CN106205924A - 一种高性能钕铁硼磁体的制备方法 - Google Patents
一种高性能钕铁硼磁体的制备方法 Download PDFInfo
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- 238000009792 diffusion process Methods 0.000 claims abstract description 47
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 47
- GZCRRIHWUXGPOV-UHFFFAOYSA-N terbium atom Chemical compound [Tb] GZCRRIHWUXGPOV-UHFFFAOYSA-N 0.000 claims abstract description 32
- 229910052771 Terbium Inorganic materials 0.000 claims abstract description 30
- KBQHZAAAGSGFKK-UHFFFAOYSA-N dysprosium atom Chemical compound [Dy] KBQHZAAAGSGFKK-UHFFFAOYSA-N 0.000 claims abstract description 30
- 229910052692 Dysprosium Inorganic materials 0.000 claims abstract description 29
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- QJVKUMXDEUEQLH-UHFFFAOYSA-N [B].[Fe].[Nd] Chemical compound [B].[Fe].[Nd] QJVKUMXDEUEQLH-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 3
- 229910052791 calcium Inorganic materials 0.000 claims abstract description 3
- 229910052802 copper Inorganic materials 0.000 claims abstract description 3
- 229910052733 gallium Inorganic materials 0.000 claims abstract description 3
- 229910052749 magnesium Inorganic materials 0.000 claims abstract description 3
- 229910052758 niobium Inorganic materials 0.000 claims abstract description 3
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 3
- 229910052726 zirconium Inorganic materials 0.000 claims abstract description 3
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 14
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- 229910052751 metal Inorganic materials 0.000 claims description 10
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- 229910017086 Fe-M Inorganic materials 0.000 claims description 2
- 229910052742 iron Inorganic materials 0.000 claims description 2
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- 238000003682 fluorination reaction Methods 0.000 description 2
- 230000005389 magnetism Effects 0.000 description 2
- FWQVINSGEXZQHB-UHFFFAOYSA-K trifluorodysprosium Chemical compound F[Dy](F)F FWQVINSGEXZQHB-UHFFFAOYSA-K 0.000 description 2
- 229910052779 Neodymium Inorganic materials 0.000 description 1
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- 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
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- 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
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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
- H01F41/0266—Moulding; Pressing
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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
- 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
Abstract
本发明公开一种高性能烧结钕铁硼磁体的制备方法，主要通过制造一种辅助扩散合金，该辅助扩散合金粉末与正常钕铁硼磁体粉末混合烧结后在晶界处进行镝、铽元素扩散而成，所述的辅助扩散合金的主要组分为Nd‑Fe‑M，其中Nd为Nd元素，Fe为Fe元素，M为Al、Cu、Ga、Mg、Ca、Zr、Ti、Co、Nb的一种或多种元素的组合，其中Nd的比例为60‑80wt%，Fe的比例为5‑15%，M的比例为5‑35wt%。与现有技术相比，通过本发明的技术方案使得镝、铽在晶界处富集，提供晶界扩散通道，抑制镝、铽向主相晶粒内部扩散，提高镝、铽有效扩散利用率，提高磁体矫顽力。
Description
技术领域
本发明涉及磁体领域，特别是一种高性能烧结钕铁硼磁体的制备方法。
技术背景
烧结钕铁硼磁体由于其优良的性能，在汽车、电子、能源等众多领域获得了广泛应用。随着应用范围的扩大，对于高性能钕铁硼磁体的需求量越来越多，也越来越迫切。镝、铽等重稀土元素的添加可显著提高烧结钕铁硼磁体的矫顽力，因此镝、铽等重稀土元素是高性能钕铁硼磁体的生产制造中不可缺少的重要组分元素。但镝、铽等重稀土是稀有的不可再生资源，在坚持可持续发展以及坚持科学技术进步的同时，如何有效提高镝、铽等重稀土元素的有效利用率成为众多学者关注的重要课题，即在保持剩磁的不变条件下，使用尽可能少的镝、铽或的尽可能高的矫顽力。
如何在减少镝、铽等重稀土的使用量的基础上获得高性能烧结钕铁硼磁体，众多学者及厂家从不同方向上了取得了不菲的成果，最为熟知的技术有3种，一为双合金技术，一为细晶技术，一为晶界扩散技术。双合金技术工艺简单，但镝、铽重稀土元素在晶界处的集中度较低，相对于传统工艺矫顽力提升有限；细晶工艺通过改进制粉工艺获得更为接近单晶状态的合金粉末，从而获得较高的矫顽力，较传统工艺矫顽力可提升1-2kOe；晶界扩散技术是通过浸蘸、喷涂等方式，在磁体表面涂覆一层镝、铽元素扩散源，镝、铽元素通过晶界相向磁体内部扩散，与晶界中的富钕相的Nd发生置换，在主相晶粒周围形成(Dy/Tb)2Fe14B，提高晶界处的各项异性，到达提高矫顽力的目的，矫顽力提升可高达4-12kOe。
但是在晶界扩散时，由于主相晶粒与晶界相的微观组织结构的影响，一部分镝、铽并没有延晶界相向磁体内部继续扩散，反而进入到主相晶粒中，与主相晶粒中Nd进行置换，降低了主相晶粒的饱和磁化强度，导致磁体剩磁降低，晶界处发生置换反应形成的(Dy/Tb)2Fe14B相对减少，抑制了磁体的矫顽力的提升。
发明内容
本发明的目的在于有效提高镝、铽稀土元素在晶界相中的扩散，抑制其向主相晶粒中的扩散，提高镝、铽元素的有效扩散利用率，大幅提高磁体矫顽力。
为实现该目的，本发明采用的技术路线是主要通过制造一种辅助扩散合金，该辅助扩散合金粉末与正常钕铁硼磁体粉末混合烧结后在晶界处进行镝、铽元素扩散而成，所述的辅助扩散合金的主要组分为Nd-Fe-M，其中Nd为Nd元素，Fe为Fe元素，M为Al、Cu、Ga、Mg、Ca、Zr、Ti、Co、Nb的一种或多种元素的组合，其中Nd的比例为60-80wt%，Fe的比例为5-15%，M的比例为5-35wt%。
为实现该目的，本发明采用如下技术方案，具体步骤如下：
a)分别熔炼钕铁硼磁体鳞片和辅助扩散合金鳞片备用；
b)分别将钕铁硼鳞片和辅助扩散合金鳞片进行HD、中磨、气流磨；钕铁硼合金粉末粒度为2-10μm；辅助扩散合金粉末粒度为4-10μm；将辅助扩散合金粉末与钕铁硼磁体粉末混合，辅助扩散合金粉末占总量的比例为0.5-10wt%；
c)将混合均匀后的粉末在充磁场中取向压型；成型后坯体经冷等静压形成生坯；将生坯在真空烧结炉中真空烧结，烧结温度为900-1200℃，保温时间为2-10h；
d)烧结后的坯体加工成薄片磁体，薄片厚度为0.5-20mm；
e)将镝和/或铽的金属或氟化物的一种或多种与乙醇混合，形成混合浆料，镝和/或铽的金属或氟化物占混合浆料的1-10%；
f)将混合浆料涂覆在每个薄片磁体上，在磁体表面形成镝和/或铽的金属或氟化物层，涂覆后磁体增重比为0.5-2wt%，然后在惰性气体Ar2气氛中进行扩散，扩散温度控制在800-1000℃，时间为2-10h；扩散后进行时效，时效温度控制在450-650℃，时间为1-10h。
进一步地，步骤b)中钕铁硼合金粉末粒度优选为4-8μm；辅助扩散合金粉末粒度优选为6-10μm；辅助扩散合金粉末占总量的比例优选为1-5wt%。
进一步地，步骤e)中镝和/或铽的金属或氟化物占混合浆料的比例优选为2-5wt%。与现有技术相比，通过本发明的技术方案可提供晶界扩散通道，抑制镝、铽向主相晶粒内部扩散，使得镝、铽在晶界处富集，提高镝、铽有效扩散利用率，提高磁体矫顽力。
具体实施方式
以下实施例进一步说明本发明的实施方式，但不限制本发明的实施范围。
实施例1：
表1 钕铁硼合金和辅助扩散合金鳞片
按照表1组分所示，熔炼钕铁硼合金鳞片和辅助扩散合金鳞片。两种合金分别经HD、中磨、气流磨研磨制粉，钕铁硼合金粉末粒度5μm，辅助扩散合金粉末粒度为9μm。钕铁硼合金粉末单独压制成型，1050℃保温5h烧结成坯，制备磁体M1；辅助扩散合金粉末按照1.5wt%比例与钕铁硼合金粉末混合，压制成型，1050℃保温5h烧结成坯，制备磁体M2。两种磁体均加工为15-15-4薄片，表面涂覆混合浆料（金属镝粉末按照4%比例与乙醇混合），涂覆前后磁体增重比均为1.0%，920℃扩散处理8h，然后500℃时效处理3小时。
将扩散前后的磁体进行性能测试，测试数据如表2所示：
表2扩散前后磁体磁性能数据
实施例2：
表3 钕铁硼合金和辅助扩散合金鳞片
按照表3组分所示，熔炼钕铁硼合金鳞片和辅助扩散合金鳞片。两种合金分别经HD、中磨、气流磨研磨制粉，钕铁硼合金粉末粒度6μm，辅助扩散合金粉末粒度为8μm。钕铁硼合金粉末单独压制成型，1080℃保温4h烧结成坯，制备磁体M3；辅助扩散合金粉末按照1.2wt%比例与钕铁硼合金粉末混合，压制成型，1080℃保温4h烧结成坯，制备磁体M4。两种磁体均加工为15-15-4薄片，表面涂覆混合浆料（氟化镝粉末按照4.5%比例与乙醇混合），涂覆前后磁体增重比均为0.8%，940℃扩散处理8h，然后520℃时效处理3小时。
将扩散前后的磁体进行性能测试，测试数据如表4所示：
表4扩散前后磁体磁性能数据
实施例3：
表5 钕铁硼合金和辅助扩散合金鳞片
按照表5组分所示，熔炼钕铁硼合金鳞片和辅助扩散合金鳞片。两种合金分别经HD、中磨、气流磨研磨制粉，钕铁硼合金粉末粒度6μm，辅助扩散合金粉末粒度为10μm。钕铁硼合金粉末单独压制成型，1060℃保温5h烧结成坯，制备磁体M5；辅助扩散合金粉末按照2.2wt%比例与钕铁硼合金粉末混合，压制成型，1060℃保温5h烧结成坯，制备磁体M6。两种磁体均加工为15-15-4薄片，表面涂覆混合浆料（金属铽粉末按照3.5%比例与乙醇混合），涂覆前后磁体增重比均为0.8%，920℃扩散处理8h，然后490℃时效处理3小时。
将扩散前后的磁体进行性能测试，测试数据如表6所示：
表6扩散前后磁体磁性能数据
实施例4：
表7钕铁硼合金和辅助扩散合金鳞片
按照表7组分所示，熔炼钕铁硼合金鳞片和辅助扩散合金鳞片。两种合金分别经HD、中磨、气流磨研磨制粉，钕铁硼合金粉末粒度4μm，辅助扩散合金粉末粒度为8μm。钕铁硼合金粉末单独压制成型，1030℃保温5h烧结成坯，制备磁体M7；辅助扩散合金粉末按照3.2wt%比例与钕铁硼合金粉末混合，压制成型，1030℃保温5h烧结成坯，制备磁体M8。两种磁体均加工为15-15-4薄片，表面涂覆混合浆料（氟化铽粉末按照3.0%比例与乙醇混合），涂覆前后磁体增重比均为1.2%，910℃扩散处理8h，然后520℃时效处理3小时。
将扩散前后的磁体进行性能测试，测试数据如表8所示：
表8扩散前后磁体磁性能数据
实施例5：
表9钕铁硼合金和辅助扩散合金鳞片
按照表9组分所示，熔炼钕铁硼合金鳞片和辅助扩散合金鳞片。两种合金分别经HD、中磨、气流磨研磨制粉，钕铁硼合金粉末粒度8μm，辅助扩散合金粉末粒度为9μm。钕铁硼合金粉末单独压制成型，1100℃保温7h烧结成坯，制备磁体M9；辅助扩散合金粉末按照4.5wt%比例与钕铁硼合金粉末混合，压制成型，1100℃保温7h烧结成坯，制备磁体M10。两种磁体均加工为15-15-4薄片，表面涂覆混合浆料（氟化铽粉末1.8%+氟化镝1%比例与乙醇混合），涂覆前后磁体增重比均为1.5%，930℃扩散处理8h，然后550℃时效处理3小时。
将扩散前后的磁体进行性能测试，测试数据如表10所示：
表10扩散前后磁体磁性能数据
Claims (4)
1.一种高性能烧结钕铁硼磁体的制备方法，其特征在于：由钕铁硼磁体粉末和辅助扩散合金粉末混合烧结后在晶界处进行镝、铽元素扩散而成，所述的辅助扩散合金的主要组分为Nd-Fe-M，其中Nd为Nd元素，Fe为Fe元素，M为Al、Cu、Ga、Mg、Ca、Zr、Ti、Co、Nb的一种或多种元素的组合，其中Nd的比例为60-80wt%，Fe的比例为5-15%，M的比例为5-35wt%。
2.根据权利要求1所述的一种高性能烧结钕铁硼磁体的制备方法，其特征在于：
具体包含如下步骤：
a)分别熔炼钕铁硼磁体鳞片和辅助扩散合金鳞片备用；
b)分别将钕铁硼鳞片和辅助扩散合金鳞片进行HD、中磨、气流磨；钕铁硼合金粉末粒度为2-10μm；辅助扩散合金粉末粒度为4-10μm；将辅助扩散合金粉末与钕铁硼磁体粉末混合，辅助扩散合金粉末占总量的比例为0.5-10wt%；
c)将混合均匀后的粉末在充磁场中取向压型；成型后坯体经冷等静压形成生坯；将生坯在真空烧结炉中真空烧结，烧结温度为900-1200℃，保温时间为2-10h；
d)烧结后的坯体加工成薄片磁体，薄片厚度为0.5-20mm；
e)将镝和/或铽的金属或氟化物的一种或多种与乙醇混合，形成混合浆料，镝和/或铽的金属或氟化物占混合浆料的1-10%；
f)将混合浆料涂覆在每个薄片磁体上，在磁体表面形成镝和/或铽的金属或氟化物层，涂覆后磁体增重比为0.5-2%，然后在惰性气体Ar2气氛中进行扩散，扩散温度控制在800-1000℃，时间为2-10h；扩散后进行时效，时效温度控制在450-650℃，时间为1-10h。
3.根据权利要求2所述的一种高性能烧结钕铁硼磁体的制备方法，其特征在于：步骤b)中钕铁硼合金粉末粒度为4-8μm；辅助扩散合金粉末粒度为6-10μm；辅助扩散合金粉末占总量的比例为1-5wt%。
4.根据权利要求2所述的一种高性能烧结钕铁硼磁体的制备方法，其特征在于：步骤e)中镝和/或铽的金属或氟化物占混合浆料的2-5%。
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