CN112750586A - 混合稀土烧结钕铁硼永磁体及其制备方法 - Google Patents

混合稀土烧结钕铁硼永磁体及其制备方法 Download PDF

Info

Publication number
CN112750586A
CN112750586A CN202011581413.5A CN202011581413A CN112750586A CN 112750586 A CN112750586 A CN 112750586A CN 202011581413 A CN202011581413 A CN 202011581413A CN 112750586 A CN112750586 A CN 112750586A
Authority
CN
China
Prior art keywords
rare earth
equal
less
permanent magnet
percent
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN202011581413.5A
Other languages
English (en)
Other versions
CN112750586B (zh
Inventor
任少卿
吕科
孟恒
赵明静
李泉
高岩
付建龙
刘国征
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Baotou Rare Earth Research Institute
Ruike Rare Earth Metallurgy and Functional Materials National Engineering Research Center Co Ltd
Original Assignee
Baotou Rare Earth Research Institute
Ruike Rare Earth Metallurgy and Functional Materials National Engineering Research Center Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Baotou Rare Earth Research Institute, Ruike Rare Earth Metallurgy and Functional Materials National Engineering Research Center Co Ltd filed Critical Baotou Rare Earth Research Institute
Priority to CN202011581413.5A priority Critical patent/CN112750586B/zh
Publication of CN112750586A publication Critical patent/CN112750586A/zh
Application granted granted Critical
Publication of CN112750586B publication Critical patent/CN112750586B/zh
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
    • H01F1/04—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys
    • H01F1/047—Alloys characterised by their composition
    • H01F1/053—Alloys characterised by their composition containing rare earth metals
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
    • H01F1/04—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys
    • H01F1/047—Alloys characterised by their composition
    • H01F1/053—Alloys characterised by their composition containing rare earth metals
    • H01F1/0536—Alloys characterised by their composition containing rare earth metals sintered
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
    • H01F1/04—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys
    • H01F1/047—Alloys characterised by their composition
    • H01F1/053—Alloys characterised by their composition containing rare earth metals
    • H01F1/055—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
    • H01F1/057—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
    • H01F1/04—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys
    • H01F1/047—Alloys characterised by their composition
    • H01F1/053—Alloys characterised by their composition containing rare earth metals
    • H01F1/055—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
    • H01F1/057—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B
    • H01F1/0571—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes
    • H01F1/0575—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together
    • H01F1/0576—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together pressed, e.g. hot working
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
    • H01F1/04—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys
    • H01F1/047—Alloys characterised by their composition
    • H01F1/053—Alloys characterised by their composition containing rare earth metals
    • H01F1/055—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
    • H01F1/057—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B
    • H01F1/0571—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes
    • H01F1/0575—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together
    • H01F1/0577—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together sintered
    • 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
    • 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
    • H01F41/0266—Moulding; Pressing
    • 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
    • H01F41/0293—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 diffusion of rare earth elements, e.g. Tb, Dy or Ho, into permanent magnets

Landscapes

  • Engineering & Computer Science (AREA)
  • Power Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Chemical & Material Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Hard Magnetic Materials (AREA)
  • Manufacturing Cores, Coils, And Magnets (AREA)

Abstract

本发明公开了一种混合稀土烧结钕铁硼永磁体及其制备方法，按照(MMxRE1‑x)aFe100‑a‑b‑ cBbMc成分配料，采用速凝甩带技术得到厚度为0.2～0.5mm的速凝甩带片，然后经过氢破碎和气流磨制成平均粒度为2～5μm的磁粉；将磁粉在氮气保护下在混料罐中混合，混合均匀后在磁场下取向成型，经冷等静压制成生坯；将生坯放在真空烧结炉中进行烧结，烧结温度为950～1100℃，保温得到烧结态磁体；对烧结态磁体进行回火处理，回火温度为420～650℃，得到混合稀土烧结钕铁硼永磁体。本发明通过调整稀土元素与硼元素的比例，制备工艺采用一级回火处理，从而改善了永磁体磁性能。

Description

混合稀土烧结钕铁硼永磁体及其制备方法
技术领域
本发明涉及稀土永磁材料制备领域，具体涉及一种混合稀土烧结钕铁硼永磁体及其制备方法。
背景技术
钕铁硼永磁体是第三代永磁材料，拥有优良的综合磁性能，被广泛地应用于电子行业、航空航天、医疗器械、风力发电、电动汽车、机器人等诸多领域，是目前市场应用最多的永磁材料。稀土永磁制造业主要以镨钕合金作为原料制造钕铁硼永磁体，而我国轻稀土主要产地白云鄂博矿中含有大量的La、Ce稀土元素，难以得到有效利用。混合稀土(Mischmetal,MM)中La、Ce、Pr、Nd各组分比例维持了矿石中的比例。由于减少了稀土元素分离的工艺流程，混合稀土合金不仅更加环保而且具有明显的价格优势。使用混合稀土作为原料制造稀土永磁体，能够显著降低永磁体的成本，同时还有利于稀土资源的平衡利用。
商用磁体一般要求矫顽力达到12KOe以上。由于混合稀土中La和Ce的高含量，若制造纯MMFeB合金，其磁性能下降严重，难以满足应用需求。近年来，MM部分替代PrNd生产低成本钕铁硼磁体的工作取得的成果表明，非均质钕铁硼合金可以保持较高的磁性能，从而为低成本磁体的生产带来了希望。
传统烧结永磁体工艺路线采用二级回火，但是对于(MM，Nd)-Fe-B磁体而言，难以避免化学元素均质化对磁性能的损害，并且制备成本高。
中国专利公开号CN 107146674 A公开了一种免于热处理的富铈稀土永磁体及其生产方法，该技术中磁体包括多个主相。工艺不经后续热处理工序，其磁体性能是通过磁体包含的多个主相来实现的。
发明内容
本发明的目的在于提供一种混合稀土烧结钕铁硼永磁体及其制备方法，通过调整稀土元素与硼元素的比例，制备工艺采用一级回火处理，从而改善了永磁体磁性能，在保持较高磁性能的同时，降低永磁体的原材料成本以及制造能耗。
为达到上述目的，本发明使用的技术解决方案是：
混合稀土烧结钕铁硼永磁体，质量百分数通式为：(MMxRE1-x)aFe100-a-b-cBbMc，MM为混合稀土合金，MM的质量百分比；Ce>48％，La 20～35％，Pr4～7％，Nd 10～20％，Sm≤0.3％，Fe≤1％，Mg≤0.8％，Si≤0.2％，Ca≤0.03％，S≤0.02％，P≤0.01％；RE为Pr、Nd、Sm、Eu、Gd、Ho、Dy、Tb元素中的一种或者多种，B为硼元素，M为Nb、V、Ti、Co、Cr、Mo、Mn、Ni、Ga、Zr、Ta、Ag、Au、Al、Pb、Cu、Si元素中一种或多种，其中29≤a≤35、0.85≤b≤1、0.5≤c≤5、10≤x≤40。
进一步，31≤a≤33，0.9≤b≤0.95，1.2≤c≤2.5，20≤x≤30。
进一步，磁体稀土总量a＝32，硼含量b＝0.92。
进一步，磁体稀土总量a＝33，硼含量b＝0.9。
混合稀土烧结钕铁硼永磁体的制备方法，包括：
按照(MMxRE1-x)aFe100-a-b-cBbMc成分配料，采用速凝甩带技术得到厚度为0.2～0.5mm的速凝甩带片，速凝甩带片经过氢破碎和气流磨制成平均粒度为2～5μm的磁粉；
将磁粉在氮气保护下混合，在混料罐中混合1～3h，混合均匀后在1.5T～2T的磁场下取向成型，经冷等静压制成生坯；
将生坯放在真空烧结炉中进行烧结，烧结温度为950～1100℃，保温1～10h得到烧结态磁体；
对烧结态磁体进行回火处理，回火温度为420～650℃，得到混合稀土烧结钕铁硼永磁体。
优选的，在470～530℃之间进行保温2～5h的回火热处理。
优选的，通过控制稀土总量以及硼的含量，使得31≤a≤33，0.9≤b≤0.95。
优选的，制备成平均粉末粒度小于3.5μm的粉末，在氮气保护下将磁粉在2T磁场下取向成型，经冷等静压200MPa制成生坯。
优选的，将生坯放入真空烧结炉中，在1060℃烧结保温5小时，然后在500℃进行回火处理3h。
本发明技术效果包括：
本发明通过调整稀土元素与硼元素的比例，采用一级回火处理，制造矫顽力大于12KOe的混合稀土烧结钕铁硼永磁体((MM，Nd)-Fe-B磁体)。在保持较高磁性能的同时，降低磁体的原材料成本以及制造能耗。
(1)本发明所提供的磁体，利用了混合稀土。
混合稀土中La、Ce、Pr、Nd各组分比例维持了我国轻稀土主要产地白云鄂博矿石中各元素的比例。由于减少了稀土元素分离的工艺流程，混合稀土合金不仅更加环保而且具有明显的价格优势。本发明利用MM部分取代Nd进行稀土永磁体的制备和生产，实现成本控制。
(2)本发明通过控制稀土总量以及硼的含量，保证永磁体液相烧结过程中富稀土相的含量，从而改善了磁性能。
(3)本发明采用一级回火的工艺路线，相较传统永磁体制造的二级回火工艺路线，大幅度降低了生产能耗。
本发明采用一级回火，有利于避免化学元素均质化对磁性能的损害，制造工艺流程更短的(MM,Nd)-Fe-B磁体，不仅减少了原材料成本，还能降低制造过程中的能耗，对低成本磁体的生产具有重大意义。
具体实施方式
以下描述充分地示出本发明的具体实施方案，以使本领域的技术人员能够实践和再现。
混合稀土烧结钕铁硼永磁体的制备方法，步骤如下：
步骤1：按照(MMxRE1-x)aFe100-a-b-cBbMc成分配料，采用速凝甩带技术得到厚度为0.2～0.5mm的速凝甩带片，然后经过氢破碎和气流磨制成平均粒度为2～5μm的磁粉；
步骤2：将磁粉在氮气保护下混合，在混料罐中混合1～3h，混合均匀后在1.5T～2T的磁场下取向成型，经冷等静压制成生坯；
冷等静压的压力为200MPa。
步骤3：将生坯放在真空烧结炉中进行烧结，烧结温度为950～1100℃，保温1～10h得到烧结态磁体；
步骤4：对烧结态磁体进行回火处理，回火温度为420～650℃，得到混合稀土烧结钕铁硼永磁体。
本优选实施例中，采用一级回火的工艺路线，优选的回火处理温度为470～530℃，在470～530℃之间选取一个温度，进行保温2～5h的回火热处理。本发明中涉及的混合稀土烧结钕铁硼永磁体中包含La、Ce、Pr、Nd四种稀土金属。
本发明得到混合稀土烧结钕铁硼永磁体，仅有一个主相，由于调整了稀土总量及硼的含量，可以仅通过一级回火，即可获得良好的磁性能。较高的稀土总量以及较低的硼含量保证了磁体中有较多的富钕相的存在，该富钕相主要由稀土、铁以及一定量的氧及其他小量金属构成，这种成分的富钕相是一级回火既能有效改善磁体的显微结构的原因。一级回火工艺是基于本发明所述磁体化学元素配比，即本发明的两个发明点是互为依托的。
混合稀土烧结钕铁硼永磁体属于(MM，Nd)-Fe-B磁体，质量百分数通式为：(MMxRE1-x)aFe100-a-b-cBbMc，MM为混合稀土合金，MM的质量百分比：Ce>48％，La 20～35％，Pr4～7％，Nd 10～20％，Sm≤0.3％，Fe≤1％，Mg≤0.8％，Si≤0.2％，Ca≤0.03％，S≤0.02％，P≤0.01％；RE为Pr、Nd、Sm、Eu、Gd、Ho、Dy、Tb元素中的一种或者几种，B为硼元素，M为Nb、V、Ti、Co、Cr、Mo、Mn、Ni、Ga、Zr、Ta、Ag、Au、Al、Pb、Cu、Si元素中一种或几种，其中29≤a≤35、0.85≤b≤1、0.5≤c≤5、10≤x≤40。
本优选实施例中，31≤a≤33，0.9≤b≤0.95，1.2≤c≤2.5，20≤x≤30。通过控制稀土总量以及硼的含量，使得31≤a≤33，0.9≤b≤0.95保证永磁体液相烧结过程中富稀土相的含量，从而改善磁性能。
通过控制稀土总量以及硼的含量，保证了速凝甩带的显微结构由良好的柱状晶组成，且柱状晶之间填充富稀土相，这是磁体磁性能的前提保证。之后的一级回火工艺，有效调控了富稀土相的构成，形成了良好的晶界结构，提高了磁体的矫顽力。本发明所述化学成分的混合稀土烧结钕铁硼永磁体，其晶界结构不需要高温阶段的时效处理，仅经过低温阶段的时效处理即可达到矫顽力最优值。
对比例1
将质量百分数为(MM0.25Re0.75)30FebalB1Co0.5Al0.4Ga0.2Cu0.1Zr0.1的化学成分配料，采用速凝甩带、氢破碎和气流磨的工艺流程，制备成平均粉末粒度小于3.5μm的粉末。在磁粉中添加润滑剂与防氧化剂并混合均匀后，在氮气保护下将磁粉在2T磁场下取向成型，并经200MPa冷等静压制成生坯。将生坯放入真空烧结炉中，在1060℃烧结保温5小时；然后在900℃一级回火热处理3h，然后在500℃进行二级回火处理3h，所得磁体磁性能如表1所示。
对比例2
将质量百分数为(MM0.25Re0.75)32FebalB0.92Co0.5Al0.4Ga0.2Cu0.1Zr0.1的化学成分配料，采用速凝甩带、氢破碎和气流磨的工艺流程，制备成平均粉末粒度小于3.5μm的粉末。在磁粉中添加润滑剂与防氧化剂并混合均匀后，在氮气保护下将磁粉在2T磁场下取向成型，并经200MPa冷等静压制成生坯。将生坯放入真空烧结炉中，在1060℃烧结保温5小时；然后在900℃一级回火热处理3h，然后在500℃进行二级回火处理3h，所得磁体磁性能如表1所示。
实施例1
将质量百分数为(MM0.25Re0.75)32FebalB0.92Co0.5Al0.4Ga0.2Cu0.1Zr0.1的化学成分配料，采用速凝甩带、氢破碎和气流磨的工艺流程，制备成平均粉末粒度小于3.5μm的粉末。在磁粉中添加润滑剂与防氧化剂并混合均匀后，在氮气保护下将磁粉在2T磁场下取向成型，并经200MPa冷等静压制成生坯。将生坯放入真空烧结炉中，在1060℃烧结保温5小时；然后在500℃进行回火处理3h，所得磁体磁性能如表1所示
表1
性能参数 Br/kGs Hcj/kOe (BH)max/MGOe 方形度/％
对比例1 13.08 7.698 37.68 76.2
对比例2 13.03 12.19 40.96 96.7
实施例1 12.88 11.89 40.14 95.1
说明：对比例1中磁体稀土总含量a＝30，硼含量b＝1，其磁性较低。
实施例1中磁体稀土总量优选的为a＝32，硼含量b＝0.92，其磁性能显著高于对比例1。实施例1中的磁体没有经过900℃回火3h的处理，仍然保持了与对比例2相当的磁性能。上述对比说明合适的稀土总量能够保证永磁体较高的磁性能，本发明不仅缩短了工艺流程，降低了生产能耗，而且磁体也能获得较好的磁性能。
对比例3
将质量百分数为(MM0.25Re0.75)33FebalB0.9Co0.5Al0.4Ga0.2Cu0.1Zr0.1的化学成分配料，采用速凝甩带、氢破碎和气流磨的工艺流程，制备成平均粉末粒度小于3.5μm的粉末。在磁粉中添加润滑剂与防氧化剂并混合均匀后，在氮气保护下将磁粉在2T磁场下取向成型，并经200MPa冷等静压制成生坯。将生坯放入真空烧结炉中，在1060℃烧结保温5小时；然后在900℃一级回火热处理3h，然后在500℃进行二级回火处理3h，所得磁体磁性能如表2所示。
对比例4
将质量百分数为(MM0.25Re0.75)30FebalB1Co0.5Al0.4Ga0.2Cu0.1Zr0.1的化学成分配料，采用速凝甩带、氢破碎和气流磨的工艺流程，制备成平均粉末粒度小于3.5μm的粉末。在磁粉中添加润滑剂与防氧化剂并混合均匀后，在氮气保护下将磁粉在2T磁场下取向成型，并经200MPa冷等静压制成生坯。将生坯放入真空烧结炉中，在1060℃烧结保温5小时，然后在500℃进行一级回火处理3h，所得磁体磁性能如表3所示。
实施例2
将质量百分数为(MM0.25Re0.75)33FebalB0.9Co0.5Al0.4Ga0.2Cu0.1Zr0.1的化学成分配料，采用速凝甩带、氢破碎和气流磨的工艺流程，制备成平均粉末粒度小于3.5μm的粉末。在磁粉中添加润滑剂与防氧化剂并混合均匀后，在氮气保护下将磁粉在2T磁场下取向成型，并经200Mpa冷等静压制成生坯。将生坯放入真空烧结炉中，在1060℃烧结保温5小时，然后在500℃进行一级回火处理3h，所得磁体磁性能如表2所示。
表2
性能参数 Br/kGs Hcj/kOe (BH)max/MGOe 方形度/％
对比例3 12.77 12.07 39.74 97
对比例4 13.05 9.00 38.88 73.1
实施例2 12.88 12.09 40.73 98.5
说明：通过对比例3和实施例2的比较可以发现，实施例2中的磁体没有经过900℃回火3h的处理，仍然保持了与对比例3相当的磁性能，其磁能积甚至明显高于多一段回火处理的对比例3。上述对比说明本发明不仅缩短了工艺流程，降低了生产能耗，而且磁体也能获得较好的磁性能。
对比例4中磁体稀土总含量a＝30，硼含量b＝1，其磁性较低。
实施例2中磁体稀土总量优选的为a＝33，硼含量b＝0.9，其磁性能显著高于对比例4。上述对比说明合理的稀土总量以及硼的含量是保证磁体性能的前提条件，
本发明所用的术语是说明和示例性、而非限制性的术语。由于本发明能够以多种形式具体实施而不脱离发明的精神或实质，所以应当理解，上述实施例不限于任何前述的细节，而应在随附权利要求所限定的精神和范围内广泛地解释，因此落入权利要求或其等效范围内的全部变化和改型都应为随附权利要求所涵盖。

Claims (9)

1.一种混合稀土烧结钕铁硼永磁体，其特征在于，质量百分数通式为：(MMxRE1-x)aFe100-a-b-cBbMc，MM为混合稀土合金，MM的质量百分比；Ce>48％，La 20～35％，Pr4～7％，Nd10～20％，Sm≤0.3％，Fe≤1％，Mg≤0.8％，Si≤0.2％，Ca≤0.03％，S≤0.02％，P≤0.01％；RE为Pr、Nd、Sm、Eu、Gd、Ho、Dy、Tb元素中的一种或者多种，B为硼元素，M为Nb、V、Ti、Co、Cr、Mo、Mn、Ni、Ga、Zr、Ta、Ag、Au、Al、Pb、Cu、Si元素中一种或多种，其中29≤a≤35、0.85≤b≤1、0.5≤c≤5、10≤x≤40。
2.如权利要求1所述的混合稀土烧结钕铁硼永磁体，其特征在于，31≤a≤33，0.9≤b≤0.95，1.2≤c≤2.5，20≤x≤30。
3.如权利要求1所述的混合稀土烧结钕铁硼永磁体，其特征在于，磁体稀土总量a＝32，硼含量b＝0.92。
4.如权利要求1所述的混合稀土烧结钕铁硼永磁体，其特征在于，磁体稀土总量a＝33，硼含量b＝0.9。
5.如权利要求1～4任一项所述的混合稀土烧结钕铁硼永磁体的制备方法，包括：
按照(MMxRE1-x)aFe100-a-b-cBbMc成分配料，采用速凝甩带技术得到厚度为0.2～0.5mm的速凝甩带片，速凝甩带片经过氢破碎和气流磨制成平均粒度为2～5μm的磁粉；
将磁粉在氮气保护下混合，在混料罐中混合1～3h，混合均匀后在1.5T～2T的磁场下取向成型，经冷等静压制成生坯；
将生坯放在真空烧结炉中进行烧结，烧结温度为950～1100℃，保温1～10h得到烧结态磁体；
对烧结态磁体进行回火处理，回火温度为420～650℃，得到混合稀土烧结钕铁硼永磁体。
6.如权利要求5所述的混合稀土烧结钕铁硼永磁体的制备方法，其特征在于，在470～530℃之间进行保温2～5h的回火热处理。
7.如权利要求5所述的混合稀土烧结钕铁硼永磁体的制备方法，其特征在于，通过控制稀土总量以及硼的含量，使得31≤a≤33，0.9≤b≤0.95。
8.如权利要求5所述的混合稀土烧结钕铁硼永磁体的制备方法，其特征在于，制备成平均粉末粒度小于3.5μm的粉末，在氮气保护下将磁粉在2T磁场下取向成型，经冷等静压200MPa制成生坯。
9.如权利要求5所述的混合稀土烧结钕铁硼永磁体的制备方法，其特征在于，将生坯放入真空烧结炉中，在1060℃烧结保温5小时，然后在500℃进行回火处理3h。
CN202011581413.5A 2020-12-28 2020-12-28 混合稀土烧结钕铁硼永磁体及其制备方法 Active CN112750586B (zh)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202011581413.5A CN112750586B (zh) 2020-12-28 2020-12-28 混合稀土烧结钕铁硼永磁体及其制备方法

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202011581413.5A CN112750586B (zh) 2020-12-28 2020-12-28 混合稀土烧结钕铁硼永磁体及其制备方法

Publications (2)

Publication Number Publication Date
CN112750586A true CN112750586A (zh) 2021-05-04
CN112750586B CN112750586B (zh) 2024-03-29

Family

ID=75646265

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202011581413.5A Active CN112750586B (zh) 2020-12-28 2020-12-28 混合稀土烧结钕铁硼永磁体及其制备方法

Country Status (1)

Country Link
CN (1) CN112750586B (zh)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113421761A (zh) * 2021-06-12 2021-09-21 山西汇镪磁性材料制作有限公司 一种降低改性磁粉吸附能的高性能烧结钕铁硼制备方法
CN114038641A (zh) * 2021-11-17 2022-02-11 山西御成新材料科技有限公司 一种含银的混合稀土铁硼烧结永磁体及其制备方法

Citations (14)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2006104050A (ja) * 2004-09-10 2006-04-20 Neomax Co Ltd 酸化物磁性材料および焼結磁石
CN101325109A (zh) * 2008-04-08 2008-12-17 浙江大学 晶界相重构的高强韧性烧结钕铁硼磁体及其制备方法
CN101901657A (zh) * 2009-05-27 2010-12-01 比亚迪股份有限公司 一种烧结钕铁硼永磁材料及其制备方法
US20110074530A1 (en) * 2009-09-30 2011-03-31 General Electric Company Mixed rare-earth permanent magnet and method of fabrication
US20120280775A1 (en) * 2011-05-02 2012-11-08 Shin-Etsu Chemical Co., Ltd. Rare earth permanent magnets and their preparation
CN104124052A (zh) * 2014-07-25 2014-10-29 安徽大地熊新材料股份有限公司 一种高性能稀土－铁－硼系烧结永磁体的制备方法
CN104275487A (zh) * 2014-08-26 2015-01-14 宁波鑫丰磁业有限公司 一种添加mm合金的烧结钕铁硼的制备方法
CN106971802A (zh) * 2017-04-14 2017-07-21 钢铁研究总院 一种再生烧结钕铁硼永磁体制备方法
WO2018040299A1 (zh) * 2016-08-31 2018-03-08 浙江东阳东磁稀土有限公司 一种制备稀土永磁材料的方法
CN108242303A (zh) * 2017-12-26 2018-07-03 钢铁研究总院 一种混合稀土永磁材料及其制备方法
CN108565086A (zh) * 2018-05-11 2018-09-21 包头稀土研究院 高磁能积高矫顽力烧结钕铁硼磁体的制备方法
JP2018182299A (ja) * 2017-04-19 2018-11-15 トヨタ自動車株式会社 希土類磁石の製造方法
CN110895985A (zh) * 2019-11-06 2020-03-20 包头稀土研究院 混合稀土烧结钕铁硼永磁体及其制备方法
CN111341512A (zh) * 2020-03-09 2020-06-26 钢铁研究总院 一种高性价比稀土永磁体及制备方法

Patent Citations (14)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2006104050A (ja) * 2004-09-10 2006-04-20 Neomax Co Ltd 酸化物磁性材料および焼結磁石
CN101325109A (zh) * 2008-04-08 2008-12-17 浙江大学 晶界相重构的高强韧性烧结钕铁硼磁体及其制备方法
CN101901657A (zh) * 2009-05-27 2010-12-01 比亚迪股份有限公司 一种烧结钕铁硼永磁材料及其制备方法
US20110074530A1 (en) * 2009-09-30 2011-03-31 General Electric Company Mixed rare-earth permanent magnet and method of fabrication
US20120280775A1 (en) * 2011-05-02 2012-11-08 Shin-Etsu Chemical Co., Ltd. Rare earth permanent magnets and their preparation
CN104124052A (zh) * 2014-07-25 2014-10-29 安徽大地熊新材料股份有限公司 一种高性能稀土－铁－硼系烧结永磁体的制备方法
CN104275487A (zh) * 2014-08-26 2015-01-14 宁波鑫丰磁业有限公司 一种添加mm合金的烧结钕铁硼的制备方法
WO2018040299A1 (zh) * 2016-08-31 2018-03-08 浙江东阳东磁稀土有限公司 一种制备稀土永磁材料的方法
CN106971802A (zh) * 2017-04-14 2017-07-21 钢铁研究总院 一种再生烧结钕铁硼永磁体制备方法
JP2018182299A (ja) * 2017-04-19 2018-11-15 トヨタ自動車株式会社 希土類磁石の製造方法
CN108242303A (zh) * 2017-12-26 2018-07-03 钢铁研究总院 一种混合稀土永磁材料及其制备方法
CN108565086A (zh) * 2018-05-11 2018-09-21 包头稀土研究院 高磁能积高矫顽力烧结钕铁硼磁体的制备方法
CN110895985A (zh) * 2019-11-06 2020-03-20 包头稀土研究院 混合稀土烧结钕铁硼永磁体及其制备方法
CN111341512A (zh) * 2020-03-09 2020-06-26 钢铁研究总院 一种高性价比稀土永磁体及制备方法

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
任少卿 等: ""CuGa 晶界添加对烧结钕铁硼永磁体磁性能及热稳定性的影响"", 《稀土》, vol. 5, no. 41, pages 40 - 49 *
刘小鱼;刘国征;赵明静;鲁富强;武斌;: "双合金工艺制备钕铁硼永磁体的性能和显微组织的研究", 金属功能材料, no. 06, pages 5 - 8 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113421761A (zh) * 2021-06-12 2021-09-21 山西汇镪磁性材料制作有限公司 一种降低改性磁粉吸附能的高性能烧结钕铁硼制备方法
CN114038641A (zh) * 2021-11-17 2022-02-11 山西御成新材料科技有限公司 一种含银的混合稀土铁硼烧结永磁体及其制备方法

Also Published As

Publication number Publication date
CN112750586B (zh) 2024-03-29

Similar Documents

Publication Publication Date Title
US11195645B2 (en) Ce-containing sintered rare-earth permanent magnet with having high toughness and high coercivity, and preparation method therefor
US11062827B2 (en) Sintered magnet composition without heavy rare earth element and a method of making the sintered magnet
CN101266855B (zh) 稀土永磁材料及其制造方法
CN106601407B (zh) 提高钕铁硼磁体矫顽力的方法
CN101853725B (zh) 烧结钕铁硼永磁材料的制备方法
EP3975212A1 (en) A method for preparation of a sintered type ndfeb permanent magnet with an adjusted grain boundary
CN104681268B (zh) 一种提高烧结钕铁硼磁体矫顽力的处理方法
CN103794322A (zh) 一种超高矫顽力烧结钕铁硼磁体及其制备方法
CN107275027B (zh) 应用钇的富铈稀土永磁体及其制备方法
CN112863848B (zh) 高矫顽力烧结钕铁硼磁体的制备方法
CN103985533A (zh) 共晶合金氢化物掺杂提高烧结钕铁硼磁体矫顽力的方法
CN110895985A (zh) 混合稀土烧结钕铁硼永磁体及其制备方法
CN104575920A (zh) 稀土永磁体及其制备方法
CN104575901A (zh) 一种添加铽粉的钕铁硼磁体及其制备方法
CN104575903A (zh) 一种添加Dy粉末的钕铁硼磁体及其制备方法
CN111378907A (zh) 一种提高钕铁硼永磁材料矫顽力的辅助合金及应用方法
CN112750586B (zh) 混合稀土烧结钕铁硼永磁体及其制备方法
CN101719405A (zh) 低能耗耐腐蚀铝合金与钕铁硼型稀土永磁的双相复合材料
CN110033914B (zh) 提高烧结钕铁硼磁体的矫顽力的方法
CN108447638A (zh) 一种新能源汽车电机用超高矫顽力钕铁硼永磁体及其制备方法
CN109545491B (zh) 一种钕铁硼永磁材料及其制备方法
CN109585112B (zh) 一种具有改进的晶体结构的高性能稀土永磁材料
CN108364739B (zh) 钕铁硼磁体及其制备方法
CN114255951B (zh) 高性能烧结钕铁硼磁体及其制备方法
CN106920614B (zh) 一种高磁性因子烧结钕铁硼的制备方法

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant