CN104464997B - A kind of preparation method of high coercive force NdFeB permanent magnet material - Google Patents
A kind of preparation method of high coercive force NdFeB permanent magnet material Download PDFInfo
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Abstract
Description
技术领域 technical field
本发明属于磁性功能材料领域，具体涉及一种高矫顽力钕铁硼永磁材料的制备方法。 The invention belongs to the field of magnetic functional materials, and in particular relates to a preparation method of a high-coercivity neodymium-iron-boron permanent magnet material.
背景技术 Background technique
自从1983年Sagawa等人发现钕铁硼磁体以来，其优异的磁性能创造了当时的最高纪录，从而宣告了第三代稀土永磁体的诞生，理论磁能积(BH)可达64MGOe(509kJ/m3)，实验室磁能积(BH)已达59MGOe(469kJ/m3)，工业规模可生产磁能积(BH)高达52MGOe(413kJ/m3)的磁体。然而，由于烧结NdFeB磁体的温度稳定性较差，而稳定性的提高需要磁体矫顽力的改善，因此开发具有高磁能积(BH)和高矫顽力(Hi)的烧结磁体也是NdFeB研究者的主要目标。随着应用市场的不断扩大，烧结钕铁硼的研发和产业化速度很快，这是其它永磁材料所无法比拟的。近年来对计算机、通讯器材以及汽车用电机在小型化、轻量化及节能环保等方面的要求，也必然会对磁体性能的要求越来越高。一种低成本烧结钕铁硼磁体及其制备方法，申请号：201210068196.9。该发明用低成本的稀有金属钬替代的高成本的稀有金属镝，同时不影响烧结钕铁硼磁体的磁性能，从而降低产品的生产成本。其主要技术指标达到以下参数：剩磁(Br) 1.18～1.22 mT；磁感应矫顽力(bHc)≥860 kA/m；内禀矫顽力(jHc) ≥1353 kA/m。最大磁能积(BH)max 263～295 kJ/m3。 Since Sagawa and others discovered NdFeB magnets in 1983, their excellent magnetic properties have created the highest record at that time, thus announcing the birth of the third generation of rare earth permanent magnets. The theoretical magnetic energy product (BH) can reach 64MGOe (509kJ/m 3 ), the magnetic energy product (BH) in the laboratory has reached 59MGOe (469kJ/m 3 ), and the industrial scale can produce magnets with a magnetic energy product (BH) as high as 52MGOe (413kJ/m 3 ). However, since the temperature stability of sintered NdFeB magnets is poor, and the improvement of stability requires the improvement of magnet coercivity, the development of sintered magnets with high magnetic energy product (BH) and high coercive force (Hi) is also an important issue for NdFeB researchers. main goal of . With the continuous expansion of the application market, the R&D and industrialization speed of sintered NdFeB is very fast, which is unmatched by other permanent magnet materials. In recent years, the requirements for miniaturization, light weight, energy saving and environmental protection of computers, communication equipment and motors for automobiles will inevitably lead to higher and higher requirements for the performance of magnets. A low-cost sintered NdFeB magnet and its preparation method, application number: 201210068196.9. The invention replaces the high-cost rare metal dysprosium with the low-cost rare metal holmium without affecting the magnetic properties of the sintered NdFeB magnet, thereby reducing the production cost of the product. Its main technical indicators reach the following parameters: remanence (Br) 1.18-1.22 mT; magnetic induction coercive force (bHc) ≥ 860 kA/m; intrinsic coercive force (jHc) ≥ 1353 kA/m. Maximum magnetic energy product (BH) max 263 ~ 295 kJ/m 3 .
发明内容 Contents of the invention
本发明目的在于克服现有技术中的不足，提供一种高矫顽力钕铁硼永磁材料的制备方法，该高矫顽力钕铁硼永磁材料，具有更高的矫顽力，而且有效保证了其高的磁能积，获得高矫顽力与高磁能积的均衡。 The purpose of the present invention is to overcome the deficiencies in the prior art and provide a method for preparing a high-coercivity NdFeB permanent magnet material. The high-coercivity NdFeB permanent magnet material has a higher coercivity, and It effectively guarantees its high magnetic energy product, and obtains a balance between high coercive force and high magnetic energy product.
本发明高矫顽力钕铁硼永磁材料；由以下组分及质量百分比的合金粉末：Nd 16～24%、B 0.95～1.12%、Cu 0.12～0.19%、Co 0.21～0.32%、Ga 0.05～0.13%、Nb 0.28～0.40%、Pr 2.1～3.1%、Tb 0.12～0.25%、余量为 Fe；添加纳米钯黑、纳米钛粉、纳米氮化钛粉烧结而成。 The high-coercivity NdFeB permanent magnet material of the present invention consists of alloy powder with the following components and mass percentages: Nd 16-24%, B 0.95-1.12%, Cu 0.12-0.19%, Co 0.21-0.32%, Ga 0.05 ～0.13%, Nb 0.28～0.40%, Pr 2.1～3.1%, Tb 0.12～0.25%, the balance is Fe; it is sintered by adding nano-palladium black, nano-titanium powder and nano-titanium nitride powder.
作为优化，该高矫顽力钕铁硼永磁材料，所述纳米钯黑平均粒径为10nm、纳米钛粉平均粒径为40nm、纳米氮化钛粉平均粒径为60nm。 As an optimization, the high coercive force NdFeB permanent magnet material, the average particle size of the nano-palladium black is 10nm, the average particle size of the nano-titanium powder is 40nm, and the average particle size of the nano-titanium nitride powder is 60nm.
制备该高矫顽力钕铁硼永磁材料的方法，包括以下步骤： The method for preparing the high-coercivity NdFeB permanent magnet material comprises the following steps:
（1）按照质量百分比Nd 23.6%、B 1.11%、Cu 0.19%、Co 0.32%、Ga 0.13%、Nb 0.39%、Pr 3.1%、Tb 0.25%、余量为 Fe配比原料，将该原料放入真空速凝甩带炉中，熔炼成厚度在0.15～0.25mm 之间的薄片； (1) According to the mass percentage of Nd 23.6%, B 1.11%, Cu 0.19%, Co 0.32%, Ga 0.13%, Nb 0.39%, Pr 3.1%, Tb 0.25%, and the balance is Fe. Put it into the vacuum quick-setting throwing belt furnace, and smelt it into thin slices with a thickness between 0.15 and 0.25mm;
（2）将步骤（1）中的薄片，加入氢破炉，并在550～570℃脱氢6小时制成氢爆粉；然后经过气流磨后制成平均粒度均为1～2μm 的磁粉； (2) Put the flakes in step (1) into a hydrogen blasting furnace, and dehydrogenate them at 550-570°C for 6 hours to make hydrogen blasting powder; then pass through a jet mill to make magnetic powder with an average particle size of 1-2 μm;
（3）按照质量百分比Nd 14.2%、B 0.96%、Cu 0.13%、Co 0.22%、Nb 0.30%、Pr 2.6%、余量为 Fe配比原料，将该原料放入真空速凝甩带炉中，熔炼成厚度在0.25～0.35mm 之间的薄片； (3) According to the mass percentage of Nd 14.2%, B 0.96%, Cu 0.13%, Co 0.22%, Nb 0.30%, Pr 2.6%, and the balance is Fe, the raw material is put into the vacuum quick-setting throwing belt furnace , smelted into thin slices with a thickness between 0.25 and 0.35mm;
（4）将步骤（3）中的薄片，加入氢破炉，并在580～590℃脱氢4小时制成氢爆粉；然后经过气流磨后制成平均粒度均为2.5～3.5μm 的磁粉； (4) Put the flakes in step (3) into a hydrogen blasting furnace, and dehydrogenate them at 580-590°C for 4 hours to make hydrogen blasting powder; then pass through a jet mill to make magnetic powder with an average particle size of 2.5-3.5 μm ;
（5）将步骤（2）和步骤（4）中的磁粉、纳米钯黑、纳米钛粉、纳米氮化钛粉按质量比为850:150:4:9:18加入到混合机中混合均匀，得混合粉料； (5) Add the magnetic powder, nano-palladium black, nano-titanium powder, and nano-titanium nitride powder in step (2) and step (4) into the mixer at a mass ratio of 850:150:4:9:18 and mix evenly , get mixed powder;
（6）将步骤（5）中的混合粉料在磁场压机中取向，冷等静压成型，放入高真空烧结炉内1030～1065℃烧结2小时，快冷风冷后，抽真空在1100～1140℃二次烧结2小时，经815～855℃回火处理3 h取出得到成品。 (6) Orient the mixed powder in step (5) in a magnetic field press, cold isostatic pressing, and put it into a high vacuum sintering furnace for sintering at 1030-1065°C for 2 hours. Secondary sintering at 1100-1140°C for 2 hours, and tempering at 815-855°C for 3 hours to obtain the finished product.
本发明由不同粒径的磁粉，添加多种活性纳米粉末，混合均匀通过特殊烧结工艺烧结而成，通过该工艺形成晶粒细小、晶界相均匀分布与晶粒取向完整的钕铁硼磁体，该钕铁硼磁体具有更高的矫顽力，而且有效保证了其高的磁能积，获得高矫顽力与高磁能积的均衡。 用NIM-10000型磁性能测试仪测量样品的磁性能，结果如下见表1。 The invention is composed of magnetic powders with different particle sizes, adding various active nano-powders, mixing them uniformly and sintering through a special sintering process, through which a NdFeB magnet with fine grains, uniform distribution of grain boundary phases and complete grain orientation is formed. The NdFeB magnet has a higher coercive force, and effectively ensures its high magnetic energy product, achieving a balance between high coercive force and high magnetic energy product. The magnetic properties of the samples were measured with a NIM-10000 magnetic property tester, and the results are shown in Table 1 as follows.
具体实施方式 detailed description
下面给出的实施例拟对本发明作进一步说明，但不能理解为是对本发明保护范围的限制，本领域技术人员根据本发明内容对本发明的一些非本质的改进和调整，仍属于本发明的保护范围。 The embodiment given below intends to further illustrate the present invention, but can not be interpreted as the restriction to protection scope of the present invention, those skilled in the art still belongs to the protection of the present invention to some non-essential improvements and adjustments of the present invention according to the content of the present invention scope.
实施例1：（1）按照质量百分比Nd 23.6%、B 1.11%、Cu 0.19%、Co 0.32%、Ga 0.13%、Nb 0.39%、Pr 3.1%、Tb 0.25%、余量为 Fe配比原料，将该原料放入真空速凝甩带炉中，熔炼成厚度在0.15～0.25mm 之间的薄片； Example 1: (1) According to the mass percentage of Nd 23.6%, B 1.11%, Cu 0.19%, Co 0.32%, Ga 0.13%, Nb 0.39%, Pr 3.1%, Tb 0.25%, and the balance is Fe proportioning raw materials, The raw material is put into a vacuum quick-setting throwing belt furnace, and melted into thin slices with a thickness between 0.15 and 0.25 mm;
（2）将步骤（1）中的薄片，加入氢破炉，并在560℃脱氢6小时制成氢爆粉；然后经过气流磨后制成平均粒度均为1～2μm 的磁粉； (2) Put the flakes in step (1) into a hydrogen blasting furnace, and dehydrogenate them at 560°C for 6 hours to make hydrogen blasting powder; then pass through a jet mill to make magnetic powder with an average particle size of 1-2 μm;
（3）按照质量百分比Nd 14.2%、B 0.96%、Cu 0.13%、Co 0.22%、Nb 0.30%、Pr 2.6%、余量为 Fe配比原料，将该原料放入真空速凝甩带炉中，熔炼成厚度在0.25～0.35mm 之间的薄片； (3) According to the mass percentage of Nd 14.2%, B 0.96%, Cu 0.13%, Co 0.22%, Nb 0.30%, Pr 2.6%, and the balance is Fe, the raw material is put into the vacuum quick-setting throwing belt furnace , smelted into thin slices with a thickness between 0.25 and 0.35mm;
（4）将步骤（3）中的薄片，加入氢破炉，并在585℃脱氢4小时制成氢爆粉；然后经过气流磨后制成平均粒度均为2.5～3.5μm 的磁粉； (4) Put the flakes in step (3) into a hydrogen blasting furnace, and dehydrogenate them at 585°C for 4 hours to make hydrogen blasting powder; then pass through a jet mill to make magnetic powder with an average particle size of 2.5-3.5 μm;
（5）取步骤（2）的磁粉85千克、步骤（4）中的磁粉15千克、纳米钯黑0.4千克、纳米钛粉0.9千克、纳米氮化钛粉1.8千克加入到混合机中混合均匀，使纳米粉末均匀吸附于钕铁硼磁粉主相周围，得混合粉料； (5) Take 85 kg of magnetic powder in step (2), 15 kg of magnetic powder in step (4), 0.4 kg of nano-palladium black, 0.9 kg of nano-titanium powder, and 1.8 kg of nano-titanium nitride powder into the mixer and mix evenly. The nano powder is evenly adsorbed around the main phase of the NdFeB magnetic powder to obtain a mixed powder;
（6）将步骤（5）中的混合粉料在磁场压机中取向，冷等静压成型，放入高真空烧结炉内1050℃烧结2小时，快冷风冷后，抽真空在1120℃二次烧结2小时，经845℃回火处理3 h取出得到成品。 (6) Orient the mixed powder in step (5) in a magnetic field press, cold isostatic pressing, put it into a high-vacuum sintering furnace for sintering at 1050°C for 2 hours, and after rapid cooling and air cooling, vacuumize at 1120°C Secondary sintering for 2 hours, tempering at 845°C for 3 hours, and taking out the finished product.
实施例2：（1）按照质量百分比Nd 23.8%、B 1.11%、Cu 0.19%、Co 0.31%、Ga 0.13%、Nb 0.39%、Pr 3.1%、Tb 0.25%、余量为 Fe配比原料，将该原料放入真空速凝甩带炉中，熔炼成厚度在0.15～0.25mm 之间的薄片； Example 2: (1) According to the mass percentage of Nd 23.8%, B 1.11%, Cu 0.19%, Co 0.31%, Ga 0.13%, Nb 0.39%, Pr 3.1%, Tb 0.25%, and the balance is Fe proportioning raw materials, The raw material is put into a vacuum quick-setting throwing belt furnace, and melted into thin slices with a thickness between 0.15 and 0.25 mm;
（2）将步骤（1）中的薄片，加入氢破炉，并在550℃脱氢6小时制成氢爆粉；然后经过气流磨后制成平均粒度均为1～2μm 的磁粉； (2) Put the flakes in step (1) into a hydrogen blasting furnace, and dehydrogenate them at 550°C for 6 hours to make hydrogen blasting powder; then pass through a jet mill to make magnetic powder with an average particle size of 1-2 μm;
（3）按照质量百分比Nd 14.1%、B 0.96%、Cu 0.12%、Co 0.23%、Nb 0.29%、Pr 2.6%、余量为 Fe配比原料，将该原料放入真空速凝甩带炉中，熔炼成厚度在0.25～0.35mm 之间的薄片； (3) According to the mass percentage of Nd 14.1%, B 0.96%, Cu 0.12%, Co 0.23%, Nb 0.29%, Pr 2.6%, and the balance is Fe, the raw material is put into the vacuum quick-setting throwing belt furnace , smelted into thin slices with a thickness between 0.25 and 0.35mm;
（4）将步骤（3）中的薄片，加入氢破炉，并在580℃脱氢4小时制成氢爆粉；然后经过气流磨后制成平均粒度均为2.5～3.5μm 的磁粉； (4) Put the flakes in step (3) into a hydrogen blasting furnace, and dehydrogenate them at 580°C for 4 hours to make hydrogen blasting powder; then pass through a jet mill to make magnetic powder with an average particle size of 2.5-3.5 μm;
（5）取步骤（2）的磁粉85千克、步骤（4）中的磁粉15千克、纳米钯黑0.4千克、纳米钛粉0.9千克、纳米氮化钛粉1.8千克加入到混合机中混合均匀，得混合粉料； (5) Take 85 kg of magnetic powder in step (2), 15 kg of magnetic powder in step (4), 0.4 kg of nano-palladium black, 0.9 kg of nano-titanium powder, and 1.8 kg of nano-titanium nitride powder into the mixer and mix evenly. get mixed powder;
（6）将步骤（5）中的混合粉料在磁场压机中取向，冷等静压成型，放入高真空烧结炉内1030℃烧结2小时，快冷风冷后，抽真空在1100℃二次烧结2小时，经815℃回火处理3 h取出得到成品。 (6) Orient the mixed powder in step (5) in a magnetic field press, cold isostatic pressing, put it into a high-vacuum sintering furnace for sintering at 1030°C for 2 hours, and after rapid cooling and air cooling, vacuumize at 1100°C Secondary sintering for 2 hours, tempering at 815°C for 3 hours and taking out the finished product.
实施例3：（1）按照质量百分比Nd 23.8%、B 1.05%、Cu 0.19%、Co 0.32%、Ga 0.13%、Nb 0.37%、Pr 3.1%、Tb 0.22%、余量为 Fe配比原料，将该原料放入真空速凝甩带炉中，熔炼成厚度在0.15～0.25mm 之间的薄片； Example 3: (1) According to the mass percentage of Nd 23.8%, B 1.05%, Cu 0.19%, Co 0.32%, Ga 0.13%, Nb 0.37%, Pr 3.1%, Tb 0.22%, and the balance is Fe proportioning raw materials, The raw material is put into a vacuum quick-setting throwing belt furnace, and melted into thin slices with a thickness between 0.15 and 0.25 mm;
（2）将步骤（1）中的薄片，加入氢破炉，并在570℃脱氢6小时制成氢爆粉；然后经过气流磨后制成平均粒度均为1～2μm 的磁粉； (2) Put the flakes in step (1) into a hydrogen blasting furnace, and dehydrogenate them at 570°C for 6 hours to make hydrogen blasting powder; then pass through a jet mill to make magnetic powder with an average particle size of 1-2 μm;
（3）按照质量百分比Nd 14.0%、B 0.99%、Cu 0.13%、Co 0.22%、Nb 0.28%、Pr 2.7%、余量为 Fe配比原料，将该原料放入真空速凝甩带炉中，熔炼成厚度在0.25～0.35mm 之间的薄片； (3) According to the mass percentage of Nd 14.0%, B 0.99%, Cu 0.13%, Co 0.22%, Nb 0.28%, Pr 2.7%, and the balance is Fe, the raw material is put into the vacuum quick-setting throwing belt furnace , smelted into thin slices with a thickness between 0.25 and 0.35mm;
（4）将步骤（3）中的薄片，加入氢破炉，并在590℃脱氢4小时制成氢爆粉；然后经过气流磨后制成平均粒度均为2.5～3.5μm 的磁粉； (4) Put the flakes in step (3) into a hydrogen blasting furnace, and dehydrogenate them at 590°C for 4 hours to make hydrogen blasting powder; then pass through a jet mill to make magnetic powder with an average particle size of 2.5-3.5 μm;
（5）取步骤（2）的磁粉85千克、步骤（4）中的磁粉15千克、纳米钯黑0.4千克、纳米钛粉0.9千克、纳米氮化钛粉1.8千克加入到混合机中混合均匀，得混合粉料； (5) Take 85 kg of magnetic powder in step (2), 15 kg of magnetic powder in step (4), 0.4 kg of nano-palladium black, 0.9 kg of nano-titanium powder, and 1.8 kg of nano-titanium nitride powder into the mixer and mix evenly. get mixed powder;
（6）将步骤（5）中的混合粉料在磁场压机中取向，冷等静压成型，放入高真空烧结炉内1065℃烧结2小时，快冷风冷后，抽真空在1140℃二次烧结2小时，经855℃回火处理3 h取出得到成品。 (6) Orient the mixed powder in step (5) in a magnetic field press, cold isostatic pressing, put it into a high vacuum sintering furnace for sintering at 1065°C for 2 hours, and after rapid cooling and air cooling, vacuumize at 1140°C Secondary sintering for 2 hours, tempering at 855°C for 3 hours and taking out the finished product.
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