CN111933374B - 一种烧结钕铁硼永磁材料及其制备方法 - Google Patents
一种烧结钕铁硼永磁材料及其制备方法 Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 38
- 229910001172 neodymium magnet Inorganic materials 0.000 title claims abstract description 37
- 238000002360 preparation method Methods 0.000 title abstract description 9
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 39
- 229910000676 Si alloy Inorganic materials 0.000 claims abstract description 23
- CSDREXVUYHZDNP-UHFFFAOYSA-N alumanylidynesilicon Chemical compound [Al].[Si] CSDREXVUYHZDNP-UHFFFAOYSA-N 0.000 claims abstract description 23
- BAFKVXDNLXTDDD-UHFFFAOYSA-N aluminum rhenium Chemical compound [Al].[Re] BAFKVXDNLXTDDD-UHFFFAOYSA-N 0.000 claims abstract description 23
- 229910000691 Re alloy Inorganic materials 0.000 claims abstract description 22
- AYIZIASFKOYHAN-UHFFFAOYSA-N [Fe].[Pr] Chemical compound [Fe].[Pr] AYIZIASFKOYHAN-UHFFFAOYSA-N 0.000 claims abstract description 22
- QYHKLBKLFBZGAI-UHFFFAOYSA-N boron magnesium Chemical compound [B].[Mg] QYHKLBKLFBZGAI-UHFFFAOYSA-N 0.000 claims abstract description 22
- ZAUUZASCMSWKGX-UHFFFAOYSA-N manganese nickel Chemical compound [Mn].[Ni] ZAUUZASCMSWKGX-UHFFFAOYSA-N 0.000 claims abstract description 22
- JLMHVMIMUYHBRQ-UHFFFAOYSA-N neodymium zinc Chemical compound [Zn].[Nd] JLMHVMIMUYHBRQ-UHFFFAOYSA-N 0.000 claims abstract description 22
- 229910000640 Fe alloy Inorganic materials 0.000 claims abstract description 21
- 229910000861 Mg alloy Inorganic materials 0.000 claims abstract description 21
- 229910000583 Nd alloy Inorganic materials 0.000 claims abstract description 21
- 229910000990 Ni alloy Inorganic materials 0.000 claims abstract description 21
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 21
- 239000000956 alloy Substances 0.000 claims abstract description 21
- 230000001681 protective effect Effects 0.000 claims abstract description 19
- YXTPWUNVHCYOSP-UHFFFAOYSA-N bis($l^{2}-silanylidene)molybdenum Chemical compound [Si]=[Mo]=[Si] YXTPWUNVHCYOSP-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229910021343 molybdenum disilicide Inorganic materials 0.000 claims abstract description 18
- 239000002994 raw material Substances 0.000 claims abstract description 17
- ZRBFEDMQRDRUDG-UHFFFAOYSA-N silicon hexaboride Chemical compound B12B3[Si]45B3B2B4B51 ZRBFEDMQRDRUDG-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000000696 magnetic material Substances 0.000 claims abstract description 9
- QJVKUMXDEUEQLH-UHFFFAOYSA-N [B].[Fe].[Nd] Chemical compound [B].[Fe].[Nd] QJVKUMXDEUEQLH-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000004544 sputter deposition Methods 0.000 claims description 25
- 239000000843 powder Substances 0.000 claims description 22
- 238000002156 mixing Methods 0.000 claims description 19
- 238000010438 heat treatment Methods 0.000 claims description 15
- 239000000758 substrate Substances 0.000 claims description 15
- 229910052743 krypton Inorganic materials 0.000 claims description 14
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 12
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 12
- 229910052710 silicon Inorganic materials 0.000 claims description 12
- 239000010703 silicon Substances 0.000 claims description 12
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 11
- 229910052742 iron Inorganic materials 0.000 claims description 11
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 10
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 10
- 229910052782 aluminium Inorganic materials 0.000 claims description 10
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical group [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 10
- 239000001257 hydrogen Substances 0.000 claims description 10
- 229910052739 hydrogen Inorganic materials 0.000 claims description 10
- 230000001105 regulatory effect Effects 0.000 claims description 10
- 238000005266 casting Methods 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 7
- DNNSSWSSYDEUBZ-UHFFFAOYSA-N krypton atom Chemical compound [Kr] DNNSSWSSYDEUBZ-UHFFFAOYSA-N 0.000 claims description 7
- -1 krypton ions Chemical class 0.000 claims description 7
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 6
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 6
- 238000000748 compression moulding Methods 0.000 claims description 6
- 229910052759 nickel Inorganic materials 0.000 claims description 6
- 229910052697 platinum Inorganic materials 0.000 claims description 6
- 229910052702 rhenium Inorganic materials 0.000 claims description 6
- WUAPFZMCVAUBPE-UHFFFAOYSA-N rhenium atom Chemical compound [Re] WUAPFZMCVAUBPE-UHFFFAOYSA-N 0.000 claims description 6
- 229910052715 tantalum Inorganic materials 0.000 claims description 6
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 claims description 6
- 229910052725 zinc Inorganic materials 0.000 claims description 6
- 239000011701 zinc Substances 0.000 claims description 6
- 229910052726 zirconium Inorganic materials 0.000 claims description 6
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims description 5
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical group [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 5
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical group [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 claims description 5
- 229910052779 Neodymium Inorganic materials 0.000 claims description 5
- 229910052777 Praseodymium Inorganic materials 0.000 claims description 5
- 238000003723 Smelting Methods 0.000 claims description 5
- 229910052786 argon Inorganic materials 0.000 claims description 5
- 229910052796 boron Inorganic materials 0.000 claims description 5
- 238000011049 filling Methods 0.000 claims description 5
- 230000003116 impacting effect Effects 0.000 claims description 5
- 229910052749 magnesium Inorganic materials 0.000 claims description 5
- 239000011777 magnesium Substances 0.000 claims description 5
- 229910052748 manganese Inorganic materials 0.000 claims description 5
- 239000011572 manganese Substances 0.000 claims description 5
- 238000004519 manufacturing process Methods 0.000 claims description 5
- QEFYFXOXNSNQGX-UHFFFAOYSA-N neodymium atom Chemical compound [Nd] QEFYFXOXNSNQGX-UHFFFAOYSA-N 0.000 claims description 5
- PUDIUYLPXJFUGB-UHFFFAOYSA-N praseodymium atom Chemical compound [Pr] PUDIUYLPXJFUGB-UHFFFAOYSA-N 0.000 claims description 5
- 238000010298 pulverizing process Methods 0.000 claims description 5
- 238000005303 weighing Methods 0.000 claims description 5
- 238000000034 method Methods 0.000 claims 4
- 239000000203 mixture Substances 0.000 claims 1
- 238000000576 coating method Methods 0.000 abstract description 7
- 238000005260 corrosion Methods 0.000 abstract description 7
- 230000007797 corrosion Effects 0.000 abstract description 7
- 239000011248 coating agent Substances 0.000 abstract description 6
- 230000005389 magnetism Effects 0.000 abstract description 2
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 6
- 230000003647 oxidation Effects 0.000 description 5
- 238000007254 oxidation reaction Methods 0.000 description 5
- 239000012071 phase Substances 0.000 description 5
- 230000002411 adverse Effects 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 229910052761 rare earth metal Inorganic materials 0.000 description 3
- 238000005245 sintering Methods 0.000 description 3
- 241000894006 Bacteria Species 0.000 description 2
- 229910052692 Dysprosium Inorganic materials 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- 229910052771 Terbium Inorganic materials 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000003064 anti-oxidating effect Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000001627 detrimental effect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000005984 hydrogenation reaction Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 238000010301 surface-oxidation reaction Methods 0.000 description 1
- 238000005496 tempering Methods 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
- H01F1/0575—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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Abstract
本发明涉及永磁材料技术领域,尤其涉及一种烧结钕铁硼永磁材料及其制备方法,该永磁材料由以下质量份的原料制成:锌钕合金5‑10份、镨铁合金8‑10份、二硅化钼0.3‑0.8份、六硼化硅0.1‑0.5份、铝铼合金0.01‑0.1份、铝硅合金0.2‑0.9份、锰镍合金1‑3份、硼镁合金1‑5份、铁粉50‑65份、保护膜合金5‑7份。本发明提高磁材料的剩磁性、最大磁能积;利用磁材料表面镀膜的方式,在磁体表面形成高效的稳定膜,在兼顾磁体性能和防腐蚀的前提之下有效降低成本。
Description
技术领域
本发明涉及永磁体技术领域,尤其涉及一种烧结钕铁硼永磁材料及其制备方法。
背景技术
烧结钕铁硼磁体主要由Nd2Fe14B,富Nd相和富B相组成,其中Nd2Fe14B是磁性相,决定剩磁和磁能积,富Nd相和磁体的微观结构决定磁体的矫顽力。从烧结钕铁硼的反磁化机理来看,主要是反磁化畴在晶界处形核机制,磁性相的边界结构和物理特性对磁体的矫顽力具有重要的影响。(Dy,Tb)2Fe14B的各向异性场高于Nd2Fe14B的各向异性场,因此添加重稀土元素Dy和Tb都能使磁体矫顽力大幅度增加,显著提高NdFeB磁体的使用温度。
但是在当前永磁体的生产研究中,主要侧重于磁性能的提升,对于磁性能的稳定性,没有进行针对性的技术储备。如专利号为CN201810343442.4的一种钕铁硼磁体,通过两种配方的第一钕铁硼合金和第二钕铁硼合金经过二次压制成型和高温烧结制得,达到降低重稀土元素的使用量,降低生产成本,获得综合磁性能较好的目的;但是对于磁体的性能延续性并没有做出尝试,不利于磁体的整体性能提升。又如专利号为CN201810254057.2的一种防氧化钕铁硼磁体的制备方法,通过将钕铁硼磁体生坯烧结、回火后得钕铁硼磁体,防止了钕铁硼磁体生坯中稀土与氧反应,避免造成烧结的时候液相收缩差异,造成氧化变形;但是其只能防止在生产环节中的氧化,对于磁体在使用环境中面对的氧化、腐蚀等环境变量缺乏考量。所以,研究一种性能全面,可以有效应对环境变化带来的不利因素的磁体极有必要。
发明内容
为了解决现有技术中存在的问题,本发明提供一种烧结钕铁硼永磁材料,以增强永磁材料的抗氧化性,延长磁材料的使用时间,该永磁材料由以下质量份的原料制成:锌钕合金5-10份、镨铁合金8-10份、二硅化钼0.3-0.8份、六硼化硅0.1-0.5份、铝铼合金0.01-0.1份、铝硅合金0.2-0.9份、锰镍合金1-3份、硼镁合金1-5份、铁粉50-65份、保护膜合金5-7份;所述锌钕合金中钕质量百分比为15-18%,余量为锌;所述镨铁合金中镨质量百分比为1-3%,余量为铁;所述铝铼合金中铼质量百分比为1-4%,余量为铝;所述铝硅合金中硅质量百分比为8-12%,余量为铝;所述锰镍合金中镍质量百分比为0.8-3%,余量为锰;所述硼镁合金中硼质量百分比为5-10%,余量为镁。
进一步的,所述保护膜合金,以质量百分比计,其成分为9:1:0.2:0.1:0.1的铂、铁、硅、锆、钽。
本发明所述的烧结钕铁硼永磁材料,制备方法如下:
(1)按配比称取锌钕合金、镨铁合金、二硅化钼、六硼化硅、铝铼合金、铝硅合金、锰镍合金、硼镁合金、铁粉,在真空度为0.1pa的熔炼炉中,先加入二硅化钼、六硼化硅、铁粉混合均匀,加热到2200-2300℃,混炼1-2h,将温度降低至1500-1600℃,加入锌钕合金、镨铁合金、铝铼合金、铝硅合金、锰镍合金、硼镁合金混炼30-50min,浇注成甩带片;
(2)将甩带片在真空炉中加热至温度300-400℃,保温50-70min,再将温度升高到440-450℃,用微波处理20-30min,然后充入氢气使得炉内气压升高至500-800pa,用微波处理30-50min,保温3-5h,将温度升高至700-800℃除去氢得到粉体;
(3)将所述粉体经气流磨粉碎为超细粉,将超细粉倒入模具压制成型中,真空氩气保护下,在1000-1100℃的温度下保温5-8h,然后将模具降温至400-500℃,保温2-4h,再次加热到1000-1100℃的温度下保温6-10h,然后将温度降低至510-530℃,保温1-2h即可;
(4)将上一步骤制得的钕铁硼磁体在真空炉内通入压强为5-8Pa的氪气,衬底偏压调至-500V,用氪离子离子冲击;将炉内压强降低至0.2-0.7pa,衬底偏压调至-150V,溅射电流5A,溅射10min;再将压强降低至0.01-0.08pa,衬底偏压调至-250V,溅射电流15A,溅射25min,溅射保护膜合金靶材;
(5)将上一步骤得到的磁体在400-450℃保温10-15min即得。
进一步的,步骤(2)中,所述微波频率2400-2500mhz,微波功率800-900W。
进一步的,步骤(3)中,所述超细粉细度为13-25um。
进一步的,步骤(3)中,所述模具降温速度为8-10℃/min。
进一步的,步骤(4)中,所述氪离子冲击时间为5min。
与现有技术相比,本发明的技术效果体现在:
本发明通过在磁体中引入锌、硅、钼、铼、锰、镍等元素,使得磁体均匀度增高,排列规则,利用不同材料晶体的微观尺度差异,促进钕铁硼晶体的有序组合,有效增强原料颗粒间的粘结,提高磁体的磁稳定性,使得磁体的均一度好,可以最大限度的发挥磁体性能,显著提高剩磁性、最大磁能积。
特别的,本发明通过在磁体材料中使用二硅化钼,利用且两种原子的半径相近,电负性比较接近,使得制得的永磁材料在高温下稳定性更好,提高磁体的高温氧化性,在实际使用中,即便保护膜合金磨损,内部永磁材料也能保证很好的稳定性。通过在磁体材料中使用铝铼合金,使得熔炼的原料熔融体延展性更好,提高其加工特性,便于不同形状永磁体的塑形,提高永磁体材料在常温常压下的抵抗碱、抗酸能力。通过在磁体材料中使用铝硅合金,利用硅元素的存在能够改善原料间的流动性,降低热裂倾向,减少疏松,促进锌钕、镨铁、二硅化钼、六硼化硅、铝铼、锰镍、硼镁、铁粉的混合,通过连接其他原料成分促进永磁材料力学性能的提升,使得多种耐高温抗腐蚀的成分相互促进,进一步提升材料的整体抗性。通过在磁体材料中使用铝硅合金,提高原料的均一度,使得原料高温性能进一步增强。
本发明利用磁材料表面镀膜的方式,在磁体表面形成高效的稳定膜,有效防止使用时不利因素导致的磁体分裂或者磁体磁性能的降低,并且磁体和磁材料形成有机的整体,在表面抗性形成的前提之下,磁体本身也具有一定的防腐蚀能力,使得磁体内外形成高低搭配,在完美兼顾磁体性能和防腐蚀的前提之下有效降低成本。而且使用铂、铁、硅、锆、钽混合镀膜,使得保护膜合金颗粒交织在磁材料表面,形成延展度好贴合度高的磨体,提高磁材料的抗干扰能力,提高磁体的高温性能和矫顽力。
本发明根据材料特性,在制作中使用微波处理,利用微波携带的能量和穿透性,有效促进金属原料之间的相互运动,提高原料组分的均一度,同时利用微波的偶极涡流、离子传导和高频率摩擦,提高原料金属的活性,促进后续的氢化。并且在镀膜中使用氪气,利用氪气带来更大的电离度,提高镀膜效果,显著提高磁性材料的性能。使得镀膜与磁体本身粘结度好,磁性能发挥完全。
本发明通过精准科学的搭配原料,针对性的使用加工工艺,使得制备出来的永磁材料在浓度湿度58%、含有0.1%的醋酸蒸气、含有杂菌的环境中,加热到80℃,放置10天后,永磁材料的磁性能也能保持良好,表面也没有出现腐蚀。可以看出本发明的永磁材料在高温下极为稳定,耐酸耐生物腐蚀上效果优异,对于环境中的不利因素具有更好的抵抗性。
具体实施方式
下面结合具体的实施方式来对本发明的技术方案做进一步的限定,但要求保护的范围不仅局限于所作的描述。
实施例1
一种烧结钕铁硼永磁材料,由以下质量份的原料制成:锌钕合金5份、镨铁合金8份、二硅化钼0.3份、六硼化硅0.1份、铝铼合金0.01份、铝硅合金0.2份、锰镍合金1份、硼镁合金1份、铁粉50份、保护膜合金5份;所述锌钕合金中钕质量百分比为15%,余量为锌;所述镨铁合金中镨质量百分比为1%,余量为铁;所述铝铼合金中铼质量百分比为1%,余量为铝;所述铝硅合金中硅质量百分比为8%,余量为铝;所述锰镍合金中镍质量百分比为0.8%,余量为锰;所述硼镁合金中硼质量百分比为5%,余量为镁所述保护膜合金由质量比为9:1:0.2:0.1:0.1的铂、铁、硅、锆、钽混合而成。
本实施例所述的烧结钕铁硼永磁材料,制备方法如下:
(1)按配比称取锌钕合金、镨铁合金、二硅化钼、六硼化硅、铝铼合金、铝硅合金、锰镍合金、硼镁合金、铁粉,在真空度为0.1pa的熔炼炉中,先加入二硅化钼、六硼化硅、铁粉混合均匀,加热到2200℃,混炼1h,将温度降低至1500℃,加入锌钕合金、镨铁合金、铝铼合金、铝硅合金、锰镍合金、硼镁合金混炼30min,浇注成甩带片;
(2)将甩带片在真空炉中加热至温度300℃,保温50min,再将温度升高到440℃,用微波处理20min,然后充入氢气使得炉内气压升高至500pa,用微波处理30min,保温3h,将温度升高至700℃除去氢得到粉体;所述微波频率2400mhz,微波功率800W;
(3)将所述粉体经气流磨粉碎为13um的超细粉,将超细粉倒入模具压制成型中,真空氩气保护下,在1000℃的温度下保温5h,然后将模具降温至400℃,保温2h,再次加热到1000℃的温度下保温6h,然后将温度降低至510℃,保温1h即可;
(4)将上一步骤制得的钕铁硼磁体在真空炉内通入压强为5Pa的高纯氪气,衬底偏压调至-500V,氪离子离子冲击约5min;将炉内压强降低至0.2pa,衬底偏压调至-150V,溅射电流5A,溅射10min;再将压强降低至0.01pa,衬底偏压调至-250V,溅射电流15A,溅射25min,溅射保护膜合金靶材;
(5)将上一步骤得到的磁体在400℃保温10min即得。
实施例2
一种烧结钕铁硼永磁材料,由以下质量份的原料制成:锌钕合金10份、镨铁合金10份、二硅化钼0.8份、六硼化硅0.5份、铝铼合金0.1份、铝硅合金0.9份、锰镍合金3份、硼镁合金5份、铁粉65份、保护膜合金7份;所述锌钕合金中钕的质量百分比为18%,余量为锌;所述镨铁合金中镨的质量百分比为3%,余量为铁;所述铝铼合金中铼的质量百分比为4%,余量为铝;所述铝硅合金中硅的质量百分比为12%,余量为铝;所述锰镍合金中镍的质量百分比为3%,余量为锰;所述硼镁合金中硼的质量百分比为10%,余量为镁所述保护膜合金由质量比为9:1:0.2:0.1:0.1的铂、铁、硅、锆、钽混合而成。
本实施例所述的烧结钕铁硼永磁材料,制备方法如下:
(1)按配比称取锌钕合金、镨铁合金、二硅化钼、六硼化硅、铝铼合金、铝硅合金、锰镍合金、硼镁合金、铁粉,在真空度为0.1pa的熔炼炉中,先加入二硅化钼、六硼化硅、铁粉混合均匀,加热到2300℃,混炼2h,将温度降低至1600℃,加入锌钕合金、镨铁合金、铝铼合金、铝硅合金、锰镍合金、硼镁合金混炼50min,浇注成甩带片;
(2)将甩带片在真空炉中加热至温度400℃,保温70min,再将温度升高到450℃,用微波处理30min,然后充入氢气使得炉内气压升高至800pa,用微波处理50min,保温5h,将温度升高至800℃除去氢得到粉体;所述微波频率2500mhz,微波功率900W;
(3)将所述粉体经气流磨粉碎为25um的超细粉,将超细粉倒入模具压制成型中,真空氩气保护下,在1100℃的温度下保温8h,然后将模具降温至500℃,保温4h,再次加热到1100℃的温度下保温10h,然后将温度降低至530℃,保温2h即可;
(4)将上一步骤制得的钕铁硼磁体在真空炉内通入压强为8Pa的高纯氪气,衬底偏压调至-500V,氪离子离子冲击约5min;将炉内压强降低至0.7pa,衬底偏压调至-150V,溅射电流5A,溅射10min;再将压强降低至0.08pa,衬底偏压调至-250V,溅射电流15A,溅射25min,溅射保护膜合金靶材;
(5)将上一步得到的磁体在450℃保温15min即得。
实施例3
一种烧结钕铁硼永磁材料,由以下质量份的原料制成:锌钕合金7份、镨铁合金9份、二硅化钼0.5份、六硼化硅0.2份、铝铼合金0.054份、铝硅合金0.43份、锰镍合金2份、硼镁合金3份、铁粉57份、保护膜合金6份;所述锌钕合金中钕的质量百分比为16%,余量为锌;所述镨铁合金中镨的质量百分比为2%,余量为铁;所述铝铼合金中铼的质量百分比为2%,余量为铝;所述铝硅合金中硅的质量百分比为12%,余量为铝;所述锰镍合金中镍的质量百分比为0.8%,余量为锰;所述硼镁合金中硼的质量百分比为10%,余量为镁所述保护膜合金由质量比为9:1:0.2:0.1:0.1的铂、铁、硅、锆、钽混合而成。
本实施例所述的烧结钕铁硼永磁材料,制备方法如下:
(1)按配比称取锌钕合金、镨铁合金、二硅化钼、六硼化硅、铝铼合金、铝硅合金、锰镍合金、硼镁合金、铁粉,在真空度为0.1pa的熔炼炉中,先加入二硅化钼、六硼化硅、铁粉混合均匀,加热到2270℃,混炼1h,将温度降低至1600℃,加入锌钕合金、镨铁合金、铝铼合金、铝硅合金、锰镍合金、硼镁合金混炼40min,浇注成甩带片;
(2)将甩带片在真空炉中加热至温度300℃,保温70min,再将温度升高到450℃,用微波处理20min,然后充入氢气使得炉内气压升高至800pa,用微波处理30min,保温5h,将温度升高至700℃除去氢得到粉体;所述微波频率2480mhz,微波功率850W;
(3)将所述粉体经气流磨粉碎为25um的超细粉,将超细粉倒入模具压制成型中,真空氩气保护下,在1000℃的温度下保温8h,然后将模具降温至400℃,保温4h,再次加热到1000℃的温度下保温10h,然后将温度降低至510℃,保温2h即可;
(4)将上一步骤制得的钕铁硼磁体在真空炉内通入压强为8Pa的高纯氪气,衬底偏压调至-500V,氪离子离子冲击约5min;将炉内压强降低至0.2pa,衬底偏压调至-150V,溅射电流5A,溅射10min;再将压强降低至0.08pa,衬底偏压调至-250V,溅射电流15A,溅射25min,溅射保护膜合金靶材;
(5)将上一步得到的磁体在400℃保温15min即得。
对比例设置:
试验例:
分别按照实施例1-3、对比例1-10制作永磁体,测试各组磁体的磁性能,将磁体置于浓度湿度58%、含有0.1%的醋酸蒸气、含有杂菌的环境中,加热到80℃,放置10天,观察磁体表面氧化情况。如下表:
可以看出,实施例1-3的磁体性能优异,显著优于对照组1-10;对照组5、6保护膜合金成分变化,受到轻微氧化,对比例10未进行镀层,表面氧化严重;所以本发明在兼顾磁体主要性能的同时,通过镀膜工艺有效提高了磁体在复杂环境中的稳定性。
Claims (7)
1.一种烧结钕铁硼永磁材料,其特征在于,由以下质量份的原料制成:锌钕合金5-10份、镨铁合金8-10份、二硅化钼0.3-0.8份、六硼化硅0.1-0.5份、铝铼合金0.01-0.1份、铝硅合金0.2-0.9份、锰镍合金1-3份、硼镁合金1-5份、铁粉50-65份、保护膜合金5-7份;所述锌钕合金中钕的质量百分比为15-18%,余量为锌;所述镨铁合金中镨的质量百分比为1-3%,余量为铁;所述铝铼合金中铼的质量百分比为1-4%,余量为铝;所述铝硅合金中硅的质量百分比为8-12%,余量为铝;所述锰镍合金中镍的质量百分比为0.8-3%,余量为锰;所述硼镁合金中硼的质量百分比为5-10%,余量为镁。
2.如权利要求1所述的烧结钕铁硼永磁材料,其特征在于,所述保护膜合金,以质量百分比计,其成分为9:1:0.2:0.1:0.1的铂、铁、硅、锆、钽。
3.一种如权利要求1所述的烧结钕铁硼永磁材料的制备方法,其特征在于,步骤如下:
(1)按配比称取锌钕合金、镨铁合金、二硅化钼、六硼化硅、铝铼合金、铝硅合金、锰镍合金、硼镁合金、铁粉,在真空度为0.1pa的熔炼炉中,先加入二硅化钼、六硼化硅、铁粉混合均匀,加热到2200-2300℃,混炼1-2h,将温度降低至1500-1600℃,加入锌钕合金、镨铁合金、铝铼合金、铝硅合金、锰镍合金、硼镁合金混炼30-50min,浇注成甩带片;
(2)将甩带片在真空炉中加热至温度300-400℃,保温50-70min,再将温度升高到440-450℃,用微波处理20-30min,然后充入氢气使得炉内气压升高至500-800pa,用微波处理30-50min,保温3-5h,将温度升高至700-800℃除去氢得到粉体;
(3)将所述粉体经气流磨粉碎为超细粉,将超细粉倒入模具压制成型中,真空氩气保护下,在1000-1100℃的温度下保温5-8h,然后将模具降温至400-500℃,保温2-4h,再次加热到1000-1100℃的温度下保温6-10h,然后将温度降低至510-530℃,保温1-2h即可;
(4)将上一步骤制得的钕铁硼磁体在真空炉内通入压强为5-8Pa的氪气,衬底偏压调至-500V,用氪离子离子冲击;将炉内压强降低至0.2-0.7pa,衬底偏压调至-150V,溅射电流5A,溅射10min;再将压强降低至0.01-0.08pa,衬底偏压调至-250V,溅射电流15A,溅射25min,溅射保护膜合金靶材;
(5)将上一步骤得到的磁体在400-450℃保温10-15min即得。
4.如权利要求3所述的烧结钕铁硼永磁材料的制备方法,其特征在于,步骤(2)中,所述微波频率2400-2500mhz,微波功率800-900W。
5.如权利要求3所述的烧结钕铁硼永磁材料的制备方法,其特征在于,步骤(3)中,所述超细粉细度为13-25um。
6.如权利要求3所述的烧结钕铁硼永磁材料的制备方法,其特征在于,步骤(3)中,所述模具降温速度为8-10℃/min。
7.如权利要求3所述的烧结钕铁硼永磁材料的制备方法,其特征在于,步骤(4)中,所述氪离子冲击时间为5min。
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