WO2005106049A1 - Procede de revenu pour aimant permanent ndfeb fritte - Google Patents

Procede de revenu pour aimant permanent ndfeb fritte Download PDF

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Publication number
WO2005106049A1
WO2005106049A1 PCT/CN2005/000380 CN2005000380W WO2005106049A1 WO 2005106049 A1 WO2005106049 A1 WO 2005106049A1 CN 2005000380 W CN2005000380 W CN 2005000380W WO 2005106049 A1 WO2005106049 A1 WO 2005106049A1
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Prior art keywords
tempering
permanent magnet
cooling
sintered
sent
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PCT/CN2005/000380
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English (en)
French (fr)
Inventor
Min Zhang
Fengrui Zhang
Zhendong Kang
Sanwen Qi
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Shanxi Huiqiang Magnetic Material Manufacturing Co., Ltd.
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Application filed by Shanxi Huiqiang Magnetic Material Manufacturing Co., Ltd. filed Critical Shanxi Huiqiang Magnetic Material Manufacturing Co., Ltd.
Publication of WO2005106049A1 publication Critical patent/WO2005106049A1/zh
Priority to US11/298,967 priority Critical patent/US7377985B2/en

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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
    • H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
    • H01F41/0253—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
    • C21D1/18—Hardening; Quenching with or without subsequent tempering
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
    • C21D1/74—Methods of treatment in inert gas, controlled atmosphere, vacuum or pulverulent material
    • C21D1/767—Methods of treatment in inert gas, controlled atmosphere, vacuum or pulverulent material with forced gas circulation; Reheating thereof

Definitions

  • the invention relates to a tempering method of a sintered NdFeB permanent magnet material.
  • NdFeB permanent magnet materials are called "Magnetic King” because of their high magnetic energy product and high coercive force. They have been widely used in many fields such as electronics, computer, automobile, machinery, energy, medical equipment and so on. According to statistics, the global production of Nd-Fe-B series permanent magnetic materials in 1997 was about 10450 tons, of which sintered Nd-Fe-B series magnets: 8,550 tons, bonded Nd-Fe-B series magnets 1900 tons, sintered Nd-Fe — B series permanent magnet materials occupy an important position.
  • the tempering process of sintered NdFeB permanent magnets includes: performing a primary or secondary tempering treatment on the sintered permanent magnet material, that is, heating the sintered and cooled permanent magnet blank in a vacuum furnace to a tempering temperature for holding, and then Filled with inert gas to quench the first-level tempering treatment; or sintered and cooled permanent magnet blanks are first heated to the first-stage tempering temperature in a vacuum furnace, then filled with inert gas to quench and cool, and then heated to
  • the secondary tempering temperature is a secondary tempering treatment in which an inert gas is quenched after the temperature is maintained. Tempering treatment can significantly improve the magnetic properties of NdFeB permanent magnets, especially the coercive force.
  • the purpose of the present invention is to overcome the shortcomings of the prior art and provide a tempering process for sintered NdFeB permanent magnets. By improving the cooling rate after tempering, the microstructure of NdFeB magnets is optimized. Improve the coercive force and consistency of magnets.
  • a kind of tempering process for sintered neodymium iron boron permanent magnets including: sintering the neodymium iron boron permanent magnet blanks with secondary tempering treatment, that is, heating the sintered and cooled permanent magnet blanks in a vacuum furnace heating chamber to the first temperature.
  • the first-level tempering temperature After the end of the heat preservation, the billet is sent to the vacuum furnace cooling chamber to be filled with inert gas quenching, and then the billet is sent to the heating chamber to rise to the second-level tempering temperature.
  • the cooling chamber is subjected to gas quenching cooling, and is characterized in that: after the tempering and heat preservation is completed, the permanent magnet blank is quickly sent to the cooling chamber and immersed in a container containing a liquid substance at normal temperature in the chamber, and the vacuum furnace is charged with The inert gas is increased by 1.8 to 3.5 times the volume of nitrogen or argon as a cooling exchange carrier gas, and then the air-cooled motor is quickly started to perform rapid cooling.
  • the first-stage tempering temperature of the secondary tempering process is 900 ⁇ 93 (TC, holding time is 2 ⁇ 3h, the second-stage tempering temperature is 500 ⁇ 630 ° C, and the holding time is 2 ⁇ 4. 5h.
  • the cooling rate is increased to 80 ⁇ 120 ° C / min.
  • the cooling rate is increased during tempering, so that the magnet is cooled down in a very short time, and the grain boundary structure of the magnet is optimized to achieve a more ideal state. Improved intrinsic coercivity and consistency. This is because when the sintered neodymium-iron-boron magnet is cooled, a non-equilibrium eutectic reaction occurs on the surface of the main phase (Nd 2 Fe 14 B) grains.
  • the content of carbon (C) is higher than that of the main phase, and the interface between the Nd-rich phase layer and the epitaxial layer in the central boundary region is neither straight nor clear.
  • the anisotropic field of the epitaxial layer is lower, the scattered magnetic field at the interface is higher, and it is easier to form demagnetized domain nuclei, so the intrinsic coercivity of the magnet after sintering is lower.
  • the primary-phase grain epitaxial layer must be hardened by primary or secondary tempering. During the primary and secondary tempering, the Nd, 0 and C atoms in the main 3 ⁇ 4 grain epitaxial layer diffuse into the Nd-rich phase region, while the iron (Fe) and boron (B) atoms in the Nd-rich phase region diffuse to the main phase.
  • the cooling method used in the present invention increases the cooling rate, makes the grain boundary components solidify in a very short time, improves the grain boundary morphology, and optimizes the boundary composition, thereby ensuring the straightness and smoothness of the interface. It is smooth, reduces the scattered magnetic field, and fully improves the intrinsic coercive force and its consistency.
  • the billet is still sent to the cooling chamber for gas quenching and cooling; the other half of the billet is cooled according to the process of the present invention, that is, the sintered and cooled permanent magnet billet is placed in a vacuum.
  • the furnace heating chamber heats up to the same tempering temperature and keeps it for the same time.
  • the tempering and heat preservation is completed, it is quickly sent to the cooling chamber and immersed in the container containing the liquid substances at room temperature.
  • the vacuum furnace is filled with an inert gas such as argon.
  • the volume of the filled gas is increased to 1. 8 ⁇ 3. 5 times compared to the prior art, and then the air-cooled motor is quickly started for fast cool down.
  • the first-stage tempering temperature of the secondary tempering treatment is 900 ° C
  • the holding time is 2h
  • the second-stage tempering temperature is .500 ° C
  • the holding time is 2h.
  • the rapid cooling rate is increased to 80 ° C / min.
  • stage tempering treatment that is, the sintered and cooled permanent magnet blank is first heated to the first stage tempering temperature in the vacuum furnace heating chamber. After the heat preservation is completed, the blank is sent to the vacuum furnace cooling chamber and filled with inert gas to quench and cool. The billet is then sent to the heating chamber to be heated to the second-stage tempering temperature.
  • the billet is still sent to the cooling chamber for gas quenching and cooling; the other half of the billet is cooled according to the process of the present invention, that is, the sintered and cooled permanent magnet billet , Heating in the vacuum furnace heating chamber to the same tempering temperature for the same time, after the tempering and heat preservation, it is quickly sent to the cooling chamber immersion chamber Inside the container containing liquid materials at room temperature, an inert gas such as argon is filled into the vacuum furnace as a cooling exchange carrier gas. The volume of the filled gas is increased by 1.8 to 3.5 times compared with the prior art. Cold motor for rapid cooling.
  • the first tempering temperature is 93CTC
  • the holding time is 3 hours
  • the second tempering temperature is 630 ° C
  • the holding time is 4.5h.
  • the cooling rate is increased to 120 ° C / minute.
  • Example 1 and Example 2 are respectively compared with the products of low coercivity and high coercivity according to the prior art and the present invention.
  • Example 1 The test data of Example 1 are listed in Tables 1 and 2.
  • the test data of Example 2 are listed in Tables 3 and 4.
  • Table 1 Testing results of the magnetic properties after tempering of the existing cooling technology.
  • Example 1 after increasing the tempering cooling rate, the intrinsic coercive force increased by an average of 1.336KOe, and the range value was reduced from 0. 403K0e to 0. 19 ⁇ 0 ⁇
  • Example 2 It can be seen from Example 2 that after raising the tempering cooling speed, the intrinsic coercive force increased by 1.790K0e on average, and the range value was reduced from 0.520K0e to 0.210K0e.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Power Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Powder Metallurgy (AREA)
  • Hard Magnetic Materials (AREA)
  • Manufacturing Cores, Coils, And Magnets (AREA)

Description

烧结钕铁硼永磁体的回火工艺
技术领域：
本发明涉及烧结钕铁硼永磁材料的回火方法。
背景技术：
钕铁硼永磁材料由于其高磁能积、 高矫顽力而被称为 "磁王"， 已广 泛用于电子、计算机、汽车、机械、能源、医疗器械等众多领域。据统计， 全球 1997年生产 Nd-Fe-B系永磁材料约 10450吨，其中烧结 Nd- Fe— B系磁 ：体 8550吨， 粘结 Nd-Fe-B系磁体 1900吨， 烧结 Nd- Fe— B系永磁材料占有 重要的地位。 周寿增著"超强永磁体"（冶金工业出版社 2004)—书中介 绍， 烧结 Nd-Fe-B系永磁材料的制造工艺流程如下： 原材料准备一冶炼一 铸锭一破碎制粉一磁场取向、压型一烧结一回火一机加工、表面处理一检 测。烧结 Nd- Fe-B系永磁合金的磁性能对工艺因素十分敏感， 相同成分的 合金由于烧结和回火工艺不同， 其磁性能可以几倍， 几十倍， 甚至几百倍 的变化。掌握烧结、回火工艺对磁性能的影响规律是十分重要的。烧结钕 铁硼永磁体的回火工艺包括:烧结后的永磁体 料进行一级或二级回火处 理， 即：将烧结冷却后的永磁体坯料在真空炉内升温至回火温度保温， 然 后充入惰性气体气淬冷却的一级回火处理；或将烧结冷却后的永磁体坯料 在真空炉内先升温至第一级回火温度保温后充入惰性气体气淬冷却，然后 再升温至第二级回火温度保温后充入惰性气体气淬冷却的二级回火处理。 回火处理可显著提高钕铁硼永磁体的磁性能， 尤其是矫顽力。 由于烧结 Nd - Fe-B系永磁合金的磁性能， 尤其是矫顽力对其显微组织、 畴结构十分 敏感， 为了获得较好的磁性能， 回火处理后应快速冷却。但是现有技术的 回火工艺， 由于冷却速度较低， 不能有效增加磁体内禀矫顽力， 并且未能 使内禀矫顽力一致性达到优异状态。
发明内容：
本发明的目的在于克服现有技术的缺点， 提供一种烧结钕铁硼永磁体 的回火工艺，通过提高回火后的冷却速度，优化钕铁硼磁体显微组织结构， 提高磁体内禀矫顽力及其一致性。
本发明解决上述技术问题所采用的技术方案为：
—种烧结钕铁硼永磁体的回火工艺， 包括： 烧结后的钕铁硼永磁体坯 料进行二级回火处理， 即：将烧结冷却后的永磁体坯料在真空炉加热室内 先升温至第一级回火温度，保温结束后将坯料送至真空炉冷却室充入惰性 气体气淬冷却，然后再将坯料送至加热室升温至第二级回火温度，保温结 束后仍将坯料送至冷却室进行气淬冷却，其特征在于：所述的永磁体坯料 在回火保温结束后， 快速送至冷却室浸入室内盛有常温液态物质的容器 内， 同时向真空炉内充入较所述惰性气体增加 1. 8〜3. 5倍体积的氮气或 氩气作为冷却交换载气， 之后迅速启动风冷电机， 进行快速冷却。
所述二级回火处理的第一级回火温度为 900〜93(TC， 保温时间为 2〜 3h, 第二级回火温度为 500〜630°C, 保温时间为 2〜4. 5h。
所述的快速冷却， 其冷却速度提高至 80〜120°C/分钟。
由于本发明的钕铁硼磁体烧结结束后， 进行回火时提高了冷却速度， 使磁体在极短的时间内冷却下来，对磁体晶粒边界组织迸行了优化，从而 达到较为理想的状态，提髙了内禀矫顽力及其一致性。这是因为烧结后的 钕铁硼磁体在进行冷却时， 富钕（Nd)相在主相（Nd2Fe14B)晶粒表面发 生非平衡共晶反应， 其钕（Nd)、氧（0)、 碳（C)的含量均比主相的高， 并且边界中央区的富 Nd相层与外延层之间的界面既不平直又不清晰。外 延层的各向异性场较低，界面处的散磁场较高， 较易形成反磁化畴核， 因 此烧结后磁体的内禀矫顽力较低。若要提高内禀矫顽力，必须通过一、二 级回火使主相晶粒外延层硬化。在迸行一、二级回火时， 主 ¾晶粒外延层 的 Nd、 0和 C原子 向富 Nd相区扩散， 而富 Nd相区的铁（Fe)、硼 (B) 原子向主相晶粒内扩散， 其结果是使 Nd2Fe14B晶粒外延层的成份和结构 向 Nd2Fe14B 相的成份和结构过渡， 界面变的平直和光滑， 使之具有 Nd2Fe14B相的各向异性与形核场， 散磁场也降低， 从而提高矫顽力。 然 而现有技术在回火冷却时冷却速度较低，其晶界成份不能保证与在保温状 态时的成份一致，从而不能充分降低散磁场，不能使内禀矫顽力得到充分 的提高。与现有技术相比， 本发明使用的冷却方式增大了冷却速度， 使晶 界成份在极短的时间内凝固下来， 改善晶界形貌，优化边界成份， 从而保 证了界面的平直和光滑，降低了散磁场，充分提高了内禀矫顽力及其一致 性。
具体的实施方式：
实施例 1
选一种合金成分相同的烧结钕铁硼磁体， 进行不同回火工艺的回火试 验， 即将一批钕铁硼磁体进行烧结、冷却结束后，其中一半坯料按现有技 术的工艺进行二级回火处理， 即：将烧结冷却后的永磁体坯料在真空炉加 热室内先升温至第一级回火温度，保温结束后将坯料送至真空炉冷却室充 入惰性气体气淬冷却， 然后再将坯料送至加热室升温至第二级回火温度， 保温结束后仍将坯料送至冷却室进行气淬冷却；另一半坯料按本发明的工 艺冷却， 即将烧结冷却后的永磁体坯料，在真空炉加热室升温至同样的回 火温度保温同样的时间，在回火保温结束后，快速送至冷却室浸入室内盛 有常温液态物质的容器内，同时向真空炉内充入氩气等惰性气体作为冷却 交换载气， 充入气体的体积与现有技术相比增加到 1. 8〜3. 5倍， 之后迅 速启动风冷电机进行快速冷却。
所述二级回火处理的第一级回火温度为 900°C , 保温时间为 2h， 第二 级回火温度为 .500°C，保温时间为 2h。所述快速冷却速度提高至 80°C/分。
实施例 2
选另一种合金成分相同的烧结钕铁硼磁体， 进行不同回火工艺的回火 试验， 即将一批钕铁硼磁体进行烧结、冷却结束后， 其中一半坯料按现有 技术的工艺迸行二级回火处理，即：将烧结冷却后的永磁体坯料在真空炉 加热室内先升温至第一级回火温度，保温结束后将坯料送至真空炉冷却室 充入惰性气体气淬冷却， 然后再将坯料送至加热室升温至第二级回火温 度，保温结束后仍将坯料送至冷却室迸行气淬冷却；另一半坯料按本发明 的工艺冷却，即将烧结冷却后的永磁体坯料，在真空炉加热室升温至同样 的回火温度保温同样的时间，在回火保温结束后，快速送至冷却室浸入室 内盛有常温液态物质的容器内，同时向真空炉内充入氩气等惰性气体作为 冷却交换载气， 充入气体的体积与现有技术相比增加到 1.8〜3.5倍， 之 后迅速启动风冷电机进行快速冷却。
所述二级回火处理的第一级回火温度为 93CTC, 保温时间为 3h， 第二 级回火温度为 630Ό, 保温时间为 4.5h。
所述快速冷却， 其冷却速度提高至 120°C/分钟。
实施例 1和实施例 2是分别针对低矫顽力和高矫顽力两种牌号的产品 按现有技术和本发明迸行比较的。
实施例 1的检测数据列于表 1和表 2， 实施例 2的检测数据列于表 3 和表 4。
表 1: 现有冷却技术回火后的磁性能检测结果 序 剩磁 内禀 磁能积 序 剩磁 内禀 磁能积 号 Br 矫顽力 (BH)max 号 Br 矫顽力 (BH)max
Hci Hci
(KGs) (KOe) (MGOe) (KGs) (KOe) (MGOe)
1 13.01 12.79 41.48 6 13.08 12.88 41.54
2 12.96 12.87 41.00 7 13.06 12.91 41.42
3 12.96 12.93 41.24 8 13.06 12.66 41.19
4 12.99 12.62 41.27 9 12.98 13.05 41.00
5 13.00 13.02 41.42 10 12.99 12.95 41.08 表 2 ： 提高冷速回火后的磁性能检测结果
序 剩磁 内禀 磁能积 序 剩磁 内禀 磁能积 号 Br 矫顽力 (BH)raax 号 Br 矫顽力 (BH) max
Hci Hci
(KGs) (KOe) (MGOe) (KGs) (KOe) (MGOe)
1 12.99 14.14 41.02 6 13.09 14.20 41.52
2 12.97 14.17 40.95 7 13.03 14.22 41.31
3 13.02 14.16 41.12 8 12.97 14.33 41.08
4 12.95 14.22 40.90 9 12, 99 14.17 40.99
5 12.97 14.25 40.98 10 13.05 14.18 41.42 表 3: 现有冷却技术回火后的磁性能检测结果
Figure imgf000006_0001
从实施例 1可见， 提高回火冷速后， 内禀矫顽力平均增高 1. 336KOe， 范围值由 0. 403K0e缩小至 0. 19Κ0βο
从实施例 2可见， 提髙回火冷速后， 内禀矫顽力平均增高 1. 790K0e， 范围值由 0. 520K0e缩小至 0. 210K0e。
试验表明：本发明对提高烧结钕铁硼磁体内禀矫顽力及其一致性效果 显著。

Claims

权 利 要 求
1、 一种烧结钕铁硼永磁体的回火工艺， 包括： 烧结后的钕铁硼 永磁体坯料进行二级回火处理， 即：将烧结冷却后的永磁体坯料在真 空炉加热室内先升温至第一级回火温度，保温结束后将坯料送至真空 炉冷却室充入惰性气体气淬冷却，然后再将坯料送至加热室升温至第 一.级回火温度，保温结束后仍将坯料送至冷却室进行气淬冷却， 其特 征在于：所述的永磁体坯料在回火保温结束后，快速送至冷却室浸入 室内盛有常温液态物质的容器内，同时向真空炉内充入较所述惰性气 体增加 1. 8〜3. 5倍体积的氩气或氮气作为冷却交换载气， 之后迅速 启动风冷电机， 进行快速冷却。
2、 按照权利要求 1所述的烧结钕铁硼永磁体的回火工艺， 其特 征在于： 所述的二级回火处理的第一级回火温度为 900〜930°C， 保 温时间为 2〜3h, 第二级回火温度为 500〜630°C， 保温时间为 2〜 4. 5h。
3、 按照权利要求 1所述的烧结钹铁硼永磁体的回火工艺， 其特 征在于： 所述的快速冷却， 其冷却速度提高至 80〜120 C/分钟。
PCT/CN2005/000380 2004-04-29 2005-03-25 Procede de revenu pour aimant permanent ndfeb fritte WO2005106049A1 (fr)

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