CN103996476B - A method for preparing rare earth permanent magnet alloy ribbon of quenched - Google Patents

A method for preparing rare earth permanent magnet alloy ribbon of quenched Download PDF

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CN103996476B
CN103996476B CN201410212022.4A CN201410212022A CN103996476B CN 103996476 B CN103996476 B CN 103996476B CN 201410212022 A CN201410212022 A CN 201410212022A CN 103996476 B CN103996476 B CN 103996476B
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alloy
permanent magnet
quenched
rare earth
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CN103996476A (en
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谭晓华
徐晖
黄正
梁永
产斯飞
李维丹
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上海大学
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Abstract

本发明涉及一种重复性好、磁性能优异的稀土永磁合金条带的制备方法,其特点在于同时控制快淬过程中的熔体温度和腔室压力。 The present invention relates to a reproducible process for preparing rare earth permanent magnet having excellent magnetic alloy strip, characterized in that while controlling the melt temperature and chamber pressure during rapid quenching. 制备过程和步骤如下:(1)按Nd 21.91%,Fe 67.88%,Co 4.71%,Zr 4.38%,B 1.12%(质量百分含量)合金组成配方进行配料;然后用真空非自耗电弧炉在氩气保护下进行熔炼,熔炼电流密度为100~220 A/cm2,将合金反复熔炼3~5次,制得母合金;(2) 采用真空快淬炉制备合金薄带,腔室在抽真空后充入氩气或者氦气作为保护气氛,压力为0.01~0.08 MPa;根据腔室压力的不同,调节快淬时的熔体温度,调整范围在Tm~Tm+200 ℃,采用合适的快淬速度15 m/s甩带,最终制得永磁合金条带。 And preparation steps are as follows: (1) by Nd 21.91%, Fe 67.88%, Co 4.71%, Zr 4.38%, B 1.12% (mass percentage) alloy recipe ingredients; then dried in vacuo non-consumable arc furnace carried out under argon smelting, smelting current density of 100 ~ 220 A / cm2, the alloy is repeatedly melted 3 to 5 times, to obtain master alloy; (2) vacuum preparation alloy ribbon quenched furnace chamber evacuated vacuum filling with argon or helium gas as a protective atmosphere, the pressure is 0.01 ~ 0.08 MPa; depending on the chamber pressure, regulating the melt temperature during rapid quenching, the adjustment range in Tm ~ Tm + 200 ℃, using a suitable fast wheel speed 15 m / s the melt spinning, the finally obtained permanent magnet alloy ribbon. 本发明可通过直接快淬得到可重复性好,稳定性好的批量条带样品,简化了工艺,降低了生产成本。 The present invention may be obtained by direct good repeatability quenched, tape sample batch and good stability, simplifying the process and reducing production costs.

Description

一种稀土永磁合金快淬条带的制备方法 A method for preparing rare earth permanent magnet alloy ribbon of quenched

技术领域 FIELD

[0001] 本发明涉及一种重复性好、磁性能优异的稀土永磁合金快淬条带的制备方法,属磁性合金材料及加工工艺技术领域。 [0001] The present invention relates to one kind of good reproducibility, an excellent method for preparing rare earth permanent magnetic alloy strip is quenched, the magnetic alloy material and metal processing art.

背景技术 Background technique

[0002] 熔体快淬法是目前制备稀土永磁材料条带样品最常用的方法,其操作简单,便于工业化生产。 [0002] The melt-spinning method is the most commonly used method for preparing a rare earth permanent magnet material sample strip, its operation is simple, convenient for industrial production. 熔体快淬法又可分为两种:非晶晶化法和直接快淬法。 Melt-quenching method can be divided into two types: amorphous bulk quick quenching method and the direct method. 前者是用快淬法先制备出具有非晶结构的薄带,然后通过后续的退火处理得到永磁合金。 The former method is first prepared by rapid quenching a ribbon having an amorphous structure, and permanent magnet alloy obtained by subsequent annealing. 但是这种方法制得的合金的磁性能与快淬条带的淬态结构有着密切的关系,而且在退火过程中容易造成磁性相的晶粒长大,使材料的磁性能降低。 But the structure of the magnetic quenched alloy prepared in this way with the band rapidly quenched strip is closely related to, and during annealing is likely to cause magnetic phase grains grow, the magnetic material can be reduced.

[0003] 直接快淬法是用快淬法直接制备出具有良好磁性能的薄带样品,其综合磁性能甚至优于用非晶晶化法制备的合金。 [0003] directly prepared by rapid quenching method is a method of directly quenched ribbon sample having good magnetic properties, the comprehensive magnetic amorphous bulk alloy was prepared even better. 另外,这种方法相比于非晶晶化法不但会降低成本,而且操作简单,便于工业生产。 Further, this method as compared to amorphous bulk methods not only reduce cost, but also easy to operate, easy to industrial production. 但是这种方法制备得到的条带样品的稳定性比较差。 However, the relatively poor stability of the tape sample strip prepared in this method. 也就是说,用直接快淬法制备出来的条带样品存在着磁性能不均匀的现象。 That is, the article prepared by rapid quenching method directly out of the magnetic tape samples there is the phenomenon of uneven. 这主要是因为直接快淬法在制备样品的过程中,部分工艺参数的影响没有被重视,如熔体温度和腔室压力等。 This is mainly because of the direct rapid quenching method during the preparation of the sample, the influence of process parameters is not part of attention, such as melt temperature and chamber pressure. 而这些参数对于制备的条带样品的微观结构和磁性能有着重要的影响。 The microstructure and magnetic parameters for these tape samples prepared strips can have a significant impact.

[0004] 本发明专利就是同时调节熔体温度和腔室压力,制备可重复性好、磁性能优异的条带样品。 [0004] The present invention patent is simultaneously adjusted melt temperature and chamber pressure to prepare a good repeatability, an excellent magnetic tape sample. 这无论是从理论还是应用的角度上都具有重要的意义。 This matter is of great significance from both the theory and application point of view.

发明内容 SUMMARY

[0005] 本发明的目的是提供一种重复性好、磁性能优异的稀土永磁合金快淬条带的制备方法。 [0005] The object of the present invention is to provide a good repeatability, the strip preparing rare earth permanent magnet having superior magnetic alloy rapid quenching.

[0006] 本发明的目的是通过同时控制快淬过程中的熔体温度和腔室压力来实现制备快淬条带。 [0006] The object of the present invention is achieved by simultaneously controlling the strip prepared quenched melt temperature and chamber pressure during rapid quenching.

[0007] 本发明成分及其质量百分含量:在稀土永磁合金通式Re-Fe (Co) _M_B中,Re为Nd,M为Zr;即: [0007] The present invention and its components mass percentage: In the rare earth permanent magnet alloy of the general formula Re-Fe (Co) _M_B in, Re is Nd, M is Zr; namely:

[0008] Nd 21.91%,Fe 67.88%,Co 4.71%,Zr 4.38%,B 1.12%。 [0008] Nd 21.91%, Fe 67.88%, Co 4.71%, Zr 4.38%, B 1.12%.

[0009] 本发明一种稀土永磁合金快淬条带的制备方法,其特征在于具有以下的过程和步骤: [0009] The method for producing a rare earth permanent magnet alloy according to the present invention, quenched strip, characterized by the following steps and procedures:

[0010] a)将工业纯金属原料,以既定的质量百分含量计配制;按上述配方配料,然后用真空非自耗电弧炉在氩气保护下进行熔炼,熔炼电流密度为100〜220 A/cm2,将合金反复熔炼3〜5次,制得母合金; [0010] a) industrial pure metal material, at a predetermined weight percentage content of the formulation; formulation according to the above ingredients, then the non-consumable arc vacuum smelting under argon protection, a current density of 100~220 melting A / cm2, the melted alloy is repeated three to five times to prepare a mother alloy;

[0011] b)采用真空快淬炉制备合金薄带,腔室在抽真空后充入氩气或者氦气作为保护气氛,压力为0.01〜0.08 MPa;根据腔室压力的不同,调节快淬时的熔体温度,调整范围在Tm〜Tm+200 °C (Tm为熔化温度,为1174°C);铜辊线速度,即快淬甩带速度为5〜45 m/s;最终制得永磁合金快淬条带。 Depending on when the chamber pressure is adjusted quenched; [0011] b) Preparation vacuum oven quenched alloy ribbon, the chamber evacuated and filled with argon gas or helium gas as a protective atmosphere, the pressure is 0.01~0.08 MPa melt temperature adjustment range Tm~Tm + 200 ° C (Tm is the melting temperature of 1174 ° C); copper roll line speed, i.e., spun melt spinning speed of 5~45 m / s; finally obtained permanent quenched magnet alloy ribbon.

[0012] 本发明可提供可重复性好,稳定性好的批量条带样品,扩大了熔体快淬法的应用领域。 [0012] The present invention can provide good repeatability, a good stability of bulk samples strips, expanded applications of melt-quenching method. 图1为本发明应用于Nd9.5Fe76C05Zr3B6.5合金体系得到的不同条带样品的磁滞回线,可以看出,条带样品磁性能优异,且可重复性好,说明该法是确实可行的。 Figure 1 is a hysteresis loop with different sample strip applied Nd9.5Fe76C05Zr3B6.5 obtained alloy system of the present invention, it can be seen, magnetic tape sample is excellent, and good repeatability, indicating that the method is practicable .

[0013] 本发明的特点是:I)工艺简单易行,便于批量生产,降低成本;2)可重复性好、磁性能优异。 [0013] The features of the present invention are: I) the process is simple, easy to mass production, reduce cost; 2) good repeatability, excellent magnetic properties.

附图说明 BRIEF DESCRIPTION

[0014]图1为本方法制备的具有优异矫顽力的快淬条带在室温下的磁滞回线图。 FIG quenched hysteresis loop strip having an excellent coercive force produced [0014] FIG. 1 with the present method at room temperature.

具体实施方式 Detailed ways

[0015] 现将本发明的实施例具体叙述于后。 [0015] Embodiments of the invention will now be specifically described in the following.

[0016] 实施例1 [0016] Example 1

[0017] 本实施例的永磁合金的成分(质量百分含量)为:Nd 21.91%,Fe 67.88%, Co4.71%,Zr 4.38%,B 1.12%0 Component (mass percentage) of the permanent magnet alloy according to an embodiment [0017] according to: Nd 21.91%, Fe 67.88%, Co4.71%, Zr 4.38%, B 1.12% 0

[0018] a)将工业纯金属原料Nd、Fe、Co、Zr以及FeB合金,以质量百分含量计为:Nd21.91%,Fe 67.88%,Co 4.71%,Zr 4.38%,B 1.12%进行配料,然后用真空非自耗电弧炉在氩气保护下进行熔炼,熔炼电流密度为100〜220 A/cm2,将合金反复熔炼3〜5次,制得母合金; [0018] a) pure metal industrial raw materials Nd, Fe, Co, Zr and FeB alloys, in terms of mass percentage: Nd21.91%, Fe 67.88%, Co 4.71%, Zr 4.38%, B 1.12% for ingredients, and then carried out in vacuo in the non-consumable arc melting under an argon atmosphere, melting current density of 100~220 A / cm2, the melted alloy is repeated three to five times to prepare a mother alloy;

[0019] b)对铸锭进行DSC (高温差示扫描量热仪)测试,找到合金的熔化温度,为1174 V,确定快淬过程中的熔体温度为1276 °C;同时确保真空腔室气体为高纯氩(99.99 %),压力为0.02 MPa,铜辊线速度为15 m/s,到达所需条件后快淬,收集条带样品。 [0019] b) ingot of DSC (temperature differential scanning calorimetry) test, to find the melting temperature of the alloy, is 1174 V, to determine the temperature of the melt spun process is 1276 ° C; while ensuring that the vacuum chamber gas is high purity argon (99.99%), a pressure of 0.02 MPa, a copper roll line speed of 15 m / s, arriving quenched after the desired conditions, the sample collecting strips.

[0020] 本实施例中所制得的纳米晶复合永磁合金,在淬态时拥有较为优异的磁性能,且重复性好,饱和磁化强度Ms= 116.12 AmVkg,矫顽力jH。 [0020] The present nanocrystalline composite permanent magnetic alloys prepared in the examples, has a more excellent magnetic properties when quenched, and repeatable, the saturation magnetization Ms = 116.12 AmVkg, coercivity jH. = 712.52 kA/m,最大磁能积(BH)max=115.12 kj/m3,如图1所示。 = 712.52 kA / m, the maximum energy product (BH) max = 115.12 kj / m3, as shown in FIG.

[0021] 实施例2 [0021] Example 2

[0022] 本实施例的永磁合金的成分(质量百分含量)为:Nd 21.91%,Fe 67.88%, Co4.71%,Zr 4.38%,B 1.12%0 [0022] Component (mass percentage) permanent magnet alloy according to the present embodiment is: Nd 21.91%, Fe 67.88%, Co4.71%, Zr 4.38%, B 1.12% 0

[0023] a)将工业纯金属原料Nd、Fe、Co、Zr以及FeB合金,以质量百分含量计为:Nd21.91%,Fe 67.88%,Co 4.71%,Zr 4.38%,B 1.12%进行配料,然后用真空非自耗电弧炉在氩气保护下进行熔炼,熔炼电流密度为100〜220 A/cm2,将合金反复熔炼3〜5次,制得母合金; [0023] a) pure metal industrial raw materials Nd, Fe, Co, Zr and FeB alloys, in terms of mass percentage: Nd21.91%, Fe 67.88%, Co 4.71%, Zr 4.38%, B 1.12% for ingredients, and then carried out in vacuo in the non-consumable arc melting under an argon atmosphere, melting current density of 100~220 A / cm2, the melted alloy is repeated three to five times to prepare a mother alloy;

[0024] b)对铸锭进行DSC测试,确定合金的熔化温度为1174 V,确定快淬过程中的熔体温度为1203 °C;同时确保真空腔室气体为高纯氩(99.99 %),压力为0.02 MPa;铜辊线速度为15 m/s,到达所需条件后快淬,收集条带样品。 [0024] b) DSC measurements of the ingot, the melting temperature of the alloy is determined 1174 V, to determine the temperature of the melt spun process is 1203 ° C; vacuum chamber while ensuring high purity argon gas (99.99%), a pressure of 0.02 MPa; copper roll line speed of 15 m / s, arriving quenched after the desired conditions, the sample collecting strips.

[0025] 本实施例中所制得的纳米晶复合永磁合金,在淬态下即表现出良好的硬磁性能,且可重复性好。 [0025] In this embodiment the obtained nanocomposite permanent magnetic alloys, i.e. in the quenched exhibit good hard magnetic properties, and good repeatability.

Claims (1)

1.一种稀土永磁合金的制备方法,该稀土永磁合金的组成成分及其质量百分含量: 在稀土永磁合金通式Re-Fe (Co) -MB*,ReSNd,iC%Zr;gp: Nd 21.91%,Fe 67.88%,Co 4.71%,Zr 4.38%,B 1.12%; 其特征在于具有以下的过程和步骤: a)将工业纯金属原料,按上述配方配料,然后用真空非自耗电弧炉在氩气保护下进行熔炼,熔炼电流密度为100〜220A/cm2,将合金反复熔炼3〜5次,制得母合金; b)采用真空快淬炉制备合金薄带,腔室在抽真空后充入氩气或者氦气作为保护气氛,压力为0.0I〜0.08MPa;根据腔室压力的不同,调节快淬时的熔体温度,调整范围在Tm〜Tm+2000C,Tm为熔化温度,为1174°C ;并采用合适的快淬速度甩带,其速度为15m/s;最终制得永磁合金快淬条带。 1. A method for preparing a rare earth permanent magnet alloy, the rare earth permanent magnet alloy composition and the mass percentage: In the rare earth permanent magnet alloy of the general formula Re-Fe (Co) -MB *, ReSNd, iC% Zr; gp: Nd 21.91%, Fe 67.88%, Co 4.71%, Zr 4.38%, B 1.12%; characterized by having the following processes and steps of: a) commercially pure metal raw material, according to the above formula ingredients, and then vacuum non in consumable arc melting under an argon atmosphere, melting current density 100~220A / cm2, the melted alloy is repeated three to five times to prepare a mother alloy; b) preparing a vacuum oven quenched alloy ribbon, the chamber after evacuation and backfilled with argon or helium gas as a protective atmosphere, the pressure is 0.0I~0.08MPa; depending on the chamber pressure, regulating the melt temperature during rapid quenching, adjustment range Tm~Tm + 2000C, Tm is melting temperature of 1174 ° C; and spun using a suitable speed melt spinning, a velocity of 15m / s; finally obtained permanent quenched alloy ribbon.
CN201410212022.4A 2014-05-19 2014-05-19 A method for preparing rare earth permanent magnet alloy ribbon of quenched CN103996476B (en)

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