CN102832001B - Iron-base multiphase magnetic alloy material and preparation method thereof - Google Patents
Iron-base multiphase magnetic alloy material and preparation method thereof Download PDFInfo
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Abstract
本发明提供一种铁基复相磁性合金及其制备方法，该合金不仅具有低的铁损和高韧性，而且合金熔化也容易操作。该制备方法工艺简单，生产成本低，适于工业化生产。该合金材料各成分的重量百分含量为：Gd3.0-6.0％，Si1.0-3.0％，Al1.0-3.0％，B 3.0-6.0％，Re0.05-0.09％， Tb0.01-0.03％，Co1.0-3.0％，其余为Fe。
The invention provides an iron-based multi-phase magnetic alloy and a preparation method thereof. The alloy not only has low iron loss and high toughness, but also is easy to operate when melting the alloy. The preparation method has simple process, low production cost and is suitable for industrialized production. The weight percentage of each component of the alloy material is: Gd3.0-6.0%, Si1.0-3.0%, Al1.0-3.0%, B 3.0-6.0%, Re0.05-0.09%, Tb0.01- 0.03%, Co1.0-3.0%, and the rest is Fe.
Description
技术领域 technical field
本发明属于金属材料技术领域，涉及一种铁基复相磁性合金及其制备方法。 The invention belongs to the technical field of metal materials, and relates to an iron-based multiphase magnetic alloy and a preparation method thereof.
背景技术 Background technique
200510128543.2号申请提供一种在交流下的软磁特性优异的Fe基非晶质合金薄带，它是通过有槽缝状开口部的浇注喷嘴使熔融合金喷出到移动的冷却基板上，使之急冷凝固而得到的，所述薄带的组成按原子％计为Fe：78％以上86％以下、Si：2％以上但不到4％、B：2％以上15％以下、C：0.02％ 以上4％以下、用符号M表示P、As、Bi、S、Se、Te的1种或2种以上为M：1％以上14％以下、且B+M：12％以上20％以下，而且将薄带宽度方向的各部位的退火后的铁损最大值记为Wmax、最小值记为Wmin 的场合，(Wmax-Wmin)/Wmin为0.4以下。在含有0.2原子％以上12原子％以下的P的非晶质母相的至少一侧的薄带表面，有厚度为5nm以上20nm以下的极薄氧化层。外加频率50Hz、最大外加 磁场80A/m交流磁场的场合在ΔTA≥80℃、ΔTB≥60℃的宽幅的退火温度范围下得到的最大磁通密度B80≥1.35T、B80的标准偏差不到0.1、铁 损≤0.12W/kg。而且，得到εf≥0.01的优异的耐脆化特性。 Application No. 200510128543.2 provides a thin strip of Fe-based amorphous alloy with excellent soft magnetic properties under alternating current. It sprays molten alloy onto a moving cooling substrate through a pouring nozzle with a slot-like opening to make it Obtained by rapid cooling and solidification, the composition of the ribbon is Fe: 78% to 86%, Si: 2% to less than 4%, B: 2% to 15%, C: 0.02% in atomic % The above 4% or less, one or more of P, As, Bi, S, Se, Te represented by the symbol M is M: 1% to 14% and B+M: 12% to 20%, and When the maximum value of iron loss after annealing at each location in the width direction of the strip is expressed as Wmax and the minimum value is expressed as Wmin, (Wmax-Wmin)/Wmin is 0.4 or less. An extremely thin oxide layer with a thickness of 5 nm to 20 nm is present on at least one surface of the ribbon of the amorphous matrix phase containing 0.2 atomic % to 12 atomic % of P. The standard of the maximum magnetic flux density B 80 ≥ 1.35T, B 80 obtained under the wide annealing temperature range of ΔT A ≥ 80°C and ΔT B ≥ 60°C when the applied frequency is 50Hz and the maximum applied magnetic field is 80A/m AC magnetic field Deviation less than 0.1, iron loss ≤0.12W/kg. Furthermore, excellent embrittlement resistance characteristics of ε f ≧0.01 are obtained.
但是其合金体系中的Te的沸点为1390℃， S的沸点为444.674℃，熔化时很难操作。Bi的熔点为271.3℃，高于熔点，金属很容易氧化。另外该合金的铁损也需要改善。 However, the boiling point of Te in the alloy system is 1390°C, and the boiling point of S is 444.674°C, so it is difficult to handle when melting. The melting point of Bi is 271.3°C, which is higher than the melting point, and the metal is easily oxidized. In addition, the iron loss of the alloy also needs to be improved.
发明内容 Contents of the invention
本发明的目的就是针对上述技术缺陷，提供一种铁基复相磁性合金，该合金不仅具有低的铁损和高韧性，而且合金熔化也容易操作。 The object of the present invention is to address the above-mentioned technical defects and provide an iron-based multi-phase magnetic alloy, which not only has low iron loss and high toughness, but also is easy to operate when melting the alloy.
本发明的另一目的是提供一种铁基复相磁性合金制备方法，该制备方法工艺简单，生产成本低，适于工业化生产。 Another object of the present invention is to provide a method for preparing an iron-based multiphase magnetic alloy. The preparation method has simple process, low production cost and is suitable for industrial production.
本发明的目的是通过以下技术方案实现的： The purpose of the present invention is achieved through the following technical solutions:
一种铁基复相磁性合金材料，其特征是：该合金材料中各成分的重量百分含量为： Gd 3.0-6.0％，Si 1.0-3.0％，Al 1.0-3.0％ ，B 3.0-6.0％，Re 0.05-0.09％，Tb 0.01-0.03％，Co 1.0-3.0％，其余为Fe。 An iron-based multiphase magnetic alloy material is characterized in that: the weight percentage of each component in the alloy material is: Gd 3.0-6.0%, Si 1.0-3.0%, Al 1.0-3.0%, B 3.0-6.0% , Re 0.05-0.09%, Tb 0.01-0.03%, Co 1.0-3.0%, and the rest is Fe.
该铁基复相磁性合金的组织特点为非晶的基体上分布着部分纳米级晶粒，纳米级晶粒所占合金材料的体积为30-40%。纳米级晶粒的尺寸为80-100nm。 The structure characteristic of the iron-based multiphase magnetic alloy is that some nano-scale grains are distributed on the amorphous matrix, and the nano-scale grains account for 30-40% of the volume of the alloy material. The size of the nanoscale grains is 80-100nm.
上述铁基复相磁性合金材料的制备方法，具体步骤如下： The preparation method of the above-mentioned iron-based multiphase magnetic alloy material, the specific steps are as follows:
（1）首先按照各成分的重量百分含量为： Gd 3.0-6.0％，Si1.0-3.0％，Al 1.0-3.0％ ，B 3.0-6.0％，Re 0.05-0.09％，Tb0.01-0.03％，Co1.0-3.0％，其余为Fe进行配料，原料Si、Al、B、Re 、Tb、Co、Fe的纯度均大于99.9％，Gd以铁钆中间合金的方式加入，铁钆合金中Gd的重量百分比为35%； (1) First, according to the weight percentage of each component: Gd 3.0-6.0%, Si1.0-3.0%, Al 1.0-3.0%, B 3.0-6.0%, Re 0.05-0.09%, Tb0.01-0.03 %, Co1.0-3.0%, and the rest is Fe for batching. The purity of raw materials Si, Al, B, Re, Tb, Co, and Fe are all greater than 99.9%. Gd is added in the form of iron-gadolinium master alloy. The weight percentage of Gd is 35%;
（2）将原料放入真空感应炉中熔炼，熔炼温度为1570-1590℃，浇注冷却后得到母合金， (2) Put the raw materials into a vacuum induction furnace for melting, the melting temperature is 1570-1590°C, pour and cool to obtain the master alloy,
（3）然后将母合金放入重熔管式坩埚中进行重熔，重熔温度为1550-1570℃，所述重熔管式坩埚置于真空感应成型炉内，重熔管式坩埚的顶部置于真空感应成型炉转轮轮缘之下2-4mm处，重熔管式坩埚内放置一个可上下移动的耐火柱塞，该耐火柱塞和管式坩埚内部的间隙为0.5-0.9mm，母合金置于管式坩埚内的耐火柱塞顶面熔化，合金熔融膨胀溢出后与旋转的转轮边缘接触，熔融金属熔潭被旋转的转轮边上的圆弧形轮缘拖拽形成合金带，（上下移动的一个耐火柱塞上行时将熔融合金液不断提供给旋转的转轮形成连续的合金带；） (3) Then put the master alloy into a remelting tubular crucible for remelting, the remelting temperature is 1550-1570°C, the remelting tubular crucible is placed in a vacuum induction forming furnace, and the top of the remelting tubular crucible Placed 2-4mm below the rim of the vacuum induction forming furnace runner, a refractory plunger that can move up and down is placed in the remelting tubular crucible, and the gap between the refractory plunger and the interior of the tubular crucible is 0.5-0.9mm. The master alloy is placed on the top surface of the refractory plunger in the tubular crucible and melted. After the alloy melts and expands and overflows, it contacts the edge of the rotating runner. The molten metal pool is dragged by the arc-shaped rim on the side of the rotating runner to form an alloy. Belt, (a refractory plunger that moves up and down continuously provides molten alloy liquid to the rotating runner to form a continuous alloy belt;)
（4）然后将合金带置于200-300℃，保温2-4小时得到高耐脆性铁基复相磁性合金。 (4) Then place the alloy strip at 200-300°C and keep it warm for 2-4 hours to obtain a high-brittleness-resistant iron-based multiphase magnetic alloy.
步骤4）中真空感应成型炉转轮轮缘的旋转线速度为26～28m/s，所得合金带的厚度为100-300μm，宽度为3-5 mm。 In step 4), the rotational speed of the rim of the vacuum induction forming furnace runner is 26-28 m/s, and the obtained alloy strip has a thickness of 100-300 μm and a width of 3-5 mm.
本发明相比现有技术具有如下有益效果：Compared with the prior art, the present invention has the following beneficial effects:
本发明合金材料采用的Tb、 Si、B、Gd都可提高非晶形成能力。成份中的Tb、 Si、B、Gd共同存在可使团簇中原子间相互作用强, 则原子扩散便困难，因此提高材料非晶形成能力。 The Tb, Si, B, and Gd used in the alloy material of the present invention can all improve the amorphous forming ability. The co-existence of Tb, Si, B, and Gd in the composition can make the interaction between atoms in the cluster strong, and the diffusion of atoms will be difficult, thus improving the ability of the material to form amorphous.
合金材料中的Al和 Co为纳米晶形核提供位置。Al和 Co共同作用，能保证纳米晶的形成。 Al and Co in alloy materials provide sites for nanocrystalline nucleation. Al and Co work together to ensure the formation of nanocrystals.
合金材料中的Re、B 可阻碍晶粒长大。Re、Tb、 Si、B结合可有效控制纳米晶的形成及长大。 Re and B in alloy materials can hinder grain growth. The combination of Re, Tb, Si, and B can effectively control the formation and growth of nanocrystals.
合金材料中的Re、 Al、Gd、Tb配合可改善晶界结构，化解局部应力，因此可有效降低材料的脆性。 The combination of Re, Al, Gd, and Tb in the alloy material can improve the grain boundary structure and resolve local stress, so it can effectively reduce the brittleness of the material.
合金材料中的Co 提高高温磁性能, 非晶的居里温度随着 Co含量的增加而增大, 高温磁导率也随 Co含量增加而增大,这是因为随 Co含量增大, 纳米晶体积分数增大,晶粒间磁耦合加强。Al有助于提高软磁性能。Al和Co结合强化了铁磁性作用，有效提高了材料的磁通量和降低了材料的铁损。 Co in the alloy material improves the high-temperature magnetic properties, the Curie temperature of the amorphous increases with the increase of the Co content, and the high-temperature magnetic permeability also increases with the increase of the Co content, because as the Co content increases, the nanocrystals As the integral number increases, the magnetic coupling between grains strengthens. Al contributes to the improvement of soft magnetic properties. The combination of Al and Co strengthens the ferromagnetic effect, effectively increases the magnetic flux of the material and reduces the iron loss of the material.
本发明合金在凝固中，采用快速冷却和合金化结合，可以有效减小合金中的相尺寸，保证化学成分的均匀分布，既保证了合金的磁性能，也保证了合金的力学性能。热处理可降低快速冷却造成的内应力，改善合金的韧性。 During the solidification of the alloy, the combination of rapid cooling and alloying can effectively reduce the phase size in the alloy, ensure uniform distribution of chemical components, and ensure both the magnetic properties of the alloy and the mechanical properties of the alloy. Heat treatment can reduce the internal stress caused by rapid cooling and improve the toughness of the alloy.
本发明制备中，没有大量使用稀贵元素，所取原料成本降低；另外合金经过快速冷却，保证了合金成分、组织和性能的均匀性，因此也就保证了合金的质量。该合金制备工艺简便，过程简单，生产的合金具有良好的性能，非常便于工业化生产。本发明的合金性能见表1。 In the preparation of the present invention, a large amount of rare and precious elements is not used, and the cost of the raw materials is reduced; in addition, the alloy is rapidly cooled to ensure the uniformity of the alloy composition, structure and performance, thereby ensuring the quality of the alloy. The preparation process of the alloy is simple and simple, the produced alloy has good properties, and is very convenient for industrialized production. The properties of the alloy of the present invention are shown in Table 1.
附图说明 Description of drawings
图1为本发明实施例1得到的材料的金相组织图。 Fig. 1 is a metallographic structure diagram of the material obtained in Example 1 of the present invention.
由图1中可以看出，本发明的铁基复相磁性合金的组织致密均匀。该纳米晶粒所占的体积份额为30%。 It can be seen from FIG. 1 that the structure of the iron-based multi-phase magnetic alloy of the present invention is dense and uniform. The volume share of the nanocrystals is 30%.
具体实施方式 Detailed ways
实施例一：Embodiment one:
本发明铁基复相磁性合金材料的制备方法，具体步骤如下： The preparation method of the iron-based multiphase magnetic alloy material of the present invention, the specific steps are as follows:
（1）首先按照各成分的重量百分含量为： Gd 3.0％，Si 1.0％，Al 1.0％ ，B 3.0％，Re 0.05％，Tb 0.01％，Co 1.0％，其余为Fe进行配料，原料Si、Al、B、Re 、Tb、Co、Fe的纯度均大于99.9％，Gd以铁钆中间合金的方式加入，铁钆合金中Gd的重量百分比为35%； (1) First, according to the weight percentage of each component: Gd 3.0%, Si 1.0%, Al 1.0%, B 3.0%, Re 0.05%, Tb 0.01%, Co 1.0%, the rest is Fe for batching, raw material Si , Al, B, Re, Tb, Co, Fe have a purity greater than 99.9%, Gd is added in the form of an iron-gadolinium master alloy, and the weight percentage of Gd in the iron-gadolinium alloy is 35%;
（2）将原料放入真空感应炉中熔炼，熔炼温度为1580℃，浇注冷却后得到母合金， (2) Put the raw materials into a vacuum induction furnace for melting, the melting temperature is 1580°C, pour and cool to obtain the master alloy,
（3）然后将母合金放入重熔管式坩埚中进行重熔，重熔温度为1560℃，所述重熔管式坩埚置于真空感应成型炉内，重熔管式坩埚的顶部置于真空感应成型炉转轮轮缘之下3mm处，重熔管式坩埚内放置一个可上下移动的耐火柱塞，该耐火柱塞和管式坩埚内部的间隙为0.6mm，母合金置于管式坩埚内的耐火柱塞顶面熔化，合金熔融膨胀溢出后与旋转的转轮边缘接触，熔融金属熔潭被旋转的转轮边上的圆弧形轮缘拖拽形成合金带，上下移动的一个耐火柱塞上行时将熔融合金液不断提供给旋转的转轮形成连续的合金带。真空感应成型炉转轮轮缘的旋转线速度为27m/s，所得合金带的厚度为150-250μm，宽度为3-5mm。 (3) Then put the master alloy into a remelting tubular crucible for remelting, the remelting temperature is 1560°C, the remelting tubular crucible is placed in a vacuum induction forming furnace, and the top of the remelting tubular crucible is placed At 3mm below the rim of the vacuum induction forming furnace runner, a refractory plunger that can move up and down is placed in the remelting tubular crucible. The gap between the refractory plunger and the interior of the tubular crucible is 0.6mm. The top surface of the refractory plunger in the crucible melts, and the alloy melts and expands and overflows to contact the edge of the rotating runner. The molten metal pool is dragged by the arc-shaped rim on the side of the rotating runner to form an alloy belt, which moves up and down. When the refractory plunger goes up, the molten alloy liquid is continuously supplied to the rotating runner to form a continuous alloy belt. The rotational speed of the rim of the vacuum induction forming furnace runner is 27m/s, and the obtained alloy strip has a thickness of 150-250μm and a width of 3-5mm.
（4）然后将合金带置于250℃，保温3小时得到高耐脆性铁基复相磁性合金材料。该合金材料中纳米晶粒所占的体积份额为30%。 (4) Then place the alloy strip at 250°C and keep it warm for 3 hours to obtain a high-brittleness-resistant iron-based multiphase magnetic alloy material. The volume share of nano crystal grains in the alloy material is 30%.
实施例二：Embodiment two:
铁基复相磁性合金材料中各成分的重量百分含量为： Gd 6.0％，Si 3.0％，Al 3.0％ ，B 6.0％，Re 0.09％，Tb0.03％，Co 3.0％，其余为Fe。其制备过程同实施例一。所得合金材料中纳米晶粒所占的体积份额为40%。 The weight percentage of each component in the iron-based multiphase magnetic alloy material is: Gd 6.0%, Si 3.0%, Al 3.0%, B 6.0%, Re 0.09%, Tb0.03%, Co 3.0%, and the rest is Fe. Its preparation process is with embodiment one. The volume share of nano crystal grains in the obtained alloy material is 40%.
实施例三：Embodiment three:
铁基复相磁性合金材料中各成分的重量百分含量为：Gd 5.0％，Si 2.0％，Al 2.0％ ，B 4.0％，Re 0.07％，Tb 0.02％，Co 2.0％，其余为Fe。其制备过程同实施例一。所得合金材料中纳米晶粒所占的体积份额为35%。 The weight percentage of each component in the iron-based multiphase magnetic alloy material is: Gd 5.0%, Si 2.0%, Al 2.0%, B 4.0%, Re 0.07%, Tb 0.02%, Co 2.0%, and the rest is Fe. Its preparation process is with embodiment one. The volume share of nano crystal grains in the obtained alloy material is 35%.
实施例四：（成分配比不在本发明设计比例范围内）Embodiment four: (ingredient distribution ratio is not within the design ratio range of the present invention)
铁基复相磁性合金材料中各成分的重量百分含量为： Gd 2.0％，Si0.5％，Al0.5％ ，B 2.0％，Re 0.03％， Tb0.005％，Co0.5％，其余为Fe。其制备过程同实施例一。所得合金材料中纳米晶粒所占的体积份额为25%。 The weight percentage of each component in the iron-based multiphase magnetic alloy material is: Gd 2.0%, Si0.5%, Al0.5%, B 2.0%, Re 0.03%, Tb0.005%, Co0.5%, the rest For Fe. Its preparation process is with embodiment one. The volume share of nano crystal grains in the obtained alloy material is 25%.
实施例五：（成分配比不在本发明设计比例范围内）Embodiment five: (ingredient distribution ratio is not within the scope of the design ratio of the present invention)
铁基复相磁性合金材料中各成分的重量百分含量为： Gd 7.0％，Si4.0％，Al 4.0％ ，B 7.0％，Re 0.1％， Tb 0.04％，Co4.0％，其余为Fe。其制备过程同实施例一。所得合金材料中纳米晶粒所占的体积份额为50%。 The weight percentage of each component in the iron-based multiphase magnetic alloy material is: Gd 7.0%, Si4.0%, Al 4.0%, B 7.0%, Re 0.1%, Tb 0.04%, Co4.0%, and the rest is Fe . Its preparation process is with embodiment one. The volume share of nano crystal grains in the obtained alloy material is 50%.
实施例一至五制得的合金材料分别对应下表中的合金材料一至五，具体性能见下表表1。下表中的最大磁通密度，为磁场80A/m交流磁场的场合在ΔTA≥80℃、ΔTB≥60℃的宽幅的退火温度范围下得到。 The alloy materials prepared in Examples 1 to 5 respectively correspond to the alloy materials 1 to 5 in the table below, and the specific properties are shown in Table 1 below. The maximum magnetic flux density in the table below is obtained under a wide annealing temperature range of ΔT A ≥ 80°C and ΔT B ≥ 60°C when the magnetic field is 80A/m AC magnetic field.
表1 Table 1
由上表可以看出，本发明的材料中添加Fe 、Ni、Ho 、V 、Ru、Al、P、Gd元素，有助于合金材料软磁性能的提高。但是含量超出本申请限定的范围，软磁性能非但不提高，反而会降低。原因是Gd、Al 、Ho、V过多，会和Co反应形成非磁性化合物，从而降低了Co的有效作用。 Fe 、Ni、Ru 元素过多，不再起作用，反而浪费原材料，也降低了Co的有效作用。 It can be seen from the above table that the addition of Fe, Ni, Ho, V, Ru, Al, P, and Gd elements in the material of the present invention contributes to the improvement of the soft magnetic properties of the alloy material. However, if the content exceeds the range defined in the present application, the soft magnetic properties will not be improved, but will be reduced. The reason is that too much Gd, Al, Ho, and V will react with Co to form a non-magnetic compound, thereby reducing the effective effect of Co. Too many Fe, Ni, and Ru elements will no longer work, but waste raw materials and reduce the effective effect of Co.
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