CN103996476B - A kind of preparation method of RE permanent magnetic alloy quick quenching band - Google Patents
A kind of preparation method of RE permanent magnetic alloy quick quenching band Download PDFInfo
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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。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。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 invention relates to a preparation method of a rare-earth permanent magnetic alloy strip with good repeatability and excellent magnetic properties, which is characterized in that the melt temperature and chamber pressure in the rapid quenching process are simultaneously controlled. The preparation process and steps are as follows: (1) According to the alloy composition formula of Nd 21.91%, Fe 67.88%, Co 4.71%, Zr 4.38%, B 1.12% (mass percentage content) for batching; then use a vacuum non-consumable electric arc furnace Melting under the protection of argon, the melting current density is 100-220 A/cm 2 , the alloy is smelted repeatedly for 3-5 times to obtain the master alloy; After evacuating, fill it with argon or helium as a protective atmosphere, the pressure is 0.01-0.08 MPa; according to the different chamber pressure, adjust the melt temperature during rapid quenching, the adjustment range is T m ~ T m +200 ℃, using The appropriate rapid quenching speed is 15 m/s to throw the strip, and finally the permanent magnetic alloy strip is obtained. The invention can obtain batch strip samples with good repeatability and good stability through direct rapid quenching, which simplifies the process and reduces the production cost.
Description
技术领域technical field
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。The invention relates to a preparation method of a rare-earth permanent magnet alloy quick-quenching strip with good repeatability and excellent magnetic properties, and belongs to the technical field of magnetic alloy materials and processing techniques.
背景技术Background technique
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。熔体快淬法又可分为两种：非晶晶化法和直接快淬法。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。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。The melt quenching method is currently the most commonly used method for preparing strip samples of rare earth permanent magnet materials. It is easy to operate and convenient for industrial production. The melt rapid quenching method can be divided into two types: the amorphous crystallization method and the direct rapid quenching method. In the former, a thin strip with an amorphous structure is first prepared by a rapid quenching method, and then a permanent magnetic alloy is obtained through subsequent annealing treatment. However, the magnetic properties of the alloy prepared by this method are closely related to the as-quenched structure of the quenched strip, and the grains of the magnetic phase tend to grow during the annealing process, which reduces the magnetic properties of the material.
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。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。但是这种方法制备得到的条带样品的稳定性比较差。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。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。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 direct rapid quenching method is to directly prepare thin strip samples with good magnetic properties by rapid quenching method, and its comprehensive magnetic properties are even better than alloys prepared by amorphous crystallization method. In addition, compared with the amorphous crystallization method, this method not only reduces the cost, but also has simple operation and is convenient for industrial production. However, the stability of the strip sample prepared by this method is relatively poor. That is to say, the strip samples prepared by the direct rapid quenching method have inhomogeneous magnetic properties. This is mainly because the influence of some process parameters, such as melt temperature and chamber pressure, has not been paid attention to during the process of sample preparation by direct rapid quenching. These parameters have important influence on the microstructure and magnetic properties of the prepared strip samples.
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。这无论是从理论还是应用的角度上都具有重要的意义。The patent of the invention is to simultaneously adjust the melt temperature and chamber pressure to prepare strip samples with good repeatability and excellent magnetic properties. This is of great significance both in terms of theory and application.
发明内容Contents of the invention
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。The purpose of the present invention is to provide a preparation method of a rare earth permanent magnet alloy quick-quenching strip with good repeatability and excellent magnetic properties.
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。The object of the present invention is to realize the preparation of quick-quenched strips by simultaneously controlling the melt temperature and chamber pressure during the quick-quenching process.
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：Components of the present invention and their mass percentages: in the rare earth permanent magnet alloy general formula Re-Fe(Co)-M-B, Re is Nd, and M is Zr; that is:
Nd 21.91%，Fe 67.88%，Co 4.71%，Zr 4.38%，B 1.12%。Nd 21.91%, Fe 67.88%, Co 4.71%, Zr 4.38%, B 1.12%.
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：A kind of preparation method of rare earth permanent magnet alloy quick-quenching strip of the present invention is characterized in that having following process and step:
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；a) Prepare industrially pure metal raw materials with a predetermined mass percentage; mix ingredients according to the above formula, and then use a vacuum non-consumable electric arc furnace to smelt under the protection of argon, and the smelting current density is 100-220 A/cm 2. The alloy is smelted repeatedly for 3 to 5 times to obtain the master alloy;
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 ℃（Tm为熔化温度，为1174℃）；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。b) The alloy thin strip is prepared by vacuum quenching furnace, and the chamber is filled with argon or helium as a protective atmosphere after vacuuming, and the pressure is 0.01-0.08 MPa; according to the difference in chamber pressure, adjust the melt during rapid quenching Temperature, the adjustment range is T m ~ T m + 200 ℃ (T m is the melting temperature, which is 1174 ℃); the line speed of the copper roll, that is, the speed of the quick quenching strip is 5 ~ 45 m/s; the final permanent magnet alloy Quenched strips.
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。图1为本发明应用于Nd9.5Fe76Co5Zr3B6.5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。The invention can provide batch strip samples with good repeatability and good stability, and expands the application field of the melt rapid quenching method. Figure 1 is the hysteresis loops of different strip samples obtained by applying the present invention to the Nd 9.5 Fe 76 Co 5 Zr 3 B 6.5 alloy system. It can be seen that the strip samples have excellent magnetic properties and good repeatability, indicating that the law is indeed feasible.
本发明的特点是：1)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。The characteristics of the present invention are: 1) the process is simple and easy, which is convenient for mass production and reduces the cost; 2) the repeatability is good and the magnetic performance is excellent.
附图说明Description of drawings
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. 1 is the hysteresis loop diagram at room temperature of the rapidly quenched strip with excellent coercive force prepared by the method.
具体实施方式detailed description
现将本发明的实施例具体叙述于后。Embodiments of the present invention will now be described in detail below.
实施例1Example 1
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%。The composition (mass percentage) of the permanent magnet alloy of this embodiment is: Nd 21.91%, Fe 67.88%, Co 4.71%, Zr 4.38%, B 1.12%.
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；a) The industrial pure metal raw materials Nd, Fe, Co, Zr and FeB alloy are calculated by mass percentage as: Nd21.91%, Fe 67.88%, Co 4.71%, Zr 4.38%, B 1.12% for batching, and then Use a vacuum non-consumable electric arc furnace to smelt under the protection of argon, with a smelting current density of 100-220 A/cm 2 , and repeatedly smelt the alloy for 3-5 times to obtain a master alloy;
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 ℃，确定快淬过程中的熔体温度为1276 ℃；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。b) Carry out DSC (high temperature differential scanning calorimeter) test on the ingot to find the melting temperature of the alloy, which is 1174 °C, and determine that the melt temperature during the rapid quenching process is 1276 °C; at the same time, ensure that the vacuum chamber gas is high-purity Argon (99.99%), the pressure is 0.02 MPa, the line speed of the copper roller is 15 m/s, after reaching the required conditions, it is rapidly quenched, and the strip samples are collected.
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 Am2/kg，矫顽力jHc= 712.52 kA/m，最大磁能积(BH)max= 115.12 kJ/m3，如图1所示。The nanocrystalline composite permanent magnet alloy prepared in this example has relatively excellent magnetic properties in the quenched state, and has good repeatability. The saturation magnetization M s = 116.12 Am 2 /kg, and the coercive force j H c = 712.52 kA/m, the maximum magnetic energy product (BH) max = 115.12 kJ/m 3 , as shown in Figure 1.
实施例2Example 2
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%。The composition (mass percentage) of the permanent magnet alloy of this embodiment is: Nd 21.91%, Fe 67.88%, Co 4.71%, Zr 4.38%, B 1.12%.
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；a) The industrial pure metal raw materials Nd, Fe, Co, Zr and FeB alloy are calculated by mass percentage as: Nd21.91%, Fe 67.88%, Co 4.71%, Zr 4.38%, B 1.12% for batching, and then Use a vacuum non-consumable electric arc furnace to smelt under the protection of argon, with a smelting current density of 100-220 A/cm 2 , and repeatedly smelt the alloy for 3-5 times to obtain a master alloy;
b)对铸锭进行DSC测试，确定合金的熔化温度为1174 ℃，确定快淬过程中的熔体温度为1203 ℃；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。b) Carry out DSC test on the ingot to confirm that the melting temperature of the alloy is 1174 °C, and determine that the melt temperature during the rapid quenching process is 1203 °C; at the same time, ensure that the gas in the vacuum chamber is high-purity argon (99.99%), and the pressure is 0.02 MPa ; The line speed of the copper roll is 15 m/s, and it is rapidly quenched after reaching the required conditions, and the strip samples are collected.
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。The nanocrystalline composite permanent magnetic alloy prepared in this embodiment exhibits good hard magnetic properties in the quenched state, and has good repeatability.
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