CN105057657B - 软-硬磁性MnBi/SiO2/FeCo纳米颗粒 - Google Patents
软-硬磁性MnBi/SiO2/FeCo纳米颗粒 Download PDFInfo
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- CN105057657B CN105057657B CN201510224110.0A CN201510224110A CN105057657B CN 105057657 B CN105057657 B CN 105057657B CN 201510224110 A CN201510224110 A CN 201510224110A CN 105057657 B CN105057657 B CN 105057657B
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 86
- 239000002105 nanoparticle Substances 0.000 title claims abstract description 77
- 239000000377 silicon dioxide Substances 0.000 title claims abstract description 45
- 229910002546 FeCo Inorganic materials 0.000 title claims abstract description 37
- 229910016629 MnBi Inorganic materials 0.000 title claims abstract description 20
- 229910052681 coesite Inorganic materials 0.000 title claims abstract description 16
- 229910052906 cristobalite Inorganic materials 0.000 title claims abstract description 16
- 229910052682 stishovite Inorganic materials 0.000 title claims abstract description 16
- 229910052905 tridymite Inorganic materials 0.000 title claims abstract description 16
- 235000012239 silicon dioxide Nutrition 0.000 title description 2
- 239000011258 core-shell material Substances 0.000 claims abstract description 31
- KYAZRUPZRJALEP-UHFFFAOYSA-N bismuth manganese Chemical compound [Mn].[Bi] KYAZRUPZRJALEP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910001152 Bi alloy Inorganic materials 0.000 claims abstract description 7
- QVYYOKWPCQYKEY-UHFFFAOYSA-N [Fe].[Co] Chemical compound [Fe].[Co] QVYYOKWPCQYKEY-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910052914 metal silicate Inorganic materials 0.000 claims description 19
- RIVZIMVWRDTIOQ-UHFFFAOYSA-N cobalt iron Chemical compound [Fe].[Co].[Co].[Co] RIVZIMVWRDTIOQ-UHFFFAOYSA-N 0.000 claims description 13
- 239000011572 manganese Substances 0.000 claims description 10
- 239000002245 particle Substances 0.000 claims description 10
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 claims description 8
- 229910045601 alloy Inorganic materials 0.000 claims description 8
- 239000000956 alloy Substances 0.000 claims description 8
- 239000011248 coating agent Substances 0.000 claims description 8
- 238000000576 coating method Methods 0.000 claims description 8
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 8
- 229920001577 copolymer Polymers 0.000 claims description 7
- 239000012448 Lithium borohydride Substances 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- -1 iron ion Chemical class 0.000 claims description 4
- 229910052742 iron Inorganic materials 0.000 claims description 3
- 230000009467 reduction Effects 0.000 claims description 3
- 150000002500 ions Chemical class 0.000 claims 2
- 229910001429 cobalt ion Inorganic materials 0.000 claims 1
- MPMSMUBQXQALQI-UHFFFAOYSA-N cobalt phthalocyanine Chemical compound [Co+2].C12=CC=CC=C2C(N=C2[N-]C(C3=CC=CC=C32)=N2)=NC1=NC([C]1C=CC=CC1=1)=NC=1N=C1[C]3C=CC=CC3=C2[N-]1 MPMSMUBQXQALQI-UHFFFAOYSA-N 0.000 claims 1
- XLJKHNWPARRRJB-UHFFFAOYSA-N cobalt(2+) Chemical compound [Co+2] XLJKHNWPARRRJB-UHFFFAOYSA-N 0.000 claims 1
- 230000000536 complexating effect Effects 0.000 claims 1
- 229910052635 ferrosilite Inorganic materials 0.000 claims 1
- 239000002086 nanomaterial Substances 0.000 claims 1
- 239000010420 shell particle Substances 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 24
- 229910052761 rare earth metal Inorganic materials 0.000 abstract description 2
- 229910000531 Co alloy Inorganic materials 0.000 abstract 1
- 239000007771 core particle Substances 0.000 abstract 1
- 150000002910 rare earth metals Chemical class 0.000 abstract 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 16
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 12
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 10
- 230000015572 biosynthetic process Effects 0.000 description 10
- 230000008859 change Effects 0.000 description 10
- 150000004678 hydrides Chemical class 0.000 description 8
- 238000003786 synthesis reaction Methods 0.000 description 8
- 235000019441 ethanol Nutrition 0.000 description 7
- 239000000696 magnetic material Substances 0.000 description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 description 6
- 230000005389 magnetism Effects 0.000 description 6
- 238000011160 research Methods 0.000 description 6
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 6
- 238000003917 TEM image Methods 0.000 description 5
- 239000003638 chemical reducing agent Substances 0.000 description 5
- 230000002045 lasting effect Effects 0.000 description 5
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 4
- QJVKUMXDEUEQLH-UHFFFAOYSA-N [B].[Fe].[Nd] Chemical compound [B].[Fe].[Nd] QJVKUMXDEUEQLH-UHFFFAOYSA-N 0.000 description 4
- 229910052797 bismuth Inorganic materials 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- 229910052748 manganese Inorganic materials 0.000 description 4
- 229910001172 neodymium magnet Inorganic materials 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 150000003839 salts Chemical class 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 230000005381 magnetic domain Effects 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 101100373011 Drosophila melanogaster wapl gene Proteins 0.000 description 2
- 229910017061 Fe Co Inorganic materials 0.000 description 2
- BZLVMXJERCGZMT-UHFFFAOYSA-N Methyl tert-butyl ether Chemical compound COC(C)(C)C BZLVMXJERCGZMT-UHFFFAOYSA-N 0.000 description 2
- 229910003978 SiClx Inorganic materials 0.000 description 2
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 2
- SWLVFNYSXGMGBS-UHFFFAOYSA-N ammonium bromide Chemical compound [NH4+].[Br-] SWLVFNYSXGMGBS-UHFFFAOYSA-N 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 238000000498 ball milling Methods 0.000 description 2
- 150000001621 bismuth Chemical class 0.000 description 2
- NSPSPMKCKIPQBH-UHFFFAOYSA-K bismuth;7,7-dimethyloctanoate Chemical compound [Bi+3].CC(C)(C)CCCCCC([O-])=O.CC(C)(C)CCCCCC([O-])=O.CC(C)(C)CCCCCC([O-])=O NSPSPMKCKIPQBH-UHFFFAOYSA-K 0.000 description 2
- 230000000903 blocking effect Effects 0.000 description 2
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 2
- 235000013339 cereals Nutrition 0.000 description 2
- GVPFVAHMJGGAJG-UHFFFAOYSA-L cobalt dichloride Chemical compound [Cl-].[Cl-].[Co+2] GVPFVAHMJGGAJG-UHFFFAOYSA-L 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000004210 ether based solvent Substances 0.000 description 2
- 229960002089 ferrous chloride Drugs 0.000 description 2
- NMCUIPGRVMDVDB-UHFFFAOYSA-L iron dichloride Chemical compound Cl[Fe]Cl NMCUIPGRVMDVDB-UHFFFAOYSA-L 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 210000004483 pasc Anatomy 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 239000012266 salt solution Substances 0.000 description 2
- 239000012279 sodium borohydride Substances 0.000 description 2
- 229910000033 sodium borohydride Inorganic materials 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000000725 suspension Substances 0.000 description 2
- 230000007704 transition Effects 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- LZDKZFUFMNSQCJ-UHFFFAOYSA-N 1,2-diethoxyethane Chemical compound CCOCCOCC LZDKZFUFMNSQCJ-UHFFFAOYSA-N 0.000 description 1
- 150000000094 1,4-dioxanes Chemical class 0.000 description 1
- JWUJQDFVADABEY-UHFFFAOYSA-N 2-methyltetrahydrofuran Chemical compound CC1CCCO1 JWUJQDFVADABEY-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- ZAFNJMIOTHYJRJ-UHFFFAOYSA-N Diisopropyl ether Chemical compound CC(C)OC(C)C ZAFNJMIOTHYJRJ-UHFFFAOYSA-N 0.000 description 1
- XTHFKEDIFFGKHM-UHFFFAOYSA-N Dimethoxyethane Chemical compound COCCOC XTHFKEDIFFGKHM-UHFFFAOYSA-N 0.000 description 1
- 229910010084 LiAlH4 Inorganic materials 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000004833 X-ray photoelectron spectroscopy Methods 0.000 description 1
- KLARSDUHONHPRF-UHFFFAOYSA-N [Li].[Mn] Chemical compound [Li].[Mn] KLARSDUHONHPRF-UHFFFAOYSA-N 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 150000003973 alkyl amines Chemical class 0.000 description 1
- 125000000217 alkyl group Chemical group 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 150000001622 bismuth compounds Chemical class 0.000 description 1
- UORVGPXVDQYIDP-UHFFFAOYSA-N borane Chemical compound B UORVGPXVDQYIDP-UHFFFAOYSA-N 0.000 description 1
- 229910010277 boron hydride Inorganic materials 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 125000003636 chemical group Chemical group 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 238000005056 compaction Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- WXGGJJDBACQMHS-UHFFFAOYSA-N iron(2+);neodymium(3+);borate Chemical compound [Fe+2].[Nd+3].[O-]B([O-])[O-] WXGGJJDBACQMHS-UHFFFAOYSA-N 0.000 description 1
- 239000012280 lithium aluminium hydride Substances 0.000 description 1
- 239000006247 magnetic powder Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000002103 nanocoating Substances 0.000 description 1
- 238000001420 photoelectron spectroscopy Methods 0.000 description 1
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- 150000003141 primary amines Chemical class 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000004080 punching Methods 0.000 description 1
- 239000011541 reaction mixture Substances 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 150000004760 silicates Chemical class 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- QBVXKDJEZKEASM-UHFFFAOYSA-M tetraoctylammonium bromide Chemical compound [Br-].CCCCCCCC[N+](CCCCCCCC)(CCCCCCCC)CCCCCCCC QBVXKDJEZKEASM-UHFFFAOYSA-M 0.000 description 1
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- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
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- C01G49/00—Compounds of iron
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Abstract
本发明提供了软‑硬磁性MnBi/SiO2/FeCo纳米颗粒。具体地,提供了铁‑钴合金核、氧化硅壳和氧化硅壳表面上的锰铋合金核或纳米颗粒的核‑壳‑核纳米颗粒(FeCo/SiO2/MnBi)。由于靠近软磁性铁钴的纳米级的硬磁性锰铋,该核‑壳‑核纳米颗粒是稀土永磁体的替代材料。
Description
发明背景
发明领域
本发明涉及纳米颗粒的磁性纳米聚集体,该纳米颗粒具有铁钴合金核与中间氧化硅壳和遍布其中分散的锰铋合金纳米颗粒。这些纳米颗粒组合软磁性MnBi并且提供了适合用于制备永磁体的纳米颗粒材料,该永磁体为标准钕铁硼(neodymium iron borate)永磁体材料的不含稀土元素的替代物。
背景讨论
发明人正在进行采用由湿化学合成方法获得的纳米颗粒材料所获得的软磁性材料和硬磁性材料两者的研究项目。因此2013年9月12 日提交的美国申请号14/025,033公开了作为硬磁性材料来源的具有5 至200nm的颗粒尺寸的MnBi纳米颗粒。另外,2014年4月14日提交的U.S.14/252,036公开了作为软磁性材料来源的核-壳纳米颗粒,该核-壳纳米颗粒具有小于200nm的铁钴纳米颗粒核与氧化硅壳和金属硅酸盐界面。通过引用将两个申请的公开内容以其全文并入本文。
磁性材料通常分为两类,其指定为可被永久磁化的硬磁物质或在低的施加场下磁性可以翻转的软磁性材料。在软磁性材料中保持能量损耗(通常称为“芯损耗”)为最小是重要的,而在硬磁性材料中优选抵抗磁化的变化。高的芯损耗因此是永磁材料的特点并且在软磁性材料中是不需要的。
许多如今的先进技术需要有效和强的硬磁体作为装置结构的基本部件。这样的装置从移动电话延伸到高性能电动机,并且显著的努力在整个行业中持续以发现不仅满足目前需要而且还满足对于有效、较廉价并且容易制备的硬磁体材料的日益增加的需求的材料。
常规地,通常认为钕铁硼为可获得的最强、表现最好的硬磁体材料之一。然而,因为这种材料基于稀土元素钕,所以它是昂贵的并且可获得的供应经常不是稳定的。因此,需要作为硬磁体表现等同于或优于钕铁硼但是其基于可容易获得的并且较廉价的组分材料的材料。
通过将粉末压实成限定的形状并且然后在200℃或更高的温度下烧结该压实体来由粉末构造磁性装置零件。在压实后烧结该零件对于通过提供颗粒至颗粒结合并且因此提供强度来在该零件中实现令人满意的力学性质是必要的。
在通信和发电领域的所有方面中的技术进步需要日益增加的强大磁性粉末,该磁性粉末具有可控制或可调节的磁性性质,其允许制备为经济的并且可容易获得的经调整的磁性零件。
因此,本发明的目的是提供用于制备永磁性零件的具有高矫顽力的硬磁性粉末。该粉末与常规永磁性材料相比必须为经济的并且必须为可容易获得的。
发明内容
根据本发明实现了这些目的和其它目的,本发明的第一实施方案包括核-壳-核纳米颗粒,其包含:包含铁钴合金的超顺磁性核;涂覆该核的二氧化硅中间壳;中间二氧化硅壳上的另一个锰铋合金纳米颗粒核;和该核与二氧化硅壳之间的金属硅酸盐界面层;其中铁钴合金核的直径为200nm或更小。
在一个实施方案中,MnBi核的直径可为从0.5到200nm。
在任一个上述实施方案的一个方面,该金属硅酸盐界面的厚度可为从0.5到10nm并且可通过用于制备二氧化硅壳的湿合成的时间长度控制该厚度。
前述段落通过整体介绍而提供,并不旨在限制以下权利要求的范围。参考结合附图的以下详细描述将最好地理解目前优选的实施方案连同进一步的优点。
附图说明
图1显示了在实施例中制备的核-壳-核纳米颗粒的TEM图像。
图2显示了在实施例中制备的核-壳-核纳米颗粒的DSC扫描和 M(T)数据。
图3显示了在实施例中制备的核-壳-核纳米颗粒的Z衬度TEM图像。
具体实施方式
在整个该说明书中所描述的所有范围包括其中的所有值和子范围,除非另外说明。
另外,在整个说明书中不定冠词“一个(a)”或“一个(an)”带有“一个或多个”的含义,除非另有说明。
在磁性材料并且特别是纳米颗粒磁性材料的持续研究中,本发明人确定了纳米颗粒形式的锰铋合金作为具有作为用于制造永磁体的钕铁硼的替代品的潜在用途的材料。预测MnBi纳米颗粒呈现高达4T的矫顽力。2013年9月12日提交的美国申请号14/025,033公开了该工作的一些结果。
发明人还在进行对软磁性纳米颗粒材料的持续研究,例如2014 年4月14日提交的U.S.14/252,036中公开的,其中公开的核-壳纳米颗粒具有小于200nm的铁钴纳米颗粒核与氧化硅壳和金属硅酸盐界面。
在对这些和其它的体系的持续研究中,发明人出乎预料地发现通过向FeCo合金核氧化硅涂层核-壳纳米颗粒施加锰铋纳米涂层而获得的核-壳-核纳米颗粒提供了根据核-壳-壳组分各自的相对尺寸和属性具有高度可调节的磁性性质的材料。在一个纳米颗粒内这样的软磁性组分与硬磁性组分的复杂组合是新颖的并且提供许多发现和开发新型磁性材料和装置的机会。
在第一实施方案中,本发明包括核-壳-核纳米颗粒,其包含:
包含铁钴合金的超顺磁性核;
涂覆该核的二氧化硅中间壳;
中间二氧化硅壳上的外锰铋合金纳米颗粒,也称为基于MnBi纳米颗粒的球形纳米级属性的核;和
该核与二氧化硅壳之间的金属硅酸盐界面层;
其中铁钴合金核的直径为200nm或更小。
发明人发现可以经由可改变的湿化学方法实现涂覆有各种厚度的氧化硅壳的单个FeCo合金纳米颗粒的形成。出乎预料地,发明人发现界面金属硅酸盐的形成可显著改变这些超高表面积FeCo合金纳米颗粒体系中的纳米磁性。在Fe和Co的2p跃迁内收集的X射线光电子能谱中观察到金属硅酸盐界面层形成的证据;并且随着氧化硅壳的厚度增加(通过改变氧化硅反应的持续时间),形成较厚的界面金属硅酸盐层,增加了纳米颗粒的总体磁各向异性,这由增加的阻挡温度和改变的矫顽力证明。因此发明人出乎预料地发现通过采用不同程度的湿合成处理时间制备包封在氧化硅壳中的超顺磁铁钴合金纳米颗粒,可获得具有不同的纳米磁性性质的核壳FeCo纳米颗粒。在某些实施方案中,铁钴合金纳米颗粒核的直径为100nm或更小,并且在其它实施方案中,铁钴合金纳米颗粒核的直径为从2nm到50nm。
根据本发明,铁钴合金纳米颗粒晶粒为铁钴合金的单个颗粒磁畴的尺寸或接近该尺寸,并且因此为超顺磁的。虽然不受理论束缚,但是发明人认为将晶粒尺寸控制为接近颗粒磁畴的尺寸是促进根据本发明的磁性芯的减小的滞后的因素。此外,在核晶粒附近隔离的氧化硅壳的存在是促进根据本发明的磁性芯的低涡流形成的因素。
常规已知对于单个磁畴颗粒表现出超顺磁性的颗粒尺寸范围具有该颗粒化学组成的上边界特性。
发明人发现在二氧化硅壳的合成期间同时形成了金属硅酸盐薄层界面。在Fe和Co的2p跃迁内收集的X射线光电子能谱中观察到金属硅酸盐界面层形成的证据;并且随着氧化硅壳的厚度增加(通过改变氧化硅反应的持续时间),形成较厚的界面金属硅酸盐层,增加了纳米颗粒的总体磁各向异性,这由增加的阻挡温度和改变的矫顽力证明。发明人认识到这种界面金属硅酸盐层对控制磁性性质的效果的理解是在将这些材料在应用中有效用作低损耗变压器芯的关键要素。
在FeCo合金核壳纳米颗粒的研究中,发明人发现在二氧化硅壳涂层合成期间形成的界面金属硅酸盐改变了作为较高各向异性相的纳米颗粒的总体磁各向异性,该较高各向异性相为Fe基和Co基硅酸盐的组合,与裸FeCo纳米颗粒相比起到增加纳米颗粒的“磁性活性体积”的作用。
合成了二元合金FeCo单个磁畴纳米颗粒样品(参见实施例),不同之处在于改变SiO2反应时间的持续时间,这导致不同厚度的SiO2壳:1分钟反应时间产生3nm厚的壳,10分钟产生4nm厚的壳,并且20分钟产生6nm厚的壳。确定了平均FeCo纳米颗粒直径和SiO2壳厚度,并且对于所有三种核/壳纳米颗粒样品(FeCo/SiO2(3nm), FeCo/SiO2(4nm)和FeCo/SiO2(6nm)),发现平均FeCo核直径为4± 1nm,这表明纳米颗粒核合成中的高程度可再现性。以类似的方式确定了氧化硅壳的厚度并且发现对于FeCo/SiO2(3nm)、FeCo/SiO2(4nm) 和FeCo/SiO2(6nm)样品其分别为3±1nm、4±1nm和6±1nm。从TEM图像观察到FeCo核完全由氧化硅壳覆盖。X射线衍射图案分析表明Fe硅酸盐和Co硅酸盐两者的存在。然而,相对比例似乎是可变化的,并且尽管不希望受理论束缚,发明人仍认为金属硅酸盐含量可与金属硅酸盐形成的热力学能有关。研究显示在合成过程期间Fe硅酸盐和Co硅酸盐在FeCo纳米颗粒核与SiO2壳之间的界面处形成。然而,不同核/壳纳米颗粒体系的Fe°和Co°金属峰的相对积分区域表明Fe硅酸盐可比Co硅酸盐优先形成。
可通过硼氢化钠与二氯化铁和二氯化钴在氢氧化钠与四辛基溴化铵的溶液中的乙醇反应来合成Fe-Co/SiO2纳米颗粒。可使用三乙胺作为基础(base)催化剂用处于水乙醇混合物中的原硅酸四乙酯处理所获得的纳米颗粒以形成氧化硅壳。然后可使用含水乙醇冲洗来净化这些颗粒。
如指出的,Fe-Co纳米颗粒的处理长度确定二氧化硅涂层的宽度,并且相应地确定金属硅酸盐层的宽度。处理时间越长,涂层的量越大并且金属硅酸盐层的宽度越大。
可进行该合成持续对于制备0.5至20nm、优选0.8至10nm并且最优选1.0至8nm的金属硅酸盐层为必要的时间。
可通过包括如下步骤的方法形成锰-铋合金涂层:在FeCo氧化硅核壳纳米颗粒的存在下用氢化物还原剂处理Mn粉末并通过球磨合并;向Mn-氢化物还原剂混合物添加烷基胺和长链羧酸盐的铋盐溶液,同时持续搅拌;完成铋盐溶液添加时,继续搅拌以形成核-壳-核 FeCo/SiO2/MnBi纳米颗粒。
用于氢化物处理的醚溶剂可为与氢化物反应条件兼容的任何醚。合适的醚溶剂包括四氢呋喃(THF)、2-甲基四氢呋喃、二乙醚、二异丙基醚、1,4-二噁烷、二甲氧基乙烷、二乙二醇二乙醚、2-(2-甲氧基乙氧基)乙醇和甲基叔丁基醚。THF可为优选的溶剂。
氢化物还原剂可为能够与锰反应以形成锰还原剂络合物的任何材料并且包括NaH、LiH、CaH2、LiAlH4和LiBH4。LiBH4可为优选的氢化物处理剂。
可通过在行星式球磨机中以150至400rpm球磨锰粉末与氢化物还原剂至多4小时来完成锰硼氢化锂还原剂络合物的形成。可优化这种工序的变体以大致改变所获得的性质,并且其会得到本领域普通技术人员的理解。
另外,可以改变氢化物处理剂的量以改变条件和所获得的纳米颗粒的性质并且其可以以从1/1到100/1的氢化物与Mn的当量比改变。
可以以任何醚可溶盐形式添加铋并且优选作为长链羧酸的盐添加铋。在一个优选的实施方案中,以新癸酸铋添加Bi。Bi与Mn的摩尔比可为从0.8/1到1.2/1。优选地Bi/Mn的比例为从0.9/1到1.1/1,并且最优选地Bi/Mn的比例为1/1。可以改变铋化合物的添加时间以优化和改变MnBi的尺寸和性质。宽度可为从0.5到200nm,优选1.0 至100nm并且最优选2至20nm。优选地添加时间小于一小时并且在一个优选的实施方案中,添加时间为约20分钟。
可以向该反应任选添加烷基胺(优选具有从6到12个碳的碳链的伯胺)。
如图2所示,当在退火过程中热处理本发明的核-壳-核纳米颗粒时,软相FeCo和硬相MnBi两者分别在FeCo和MnBi的特性温度下退火。
已经整体上描述本发明,可参考一些特定实施例来获得进一步的理解,在本文中提供一些特定实施例仅出于说明的目的而不旨在进行限制,除非另外说明。
实施例
核-壳-核铁-钴/氧化硅/锰铋纳米颗粒
将0.489g氢氧化钠、12.892g四辛基溴化铵、10.922g四水合二氯化铁和12.042g六水合氯化钴溶解在250mL乙醇中并且置于氩下。随后向该铁钴混合物添加溶解于450mL乙醇中的12.258g硼氢化钠的溶液。在完成硼氢化物添加时,用100mL水稀释该反应混合物。然后用70%水/30%乙醇洗涤产物FeCo纳米颗粒。
随后将FeCo纳米颗粒悬浮在625mL水和2mL三乙胺的混合物中。然后向该FeCo悬浮液添加处于390mL乙醇中的0.5mL原硅酸四乙酯的溶液并且使所获得的混合物反应15分钟以获得涂覆氧化硅的纳米颗粒。随后用乙醇洗涤该经涂覆的纳米颗粒。
将涂覆氧化硅的FeCo纳米颗粒(0.27g)悬浮在200mL THF中。向该FeCo纳米颗粒悬浮液添加0.152g庚基氰、0.008g硼氢化锂和 0.012g Mn(LiBH4)2。然后向该搅拌的悬浮液逐滴添加处于15mL THF 中的0.082克新癸酸铋的溶液。最后用THF洗涤该产物。
在图1中显示了所制备的核-壳-核纳米颗粒的TEM图像。
图3的Z衬度TEM图像显示MnBi相如何在整个FeCo/SiO2中具有岛状分布。
图2显示了在温度范围内的DSC和M(T)数据,在该温度范围由两组数据所观察到的性质显示FeCo软磁性相和MnBi硬磁性相的不同存在,从而证实了两种相在核-壳-核纳米结构中的存在。
Claims (8)
1.核-壳-核纳米颗粒体系,其包含:
包含铁钴合金的超顺磁性核;
涂覆该核的二氧化硅中间壳;
中间二氧化硅壳上的锰铋合金外核;和
该超顺磁性核与二氧化硅壳之间的金属硅酸盐界面层;
其中
铁钴合金核的直径为200nm或更小。
2.根据权利要求1的核-壳-核纳米颗粒体系,其中MnBi核的直径为从0.5到200nm。
3.根据权利要求1的核-壳-核纳米颗粒体系,其中该界面层的金属硅酸盐包含硅酸铁和硅酸钴中的至少一种。
4.根据权利要求1的核-壳-核纳米颗粒体系,其中该金属硅酸盐界面层的厚度为从0.5nm到15nm。
5.根据权利要求1的核-壳-核纳米颗粒体系,其中该超顺磁性核由铁钴合金组成。
6.根据权利要求1的核-壳-核纳米颗粒体系,其中铁钴核的直径为从2到75nm。
7.制备核-壳-核FeCo/SiO2/MnBi纳米颗粒的方法,其包括:
由普通溶液将铁离子和钴离子共还原以制备FeCo合金纳米颗粒;
将该FeCo纳米颗粒从还原混合物分离;
在该FeCo纳米颗粒上形成氧化硅涂层以获得核-壳纳米颗粒;
和
通过用Mn和硼氢化锂还原络合物离子还原Bi离子以获得氧化硅壳上的MnBi合金纳米颗粒,在该核-壳纳米颗粒上形成MnBi合金纳米颗粒。
8.FeCo/SiO2纳米颗粒的核-壳-核纳米聚集体,其具有附着于氧化硅壳表面的MnBi纳米颗粒。
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CN102266740A (zh) * | 2010-06-04 | 2011-12-07 | 韩国科学技术研究院 | 超顺磁团簇-纳米颗粒-多孔复合珠及其制备方法 |
CN102728385A (zh) * | 2011-04-12 | 2012-10-17 | 韩国科学技术研究院 | 复合物及制备和回收方法、催化剂、抗菌或抗病毒复合物 |
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