴60℃环境下加热；并用稀释剂以胶漆与稀释剂的比例为0.8:1来配兑稀释，稀释后的胶漆在60℃下保温40min；B. Using epoxy resin glue paint as curing agent, heat the epoxy resin glue paint in a water bath at 60°C; and use thinner to mix and dilute the glue paint and thinner at a ratio of 0.8:1. The diluted glue The paint is kept at 60℃ for 40min;
C、将预热后的纳米晶磁芯浸于配兑后的热胶漆中，采用真空含浸的方式，含浸30min，真空度为0.6Mpa；C. Immerse the preheated nanocrystalline magnetic core in the hot glue paint after blending, adopt the method of vacuum impregnation, impregnate for 30min, and the vacuum degree is 0.6Mpa;
D、将含浸后的纳米晶磁芯采用三段保温法固化，第一段温度60℃，保温40min；第二段温度100℃，保温80min；第三段温度140℃，保温80min；自然冷却。D. The impregnated nanocrystalline magnetic core is cured by three-stage heat preservation method. The temperature of the first stage is 60°C, and the heat preservation is 40min; the temperature of the second stage is 100°C, and the heat preservation is 80min; the temperature of the third stage is 140°C, and the heat preservation is 80min; Natural cooling.
实施例2Example 2
一种铁镍基纳米晶磁芯，所述铁镍基纳米晶磁芯由铁镍合金制成，所述铁镍基纳米晶带材包括如下重量百分比的元素：Ni：18%、Si：11.5%、B：3.5%、Nb：2.5%、Cu：0.35%、Co：5%，余量为Fe。An iron-nickel-based nanocrystalline magnetic core, the iron-nickel-based nanocrystalline magnetic core is made of an iron-nickel alloy, and the iron-nickel-based nanocrystalline strip includes the following elements by weight: Ni: 18%, Si: 11.5 %, B: 3.5%, Nb: 2.5%, Cu: 0.35%, Co: 5%, and the balance is Fe.
所述铁镍基纳米晶带材还包括Ga：0.5%、V：0.2%、Ti：0.3%、Mn：1.5%、Cr：0.8%、Mo：0.9%、C：1.25%、Ge：0.02%、P：0.002%、Vb：1.5%、Ta：0.4%和W：0.05%。The iron-nickel-based nanocrystalline ribbon further includes Ga: 0.5%, V: 0.2%, Ti: 0.3%, Mn: 1.5%, Cr: 0.8%, Mo: 0.9%, C: 1.25%, Ge: 0.02% , P: 0.002%, Vb: 1.5%, Ta: 0.4% and W: 0.05%.
一种铁镍基纳米晶磁芯的制备方法，包括如下步骤：A preparation method of an iron-nickel-based nanocrystalline magnetic core, comprising the following steps:
（1）将上述组分的铁镍基纳米晶带材原料进行冶炼，得到合金熔体；(1) smelting the iron-nickel-based nanocrystalline ribbon raw materials of the above components to obtain an alloy melt;
（2）采用单辊急冷法将合金熔体进行喷制，得到铁镍基纳米晶带材；(2) The alloy melt is sprayed by a single-roller quenching method to obtain an iron-nickel-based nanocrystalline strip;
（3）将铁镍基纳米晶带材卷绕成环形纳米晶磁芯；(3) Winding the iron-nickel-based nanocrystalline ribbon into a ring-shaped nanocrystalline magnetic core;
（4）将纳米晶磁芯放入真空退火炉内进行热处理；(4) Put the nanocrystalline magnetic core into the vacuum annealing furnace for heat treatment;
（5）将热处理后的纳米晶磁芯放入真空退火炉内再次进行热处理。(5) Put the heat-treated nanocrystalline magnetic core into a vacuum annealing furnace for heat treatment again.
所述步骤（3）中，铁镍基纳米晶带材的厚度为15-25μm，宽度为20-30mm。In the step (3), the thickness of the iron-nickel-based nanocrystalline tape is 15-25 μm, and the width is 20-30 mm.
所述步骤（4）和所述步骤（5）中，热处理的步骤为：In the step (4) and the step (5), the steps of heat treatment are:
a) 经过115min把炉内温度从室温升温至645K；a) After 115min, the temperature in the furnace was raised from room temperature to 645K;
b) 在648K保温18min后，用34min升温至755K；b) After holding at 648K for 18min, heat up to 755K in 34min;
c) 在758K保温38min后，用12min升温至795K；c) After being kept at 758K for 38min, the temperature was raised to 795K in 12min;
d) 在798K保温58min后，用11min升温至830K；d) After being kept at 798K for 58min, the temperature was raised to 830K in 11min;
e) 在833K保温38min后，退出炉罩强风把炉体温度急冷至345K，打开炉门把纳米晶磁芯取出；e) After holding at 833K for 38min, exit the furnace hood with strong wind to quench the furnace body temperature to 345K, open the furnace door and take out the nanocrystalline magnetic core;
f) 把从炉内取出的纳米晶磁芯放在冷却架上再强风急冷至常温。f) Put the nanocrystalline magnetic core taken out from the furnace on the cooling rack and then quench it with strong wind to room temperature.
所述步骤（4）和所述步骤（5）中，真空退火炉内的真空度小于-0.1Mpa，真空退火炉内充有混合气体，混合气体由体积百分比为12%的氢气和体积百分比为88%的氮气组成。In the step (4) and the step (5), the vacuum degree in the vacuum annealing furnace is less than -0.1Mpa, the vacuum annealing furnace is filled with mixed gas, and the mixed gas is composed of 12% hydrogen by volume and 12% by volume. 88% nitrogen composition.
所述步骤（5）之后还包括步骤（6）将再次进行热处理后的纳米晶磁芯进行浸胶固化处理。After the step (5), it further includes a step (6) of dipping and curing the nanocrystalline magnetic core after the heat treatment again.
所述步骤（6）中，浸胶固化处理包括如下步骤：In the step (6), the dipping and curing treatment includes the following steps:
A、将纳米晶磁芯在62℃温度下进行预热；A. Preheat the nanocrystalline core at 62℃;
B、采用环氧树脂胶漆作为固化剂，将环氧树脂胶漆在水浴62℃环境下加热；并用稀释剂以胶漆与稀释剂的比例为0.9:1来配兑稀释，稀释后的胶漆在62℃下保温50min；B. Using epoxy resin glue paint as curing agent, heat epoxy resin glue paint in a water bath at 62°C; and use diluent to mix and dilute the ratio of glue paint to thinner of 0.9:1. The diluted glue The paint is kept at 62°C for 50min;
C、将预热后的纳米晶磁芯浸于配兑后的热胶漆中，采用真空含浸的方式，含浸35min，真空度为0.65Mpa；C. Immerse the preheated nanocrystalline magnetic core in the hot glue paint after blending, adopt the method of vacuum impregnation, impregnate for 35min, and the vacuum degree is 0.65Mpa;
D、将含浸后的纳米晶磁芯采用三段保温法固化，第一段温度65℃，保温50min；第二段温度105℃，保温90min；第三段温度145℃，保温90min；自然冷却。D. The impregnated nanocrystalline magnetic core is cured by three-stage heat preservation method, the temperature of the first stage is 65°C, and the heat preservation is 50min; the temperature of the second stage is 105°C, and the heat preservation is 90min; the temperature of the third stage is 145°C, and the heat preservation is 90min; and natural cooling.
实施例3Example 3
一种铁镍基纳米晶磁芯，所述铁镍基纳米晶磁芯由铁镍合金制成，所述铁镍基纳米晶带材包括如下重量百分比的元素：Ni：20%、Si：11%、B：4%、Nb：3%、Cu：0.4%、Co：6%，余量为Fe。An iron-nickel-based nanocrystalline magnetic core, the iron-nickel-based nanocrystalline magnetic core is made of an iron-nickel alloy, and the iron-nickel-based nanocrystalline strip includes the following elements by weight: Ni: 20%, Si: 11 %, B: 4%, Nb: 3%, Cu: 0.4%, Co: 6%, and the balance is Fe.
所述铁镍基纳米晶带材还包括Ga：0.6%、V：0.3%、Ti：0.4%、Mn：2%、Cr：1.0%、Mo：1.0%、C：1.3%、Ge：0.03%、P：0.003%、Vb：1.6%、Ta：0.5%和W：0.06%。The iron-nickel-based nanocrystalline ribbon further includes Ga: 0.6%, V: 0.3%, Ti: 0.4%, Mn: 2%, Cr: 1.0%, Mo: 1.0%, C: 1.3%, Ge: 0.03% , P: 0.003%, Vb: 1.6%, Ta: 0.5% and W: 0.06%.
一种铁镍基纳米晶磁芯的制备方法，包括如下步骤：A preparation method of an iron-nickel-based nanocrystalline magnetic core, comprising the following steps:
（1）将上述组分的铁镍基纳米晶带材原料进行冶炼，得到合金熔体；(1) smelting the iron-nickel-based nanocrystalline ribbon raw materials of the above components to obtain an alloy melt;
（2）采用单辊急冷法将合金熔体进行喷制，得到铁镍基纳米晶带材；(2) The alloy melt is sprayed by a single-roller quenching method to obtain an iron-nickel-based nanocrystalline strip;
（3）将铁镍基纳米晶带材卷绕成环形纳米晶磁芯；(3) Winding the iron-nickel-based nanocrystalline ribbon into a ring-shaped nanocrystalline magnetic core;
（4）将纳米晶磁芯放入真空退火炉内进行热处理；(4) Put the nanocrystalline magnetic core into the vacuum annealing furnace for heat treatment;
（5）将热处理后的纳米晶磁芯放入真空退火炉内再次进行热处理。(5) Put the heat-treated nanocrystalline magnetic core into a vacuum annealing furnace for heat treatment again.
所述步骤（3）中，铁镍基纳米晶带材的厚度为20μm，宽度为25mm。In the step (3), the thickness of the iron-nickel-based nanocrystalline tape is 20 μm and the width is 25 mm.
所述步骤（4）和所述步骤（5）中，热处理的步骤为：In the step (4) and the step (5), the steps of heat treatment are:
a) 经过120min把炉内温度从室温升温至650K；a) After 120min, the temperature in the furnace is raised from room temperature to 650K;
b) 在653K保温20min后，用36min升温至760K；b) After holding at 653K for 20min, heat up to 760K in 36min;
c) 在763K保温40min后，用13min升温至800K；c) After being kept at 763K for 40min, the temperature was raised to 800K in 13min;
d) 在803K保温60min后，用12min升温至835K；d) After keeping the temperature at 803K for 60min, use 12min to heat up to 835K;
e) 在838K保温40min后，退出炉罩强风把炉体温度急冷至350K，打开炉门把纳米晶磁芯取出；e) After holding at 838K for 40min, exit the furnace hood with strong wind to quench the furnace body temperature to 350K, open the furnace door and take out the nanocrystalline magnetic core;
f) 把从炉内取出的纳米晶磁芯放在冷却架上再强风急冷至常温。f) Put the nanocrystalline magnetic core taken out from the furnace on the cooling rack and then quench it with strong wind to room temperature.
所述步骤（4）和所述步骤（5）中，真空退火炉内的真空度小于-0.1Mpa，真空退火炉内充有混合气体，混合气体由体积百分比为15%的氢气和体积百分比为85%的氮气组成。In the step (4) and the step (5), the vacuum degree in the vacuum annealing furnace is less than -0.1Mpa, the vacuum annealing furnace is filled with mixed gas, and the mixed gas is composed of 15% hydrogen by volume and 15% by volume. 85% nitrogen composition.
所述步骤（5）之后还包括步骤（6）将再次进行热处理后的纳米晶磁芯进行浸胶固化处理。After the step (5), it further includes a step (6) of dipping and curing the nanocrystalline magnetic core after the heat treatment again.
所述步骤（6）中，浸胶固化处理包括如下步骤：In the step (6), the dipping and curing treatment includes the following steps:
A、将纳米晶磁芯在65℃温度下进行预热；A. Preheat the nanocrystalline core at 65℃;
B、采用环氧树脂胶漆作为固化剂，将环氧树脂胶漆在水浴65℃环境下加热；并用稀释剂以胶漆与稀释剂的比例为1:1来配兑稀释，稀释后的胶漆在65℃下保温60min；B. Using epoxy resin glue paint as curing agent, heat epoxy resin glue paint in a water bath at 65°C; and use thinner to mix and dilute the glue paint and thinner at a ratio of 1:1. The diluted glue The paint is kept at 65℃ for 60min;
C、将预热后的纳米晶磁芯浸于配兑后的热胶漆中，采用真空含浸的方式，含浸40min，真空度为0.7Mpa；C. Immerse the preheated nanocrystalline magnetic core in the blended hot glue paint, adopt the method of vacuum impregnation, impregnate for 40min, and the vacuum degree is 0.7Mpa;
D、将含浸后的纳米晶磁芯采用三段保温法固化，第一段温度70℃，保温60min；第二段温度110℃，保温810min；第三段温度150℃，保温100min；自然冷却。D. The impregnated nanocrystalline magnetic core is cured by a three-stage heat preservation method, the temperature of the first stage is 70°C, and the heat preservation is 60min; the temperature of the second stage is 110°C, and the heat preservation is 810min; the temperature of the third stage is 150°C, and the heat preservation is 100min; Natural cooling.
实施例4Example 4
一种铁镍基纳米晶磁芯，所述铁镍基纳米晶磁芯由铁镍合金制成，所述铁镍基纳米晶带材包括如下重量百分比的元素：Ni：22%、Si：11.5%、B：4.5%、Nb：3.5%、Cu：0.45%、Co：7%，余量为Fe。An iron-nickel-based nanocrystalline magnetic core, the iron-nickel-based nanocrystalline magnetic core is made of an iron-nickel alloy, and the iron-nickel-based nanocrystalline strip includes the following elements by weight: Ni: 22%, Si: 11.5 %, B: 4.5%, Nb: 3.5%, Cu: 0.45%, Co: 7%, and the balance is Fe.
所述铁镍基纳米晶带材还包括Ga：0.7%、V：0.4%、Ti：0.5%、Mn：2.5%、Cr：1.2%、Mo：1.1%、C：1.35%、Ge：0.04%、P：0.004%、Vb：1.7%、Ta：0.6%和W：0.07%。The iron-nickel-based nanocrystalline ribbon further includes Ga: 0.7%, V: 0.4%, Ti: 0.5%, Mn: 2.5%, Cr: 1.2%, Mo: 1.1%, C: 1.35%, Ge: 0.04% , P: 0.004%, Vb: 1.7%, Ta: 0.6% and W: 0.07%.
一种铁镍基纳米晶磁芯的制备方法，包括如下步骤：A preparation method of an iron-nickel-based nanocrystalline magnetic core, comprising the following steps:
（1）将上述组分的铁镍基纳米晶带材原料进行冶炼，得到合金熔体；(1) smelting the iron-nickel-based nanocrystalline ribbon raw materials of the above components to obtain an alloy melt;
（2）采用单辊急冷法将合金熔体进行喷制，得到铁镍基纳米晶带材；(2) The alloy melt is sprayed by a single-roller quenching method to obtain an iron-nickel-based nanocrystalline strip;
（3）将铁镍基纳米晶带材卷绕成环形纳米晶磁芯；(3) Winding the iron-nickel-based nanocrystalline ribbon into a ring-shaped nanocrystalline magnetic core;
（4）将纳米晶磁芯放入真空退火炉内进行热处理；(4) Put the nanocrystalline magnetic core into the vacuum annealing furnace for heat treatment;
（5）将热处理后的纳米晶磁芯放入真空退火炉内再次进行热处理。(5) Put the heat-treated nanocrystalline magnetic core into a vacuum annealing furnace for heat treatment again.
所述步骤（3）中，铁镍基纳米晶带材的厚度为22μm，宽度为28mm。In the step (3), the thickness of the iron-nickel-based nanocrystalline tape is 22 μm and the width is 28 mm.
所述步骤（4）和所述步骤（5）中，热处理的步骤为：In the step (4) and the step (5), the steps of heat treatment are:
a) 经过125min把炉内温度从室温升温至655K；a) After 125min, the temperature in the furnace is raised from room temperature to 655K;
b) 在658K保温22min后，用38min升温至765K；b) After being kept at 658K for 22min, the temperature was raised to 765K in 38min;
c) 在768K保温42min后，用14min升温至805K；c) After holding at 768K for 42min, heat up to 805K in 14min;
d) 在808K保温62min后，用13min升温至840K；d) After keeping the temperature at 808K for 62min, use 13min to heat up to 840K;
e) 在843K保温42min后，退出炉罩强风把炉体温度急冷至355K，打开炉门把纳米晶磁芯取出；e) After holding at 843K for 42min, exit the furnace hood with strong wind to quench the furnace body temperature to 355K, open the furnace door and take out the nanocrystalline magnetic core;
f) 把从炉内取出的纳米晶磁芯放在冷却架上再强风急冷至常温。f) Put the nanocrystalline magnetic core taken out from the furnace on the cooling rack and then quench it with strong wind to room temperature.
所述步骤（4）和所述步骤（5）中，真空退火炉内的真空度小于-0.1Mpa，真空退火炉内充有混合气体，混合气体由体积百分比为18%的氢气和体积百分比为82%的氮气组成。In the step (4) and the step (5), the vacuum degree in the vacuum annealing furnace is less than -0.1Mpa, and the vacuum annealing furnace is filled with mixed gas, and the mixed gas is composed of 18% hydrogen by volume and 18% by volume. 82% nitrogen composition.
所述步骤（5）之后还包括步骤（6）将再次进行热处理后的纳米晶磁芯进行浸胶固化处理。After the step (5), it further includes a step (6) of dipping and curing the nanocrystalline magnetic core after the heat treatment again.
所述步骤（6）中，浸胶固化处理包括如下步骤：In the step (6), the dipping and curing treatment includes the following steps:
A、将纳米晶磁芯在68℃温度下进行预热；A. Preheat the nanocrystalline core at 68℃;
B、采用环氧树脂胶漆作为固化剂，将环氧树脂胶漆在水浴68℃环境下加热；并用稀释剂以胶漆与稀释剂的比例为1.1:1来配兑稀释，稀释后的胶漆在68℃下保温70min；B. Using epoxy resin glue paint as curing agent, heat epoxy resin glue paint in a water bath at 68°C; and use thinner to mix and dilute the glue paint and thinner ratio of 1.1:1. The diluted glue The paint is kept at 68℃ for 70min;
C、将预热后的纳米晶磁芯浸于配兑后的热胶漆中，采用真空含浸的方式，含浸45min，真空度为0.75Mpa；C. Immerse the preheated nanocrystalline magnetic core in the blended hot glue paint, adopt the method of vacuum impregnation, impregnate for 45min, and the vacuum degree is 0.75Mpa;
D、将含浸后的纳米晶磁芯采用三段保温法固化，第一段温度75℃，保温70min；第二段温度115℃，保温110min；第三段温度155℃，保温110min；自然冷却。D. The impregnated nanocrystalline magnetic core is cured by three-stage heat preservation method, the temperature of the first stage is 75°C, and the heat preservation is 70min; the temperature of the second stage is 115°C, and the heat preservation is 110min; the temperature of the third stage is 155°C, and the heat preservation is 110min; Natural cooling.
实施例5Example 5
一种铁镍基纳米晶磁芯，所述铁镍基纳米晶磁芯由铁镍合金制成，所述铁镍基纳米晶带材包括如下重量百分比的元素：Ni：25%、Si：12%、B：5%、Nb：4%、Cu：0.5%、Co：8%，余量为Fe。An iron-nickel-based nanocrystalline magnetic core, the iron-nickel-based nanocrystalline magnetic core is made of an iron-nickel alloy, and the iron-nickel-based nanocrystalline strip includes the following elements by weight: Ni: 25%, Si: 12 %, B: 5%, Nb: 4%, Cu: 0.5%, Co: 8%, and the balance is Fe.
所述铁镍基纳米晶带材还包括Ga：0.8%、V：0.5%、Ti：0.6%、Mn：3%、Cr：1.5%、Mo：1.2%、C：1.4%、Ge：0.05%、P：0.005%、Vb：1.8%、Ta：0.7%和W：0.08%。The iron-nickel-based nanocrystalline ribbon further includes Ga: 0.8%, V: 0.5%, Ti: 0.6%, Mn: 3%, Cr: 1.5%, Mo: 1.2%, C: 1.4%, Ge: 0.05% , P: 0.005%, Vb: 1.8%, Ta: 0.7% and W: 0.08%.
一种铁镍基纳米晶磁芯的制备方法，包括如下步骤：A preparation method of an iron-nickel-based nanocrystalline magnetic core, comprising the following steps:
（1）将上述组分的铁镍基纳米晶带材原料进行冶炼，得到合金熔体；(1) smelting the iron-nickel-based nanocrystalline ribbon raw materials of the above components to obtain an alloy melt;
（2）采用单辊急冷法将合金熔体进行喷制，得到铁镍基纳米晶带材；(2) The alloy melt is sprayed by a single-roller quenching method to obtain an iron-nickel-based nanocrystalline strip;
（3）将铁镍基纳米晶带材卷绕成环形纳米晶磁芯；(3) Winding the iron-nickel-based nanocrystalline ribbon into a ring-shaped nanocrystalline magnetic core;
（4）将纳米晶磁芯放入真空退火炉内进行热处理；(4) Put the nanocrystalline magnetic core into the vacuum annealing furnace for heat treatment;
（5）将热处理后的纳米晶磁芯放入真空退火炉内再次进行热处理。(5) Put the heat-treated nanocrystalline magnetic core into a vacuum annealing furnace for heat treatment again.
所述步骤（3）中，铁镍基纳米晶带材的厚度为25μm，宽度为30mm。In the step (3), the iron-nickel-based nanocrystalline tape has a thickness of 25 μm and a width of 30 mm.
所述步骤（4）和所述步骤（5）中，热处理的步骤为：In the step (4) and the step (5), the steps of heat treatment are:
a) 经过130min把炉内温度从室温升温至660K；a) After 130min, the temperature in the furnace is raised from room temperature to 660K;
b) 在663K保温25min后，用40min升温至770K；b) After being kept at 663K for 25min, the temperature was raised to 770K in 40min;
c) 在773K保温45min后，用15min升温至810K；c) After being kept at 773K for 45min, the temperature was raised to 810K in 15min;
d) 在813K保温65min后，用14min升温至845K；d) After keeping the temperature at 813K for 65min, use 14min to heat up to 845K;
e) 在848K保温45min后，退出炉罩强风把炉体温度急冷至360K，打开炉门把纳米晶磁芯取出；e) After holding at 848K for 45min, exit the furnace hood with strong wind to quench the furnace body temperature to 360K, open the furnace door and take out the nanocrystalline magnetic core;
f) 把从炉内取出的纳米晶磁芯放在冷却架上再强风急冷至常温。f) Put the nanocrystalline magnetic core taken out from the furnace on the cooling rack and then quench it with strong wind to room temperature.
所述步骤（4）和所述步骤（5）中，真空退火炉内的真空度小于-0.1Mpa，真空退火炉内充有混合气体，混合气体由体积百分比为20%的氢气和体积百分比为80%的氮气组成。In the step (4) and the step (5), the vacuum degree in the vacuum annealing furnace is less than -0.1Mpa, the vacuum annealing furnace is filled with mixed gas, and the mixed gas is composed of 20% hydrogen by volume and 20% by volume. 80% nitrogen composition.
所述步骤（5）之后还包括步骤（6）将再次进行热处理后的纳米晶磁芯进行浸胶固化处理。After the step (5), it further includes a step (6) of dipping and curing the nanocrystalline magnetic core after the heat treatment again.
所述步骤（6）中，浸胶固化处理包括如下步骤：In the step (6), the dipping and curing treatment includes the following steps:
A、将纳米晶磁芯在70℃温度下进行预热；A. Preheat the nanocrystalline core at 70℃;
B、采用环氧树脂胶漆作为固化剂，将环氧树脂胶漆在水浴70℃环境下加热；并用稀释剂以胶漆与稀释剂的比例为1.2:1来配兑稀释，稀释后的胶漆在70℃下保温80min；B. Using epoxy resin glue paint as curing agent, heat the epoxy resin glue paint in a water bath at 70°C; and use thinner to mix and dilute the glue paint and thinner at a ratio of 1.2:1. The diluted glue The paint is kept at 70℃ for 80min;
C、将预热后的纳米晶磁芯浸于配兑后的热胶漆中，采用真空含浸的方式，含浸50min，真空度为0.8Mpa；C. Immerse the preheated nanocrystalline magnetic core in the hot glue paint after blending, adopt the method of vacuum impregnation, impregnate for 50min, and the vacuum degree is 0.8Mpa;
D、将含浸后的纳米晶磁芯采用三段保温法固化，第一段温度80℃，保温80min；第二段温度120℃，保温120min；第三段温度160℃，保温120min；自然冷却。D. The impregnated nanocrystalline magnetic core is cured by three-stage heat preservation method, the temperature of the first stage is 80°C, and the heat preservation is 80min; the temperature of the second stage is 120°C, and the heat preservation is 120min; the temperature of the third stage is 160°C, and the heat preservation is 120min; natural cooling.
经测试，本发明制得的纳米晶磁芯的有效磁导率μe可以达到9.1×104以上，饱和磁感应值Bs可以达到1.50T以上，矫顽力磁场强度Hc的值小于2Am-1，剩磁比小于0.1，抗直流偏置能力强，在100Oe场强下，磁导率仍然有80%以上，其中在0.2T、20k Hz条件下损耗值为1.2W/kg以下，同时磁芯在0.5T、20k Hz条件下损耗值为5.6W/kg以下，磁芯在0.5T、50k Hz条件下损耗值为16.8W/kg以下。After testing, the effective magnetic permeability μe of the nanocrystalline magnetic core prepared by the present invention can reach more than 9.1×10 4 , the saturation magnetic induction value Bs can reach more than 1.50T, the value of the coercive force magnetic field strength Hc is less than 2Am -1 , and the residual value is less than 2Am -1 . The magnetic ratio is less than 0.1, and the DC bias resistance is strong. Under the field strength of 100Oe, the magnetic permeability is still more than 80%. The loss value is below 1.2W/kg under the condition of 0.2T and 20k Hz, and the magnetic core is at 0.5 The loss value is less than 5.6W/kg under the conditions of T and 20k Hz, and the loss value of the magnetic core is less than 16.8W/kg under the conditions of 0.5T and 50k Hz.
本发明的铁镍基纳米晶磁芯具有稳定的磁导率和直流偏置能力，还具有高饱和磁感应强度、低损耗值、低矫顽力、耐高温等优点，综合性能优良。The iron-nickel-based nanocrystalline magnetic core of the invention has stable magnetic permeability and DC bias capability, and also has the advantages of high saturation magnetic induction intensity, low loss value, low coercive force, high temperature resistance, etc., and excellent comprehensive performance.
上述实施例为本发明较佳的实现方案，除此之外，本发明还可以其它方式实现，在不脱离本发明构思的前提下任何显而易见的替换均在本发明的保护范围之内。The above-mentioned embodiment is a preferred implementation scheme of the present invention. In addition, the present invention can also be implemented in other ways, and any obvious replacements are within the protection scope of the present invention without departing from the concept of the present invention.
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