CN117626134A - High frequency and high magnetic permeability iron-based nanocrystalline alloy and preparation method thereof - Google Patents
High frequency and high magnetic permeability iron-based nanocrystalline alloy and preparation method thereof Download PDFInfo
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Abstract
Description
技术领域Technical field
本发明涉及一种纳米晶合金,具体涉及一种高频高磁导率铁基纳米晶合金及其制备方法,属于合金材料领域。The invention relates to a nanocrystalline alloy, in particular to a high-frequency, high-permeability iron-based nanocrystalline alloy and a preparation method thereof, and belongs to the field of alloy materials.
背景技术Background technique
自从1988年,纳米晶合金被首次开发以来,Fe73.5Si9B13.5Nb3Cu1已取得广泛应用,几十年来,大量的科学家和工程技术人员围绕该合金做了大量研究工作。然而,目前主流应用的仍然还是该合金成分。Since the nanocrystalline alloy was first developed in 1988, Fe 73.5 Si 9 B 13.5 Nb 3 Cu 1 has been widely used. For decades, a large number of scientists and engineering technicians have done a lot of research work on this alloy. However, the current mainstream application is still the alloy composition.
随着器件往高频化方向发展,需要软磁材料的频率稳定性好,且频率稳定性好的磁导率水平尽量提高,目前常用制备超薄非晶带,外加横向磁场热处理的工艺,勉强满足高频器件对软磁材料的需求。但是为满足高频下高磁导率的要求,需要不断提高超薄非晶带的制备工艺,该方案会带来成本的大幅提升。As devices develop towards high frequencies, soft magnetic materials need to have good frequency stability and the magnetic permeability level with good frequency stability should be increased as much as possible. Currently, the process of preparing ultra-thin amorphous ribbons and applying transverse magnetic field heat treatment is commonly used. Meet the demand for soft magnetic materials for high-frequency devices. However, in order to meet the requirements of high magnetic permeability at high frequencies, the preparation process of ultra-thin amorphous ribbons needs to be continuously improved, and this solution will significantly increase the cost.
研究表明,Si含量提高能带来高频磁导率的提升,通过Si含量的调整,高硅含量的纳米晶合金会带来非晶形成能力的恶化,导致现有工艺难以制备出完全非晶的结构,后续性能根本无法得到保障。通常需要增大Nb、Mo、Cr等强非晶形成元素的含量,来保障现有工艺下制备出完全非晶的快淬条带。也有研究表明,添加Co和Ni元素也可以用来提高频率稳定性,但是该方法会带来成本的大幅降低,甚至可能大幅降低低频磁导率,所以这种方法较少采用。Research shows that increasing the Si content can lead to an increase in high-frequency magnetic permeability. By adjusting the Si content, nanocrystalline alloys with high silicon content will deteriorate the amorphous formation ability, making it difficult to prepare completely amorphous materials using existing processes. structure, subsequent performance cannot be guaranteed at all. It is usually necessary to increase the content of strong amorphous-forming elements such as Nb, Mo, and Cr to ensure that completely amorphous fast-quenching strips can be prepared under the existing process. Studies have also shown that adding Co and Ni elements can also be used to improve frequency stability, but this method will bring about a significant reduction in cost and may even significantly reduce low-frequency magnetic permeability, so this method is rarely used.
然而,添加Co、Ni、Nb、Mo等元素,通常需要大幅增加原材料的成本,在性能没有大幅提高的情况下,很难得到推广应用。所以,目前迫切需要一种不增加成本,且适应现行工艺的高频高磁导率纳米晶合金,以满足高频率下对高磁导率的使用要求。However, adding elements such as Co, Ni, Nb, and Mo usually requires a significant increase in the cost of raw materials. Without a significant improvement in performance, it is difficult to be promoted and applied. Therefore, there is an urgent need for a high-frequency and high-permeability nanocrystalline alloy that does not increase costs and is adaptable to current processes to meet the requirements for high magnetic permeability at high frequencies.
发明内容Contents of the invention
本发明的主要目的在于提供一种高频高磁导率铁基纳米晶合金及其制备方法,以克服现有技术的不足。The main purpose of the present invention is to provide a high-frequency and high-permeability iron-based nanocrystalline alloy and a preparation method thereof to overcome the shortcomings of the existing technology.
为实现前述发明目的,本发明采用的技术方案包括:In order to achieve the foregoing invention objectives, the technical solutions adopted by the present invention include:
本发明的一个方面提供了一种高频高磁导率铁基纳米晶合金,其化学式为FeaSibBcPdNbeCufMg,其中M为杂质元素,a、b、c、d、e、f和g为各元素的原子百分数含量,a+b+c+d+e+f+g=100,且15.5≤b≤20.5,g≤0.5。One aspect of the present invention provides a high-frequency, high-permeability iron-based nanocrystalline alloy whose chemical formula is Fe a Si b B c P d Nb e Cu f M g , where M is an impurity element, a, b, c , d, e, f and g are the atomic percentage contents of each element, a+b+c+d+e+f+g=100, and 15.5≤b≤20.5, g≤0.5.
进一步的,70≤a≤75,3≤c≤8,0.5≤d≤5,1.5≤e≤3.5,0.5≤f≤1.5。Further, 70≤a≤75, 3≤c≤8, 0.5≤d≤5, 1.5≤e≤3.5, 0.5≤f≤1.5.
其中,由于杂质元素种类众多,为方便计算杂质元素的含量,故而按杂质元素的质量分数并以Fe元素的原子量折算为Mg。Among them, since there are many types of impurity elements, in order to facilitate the calculation of the content of impurity elements, the mass fraction of impurity elements and the atomic weight of Fe element are converted into Mg.
进一步的,所述铁基纳米晶合金在100KHz的相对磁导率≥29000。Further, the relative magnetic permeability of the iron-based nanocrystalline alloy at 100KHz is ≥29,000.
本发明的另一个方面还提供了一种制备所述高频高磁导率铁基纳米晶合金的方法,其包括:按照所述铁基纳米晶合金的组成配制原料,并依次进行熔炼、热处理,从而制得所述铁基纳米晶合金;其中,所述热处理的至少部分操作是在磁场中进行的。Another aspect of the present invention also provides a method for preparing the high-frequency high magnetic permeability iron-based nanocrystalline alloy, which includes: preparing raw materials according to the composition of the iron-based nanocrystalline alloy, and sequentially performing smelting and heat treatment , thereby preparing the iron-based nanocrystalline alloy; wherein at least part of the heat treatment is performed in a magnetic field.
进一步的,所述磁场的强度为0.01~1T。优选的,所述磁场为恒定磁场。Further, the intensity of the magnetic field is 0.01~1T. Preferably, the magnetic field is a constant magnetic field.
进一步的,所述磁场的来源包括永磁体或电磁铁等,即,所述磁场可以由永磁体或电磁铁等施加。Further, the source of the magnetic field includes a permanent magnet or an electromagnet, that is, the magnetic field can be applied by a permanent magnet or an electromagnet.
进一步的,所述热处理包括:先在460~480℃进行第一阶段热处理,时间为30~120min;之后在540~580℃进行第二阶段热处理,时间为90~180min。Further, the heat treatment includes: first performing a first-stage heat treatment at 460-480°C for a time of 30-120 min; and then performing a second-stage heat treatment at 540-580°C for a time of 90-180 min.
在一些情况下,所述热处理的整个过程均是在所述磁场中进行的。在另一些情况下,所述第二阶段热处理是在所述磁场中进行的。但至少所述第二阶段热处理需要在所述磁场中进行。In some cases, the entire heat treatment process is performed in the magnetic field. In other cases, the second stage heat treatment is performed in the magnetic field. But at least the second stage heat treatment needs to be carried out in the magnetic field.
在一个实施例中,所述的制备方法具体包括:将所述原料冶炼成合金液后,再加工为带材,之后对所述带材进行所述热处理,从而制得所述铁基纳米晶合金。In one embodiment, the preparation method specifically includes: smelting the raw material into an alloy liquid, processing it into a strip, and then subjecting the strip to the heat treatment to prepare the iron-based nanocrystals. alloy.
在一个实施例中,所述的制备方法具体包括配料、熔炼、喷带、绕制铁芯、热处理等步骤,即:In one embodiment, the preparation method specifically includes the steps of batching, smelting, spraying tape, winding iron core, heat treatment, etc., namely:
先按所述纳米晶合金的组成配制原料,原料包括金属单质或中间合金等。First, raw materials are prepared according to the composition of the nanocrystalline alloy. The raw materials include metal elements or master alloys.
利用所得原料,经电弧或感应、电阻炉熔炼等方式形成合金,可以真空冶炼,也可经非真空方式冶炼,其中非真空方式冶炼需经熔体净化处理,以降低其中有害杂质元素或夹杂带来的危害,经冶炼形成均匀混合的合金液,合金液可以直接用于制带,也可以冷却后形成合金锭,再将合金锭熔化为合金液后用于制带。The obtained raw materials are used to form alloys through arc, induction, resistance furnace smelting, etc., which can be smelted in a vacuum or in a non-vacuum manner. Non-vacuum smelting requires melt purification to reduce harmful impurity elements or inclusion bands. After smelting, a uniformly mixed alloy liquid is formed. The alloy liquid can be directly used for strip making, or it can be cooled to form an alloy ingot, and then the alloy ingot is melted into alloy liquid and used for strip making.
之后将所述合金液经平面流铸方式获得平直条带,并可利用XRD方式检测条带的物相状态是否为完全非晶状态,将条带收集后待用。所述甩带机可以为重力或压力单辊甩带机。The alloy liquid is then subjected to planar flow casting to obtain straight strips, and the XRD method can be used to detect whether the physical phase state of the strips is completely amorphous, and the strips are collected for later use. The belt spinning machine can be a gravity or pressure single roller belt spinning machine.
收集后的条带,可以按照需要的尺寸经卷绕后可制作成相应尺寸的磁芯,磁芯需经点焊或其他方式固定,以防止磁芯散开。The collected strips can be rolled according to the required size and made into magnetic cores of corresponding sizes. The magnetic cores need to be fixed by spot welding or other methods to prevent the magnetic cores from spreading.
该磁芯经横向磁场热处理后可获得性能优异的纳米晶磁芯,处理工艺为磁场热处理,磁场的施加方式可以为永磁体或电磁铁等方式。The magnetic core can obtain a nanocrystalline magnetic core with excellent performance after transverse magnetic field heat treatment. The treatment process is magnetic field heat treatment. The magnetic field can be applied by permanent magnets or electromagnets.
相较于现有技术,本发明至少具有如下优势:Compared with the existing technology, the present invention has at least the following advantages:
(1)本发明通过将铁基纳米晶合金中的Si含量提高至15.5~20.5at.%,使合金的高频磁导率明显提高,达到100kHz下的磁导率≥29000,并通过添加P元素,有效增强了非晶形成能力,克服了Si含量提高引起的非晶形成能力不足等缺陷,且使合金的频率抗衰减特性良好,相较于添加Co、Ni、Nb、Mo等元素提高合金的高频磁导率的方式,成本更低。(1) The present invention significantly improves the high-frequency magnetic permeability of the alloy by increasing the Si content in the iron-based nanocrystalline alloy to 15.5~20.5at.%, reaching a magnetic permeability of ≥29000 at 100kHz, and by adding P element, effectively enhances the amorphous formation ability, overcomes defects such as insufficient amorphous formation ability caused by increased Si content, and makes the frequency attenuation resistance of the alloy good. Compared with adding Co, Ni, Nb, Mo and other elements to improve the alloy The high-frequency magnetic permeability method has lower cost.
(2)本发明的高频高磁导率铁基纳米晶合金可以在现有生产条件下大规模生产,只需按所述纳米晶合金的组分配制原料后,进行熔炼等工序,即可制备出完全非晶的带材,例如21±1微米规格的带材,再经卷绕成磁芯等工序,之后在磁场中进行热处理,就可以获得相应的纳米晶磁芯。相比于高Si含量的107合金,本发明的制备方法不仅提升了铁基纳米晶合金的高频磁导率,改善了铁基纳米晶合金非晶形成能力,与压力法制备的超薄带相比,制作过程更加容易,可以在性能接近的情况下,大幅降低成本。(2) The high-frequency high-permeability iron-based nanocrystalline alloy of the present invention can be mass-produced under existing production conditions. It only needs to prepare raw materials according to the composition of the nanocrystalline alloy and carry out smelting and other processes. By preparing a completely amorphous strip, such as a strip with a specification of 21±1 microns, and then winding it into a magnetic core, and then heat treating it in a magnetic field, the corresponding nanocrystalline magnetic core can be obtained. Compared with the 107 alloy with high Si content, the preparation method of the present invention not only improves the high-frequency magnetic permeability of the iron-based nanocrystalline alloy, but also improves the amorphous formation ability of the iron-based nanocrystalline alloy. It is also consistent with the ultra-thin ribbon prepared by the pressure method. In comparison, the production process is easier and the cost can be greatly reduced while the performance is close.
附图说明Description of drawings
下面结合附图和具体实施方式对本发明作进一步详细的说明。The present invention will be described in further detail below with reference to the accompanying drawings and specific embodiments.
图1为本发明实施例与对比例中铁基纳米晶合金淬态带材的XRD检测图谱。Figure 1 is the XRD detection pattern of the iron-based nanocrystalline alloy quenched strip in the Examples and Comparative Examples of the present invention.
具体实施方式Detailed ways
如前所述,鉴于实际应用中对高频高磁导率纳米晶合金的迫切需求,本发明在Fe73.5Si9B13.5Nb3Cu1的基础上,通过大幅提高Si的含量,并在剩余合金中添加P元素,保证在现有工艺条件下可以制备出完全非晶的条带,条带经横向磁场热处理后,可以保证磁导率在高频特性良好,而P的添加,还能跟Nb和Cu配合,从而达到细化纳米晶晶粒的作用,从而保证高频条件下的软磁性能,突出表现为磁导率≥29000(at 100kHz)。As mentioned above, in view of the urgent demand for high-frequency and high-permeability nanocrystalline alloys in practical applications, the present invention is based on Fe 73.5 Si 9 B 13.5 Nb 3 Cu 1 by greatly increasing the Si content and adding the remaining Adding P element to the alloy ensures that completely amorphous strips can be prepared under existing process conditions. After the strips are heat treated in a transverse magnetic field, the magnetic permeability can be ensured to be good at high frequencies. The addition of P can also follow the Nb and Cu cooperate to refine the nanocrystal grains, thus ensuring soft magnetic properties under high-frequency conditions, highlighted by magnetic permeability ≥ 29000 (at 100kHz).
如下将结合若干实施例对本发明的技术方案作进一步的说明。The technical solution of the present invention will be further described below with reference to several embodiments.
在如下实施例中,主要是利用阻抗分析仪测试磁芯在不同频率下的电感量,并根据其尺寸、质量等计算出其相应的磁导率。In the following embodiments, an impedance analyzer is mainly used to test the inductance of the magnetic core at different frequencies, and its corresponding magnetic permeability is calculated based on its size, quality, etc.
实施例1本实施例提供的一种高频高磁导率铁基纳米晶合金的制备方法包括如下步骤:Example 1 This example provides a method for preparing a high-frequency, high-permeability iron-based nanocrystalline alloy, which includes the following steps:
利用金属单质Fe、Si、Cu和中间合金FeB、FeP、FeNb来进行合金成分的称量配料获得Fe70Si20.5B4P4Nb2Cu0.5待用。Use metal elements Fe, Si, Cu and intermediate alloys FeB, FeP, FeNb to weigh and batch the alloy components to obtain Fe 70 Si 20.5 B 4 P 4 Nb 2 Cu 0.5 for later use.
利用所得原料,经电弧熔炼方式经真空冶炼形成合金,经熔体净化处理,以降低其中有害杂质元素或夹杂带来的危害,经冶炼形成均匀混合的合金液,直接用于制带。制带过程中控制合金液浇铸温度为1310~1330℃之间,将合金液经压力单辊甩带机方式获得平直的条带,利用XRD方式检测条带的物相状态是否为完全非晶状态,将条带收集后待用。The obtained raw materials are used to form an alloy through vacuum smelting through arc smelting. The melt is purified to reduce the harm caused by harmful impurity elements or inclusions. After smelting, a uniformly mixed alloy liquid is formed, which can be directly used for belt making. During the strip making process, the casting temperature of the alloy liquid is controlled between 1310 and 1330°C. The alloy liquid is passed through a pressure single-roller belt spinning machine to obtain a straight strip. The XRD method is used to detect whether the physical phase state of the strip is completely amorphous. status, collect the strips for later use.
将收集到的条带按照需要的尺寸裁切后经卷绕,可制作成外径为30mm、内径为20mm、高度为10mm的圆环形磁芯,磁芯内外层经点焊或其他方式固定,以防止磁芯散开。The collected strips are cut to the required size and then rolled to make a circular magnetic core with an outer diameter of 30mm, an inner diameter of 20mm, and a height of 10mm. The inner and outer layers of the core are fixed by spot welding or other methods. , to prevent the core from spreading.
该磁芯经横向磁场热处理后可获得性能优异的纳米晶磁芯,处理工艺为磁场热处理,磁场的施加方式为电磁铁施加,磁场强度0.1T,且在整个两阶段的热处理过程中均有施加。其中第一阶段热处理为460℃热处理120min,第二阶段热处理为540℃热处理,保温180min。After the magnetic core is subjected to transverse magnetic field heat treatment, a nanocrystalline magnetic core with excellent performance can be obtained. The treatment process is magnetic field heat treatment. The magnetic field is applied by an electromagnet. The magnetic field intensity is 0.1T and is applied during the entire two-stage heat treatment process. . The first stage of heat treatment is 460°C heat treatment for 120 minutes, and the second stage heat treatment is 540°C heat treatment with heat preservation for 180 minutes.
利用阻抗分析仪即可测试本实施例所获磁芯在不同频率下的电感量,计算可知其在100kHz下的相对磁导率为34100。The inductance of the magnetic core obtained in this embodiment at different frequencies can be tested using an impedance analyzer. Calculation shows that its relative magnetic permeability at 100 kHz is 34100.
实施例2本实施例提供的一种高频高磁导率铁基纳米晶合金的制备方法包括如下步骤:Example 2 This example provides a method for preparing a high-frequency, high-permeability iron-based nanocrystalline alloy, which includes the following steps:
利用金属单质Fe、Si、Cu和中间合金FeB、FeP、FeNb来进行合金成分的称量配料获得Fe71.5Si19B3P2.75Nb3Cu0.75待用。Use metal elements Fe, Si, Cu and intermediate alloys FeB, FeP, FeNb to weigh and batch the alloy components to obtain Fe 71.5 Si 19 B 3 P 2.75 Nb 3 Cu 0.75 for later use.
利用所得原料,可经非真空感应方式冶炼,经熔体净化处理,以降低其中有害杂质元素或夹杂带来的危害,经冶炼形成均匀混合的合金液,合金液直接用于制带。The raw materials obtained can be smelted by non-vacuum induction methods, and the melt can be purified to reduce the harm caused by harmful impurity elements or inclusions. After smelting, a uniformly mixed alloy liquid can be formed, and the alloy liquid can be directly used for belt making.
制带过程中,控制合金液浇铸温度为1330~1350℃之间,将合金液经重力制带方式获得平直的条带,利用XRD方式检测条带的物相状态是否为完全非晶状态,将条带收集后待用。During the strip making process, the casting temperature of the alloy liquid is controlled to be between 1330 and 1350°C. The alloy liquid is made into a straight strip by gravity strip making, and the XRD method is used to detect whether the physical phase state of the strip is completely amorphous. Collect the strips and set aside for later use.
将收集到的条带按照需要的尺寸裁切后经卷绕,,可制作成外径为30mm、内径为20mm、高度为10mm的圆环形磁芯,磁芯内外层经点焊或其他方式固定,以防止磁芯散开。The collected strips are cut and rolled according to the required size, and can be made into a circular magnetic core with an outer diameter of 30mm, an inner diameter of 20mm, and a height of 10mm. The inner and outer layers of the core are spot welded or otherwise. Secure to prevent the core from unraveling.
该磁芯经横向磁场热处理后可获得性能优异的纳米晶磁芯,处理工艺为磁场热处理,磁场的施加方式为电磁铁施加,磁场强度1T,在整个两阶段的热处理过程中均有施加。其中第一阶段热处理为470℃热处理60min,第二阶段热处理为560℃热处理,保温150min。After the magnetic core is subjected to transverse magnetic field heat treatment, a nanocrystalline magnetic core with excellent performance can be obtained. The treatment process is magnetic field heat treatment. The magnetic field is applied by an electromagnet. The magnetic field intensity is 1T, which is applied during the entire two-stage heat treatment process. The first stage of heat treatment is 470°C heat treatment for 60 minutes, and the second stage heat treatment is 560°C heat treatment with heat preservation for 150 minutes.
利用阻抗分析仪即可测试本实施例所获磁芯在不同频率下的电感量,计算可知其在100kHz下的相对磁导率为32400。The inductance of the magnetic core obtained in this embodiment at different frequencies can be tested using an impedance analyzer. Calculation shows that its relative magnetic permeability at 100 kHz is 32,400.
实施例3本实施例提供的一种高频高磁导率铁基纳米晶合金的制备方法包括如下步骤:Example 3 This example provides a method for preparing a high-frequency, high-permeability iron-based nanocrystalline alloy, which includes the following steps:
利用金属单质Fe、Si、Cu和中间合金FeB、FeP、FeNb来进行合金成分的称量配料获得Fe73.5Si17B4.25P2Nb2Cu1.25待用。Use metal elements Fe, Si, Cu and master alloys FeB, FeP, FeNb to weigh and batch the alloy components to obtain Fe 73.5 Si 17 B 4.25 P 2 Nb 2 Cu 1.25 for later use.
利用所得原料,经非真空方式冶炼,经熔体净化处理,以降低其中有害杂质元素或夹杂带来的危害,经冶炼形成均匀混合的合金液,合金液直接用于制带。制带过程中控制合金液浇铸温度为1370~1390℃之间,将合金液经重力单辊甩带机方式获得平直的条带,利用XRD方式检测条带的物相状态是否为完全非晶状态,将条带收集后待用。The obtained raw materials are smelted in a non-vacuum manner, and the melt is purified to reduce the harm caused by harmful impurity elements or inclusions. After smelting, a uniformly mixed alloy liquid is formed, and the alloy liquid is directly used for belt making. During the strip making process, the casting temperature of the alloy liquid is controlled between 1370 and 1390°C. The alloy liquid is passed through a gravity single-roller strip machine to obtain a straight strip. The XRD method is used to detect whether the physical phase state of the strip is completely amorphous. status, collect the strips for later use.
将收集到的条带按照需要的尺寸裁切后经卷绕,可制作成外径为30mm、内径为20mm、高度为10mm的圆环形磁芯,磁芯内外层经点焊或其他方式固定,以防止磁芯散开。The collected strips are cut to the required size and then rolled to make a circular magnetic core with an outer diameter of 30mm, an inner diameter of 20mm, and a height of 10mm. The inner and outer layers of the core are fixed by spot welding or other methods. , to prevent the core from spreading.
该磁芯经横向磁场热处理后可获得性能优异的纳米晶磁芯,处理工艺为磁场热处理,磁场的施加方式为永磁体施加,磁场强度0.1T,仅在第二阶段的热处理过程中有施加。其中第一阶段热处理为470℃热处理90min,第二阶段热处理为560℃热处理,保温150min。The magnetic core can obtain a nanocrystalline magnetic core with excellent performance after transverse magnetic field heat treatment. The treatment process is magnetic field heat treatment. The magnetic field is applied by a permanent magnet. The magnetic field intensity is 0.1T. It is only applied during the second stage of heat treatment. The first stage of heat treatment is 470°C heat treatment for 90 minutes, and the second stage heat treatment is 560°C heat treatment with heat preservation for 150 minutes.
利用阻抗分析仪即可测试本实施例所获磁芯在不同频率下的电感量,计算可知其在100kHz下的相对磁导率为31800。The inductance of the magnetic core obtained in this embodiment at different frequencies can be tested using an impedance analyzer. Calculation shows that its relative magnetic permeability at 100 kHz is 31,800.
实施例4本实施例提供的一种高频高磁导率铁基纳米晶合金的制备方法包括如下步骤:Example 4 This example provides a method for preparing a high-frequency, high-permeability iron-based nanocrystalline alloy, which includes the following steps:
利用金属单质Fe、Si、Cu和中间合金FeB、FeP、FeNb来进行合金成分的称量配料获得Fe75Si15.5B6P0.5Nb1.5Cu1.5待用。Use metal elements Fe, Si, Cu and master alloys FeB, FeP, FeNb to weigh and batch the alloy components to obtain Fe 75 Si 15.5 B 6 P 0.5 Nb 1.5 Cu 1.5 for later use.
利用所得原料,经真空感应方式冶炼,冶炼过程经熔体净化处理,以降低其中有害杂质元素或夹杂带来的危害,经冶炼形成均匀混合的合金液,冷却后形成合金锭,以备将合金锭熔化为合金液后用于制带。制带过程中控制合金液浇铸温度为1390~1410℃之间,将合金液经重力单辊甩带机方式获得平直的条带,利用XRD方式检测条带的物相状态是否为完全非晶状态,将条带收集后待用。The obtained raw materials are smelted by vacuum induction. The melt is purified during the smelting process to reduce the harm caused by harmful impurity elements or inclusions. After smelting, a uniformly mixed alloy liquid is formed. After cooling, an alloy ingot is formed to prepare the alloy. The ingot is melted into molten alloy and used to make strips. During the strip making process, the casting temperature of the alloy liquid is controlled to be between 1390 and 1410°C. The alloy liquid is passed through a gravity single-roller strip machine to obtain a straight strip. The XRD method is used to detect whether the physical phase state of the strip is completely amorphous. status, collect the strips for later use.
将收集到的条带按照需要的尺寸裁切后经卷绕,可制作成外径为30mm、内径为20mm、高度为10mm的圆环形磁芯,磁芯内外层经点焊或其他方式固定,以防止磁芯散开。The collected strips are cut to the required size and then rolled to make a circular magnetic core with an outer diameter of 30mm, an inner diameter of 20mm, and a height of 10mm. The inner and outer layers of the core are fixed by spot welding or other methods. , to prevent the core from spreading.
该磁芯经横向磁场热处理后可获得性能优异的纳米晶磁芯,处理工艺为磁场热处理,磁场的施加方式为线圈施加,磁场强度0.01T,在整个两阶段的热处理过程中均有施加。其中第一阶段热处理为480℃热处理30min,第二阶段热处理为580℃热处理,保温90min。The magnetic core can obtain a nanocrystalline magnetic core with excellent performance after transverse magnetic field heat treatment. The treatment process is magnetic field heat treatment. The magnetic field is applied by coil. The magnetic field intensity is 0.01T, which is applied during the entire two-stage heat treatment process. The first stage of heat treatment is 480°C for 30 minutes, and the second stage of heat treatment is 580°C with heat preservation for 90 minutes.
利用阻抗分析仪即可测试本实施例所获磁芯在不同频率下的电感量,计算可知其在100kHz下的相对磁导率为29300。The inductance of the magnetic core obtained in this embodiment at different frequencies can be tested using an impedance analyzer. Calculation shows that its relative magnetic permeability at 100 kHz is 29,300.
实施例5本实施例提供的一种高频高磁导率铁基纳米晶合金的制备方法包括如下步骤:Example 5 This example provides a method for preparing a high-frequency, high-permeability iron-based nanocrystalline alloy, which includes the following steps:
利用金属单质Fe、Si、Cu和中间合金FeB、FeP、FeNb来进行合金成分的称量配料获得Fe70Si15.5B8P4Nb2Cu0.5待用。Use metal elements Fe, Si, Cu and intermediate alloys FeB, FeP, FeNb to weigh and batch the alloy components to obtain Fe 70 Si 15.5 B 8 P 4 Nb 2 Cu 0.5 for later use.
利用所得原料,经真空感应方式冶炼,其中冶炼经熔体净化处理,以降低其中有害杂质元素或夹杂带来的危害,经冶炼形成均匀混合的合金液,合金液可以直接用于制带。制带过程中控制合金液浇铸温度为1330~1350℃之间,将合金液经重力单辊甩带机方式获得平直的条带,利用XRD方式检测条带的物相状态是否为完全非晶状态,将条带收集后待用。The obtained raw materials are smelted by vacuum induction. The smelting is subjected to melt purification to reduce the harm caused by harmful impurity elements or inclusions. After smelting, a uniformly mixed alloy liquid is formed, and the alloy liquid can be directly used for belt making. During the strip making process, the casting temperature of the alloy liquid is controlled to be between 1330 and 1350°C. The alloy liquid is passed through a gravity single-roller belt spinning machine to obtain a straight strip. The XRD method is used to detect whether the physical phase state of the strip is completely amorphous. status, collect the strips for later use.
将收集到的条带按照需要的尺寸裁切后经卷绕,可制作成外径为30mm、内径为20mm、高度为10mm的圆环形磁芯,磁芯内外层经点焊或其他方式固定,以防止磁芯散开。The collected strips are cut to the required size and then rolled to make a circular magnetic core with an outer diameter of 30mm, an inner diameter of 20mm, and a height of 10mm. The inner and outer layers of the core are fixed by spot welding or other methods. , to prevent the core from spreading.
该磁芯经横向磁场热处理后可获得性能优异的纳米晶磁芯,处理工艺为磁场热处理,磁场的施加方式为永磁体施加,磁场强度0.1T,在整个两阶段的热处理过程中均有施加。其中第一阶段热处理为460℃热处理90min,第二阶段热处理为570℃热处理,保温120min。After the magnetic core is subjected to transverse magnetic field heat treatment, a nanocrystalline magnetic core with excellent performance can be obtained. The treatment process is magnetic field heat treatment. The magnetic field is applied by a permanent magnet. The magnetic field intensity is 0.1T, which is applied during the entire two-stage heat treatment process. The first stage of heat treatment is 460°C heat treatment for 90 minutes, and the second stage heat treatment is 570°C heat treatment with heat preservation for 120 minutes.
利用阻抗分析仪即可测试本实施例所获磁芯在不同频率下的电感量,计算可知其在100kHz下的相对磁导率为31500。The inductance of the magnetic core obtained in this embodiment at different frequencies can be tested using an impedance analyzer. Calculation shows that its relative magnetic permeability at 100 kHz is 31,500.
实施例6本实施例提供的一种高频高磁导率铁基纳米晶合金的制备方法包括如下步骤:Example 6 This example provides a method for preparing a high-frequency, high-permeability iron-based nanocrystalline alloy, which includes the following steps:
利用金属单质Fe、Si、Cu和中间合金FeB、FeP、FeNb来进行合金成分的称量配料获得Fe73.5Si16.5B2P5Nb2Cu1待用。Use metal elements Fe, Si, Cu and master alloys FeB, FeP, FeNb to weigh and batch the alloy components to obtain Fe 73.5 Si 16.5 B 2 P 5 Nb 2 Cu 1 for later use.
利用所得原料,经非真空感应方式冶炼,其中非真空方式冶炼需经熔体净化处理,以降低其中有害杂质元素或夹杂带来的危害,经冶炼形成均匀混合的合金液,合金液冷却后形成合金锭,以备再将合金锭熔化为合金液后用于制带。制带过程中控制合金液浇铸温度为1320~1340℃之间,将合金液经压力单辊甩带机方式获得平直的条带,利用XRD方式检测条带的物相状态是否为完全非晶状态,将条带收集后待用。The obtained raw materials are smelted by non-vacuum induction method. The non-vacuum smelting method requires melt purification treatment to reduce the harm caused by harmful impurity elements or inclusions. After smelting, a uniformly mixed alloy liquid is formed. The alloy liquid is cooled to form Alloy ingots are prepared to be melted into alloy liquid and used for strip making. During the strip making process, the casting temperature of the alloy liquid is controlled between 1320 and 1340°C. The alloy liquid is passed through a pressure single-roller belt spinning machine to obtain a straight strip. The XRD method is used to detect whether the physical phase state of the strip is completely amorphous. status, collect the strips for later use.
将收集到的条带按照需要的尺寸裁切后经卷绕,可制作成外径为30mm、内径为20mm、高度为10mm的圆环形磁芯,磁芯内外层经点焊或其他方式固定,以防止磁芯散开。The collected strips are cut to the required size and then rolled to make a circular magnetic core with an outer diameter of 30mm, an inner diameter of 20mm, and a height of 10mm. The inner and outer layers of the core are fixed by spot welding or other methods. , to prevent the core from spreading.
该磁芯经横向磁场热处理后可获得性能优异的纳米晶磁芯,处理工艺为磁场热处理,磁场的施加方式为电磁铁施加,磁场强度为1T,在整个两阶段的热处理过程中均有施加。其中第一阶段热处理为470℃热处理120min,第二阶段热处理为560℃热处理,保温150min。The magnetic core can obtain a nanocrystalline magnetic core with excellent performance after transverse magnetic field heat treatment. The treatment process is magnetic field heat treatment. The magnetic field is applied by an electromagnet. The magnetic field intensity is 1T, which is applied during the entire two-stage heat treatment process. The first stage of heat treatment is 470°C heat treatment for 120 minutes, and the second stage heat treatment is 560°C heat treatment with heat preservation for 150 minutes.
利用阻抗分析仪即可测试本实施例所获磁芯在不同频率下的电感量,计算可知其在100kHz下的相对磁导率为33600。The inductance of the magnetic core obtained in this embodiment at different frequencies can be tested using an impedance analyzer. Calculation shows that its relative permeability at 100 kHz is 33600.
对比例1本对比例提供的一种高频高磁导率铁基纳米晶合金的制备方法包括如下步骤:Comparative Example 1 This comparative example provides a method for preparing a high-frequency, high-permeability iron-based nanocrystalline alloy, which includes the following steps:
利用金属单质Fe、Si、Cu和中间合金FeB、FeNb来进行合金成分的称量配料获得Fe73.5Si20.5B3Nb2Cu1待用。Use metal elements Fe, Si, Cu and intermediate alloys FeB and FeNb to weigh and batch the alloy components to obtain Fe 73.5 Si 20.5 B 3 Nb 2 Cu 1 for later use.
利用所得原料,经非真空感应方式冶炼,其中非真空方式冶炼需经熔体净化处理,以降低其中有害杂质元素或夹杂带来的危害,经冶炼形成均匀混合的合金液,合金液冷却后形成合金锭,以备再将合金锭熔化为合金液后用于制带。The obtained raw materials are smelted by non-vacuum induction method. The non-vacuum smelting method requires melt purification treatment to reduce the harm caused by harmful impurity elements or inclusions. After smelting, a uniformly mixed alloy liquid is formed. The alloy liquid is cooled to form Alloy ingots are prepared to be melted into alloy liquid and used for strip making.
制带过程中,控制合金液浇铸温度为1410~1430℃之间,将合金液经重力单辊甩带机方式获得平直的条带,利用XRD方式检测条带的物相状态是否为完全非晶状态,将条带收集后待用。检测结果表示条带为晶化状态,后续制作必然导致磁性能完全恶化。During the strip making process, the casting temperature of the alloy liquid is controlled between 1410 and 1430°C. The alloy liquid is passed through a gravity single-roller belt spinning machine to obtain a straight strip. The XRD method is used to detect whether the physical phase state of the strip is completely non-conforming. Crystallized state, collect the strips for later use. The test results indicate that the strips are in a crystallized state, and subsequent production will inevitably lead to complete deterioration of the magnetic properties.
对比例2本对比例提供的一种高频高磁导率铁基纳米晶合金的制备方法包括如下步骤:Comparative Example 2 This comparative example provides a method for preparing a high-frequency, high-permeability iron-based nanocrystalline alloy, which includes the following steps:
利用金属单质Fe、Si、Cu和中间合金FeB、FeNb来进行合金成分的称量配料获得Fe73.5Si15.5B7Nb3Cu1待用。Use metal elements Fe, Si, Cu and intermediate alloys FeB and FeNb to weigh and batch the alloy components to obtain Fe 73.5 Si 15.5 B 7 Nb 3 Cu 1 for later use.
利用所得原料,经非真空感应方式冶炼,其中非真空方式冶炼需经熔体净化处理,以降低其中有害杂质元素或夹杂带来的危害,经冶炼形成均匀混合的合金液,合金液冷却后形成合金锭,以备再将合金锭熔化为合金液后用于制带。制带过程中控制合金液浇铸温度为1430~1450℃之间,将合金液经重力单辊甩带机方式获得平直的条带,利用XRD方式检测条带的物相状态是否为完全非晶状态,将条带收集后待用。The obtained raw materials are smelted by non-vacuum induction method. The non-vacuum smelting method requires melt purification treatment to reduce the harm caused by harmful impurity elements or inclusions. After smelting, a uniformly mixed alloy liquid is formed. The alloy liquid is cooled to form Alloy ingots are prepared to be melted into alloy liquid and used for strip making. During the strip making process, the casting temperature of the alloy liquid is controlled to be between 1430 and 1450°C. The alloy liquid is passed through a gravity single-roller belt spinning machine to obtain a straight strip. The XRD method is used to detect whether the physical phase state of the strip is completely amorphous. status, collect the strips for later use.
将收集到的条带按照需要的尺寸裁切后经卷绕,可制作成外径为30mm、内径为20mm、高度为10mm的圆环形磁芯,磁芯内外层经点焊或其他方式固定,以防止磁芯散开。The collected strips are cut to the required size and then rolled to make a circular magnetic core with an outer diameter of 30mm, an inner diameter of 20mm, and a height of 10mm. The inner and outer layers of the core are fixed by spot welding or other methods. , to prevent the core from spreading.
该磁芯经横向磁场热处理后可获得性能优异的纳米晶磁芯,处理工艺为磁场热处理,磁场的施加方式为永磁体施加,磁场强度0.1T,在整个两阶段的热处理过程中均有施加。其中第一阶段热处理为470℃热处理120min,第二阶段热处理为560℃热处理,保温150min。After the magnetic core is subjected to transverse magnetic field heat treatment, a nanocrystalline magnetic core with excellent performance can be obtained. The treatment process is magnetic field heat treatment. The magnetic field is applied by a permanent magnet. The magnetic field intensity is 0.1T, which is applied during the entire two-stage heat treatment process. The first stage of heat treatment is 470°C heat treatment for 120 minutes, and the second stage heat treatment is 560°C heat treatment with heat preservation for 150 minutes.
利用阻抗分析仪即可测试本对比例所获磁芯在不同频率下的电感量,计算可知其在100kHz下的相对磁导率为26500。The inductance of the magnetic core obtained in this comparative example at different frequencies can be tested using an impedance analyzer. Calculation shows that its relative permeability at 100kHz is 26500.
对比例3本对比例提供的一种高频高磁导率铁基纳米晶合金的制备方法包括如下步骤:Comparative Example 3 This comparative example provides a method for preparing a high-frequency, high-permeability iron-based nanocrystalline alloy, which includes the following steps:
利用金属单质Fe、Si、Cu和中间合金FeB、FeP、FeNb来进行合金成分的称量配料获得Fe73.5Si14B7P1.5Nb3Cu1待用。Use metal elements Fe, Si, Cu and intermediate alloys FeB, FeP, FeNb to weigh and batch the alloy components to obtain Fe 73.5 Si 14 B 7 P 1.5 Nb 3 Cu 1 for later use.
利用所得原料,经非真空感应方式冶炼,其中非真空方式冶炼需经熔体净化处理,以降低其中有害杂质元素或夹杂带来的危害,经冶炼形成均匀混合的合金液,合金液冷却后形成合金锭,以备再将合金锭熔化为合金液后用于制带。制带过程中控制合金液浇铸温度为1400~1430℃之间,将合金液经重力单辊甩带机方式获得平直的条带,利用XRD方式检测条带的物相状态是否为完全非晶状态,将条带收集后待用。The obtained raw materials are smelted by non-vacuum induction method. The non-vacuum smelting method requires melt purification treatment to reduce the harm caused by harmful impurity elements or inclusions. After smelting, a uniformly mixed alloy liquid is formed. The alloy liquid is cooled to form Alloy ingots are prepared to be melted into alloy liquid and used for strip making. During the strip making process, the casting temperature of the alloy liquid is controlled between 1400 and 1430°C. The alloy liquid is passed through a gravity single-roller strip machine to obtain a straight strip. The XRD method is used to detect whether the physical phase state of the strip is completely amorphous. status, collect the strips for later use.
将收集到的条带按照需要的尺寸裁切后经卷绕,可制作成外径为30mm、内径为20mm、高度为10mm的圆环形磁芯,磁芯内外层经点焊或其他方式固定,以防止磁芯散开。The collected strips are cut to the required size and then rolled to make a circular magnetic core with an outer diameter of 30mm, an inner diameter of 20mm, and a height of 10mm. The inner and outer layers of the core are fixed by spot welding or other methods. , to prevent the core from spreading.
该磁芯经横向磁场热处理后可获得性能优异的纳米晶磁芯,处理工艺为磁场热处理,磁场的施加方式为永磁体施加,磁场强度0.1T,在整个两阶段的热处理过程中均有施加。其中第一阶段热处理为470℃热处理120min,第二阶段热处理为560℃热处理,保温150min。After the magnetic core is subjected to transverse magnetic field heat treatment, a nanocrystalline magnetic core with excellent performance can be obtained. The treatment process is magnetic field heat treatment. The magnetic field is applied by a permanent magnet. The magnetic field intensity is 0.1T, which is applied during the entire two-stage heat treatment process. The first stage of heat treatment is 470°C heat treatment for 120 minutes, and the second stage heat treatment is 560°C heat treatment with heat preservation for 150 minutes.
利用阻抗分析仪即可测试本对比例所获磁芯在不同频率下的电感量,计算可知其在100kHz下的相对磁导率为26800。The inductance of the magnetic core obtained in this comparative example at different frequencies can be tested using an impedance analyzer. Calculation shows that its relative permeability at 100kHz is 26800.
对比例4本对比例提供的一种高频高磁导率铁基纳米晶合金的制备方法包括如下步骤:Comparative Example 4 This comparative example provides a method for preparing a high-frequency, high-permeability iron-based nanocrystalline alloy, which includes the following steps:
利用金属单质Fe、Si、Cu和中间合金FeB、FeP、FeNb来进行合金成分的称量配料获得Fe70Si21B3P2Nb3Cu1待用。Use metal elements Fe, Si, Cu and intermediate alloys FeB, FeP, FeNb to weigh and batch the alloy components to obtain Fe 70 Si 21 B 3 P 2 Nb 3 Cu 1 for later use.
利用所得原料,经非真空感应方式冶炼,其中非真空方式冶炼需经熔体净化处理,以降低其中有害杂质元素或夹杂带来的危害,经冶炼形成均匀混合的合金液,合金液冷却后形成合金锭,以备再将合金锭熔化为合金液后用于制带。The obtained raw materials are smelted by non-vacuum induction method. The non-vacuum smelting method requires melt purification treatment to reduce the harm caused by harmful impurity elements or inclusions. After smelting, a uniformly mixed alloy liquid is formed. The alloy liquid is cooled to form Alloy ingots are prepared to be melted into alloy liquid and used for strip making.
制带过程中,控制合金液浇铸温度为1380~1400℃之间,将合金液经重力单辊甩带机方式获得平直的条带,利用XRD方式检测条带的物相状态是否为完全非晶状态,将条带收集后待用。检测结果表示条带为晶化状态,后续制作必然导致磁性能完全恶化。During the strip making process, the casting temperature of the alloy liquid is controlled to be between 1380 and 1400°C. The alloy liquid is passed through a gravity single-roller belt spinning machine to obtain a straight strip. The XRD method is used to detect whether the physical phase state of the strip is completely non-conforming. Crystallized state, collect the strips for later use. The test results indicate that the strips are in a crystallized state, and subsequent production will inevitably lead to complete deterioration of the magnetic properties.
对比例5本对比例提供的一种高频高磁导率铁基纳米晶合金的制备方法包括如下步骤:Comparative Example 5 This comparative example provides a method for preparing a high-frequency, high-permeability iron-based nanocrystalline alloy, which includes the following steps:
利用金属单质Fe、Si、Cu和中间合金FeB、FeP、FeNb来进行合金成分的称量配料获得Fe69Si20.5B0.5P6Nb3Cu1待用。Use metal elements Fe, Si, Cu and intermediate alloys FeB, FeP, FeNb to weigh and batch the alloy components to obtain Fe 69 Si 20.5 B 0.5 P 6 Nb 3 Cu 1 for later use.
利用所得原料,经非真空感应方式冶炼,其中非真空方式冶炼需经熔体净化处理,以降低其中有害杂质元素或夹杂带来的危害,经冶炼形成均匀混合的合金液,合金液冷却后形成合金锭,以备再将合金锭熔化为合金液后用于制带。制带过程中控制合金液浇铸温度为1310~1330℃之间,将合金液经重力单辊甩带机方式获得平直的条带,利用XRD方式检测条带的物相状态是否为完全非晶状态,将条带收集后待用。The obtained raw materials are smelted by non-vacuum induction method. The non-vacuum smelting method requires melt purification treatment to reduce the harm caused by harmful impurity elements or inclusions. After smelting, a uniformly mixed alloy liquid is formed. The alloy liquid is cooled to form Alloy ingots are prepared to be melted into alloy liquid and used for strip making. During the strip making process, the casting temperature of the alloy liquid is controlled to be between 1310 and 1330°C. The alloy liquid is passed through a gravity single-roller belt spinning machine to obtain a straight strip. The XRD method is used to detect whether the physical phase state of the strip is completely amorphous. status, collect the strips for later use.
将收集到的条带按照需要的尺寸裁切后经卷绕,可制作成外径为30mm、内径为20mm、高度为10mm的圆环形磁芯,磁芯内外层经点焊或其他方式固定,以防止磁芯散开。The collected strips are cut to the required size and then rolled to make a circular magnetic core with an outer diameter of 30mm, an inner diameter of 20mm, and a height of 10mm. The inner and outer layers of the core are fixed by spot welding or other methods. , to prevent the core from spreading.
该磁芯经横向磁场热处理后可获得性能优异的纳米晶磁芯,处理工艺为磁场热处理,磁场的施加方式为永磁体施加,磁场强度0.1T,在整个两阶段的热处理过程中均有施加。其中第一阶段热处理为470℃热处理120min,第二阶段热处理为560℃热处理,保温150min。After the magnetic core is subjected to transverse magnetic field heat treatment, a nanocrystalline magnetic core with excellent performance can be obtained. The treatment process is magnetic field heat treatment. The magnetic field is applied by a permanent magnet. The magnetic field intensity is 0.1T, which is applied during the entire two-stage heat treatment process. The first stage of heat treatment is 470°C heat treatment for 120 minutes, and the second stage heat treatment is 560°C heat treatment with heat preservation for 150 minutes.
利用阻抗分析仪即可测试本对比例所获磁芯在不同频率下的电感量,计算可知其在100kHz下的相对磁导率为27200。The inductance of the magnetic core obtained in this comparative example at different frequencies can be tested using an impedance analyzer. Calculation shows that its relative permeability at 100kHz is 27200.
尽管已参考说明性实施例描述了本发明,但所属领域的技术人员将理解,在不背离本发明的精神及范围的情况下可做出各种其它改变、省略及/或添加且可用实质等效物替代所述实施例的元件。另外,可在不背离本发明的范围的情况下做出许多修改以使特定情形或材料适应本发明的教示。因此,本文并不打算将本发明限制于用于执行本发明的所揭示特定实施例,而是打算使本发明将包含归属于所附权利要求书的范围内的所有实施例。Although the present invention has been described with reference to illustrative embodiments, those skilled in the art will understand that various other changes, omissions and/or additions may be made and the substance thereof may be used without departing from the spirit and scope of the invention. Elements of the described embodiments may be replaced with effective ones. In addition, many modifications may be made to adapt a particular situation or material to the teachings of the invention without departing from its scope. Therefore, it is intended that the invention not be limited to the particular embodiments disclosed for carrying out this invention, but that the invention will include all embodiments falling within the scope of the appended claims.
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崔兴华等: "铁基纳米晶共模磁芯的制备及其性能研究", 《金属功能材料》, vol. 22, no. 2, 30 April 2015 (2015-04-30), pages 8 - 9 * |
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