CN117275864A - 一种高性能钕铁硼磁体的制备方法和应用 - Google Patents
一种高性能钕铁硼磁体的制备方法和应用 Download PDFInfo
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- CN117275864A CN117275864A CN202311291591.8A CN202311291591A CN117275864A CN 117275864 A CN117275864 A CN 117275864A CN 202311291591 A CN202311291591 A CN 202311291591A CN 117275864 A CN117275864 A CN 117275864A
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- 229910001172 neodymium magnet Inorganic materials 0.000 title claims abstract description 67
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 229920001971 elastomer Polymers 0.000 claims abstract description 32
- 239000000843 powder Substances 0.000 claims abstract description 18
- 239000001257 hydrogen Substances 0.000 claims abstract description 17
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 17
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000003963 antioxidant agent Substances 0.000 claims abstract description 15
- 230000003078 antioxidant effect Effects 0.000 claims abstract description 15
- 239000000314 lubricant Substances 0.000 claims abstract description 15
- QJVKUMXDEUEQLH-UHFFFAOYSA-N [B].[Fe].[Nd] Chemical compound [B].[Fe].[Nd] QJVKUMXDEUEQLH-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000000034 method Methods 0.000 claims abstract description 13
- 229920006000 epoxidized styrene-butadiene-styrene block copolymer Polymers 0.000 claims abstract description 12
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- 238000005266 casting Methods 0.000 claims description 12
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- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- 238000003723 Smelting Methods 0.000 claims description 8
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims description 6
- 238000000227 grinding Methods 0.000 claims description 6
- HQKMJHAJHXVSDF-UHFFFAOYSA-L magnesium stearate Chemical compound [Mg+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O HQKMJHAJHXVSDF-UHFFFAOYSA-L 0.000 claims description 6
- 239000002994 raw material Substances 0.000 claims description 6
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- 229910052802 copper Inorganic materials 0.000 claims description 5
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 5
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 5
- 239000010935 stainless steel Substances 0.000 claims description 5
- 229910001220 stainless steel Inorganic materials 0.000 claims description 5
- 239000008117 stearic acid Substances 0.000 claims description 5
- 239000011701 zinc Substances 0.000 claims description 5
- 239000011787 zinc oxide Substances 0.000 claims description 5
- 230000005415 magnetization Effects 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 4
- 229910052751 metal Inorganic materials 0.000 claims description 4
- 239000002184 metal Substances 0.000 claims description 4
- NLZUEZXRPGMBCV-UHFFFAOYSA-N Butylhydroxytoluene Chemical compound CC1=CC(C(C)(C)C)=C(O)C(C(C)(C)C)=C1 NLZUEZXRPGMBCV-UHFFFAOYSA-N 0.000 claims description 3
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 3
- BGNXCDMCOKJUMV-UHFFFAOYSA-N Tert-Butylhydroquinone Chemical compound CC(C)(C)C1=CC(O)=CC=C1O BGNXCDMCOKJUMV-UHFFFAOYSA-N 0.000 claims description 3
- CEGOLXSVJUTHNZ-UHFFFAOYSA-K aluminium tristearate Chemical compound [Al+3].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O CEGOLXSVJUTHNZ-UHFFFAOYSA-K 0.000 claims description 3
- 229940063655 aluminum stearate Drugs 0.000 claims description 3
- CZBZUDVBLSSABA-UHFFFAOYSA-N butylated hydroxyanisole Chemical compound COC1=CC=C(O)C(C(C)(C)C)=C1.COC1=CC=C(O)C=C1C(C)(C)C CZBZUDVBLSSABA-UHFFFAOYSA-N 0.000 claims description 3
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- 235000019359 magnesium stearate Nutrition 0.000 claims description 3
- 229910000077 silane Inorganic materials 0.000 claims description 3
- 239000004250 tert-Butylhydroquinone Substances 0.000 claims description 3
- 235000019281 tert-butylhydroquinone Nutrition 0.000 claims description 3
- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical compound [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 claims description 3
- 239000002480 mineral oil Substances 0.000 claims description 2
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- 229910052779 Neodymium Inorganic materials 0.000 abstract description 4
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- QEFYFXOXNSNQGX-UHFFFAOYSA-N neodymium atom Chemical compound [Nd] QEFYFXOXNSNQGX-UHFFFAOYSA-N 0.000 abstract description 4
- 229910052726 zirconium Inorganic materials 0.000 abstract description 4
- 239000006087 Silane Coupling Agent Substances 0.000 abstract description 3
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- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
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- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 2
- 229910052758 niobium Inorganic materials 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
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- 238000006467 substitution reaction Methods 0.000 description 2
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 1
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 description 1
- 239000004593 Epoxy Substances 0.000 description 1
- 229910017493 Nd 2 O 3 Inorganic materials 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 230000002159 abnormal effect Effects 0.000 description 1
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- 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
- H01F1/0573—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 obtained by reduction or by hydrogen decrepitation or embrittlement
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- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/023—Hydrogen absorption
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C33/04—Making ferrous alloys by melting
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- C22C38/002—Ferrous alloys, e.g. steel alloys containing In, Mg, or other elements not provided for in one single group C22C38/001 - C22C38/60
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- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
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- 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
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Abstract
本发明涉及钕铁硼磁体技术领域,且公开了一种高性能钕铁硼磁体的制备方法和应用,加入适量Zr、Nb、Dy等调节钕铁硼磁体的组成,使晶粒均匀化、规则化;抗氧化剂和润滑剂的添加,减少钕的氧化,改善磁体在高温下的使用性能;采用速凝铸带工艺促进富钕相的弥散分布,提高磁体的取向度;采用氢破碎工艺技术,使铸锭粉化而得到微粉,降低磁粉被氧化的程度;采用垂直取向压制成型,提高了磁稳定性;利用硅烷偶联剂对磁粉表面进行改性,偶联剂的一端与磁粉表面的羟基发生键联,另一端与环氧化SBS、硅橡胶和其他助剂混炼交联,相互缠绕形成相互贯穿网络结构,提高橡胶力学性能的同时也提高了橡胶的磁性能。
Description
技术领域
本发明涉及钕铁硼磁体技术领域,具体为一种高性能钕铁硼磁体的制备方法和应用。
背景技术
钕铁硼磁体作为第三代稀土永磁材料,其优点是性价比高,体积小、重量轻、良好的机械特性和磁性强,适用于制造各种高性能、形状复杂的产品,成为许多现代工业技术中不可缺少的关键基础支撑材料,随着信息技术的快速发展,为钕铁硼产业带来更为广阔的市场前景,但是目前在市面上钕铁硼材料制备工艺复杂,不易用于广泛生产。
烧结钕铁硼磁体的组织结构导致其自身容易氧化,因此需要对磁体的表面进行处理,以提高耐氧化能力,现有技术多采用磁控溅射镀、混合镀层和磁控溅射镀,但是存在步骤繁琐,设备结构要求高的问题,且镀层和磁体的结合力比较差;另外磁粉的粒径一致性对磁粉质量和烧结磁体的各方面性能有很重要的影响,大颗粒混入到磁粉中会严重影响磁粉的质量和烧结磁体的各方面性能,不仅降低了钕铁硼粉料的成材率,浪费了稀土资源,还提高了生产成本。本发明通过优化磁体成分组成、改善制粉工艺和成型技术,克服了易氧化的问题,提高了钕铁硼磁体的综合性能。
磁性橡胶是一种新型的高分子复合材料,它将磁性材料颗粒填充到橡胶中,再用传统的橡胶加工方法进行加工成型,与传统的磁性材料相比,磁性橡胶具有密度小、抗腐蚀性好等,在电机、驱动器与强力磁铁等领域应用广泛;但是钕铁硼磁粉与橡胶有机基体之间的相容性差,导致橡胶磁在使用过程中器件易产生性能损伤或不稳定性等。本发明通过对钕铁硼磁体表面进行改性,在界面处通过化学反应形成了化学键,与橡胶的大分子链发生交联,从而提高了橡胶磁的力学性能和磁性能,拓展了其应用范围。
发明内容
(一)解决的技术问题
针对现有技术的不足,本发明提供了一种高性能钕铁硼磁体的制备方法和应用,克服了现有技术制备的钕铁硼磁体易氧化和矫顽力低的问题,同时进一步提高了橡胶的磁性和力学性能。
(二)技术方案
一种高性能钕铁硼磁体的制备方法,所述钕铁硼磁体中各成分由以下质量百分比组成,18-25%Nd、4.2-6.6%Pr、0.5-2.4%Dy、60-75%Fe、0.2-0.8%Co、0.8-2.2%B、0.06-0.11%Nb、0.1-0.5%Zr、0.4-1.5%Al和0.3-0.9%Zn;所述制备方法按以下步骤进行:
(1)将上述成分配置好的原料放入真空速凝熔炼炉,真空抽至0.01-0.03Pa,在1400-1500℃下进行熔炼,然后将熔融的金属液浇注到旋转的水冷铜辊轮上,在一定的辊轮转速下,获得一定厚度的速凝铸片。
(2)将步骤(1)中的速凝铸片放入不锈钢氢爆罐中,加入0.02-0.11%的抗氧化剂和0.03-0.08%的润滑剂,在180-220℃、压力为0.1-0.3MPa的氢气压力下吸氢1-3h,然后加热至400-600℃脱氢5-8h,气流磨制成粒径为3.5-4.5μm的粉末,得到高性能钕铁硼磁体。
进一步的,所述步骤(1)中辊轮转速为1.2-3.5m/s,铸片厚度为0.1-0.5mm。
进一步的,所述步骤(2)中抗氧化剂为2,6-二叔丁基对甲酚、叔丁基氢醌或丁基羟基茴香醚中的任意一种。
进一步的,所述步骤(2)中所述润滑剂为硬脂酸锌、硬脂酸铝、硬酯酸镁或矿物油中的任意一种。
一种如权利要求1-4任一项所述的制备方法得到的高性能钕铁硼磁体在橡胶中的应用,制备方法如下:
S1、将(3-氨基丙基)三乙氧基硅烷溶于乙醇中,搅拌稀释,将高性能钕铁硼磁体粉末加入到硅烷稀释液中,在20-35℃下搅拌分散,静置,在50-60℃下烘干,得到改性高性能钕铁硼磁体。
S2、向开炼机中加入环氧化SBS、硅橡胶、氧化锌、硬脂酸、改性高性能钕铁硼磁体、DM促进剂和TT促进剂,混炼均匀,在平板硫化机上进行硫化,硫化温度为140-160℃,硫化压力为8-12MPa,硫化时间为20-40min,接着在磁化场下进行充磁,得到高性能钕铁硼磁性橡胶。
进一步的,所述步骤S1中(3-氨基丙基)三乙氧基硅烷的质量为钕铁硼磁体粉末质量的1.5-3.5%。
进一步的,各添加物按重量份计,环氧化SBS为15-25份、硅橡胶为40-60份、氧化锌为3-6份,硬脂酸为1-3份,高性能的钕铁硼磁体为4-15份,DM促进剂为2-4份、TT促进剂为0.2-0.8份。
进一步的,磁化场强度为1300-1400kA/m,充磁时间为25-45min。
(三)有益的技术效果
本发明主要通过以下方法制备高性能钕铁硼磁体:(1)通过加入适量的合金成分如Zr、Nb等调节钕铁硼磁体的组成,使晶粒均匀化、规则化,降低材料内部的散磁场;加入抗氧化剂和润滑剂,减少钕的氧化,显著降低磁通不可逆损失,使得磁体在高温下的使用性能明显改善;(2)采用速凝铸带工艺促进富钕相的弥散分布,并使晶粒得到细化,对提高烧结钕铁硼磁体的取向度十分有利;(3)改善制粉工艺,采用氢破碎工艺技术,利用稀土永磁合金的吸氢、放氢特性,使铸锭粉化而得到微粉,降低磁粉被氧化的程度;(4)改进磁粉的烧结工艺,采用垂直取向压制成型,使得磁粉在各个方向受力差异不大,提高磁取向度,得到高性能钕铁硼体;(5)采用(3-氨基丙基)三乙氧基硅烷对磁粉表面进行改性,磁粉表面的羟基与偶联剂的硅氢键发生键联,另外一端的氨基再与环氧化SBS、硅橡胶和其他助剂混炼交联,得到高性能钕铁硼磁性橡胶。
适量硅烷偶联剂的加入能增加磁体的抗氧化能力和尺寸稳定性,在钕铁硼磁粉和环氧化SBS之间起到了“分子桥”的作用,将相容性差的两种物质在界面处通过化学反应形成了化学键,使环氧化SBS的大分子链发生交联,同时环氧化SBS与硅橡胶相容性较好,三者之间相互缠绕形成相互贯穿网络结构;钕铁硼磁粉和橡胶混炼时,橡胶的流动性好,能够充分浸润磁粉的表面,缩短了橡胶的混炼时间,防止橡胶基体出现早期硫化的现象,在提高材料力学性能的同时使材料的磁性能也得到一定的提高。
具体实施方式
下面将结合本发明实施例,对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例仅仅是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有作出创造性劳动前提下所获得的所有其他实施例,都涉及本发明保护的范围。
环氧化SBS的制备:在装有回流冷凝管、滴液漏斗的烧瓶中加入质量浓度为1g的SBS和10mL环己烷,待SBS完全溶解后,加入0.5g甲酸和0.3g过氧化氢,在70℃下反应3h,反应结束后,乙醇沉降,洗涤,得到环氧化SBS。
实施例1
(1)将按质量百分比的22%Nd、5.2%Pr、0.5%Dy、63%Fe、0.4%Co、2.1%B、0.06%Nb、0.1%Zr、0.8%Al和0.6%Zn配置好的原料放入真空速凝熔炼炉,真空抽至0.02Pa,在1450℃下进行熔炼,然后将熔融的金属液浇注到旋转的水冷铜辊轮上,辊轮转速为2.5m/s,获得厚度为0.3mm速凝铸片。
(2)将步骤(1)中的速凝铸片放入不锈钢氢爆罐中,加入0.03%丁基羟基茴香醚和0.05%的硬酯酸镁,在210℃、压力为0.3MPa的氢气压力下吸氢3h,然后加热至550℃脱氢7h,气流磨制成粒径为4.0μm的粉末,得到高性能钕铁硼磁体。
实施例2
本实施例与实施例1的区别在于,步骤(1)中Nb的质量百分比为0.07%、Zr的质量百分比为0.2%,其他条件保持一致。
实施例3
本实施例与实施例1的区别在于,步骤(1)中Nb的质量百分比为0.08%、Zr的质量百分比为0.3%,其他条件保持一致。
实施例4
本实施例与实施例1的区别在于,步骤(1)中Nb的质量百分比为0.09%、Zr的质量百分比为0.4%,其他条件保持一致。
实施例5
本实施例与实施例1的区别在于,步骤(1)中Nb的质量百分比为0.11%、Zr的质量百分比为0.5%,其他条件保持一致。
对比例1
本对比例与实施例1的区别在于,步骤(1)中不加入Nb和Zr,其他条件保持一致。
测试样品制备:钕铁硼磁体粉末置于磁场强度为2.0T的磁场中垂直取向压制成型,放入真空烧结炉中,在1100℃烧结4h结,接着在900℃下进行一次回火,保温3h,在700℃进行二次回火,保温6h,采用磁性材料测量系统测试材料磁性能。
矫顽力(kA/m) | 最大磁能积(kJ/m3) | |
实施例1 | 312.3 | 851.6 |
实施例2 | 325.1 | 880.1 |
实施例3 | 370.2 | 1010.8 |
实施例4 | 365.6 | 1048.5 |
实施例5 | 356.9 | 1020.2 |
对比例1 | 280.1 | 721.3 |
磁能积越大,产生同样效果时所需磁材料越少;矫顽力代表磁性材料抵抗退磁的能力,数值越大,耐温性能越好;添加合金元素对材料进行性能优化是一种最为常见的材料改性的方法,由上表测试数据可知,随着Zr元素和Nb元素含量的增加,矫顽力和最大磁能积得到一定程度的提高,而且提高幅度较明显,这是因为Zr元素和Nb元素的加入降低了钕铁硼磁体对烧结温度的敏感性,提高了磁体的耐烧结温度,在1100℃的烧结温度下,磁体的磁性能差异性较小,并且不会发生晶粒的异常长大,复合添加Zr和Nb克服了烧结炉内温度场分布不均匀而引起的磁体性能稳定性差的问题,起到细化晶粒,提高晶粒间的浸润性的作用,最终制备了高磁能积且性能稳定的磁体。
实施例6
(1)将按质量百分比的24%Nd、6.4%Pr、1.3%Dy、65%Fe、0.5%Co、1.8%B、0.09%Nb、0.4%Zr、0.9%Al和0.6%Zn配置好的原料放入真空速凝熔炼炉,真空抽至0.03Pa,在1500℃下进行熔炼,然后将熔融的金属液浇注到旋转的水冷铜辊轮上,辊轮转速为3.2m/s,获得厚度为0.2mm速凝铸片。
(2)将步骤(1)中的速凝铸片放入不锈钢氢爆罐中,加入0.02%的抗氧化剂2,6-二叔丁基对甲酚和0.03%的润滑剂硬脂酸锌,在190℃、压力为0.3MPa的氢气压力下吸氢3h,然后加热至500℃脱氢6h,气流磨制成粒径为3.5μm的粉末,得到高性能钕铁硼磁体。
实施例7
本实施例与实施例6的区别在于,步骤(2)中抗氧化剂的质量百分比为0.04%,润滑剂的质量百分比为0.04%,其他条件保持一致。
实施例8
本实施例与实施例6的区别在于,步骤(2)中抗氧化剂的质量百分比为0.06%,润滑剂的质量百分比为0.05%,其他条件保持一致。
实施例9
本实施例与实施例6的区别在于,步骤(2)中抗氧化剂的质量百分比为0.08%,润滑剂的质量百分比为0.06%,其他条件保持一致。
实施例10
本实施例与实施例6的区别在于,步骤(2)中抗氧化剂的质量百分比为0.11%,润滑剂的质量百分比为0.08%,其他条件保持一致。
对比例2
本对比例与实施例6的区别在于,步骤(2)中不加入抗氧化剂和润滑剂,其他条件保持一致。
剩余磁通密度(T) | |
实施例6 | 1.350 |
实施例7 | 1.364 |
实施例8 | 1.372 |
实施例9 | 1.385 |
实施例10 | 1.426 |
对比例2 | 1.208 |
钕铁硼永磁粉末颗粒的流动性较差,在磨粉过程中,钕铁硼磁体中富Nd相易被氧化形成Nd2O3,它的含量越多,永磁体的剩余磁通密度下降越大。由上表测试数据可知,随着磁体中抗氧化剂和润滑剂含量的增多,剩余磁通密度逐渐增大,对比例2未加入抗氧化剂和润滑剂,其剩余磁通密度为1.208T,而实施例10的剩余磁通密度为1.426T,这是因为磨粉过程中添加的抗氧化剂,能在粉末颗粒的表面形成一层保护膜,有效地防止了粉末进一步氧化,使磁体中Nd2O3的含量降到最少,另外润滑剂的添加使得磁性颗粒转动阻力减少,减少粉末颗粒之间的摩擦,粉末取向度提高,磁体剩磁得到提高,永磁体最终磁性能也得到提升。
实施例11
(1)将按质量百分比的25%Nd、4.6%Pr、1.9%Dy、71%Fe、0.7%Co、1.5%B、0.09%Nb、0.4%Zr、1.5%Al和0.9%Zn配置好的原料放入真空速凝熔炼炉,真空抽至0.01Pa,在1400℃下进行熔炼,然后将熔融的金属液浇注到旋转的水冷铜辊轮上,辊轮转速为2.6m/s,获得厚度为0.2mm速凝铸片。
(2)将步骤(1)中的速凝铸片放入不锈钢氢爆罐中,加入0.09%的叔丁基氢醌和0.08%的硬脂酸铝,在200℃、压力为0.3MPa的氢气压力下吸氢3h,然后加热至480℃脱氢6h,气流磨制成粒径为4.5μm的粉末,得到高性能钕铁硼磁体。
(3)将0.25g的(3-氨基丙基)三乙氧基硅烷溶于乙醇中,搅拌稀释,将10g高性能钕铁硼磁体粉末加入到硅烷稀释液中,在30℃下搅拌分散,静置,在50℃下烘干,得到改性高性能钕铁硼磁体。
(4)向开炼机中加入20g环氧化SBS、55g硅橡胶、5g氧化锌、2g硬脂酸、4g改性高性能钕铁硼磁体、3g的DM促进剂和0.5g的TT促进剂,混炼均匀,在平板硫化机上进行硫化,硫化温度为150℃,硫化压力为10MPa,硫化时间为30min,接着在磁化场强度为1350kA/m下充磁35min,得到高性能钕铁硼磁性橡胶。
实施例12
本实施例与实施例11的区别在于,步骤(4)中改性高性能钕铁硼磁体的质量为7g,其他条件保持一致。
实施例13
本实施例与实施例11的区别在于,步骤(4)中改性高性能钕铁硼磁体的质量为10g,其他条件保持一致。
实施例14
本实施例与实施例11的区别在于,步骤(4)中改性高性能钕铁硼磁体的质量为12g,其他条件保持一致。
实施例15
本实施例与实施例11的区别在于,步骤(4)中改性高性能钕铁硼磁体的质量为15g,其他条件保持一致。
由上表测试数据可知,随着磁性橡胶复合材料中改性高性能钕铁硼磁体填充量的增加,剩余磁通密度和矫顽力逐渐增大,这是因为硅烷偶联剂改性后的高性能钕铁硼磁体表面的氨基与在环氧SBS发生化学交联,促进在基体中的分散,从而避免了在加工的过程中由于磁粉局部密度过大引起的加工硬化、磁粉损伤导致性能下降等一系列的问题,保证了磁体较高的密度和磁性能。
橡胶的硬度实质上是橡胶抵抗外界压力的能力,它反映了橡胶网状结构在外力作用下的抗变形能力。由于橡胶本身的硬度高,加之钕铁硼作为稀土化合物,能够增加体系交联密度和粘度,提高分子间作用力,使材料的硬度有所提高;钕铁硼磁粉在和橡胶混炼时,橡胶的流动性好,能够充分浸润磁粉的表面,这在提高材料力学性能的同时使材料的磁性能也得到一定的提高,另一方面也缩短了橡胶的混炼时间,防止橡胶基体出现早期硫化的现象,提高了加工的安全性。
以上所述,仅为本申请的具体实施方式,但本申请的保护范围并不局限于此,任何熟悉本技术领域的技术人员在本申请揭露的技术范围内,可轻易想到变化或替换,都应涵盖在本申请的保护范围之内。因此,本申请的保护范围应以所述权利要求的保护范围为准。
Claims (8)
1.一种高性能钕铁硼磁体的制备方法,其特征在于,所述钕铁硼磁体中各成分由以下质量百分比组成,18-25%Nd、4.2-6.6%Pr、0.5-2.4%Dy、60-75%Fe、0.2-0.8%Co、0.8-2.2%B、0.06-0.11%Nb、0.1-0.5%Zr、0.4-1.5%Al和0.3-0.9%Zn;所述制备方法按以下步骤进行:
(1)将上述成分配置好的原料放入真空速凝熔炼炉,真空抽至0.01-0.03Pa,在1400-1500℃下进行熔炼,然后将熔融的金属液浇注到旋转的水冷铜辊轮上,在一定的辊轮转速下,获得一定厚度的速凝铸片;
(2)将步骤(1)中的速凝铸片放入不锈钢氢爆罐中,加入0.02-0.11%的抗氧化剂和0.03-0.08%的润滑剂,在180-220℃、压力为0.1-0.3MPa的氢气压力下吸氢1-3h,然后加热至400-600℃脱氢5-8h,气流磨制成粒径为3.5-4.5μm的粉末,得到高性能钕铁硼磁体。
2.根据权利要求1所述的高性能钕铁硼磁体的制备方法,其特征在于,所述步骤(1)中辊轮转速为1.2-3.5m/s,铸片厚度为0.1-0.5mm。
3.根据权利要求1所述的高性能钕铁硼磁体的制备方法,其特征在于,所述步骤(2)中抗氧化剂为2,6-二叔丁基对甲酚、叔丁基氢醌或丁基羟基茴香醚中的任意一种。
4.根据权利要求1所述的高性能钕铁硼磁体的制备方法,其特征在于,所述步骤(2)中所述润滑剂为硬脂酸锌、硬脂酸铝、硬酯酸镁或矿物油中的任意一种。
5.一种如权利要求1-4任一项所述的制备方法得到的高性能钕铁硼磁体在橡胶中的应用,其特征在于,制备方法如下:
S1、将(3-氨基丙基)三乙氧基硅烷溶于乙醇中,搅拌稀释,将高性能钕铁硼磁体粉末加入到硅烷稀释液中,在20-35℃下搅拌分散,静置,在50-60℃下烘干,得到改性高性能钕铁硼磁体;
S2、向开炼机中加入环氧化SBS、硅橡胶、氧化锌、硬脂酸、改性高性能钕铁硼磁体、DM促进剂和TT促进剂,混炼均匀,在平板硫化机上进行硫化,硫化温度为140-160℃,硫化压力为8-12MPa,硫化时间为20-40min,接着在磁化场下进行充磁,得到高性能钕铁硼磁性橡胶。
6.根据权利要求5所述的高性能钕铁硼磁体在橡胶中的应用,其特征在于,所述步骤S1中(3-氨基丙基)三乙氧基硅烷的质量为钕铁硼磁体粉末质量的1.5-3.5%。
7.根据权利要求5所述的高性能钕铁硼磁体在橡胶中的应用,其特征在于,各添加物按重量份计,环氧化SBS为15-25份、硅橡胶为40-60份、氧化锌为3-6份,硬脂酸为1-3份,高性能的钕铁硼磁体为4-15份,DM促进剂为2-4份、TT促进剂为0.2-0.8份。
8.根据权利要求5所述的高性能钕铁硼磁体在橡胶中的应用,其特征在于,磁化场强度为1300-1400kA/m,充磁时间为25-45min。
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