CN114823113A - 一种高矫顽力富铈稀土永磁材料的制备方法 - Google Patents
一种高矫顽力富铈稀土永磁材料的制备方法 Download PDFInfo
- Publication number
- CN114823113A CN114823113A CN202210392116.9A CN202210392116A CN114823113A CN 114823113 A CN114823113 A CN 114823113A CN 202210392116 A CN202210392116 A CN 202210392116A CN 114823113 A CN114823113 A CN 114823113A
- Authority
- CN
- China
- Prior art keywords
- equal
- rare earth
- heat treatment
- cerium
- less
- 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.)
- Pending
Links
- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 44
- 150000002910 rare earth metals Chemical class 0.000 title claims abstract description 29
- 229910052684 Cerium Inorganic materials 0.000 title claims abstract description 23
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 title claims abstract description 22
- 239000000463 material Substances 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 238000010438 heat treatment Methods 0.000 claims abstract description 37
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 34
- 239000006247 magnetic powder Substances 0.000 claims abstract description 33
- 238000000034 method Methods 0.000 claims abstract description 26
- 238000005245 sintering Methods 0.000 claims abstract description 23
- 238000007731 hot pressing Methods 0.000 claims abstract description 9
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 5
- 239000000956 alloy Substances 0.000 claims abstract description 5
- 229910052796 boron Inorganic materials 0.000 claims abstract description 5
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 4
- 229910052802 copper Inorganic materials 0.000 claims abstract description 4
- 229910052733 gallium Inorganic materials 0.000 claims abstract description 3
- 229910052748 manganese Inorganic materials 0.000 claims abstract description 3
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 3
- 229910052758 niobium Inorganic materials 0.000 claims abstract description 3
- 229910052715 tantalum Inorganic materials 0.000 claims abstract description 3
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 3
- 229910052720 vanadium Inorganic materials 0.000 claims abstract description 3
- 229910052726 zirconium Inorganic materials 0.000 claims abstract description 3
- 238000004519 manufacturing process Methods 0.000 claims abstract 4
- 229910052739 hydrogen Inorganic materials 0.000 claims description 10
- 239000001257 hydrogen Substances 0.000 claims description 10
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 7
- 238000010902 jet-milling Methods 0.000 claims description 5
- 238000002074 melt spinning Methods 0.000 claims description 5
- 229910052779 Neodymium Inorganic materials 0.000 claims description 2
- 150000002431 hydrogen Chemical class 0.000 claims description 2
- 229910052746 lanthanum Inorganic materials 0.000 claims description 2
- 238000009768 microwave sintering Methods 0.000 claims description 2
- 238000010791 quenching Methods 0.000 claims description 2
- 230000000171 quenching effect Effects 0.000 claims description 2
- 238000010583 slow cooling Methods 0.000 claims description 2
- 238000002490 spark plasma sintering Methods 0.000 claims description 2
- 229910052727 yttrium Inorganic materials 0.000 claims description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical group [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims 1
- 229910052692 Dysprosium Inorganic materials 0.000 claims 1
- 229910052688 Gadolinium Inorganic materials 0.000 claims 1
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 claims 1
- 229910052777 Praseodymium Inorganic materials 0.000 claims 1
- 229910052771 Terbium Inorganic materials 0.000 claims 1
- 239000000203 mixture Substances 0.000 claims 1
- 230000001808 coupling effect Effects 0.000 abstract description 4
- 229910052742 iron Inorganic materials 0.000 abstract description 3
- 230000005389 magnetism Effects 0.000 abstract description 3
- 230000003313 weakening effect Effects 0.000 abstract description 2
- 239000004615 ingredient Substances 0.000 abstract 1
- 238000012360 testing method Methods 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 6
- 229910001172 neodymium magnet Inorganic materials 0.000 description 6
- QJVKUMXDEUEQLH-UHFFFAOYSA-N [B].[Fe].[Nd] Chemical compound [B].[Fe].[Nd] QJVKUMXDEUEQLH-UHFFFAOYSA-N 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 3
- 230000005294 ferromagnetic effect Effects 0.000 description 3
- 230000005291 magnetic effect Effects 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 238000006356 dehydrogenation reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000007323 disproportionation reaction Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 description 1
- QEFYFXOXNSNQGX-UHFFFAOYSA-N neodymium atom Chemical compound [Nd] QEFYFXOXNSNQGX-UHFFFAOYSA-N 0.000 description 1
- 230000008520 organization Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000010248 power generation Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 1
Images
Classifications
-
- 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
- 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
-
- 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
Landscapes
- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Hard Magnetic Materials (AREA)
Abstract
本发明公开了一种高矫顽力富铈稀土永磁材料的制备方法。本发明针对成分为(A1‑aCea)bFebalMcBdGae的富铈磁体，A为稀土元素Nd、Pr、Dy、Tb、La、Y、Gd中的一种或多种，Ce为稀土元素铈，Fe为铁元素，M为合金元素Co、Ni、Al、Cu、Mn、Nb、Zr、Ti、V、Ta中的一种或多种，B为硼元素，Ga为镓元素，以质量百分数计，0.3≤a≤0.7，30≤b≤35，0≤c≤2，0.75≤d≤0.95，0.2≤e≤3。本发明高矫顽力富铈稀土永磁材料的制备方法包括：将磁粉通过烧结或热压热变形工艺制备成磁体，再进行热处理。本发明基于富铈稀土永磁材料的组织结构特征，通过提高磁体中合金元素Ga和稀土元素的含量，同时降低B元素的含量，在磁体制备过程中形成大量连续REFe2相以及部分RE6Fe13Ga相，消耗晶界相中的铁，降低晶界相的磁性，从而削弱甚至是消除主相晶粒间的短程交换耦合作用，提高磁体的矫顽力。
Description
技术领域
本发明涉及稀土永磁领域，具体涉及一种高矫顽力富铈稀土永磁材料的制备方法。
背景技术
钕铁硼是目前磁性最强、应用最广、消耗稀土最多的稀土永磁材料，广泛应用于国防和民用领域。低碳经济的全球化背景下，风力发电、新能源汽车等新兴产业蓬勃发展，钕铁硼作为关键材料，其需求量快速增长，战略性稀土元素Nd/Pr的消耗量和价格随之大幅增长。因此，近年来，高丰度稀土元素在钕铁硼中的应用技术获得广泛关注，已成为稀土永磁领域的重点发展方向。
在丰度较高的镧(La)、铈(Ce)、钇(Y)这三种稀土元素中，Ce元素的地壳丰度最高，而且Ce-Fe-B形成的Ce2Fe14B四方相的理论磁晶各向异性场HA也高于La2Fe14B和Y2Fe14B，因而成为研究焦点。然而，Ce2Fe14B四方相的内禀磁性能仍远低于Nd2Fe14B，目前高Ce替代量的富铈磁体磁性能普遍偏低，尤其是矫顽力低，远低于理论HA，无法满足商业应用要求。如果能够通过成分设计和制备技术的创新，发明高矫顽力富Ce稀土永磁材料，将有望实现高丰度稀土Ce在稀土永磁中的规模应用，促进稀土元素的高效平衡利用。
基于现有钕铁硼的研究结果，钕铁硼磁体的矫顽力远低于理论值，很大程度上归因于磁体的铁磁性晶界相，晶界相中铁含量过高，甚至达到60％以上，相邻铁磁性主相晶粒间仍存在短程交换耦合作用。在传统钕铁硼磁体中，以富钕晶界相为主；而在富Ce磁体中，除了部分富稀土晶界相，还存在大量的REFe2晶界相，并且主要以三叉晶界的形式存在，对主相晶粒的磁隔绝作用仍较小。如何有效发挥REFe2等晶界相的作用，是制备高矫顽力富铈稀土永磁材料的关键问题。
发明内容
本发明的目的是克服现有技术的不足，提供一种高矫顽力富铈稀土永磁材料的制备方法。
一种高矫顽力富铈稀土永磁材料的制备方法，包括以下步骤：
(1)制备成分为(A1-aCea)bFebalMcBdGae的磁粉，其中A为稀土元素Nd、Pr、Dy、Tb、La、Y、Gd中的一种或多种，Ce为稀土元素铈，Fe为铁元素，M为合金元素Co、Ni、Al、Cu、Mn、Nb、Zr、Ti、V、Ta中的一种或多种，B为硼元素，Ga为镓元素，以质量百分数计，0.3≤a≤0.7，30≤b≤35，0≤c≤2，0.75≤d≤0.95，0.2≤e≤3；
(2)将所得的磁粉通过烧结或热压热变形工艺制备成磁体；
(3)将所制备的磁体通过热处理，得到高矫顽力富铈稀土永磁材料。
其中，步骤(1)中磁粉的制备工艺包括：
(1)依次为甩带、氢破和气流磨；
(2)依次为快淬带和氢破；
(3)依次为吸氢、歧化、脱氢和再复合。
步骤(1)中的磁粉，通过单主相的方法直接得到或通过多主相的方法得到最终限定的成分。
步骤(2)中的烧结工艺包括：普通烧结工艺或放电等离子烧结工艺或微波烧结工艺。
步骤(3)中的热处理工艺包括：一步热处理或两步热处理或在步骤(2)烧结或热压热变形后慢速冷却。
具体地，一步热处理的热处理温度为：400～800℃，热处理时间为：0.5h～5h。
具体地，两步热处理中的第一步热处理温度为：850～950℃，热处理时间为：0.5h～4h；第二步热处理温度为：400～600℃，热处理时间为：0.5h～5h。
具体地，烧结或热压热变形后的冷却速度小于等于室温下随炉冷却速度。
本发明与现有技术相比的有益效果：
1)本发明基于大量实验研究，在掌握富铈稀土永磁材料的组织结构特征的基础上，针对不同Ce含量的磁体，通过针对性成分设计，在不同程度上提高磁体中合金元素Ga的含量，辅以Cu和Al等合金元素优化配比，同时降低B元素的含量，促进形成大量REFe2相，更重要的是，促进REFe2相延伸进入相邻主相晶粒界面区域，形成连续REFe2晶界相，并同时形成部分RE6Fe13Ga相，这些富Fe的非铁磁性晶界相会大量消耗富稀土晶界相中的铁，降低富稀土晶界相的磁性，从而削弱乃至消除主相晶粒间的短程交换耦合作用，大幅提高磁体的矫顽力。
2)本发明成分设计同时增加稀土元素的含量，并配合不同稀土元素和合金元素的配比，一方面磁粉制备过程中更有利于形成良好的组织结构，促进在烧结和热处理过程中形成大量连续REFe2相以及部分RE6Fe13Ga晶界相，另一方面提高富稀土晶界相中的稀土元素含量，相对降低其中Fe元素含量，进一步提高矫顽力。
3)本发明在针对性成分设计的同时，配合制备技术创新，创新结合不同的制粉、烧结和热处理技术，包括创新提出的烧结或热压热变形后以较慢速度冷却，冷却速度小于等于室温下随炉冷却速度等，可进一步优化晶界相的形成和分布，进而提高矫顽力，最终得到高矫顽力富铈稀土永磁材料。
附图说明
图1为背散射图对比，其中，(a)对比例1的富Ce磁体；(b)实施例1的富Ce磁体；
具体实施方式
下面结合具体实施例对本发明做进一步说明，但本发明并不仅仅局限于以下实施例：
实施例1：
(1)制备两种不同成分的磁粉，以质量百分数计，磁粉1成分为[(Pr0.2Nd0.8)0.5Ce0.5]32FebalZr0.15Cu0.12Al0.2Co0.6B0.9Ga0.5，磁粉2成分为(Pr0.2Nd0.8)32FebalZr0.15Cu0.12Al0. 2Co0.6B0.9Ga0.5，其制备工艺均依次为甩带、氢破和气流磨；
(2)将所得的磁粉1和磁粉2以4:1的质量比均匀混合后，通过普通烧结工艺制备成磁体，烧结温度为1040℃，烧结时间为4h；
(3)将所制备的磁体通过一步热处理，得到高矫顽力富铈稀土永磁材料，一步热处理温度为650℃，一步热处理时间为2h。
AMT-4永磁特性测量仪测试结果显示，烧结态磁体的矫顽力为12.0kOe，热处理态磁体的矫顽力为13.2kOe。
对比例1：
与实施例1的不同之处在于：步骤(1)磁粉的成分不同，降低稀土元素的含量，提高B元素的含量，降低Ga元素的含量，以质量百分数计，磁粉1成分为[(Pr0.2Nd0.8)0.5Ce0.5]31FebalZr0.15Cu0.12Al0.2Co0.6 B1Ga0.1，磁粉2成分为(Pr0.2Nd0.8)31FebalZr0.15Cu0.12Al0.2Co0.6B1Ga0.1。AMT-4永磁特性测量仪测试结果显示，烧结态磁体的矫顽力为8.9kOe，热处理态磁体的矫顽力为10.1kOe，远小于实施例1。
实施例1和对比例1富Ce磁体组织形貌对比如图1所示，本发明设计的磁体，形成大量连续REFe2相以及部分RE6Fe13Ga相，从而削弱甚至是消除主相晶粒间的短程交换耦合作用，提高磁体的矫顽力。
实施例2：
(1)制备磁粉，以质量百分数计，磁粉成分为[(Pr0.3Nd0.7)0.45Ce0.55]32.2FebalNb0.2Cu0.2Al0.3Co0.8B0.85Ga1，其制备工艺依次为甩带、氢破和气流磨；
(2)将所得的磁粉通过普通烧结工艺制备成磁体，烧结温度为1030℃，烧结时间为4.5h；
(3)将所制备的磁体通过一步热处理，得到高矫顽力富铈稀土永磁材料，热处理温度为630℃，热处理时间为2h。
AMT-4永磁特性测量仪测试结果显示，烧结态磁体的矫顽力为10.6kOe，热处理态磁体的矫顽力为12.0kOe。
对比例2：
与实施例2的不同之处在于：步骤(1)磁粉的成分不同，降低稀土元素的含量，提高B元素的含量，不包含Ga元素，以质量百分数计，磁粉成分为[(Pr0.3Nd0.7)0.45Ce0.55]31.6FebalNb0.2Cu0.2Al0.3Co0.8B1。AMT-4永磁特性测量仪测试结果显示，烧结态磁体的矫顽力为6.8kOe，热处理态磁体的矫顽力为7.5kOe，远小于实施例2。
实施例3：
(1)制备磁粉，以质量百分数计，磁粉成分为(Nd0.4Ce0.6)32.5FebalZr0.25Cu0.25Co0. 9B0.85Ga0.65，其制备工艺依次为吸氢、歧化、脱氢和再复合；
(2)将所得的磁粉通过热压热变形工艺制备成磁体，热压温度660℃，压力380MPa，热变形温度为800℃；
(3)所制备的磁体免于热处理，得到高矫顽力富铈稀土永磁材料。
AMT-4永磁特性测量仪测试结果显示，磁体的矫顽力为9.8kOe。
对比例3：
与实施例3的不同之处在于：步骤(1)磁粉的成分不同，降低稀土元素的含量，提高B元素的含量，不包含Ga元素，以质量百分数计，磁粉成分为(Nd0.4Ce0.6)31FebalZr0.25Cu0.25Co0.9B1。AMT-4永磁特性测量仪测试结果显示，磁体的矫顽力为5.8kOe，远小于实施例3。
实施例4：
(1)制备两种不同成分的磁粉，以质量百分数计，磁粉1成分为[(Pr0.1Nd0.9)0.5La0.2Ce0.3]31.5FebalZr0.15Al0.25Cu0.25Ti0.1B0.9Ga0.8，磁粉2成分为(Pr0.1Nd0.9)31.5FebalZr0.15Al0.25Cu0.25Ti0.1B0.9Ga0.8，其制备工艺均依次为甩带、氢破和气流磨；
(2)将所得的磁粉1和磁粉2以3:2的质量比均匀混合后，通过普通烧结工艺制备成磁体，烧结温度为1040℃，烧结时间为3h；
(3)将所制备的磁体通过一步热处理，得到高矫顽力富铈稀土永磁材料，热处理温度为480℃，热处理时间为4h。
AMT-4永磁特性测量仪测试结果显示，烧结态磁体的矫顽力为9.5kOe，热处理态磁体的矫顽力为15.7kOe。
对比例4：
与实施例4的不同之处在于：步骤(1)磁粉的成分不同，降低稀土元素的含量，提高B元素的含量，降低Ga元素的含量，以质量百分数计，磁粉1成分为[(Pr0.1Nd0.9)0.5La0.2Ce0.3]30.5FebalZr0.15Al0.25 Cu0.25Ti0.1B1Ga0.15，磁粉2成分为(Pr0.1Nd0.9)30.5FebalZr0.15Al0.25Cu0.25Ti0.1B1Ga0.15。AMT-4永磁特性测量仪测试结果显示，烧结态磁体的矫顽力为7.5kOe，热处理态磁体的矫顽力为9.6kOe，远小于实施例4。
Claims (8)
1.一种高矫顽力富铈稀土永磁材料的制备方法，其特征在于，包括以下步骤：
(1)制备成分为(A1-aCea)bFebalMcBdGae的磁粉，其中A为稀土元素Nd、Pr、Dy、Tb、La、Y、Gd中的一种或多种，Ce为稀土元素铈，Fe为铁元素，M为合金元素Co、Ni、Al、Cu、Mn、Nb、Zr、Ti、V、Ta中的一种或多种，B为硼元素，Ga为镓元素，以质量百分数计，0.3≤a≤0.7，30≤b≤35，0≤c≤2，0.75≤d≤0.95，0.2≤e≤3；
(2)将所得的磁粉通过烧结或热压热变形工艺制备成磁体；
(3)将所制备的磁体通过热处理，得到高矫顽力富铈稀土永磁材料。
2.根据权利要求1所述的制备方法，其特征在于，步骤(1)中磁粉的制备工艺包括：
(1)依次为甩带、氢破和气流磨；
(2)依次为快淬带和氢破；
(3)依次为吸氢、歧化、脱氢和再复合。
3.根据权利要求1所述的制备方法，其特征在于，步骤(1)中的磁粉，通过单主相的方法直接得到或通过多主相的方法得到最终限定的成分。
4.根据权利要求1所述的制备方法，其特征在于，步骤(2)中的烧结工艺包括：普通烧结工艺或放电等离子烧结工艺或微波烧结工艺。
5.根据权利要求1所述的制备方法，在特征在于，步骤(3)中的热处理工艺包括：一步热处理或两步热处理或在步骤(2)烧结或热压热变形后慢速冷却。
6.根据权利要求5所述的制备方法，其特征在于，一步热处理的热处理温度为：400～800℃，热处理时间为：0.5h～5h。
7.根据权利要求5所述的制备方法，其特征在于，两步热处理中的第一步热处理温度为：850～950℃，热处理时间为：0.5h～4h；第二步热处理温度为：400～600℃，热处理时间为：0.5h～5h。
8.根据权利要求5所述的制备方法，其特征在于，烧结或热压热变形后的冷却速度小于等于室温下随炉冷却速度。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210392116.9A CN114823113A (zh) | 2022-04-14 | 2022-04-14 | 一种高矫顽力富铈稀土永磁材料的制备方法 |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210392116.9A CN114823113A (zh) | 2022-04-14 | 2022-04-14 | 一种高矫顽力富铈稀土永磁材料的制备方法 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN114823113A true CN114823113A (zh) | 2022-07-29 |
Family
ID=82537345
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202210392116.9A Pending CN114823113A (zh) | 2022-04-14 | 2022-04-14 | 一种高矫顽力富铈稀土永磁材料的制备方法 |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN114823113A (zh) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115274242A (zh) * | 2022-08-30 | 2022-11-01 | 烟台东星磁性材料股份有限公司 | 铈添加re-t-b-m系烧结钕铁硼磁体 |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH09165601A (ja) * | 1995-12-12 | 1997-06-24 | Sumitomo Special Metals Co Ltd | 永久磁石用異方性希土類合金粉末及び異方性ボンド磁石の製造方法 |
| CN102800454A (zh) * | 2012-08-30 | 2012-11-28 | 钢铁研究总院 | 低成本双主相Ce永磁合金及其制备方法 |
| CN105427995A (zh) * | 2015-12-21 | 2016-03-23 | 浙江凯文磁业有限公司 | 一种有机重稀土配合物增强烧结钕铁硼矫顽力的制备方法 |
| CN106710768A (zh) * | 2016-12-27 | 2017-05-24 | 浙江大学 | 一种添加氢化钕提高钕铈铁硼烧结磁体矫顽力的方法 |
| CN106910613A (zh) * | 2017-01-13 | 2017-06-30 | 浙江大学 | 一步热处理技术生产高Ce含量稀土永磁的方法 |
| CN108922714A (zh) * | 2018-08-29 | 2018-11-30 | 南京理工大学 | 一种高矫顽力钕铈铁硼烧结磁体的制备方法 |
| CN110148507A (zh) * | 2019-05-23 | 2019-08-20 | 钢铁研究总院 | 一种含REFe2相的晶界扩散铈磁体及其制备方法 |
| CN113223849A (zh) * | 2021-05-20 | 2021-08-06 | 中国科学院宁波材料技术与工程研究所 | 一种高性能高丰度稀土铁硼永磁材料及其制备方法 |
-
2022
- 2022-04-14 CN CN202210392116.9A patent/CN114823113A/zh active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH09165601A (ja) * | 1995-12-12 | 1997-06-24 | Sumitomo Special Metals Co Ltd | 永久磁石用異方性希土類合金粉末及び異方性ボンド磁石の製造方法 |
| CN102800454A (zh) * | 2012-08-30 | 2012-11-28 | 钢铁研究总院 | 低成本双主相Ce永磁合金及其制备方法 |
| CN105427995A (zh) * | 2015-12-21 | 2016-03-23 | 浙江凯文磁业有限公司 | 一种有机重稀土配合物增强烧结钕铁硼矫顽力的制备方法 |
| CN106710768A (zh) * | 2016-12-27 | 2017-05-24 | 浙江大学 | 一种添加氢化钕提高钕铈铁硼烧结磁体矫顽力的方法 |
| CN106910613A (zh) * | 2017-01-13 | 2017-06-30 | 浙江大学 | 一步热处理技术生产高Ce含量稀土永磁的方法 |
| CN108922714A (zh) * | 2018-08-29 | 2018-11-30 | 南京理工大学 | 一种高矫顽力钕铈铁硼烧结磁体的制备方法 |
| CN110148507A (zh) * | 2019-05-23 | 2019-08-20 | 钢铁研究总院 | 一种含REFe2相的晶界扩散铈磁体及其制备方法 |
| CN113223849A (zh) * | 2021-05-20 | 2021-08-06 | 中国科学院宁波材料技术与工程研究所 | 一种高性能高丰度稀土铁硼永磁材料及其制备方法 |
Non-Patent Citations (1)
| Title |
|---|
| 严密 等: "新型富La/Ce多主相稀土永磁材料研究", 金属功能材料, vol. 25, no. 1, 28 February 2018 (2018-02-28), pages 1 - 9 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115274242A (zh) * | 2022-08-30 | 2022-11-01 | 烟台东星磁性材料股份有限公司 | 铈添加re-t-b-m系烧结钕铁硼磁体 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| JP6366666B2 (ja) | 重希土類元素を含まない焼結Ｎｄ−Ｆｅ−Ｂ磁性体の製造方法 | |
| CN101364465B (zh) | 稀土永磁材料及其制备方法 | |
| CN111210963B (zh) | 高性能钇铈基稀土永磁体及制备方法 | |
| CN107275027B (zh) | 应用钇的富铈稀土永磁体及其制备方法 | |
| CN111091944B (zh) | 一种富镧铈钇多主相细晶稀土永磁材料及其制备方法 | |
| CN110931197B (zh) | 一种用于高丰度稀土永磁体的扩散源 | |
| CN105990019A (zh) | 一种低重稀土烧结钕铁硼的制备方法 | |
| CN103056370A (zh) | 一种提高烧结钕铁硼磁材料矫顽力的方法 | |
| CN104681268A (zh) | 一种提高烧结钕铁硼磁体矫顽力的处理方法 | |
| CN104575920A (zh) | 稀土永磁体及其制备方法 | |
| CN113593873A (zh) | 一种高矫顽力混合稀土永磁材料及其制备方法 | |
| US20220319773A1 (en) | Grain boundary diffusion method for bulk rare earth permanent magnetic material | |
| CN116612956A (zh) | 一种具有核壳结构的含铈钕铁硼磁体及其制备方法和应用 | |
| CN114210976B (zh) | 一种烧结钕铁硼双合金结合晶界扩散的方法 | |
| CN114823113A (zh) | 一种高矫顽力富铈稀土永磁材料的制备方法 | |
| CN109594023B (zh) | 一种短流程Ce-Fe基烧结永磁体及其制备方法 | |
| CN112259314B (zh) | 一种R(Fe,M)12型的稀土永磁材料及其制备方法 | |
| CN114678182B (zh) | 一种低成本高性能多主相稀土永磁材料及其制备方法 | |
| CN116564639A (zh) | 一种同时提高多主相LaCe基烧结永磁材料剩磁和矫顽力的方法 | |
| CN114196864B (zh) | 一种Y-Gd基合金及包括该基合金的钕铈铁硼磁体与制备方法 | |
| CN114255951B (zh) | 高性能烧结钕铁硼磁体及其制备方法 | |
| CN113782292B (zh) | 一种具有改进温度稳定性的钇铈基稀土永磁材料 | |
| CN102208238B (zh) | 一种无钕无铽高矫顽力烧结稀土永磁体及其制备方法 | |
| CN114464443A (zh) | 一种同时提高多主相LaCe基烧结永磁材料矫顽力和耐腐蚀性的方法 | |
| CN111952031B (zh) | 含Al磁硬化层结构的低成本耐热烧结含Ce磁体及制备方法 |
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 |