JP4700374B2 - Method for producing SmCo magnetic fine particles - Google Patents

Method for producing SmCo magnetic fine particles Download PDF

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JP4700374B2
JP4700374B2 JP2005059293A JP2005059293A JP4700374B2 JP 4700374 B2 JP4700374 B2 JP 4700374B2 JP 2005059293 A JP2005059293 A JP 2005059293A JP 2005059293 A JP2005059293 A JP 2005059293A JP 4700374 B2 JP4700374 B2 JP 4700374B2
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直樹 戸嶋
幸英 白石
暢 松下
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本発明は、ＳｍＣｏ系磁性微粒子の製造方法に関するものである。   The present invention relates to a method for producing SmCo magnetic fine particles.

永久磁石として有名であり、極めて高い一軸性の結晶磁気異方性を示すＳｍＣｏ合金は、高密度記録を実現する磁気記録媒体をはじめ様々な磁性材料として魅力的な材料の一つである。
このようなＳｍＣｏ合金において、ナノレベルで制御されたナノ微粒子の作成については、物理的手法による研究はあるが、化学的手法による合成の報告は殆どない。 SmCo alloy, which is famous as a permanent magnet and exhibits extremely high uniaxial magnetocrystalline anisotropy, is one of attractive materials as various magnetic materials including magnetic recording media that realize high-density recording.
In such SmCo alloys, although there are studies by physical methods for the production of nano-particles controlled at the nano level, there are few reports of synthesis by chemical methods.

例えば、非特許文献１に、ＳｍＣｏクラスタの製造方法が開示されている。
この製造方法では、原材料として、サマリウムアセチルアセトナートＳｍ(acac)と、毒性があるコバルトカルボニルＣｏ2（ＣＯ）8が用いられている。 For example, Non-Patent Document 1 discloses a method for producing an SmCo cluster.
In this production method, samarium acetylacetonate Sm (acac) and toxic cobalt carbonyl Co 2 (CO) 8 are used as raw materials.

また、非特許文献２にも、ＳｍＣｏナノ微粒子の製造方法が開示されている。
この場合も、原材料として、サマリウムアセチルアセトナートＳｍ(acac)と、毒性があるコバルトカルボニルＣｏ2（ＣＯ）8が用いられている、 Non-Patent Document 2 also discloses a method for producing SmCo nanoparticles.
Also in this case, samarium acetylacetonate Sm (acac) and toxic cobalt carbonyl Co 2 (CO) 8 are used as raw materials.

さらに、非特許文献３に、クラスタ・ガンで気相凝縮させて、ＳｍＣｏナノ微粒子を製造する方法が開示されている。   Further, Non-Patent Document 3 discloses a method for producing SmCo nanoparticle by vapor phase condensation with a cluster gun.

また、非特許文献４に、電析によりＳｍ−Ｃｏナノ微粒子を製造する方法が開示されている。   Non-Patent Document 4 discloses a method for producing Sm—Co nanoparticles by electrodeposition.

K Orio et al「Organometallic synthesis and magnetic properties of ferromagnetic Sm-Co nanocluster 」 JOURNAL OF APPLIED PHYSICS, vol 91, number 10, (2002), page 8480K Orio et al `` Organometallic synthesis and magnetic properties of treated Sm-Co nanocluster '' JOURNAL OF APPLIED PHYSICS, vol 91, number 10, (2002), page 8480 Hongwei Gu and Bing Xu et al「Chemical synthesis of narrowly dispersed SmCo5 nanoparticles」 JOURNAL OF APPLIEDPHYSICS vol 93 number 10 (2003) page 7589Hongwei Gu and Bing Xu et al “Chemical synthesis of narrowly dispersed SmCo5 nanoparticles” JOURNAL OF APPLIEDPHYSICS vol 93 number 10 (2003) page 7589 S Stoyanov et al「High anisotropy Sm-Co nanoparticles: Preparation by cluster gun technique and their magnetic properties 」 JOURNAL OF APPLIED PHYSICS vol 93 number 10 (2003) page 7592S Stoyanov et al “High anisotropy Sm-Co nanoparticles: Preparation by cluster gun technique and their magnetic properties” JOURNAL OF APPLIED PHYSICS vol 93 number 10 (2003) page 7592 Jianqi Zhang et al「Electrodeposition of Sm-Co nanoparticles from aqueous solutions 」 Journal of Magnetism abd Magnetic Materials 283 (2004) page 89-94Jianqi Zhang et al “Electrodeposition of Sm-Co nanoparticles from aqueous solutions” Journal of Magnetism abd Magnetic Materials 283 (2004) page 89-94

本発明は、毒性があるコバルトカルボニルＣｏ2（ＣＯ）8を使うことなく、化学的方法で、ＳｍＣｏ系磁性微粒子を合成する方法を提案することを課題とする。
The present invention, without using a cobalt carbonyl Co 2 (CO) 8 which is toxic, with chemical methods, it is an object to propose a method for synthesizing a SmCo-based magnetic fine particles.

上記した課題は、請求項１に記載のＳｍＣｏ系磁性微粒子の製造方法によって解決された。
すなわち、サマリウムアセチルアセトナート水和物からなるサマリウム塩と、コバルトアセチルアセトナートからなるコバルト塩とをグリコール類に溶解して反応溶液を作る過程と、上記反応溶液を十分に攪拌する攪拌過程と、十分に攪拌された上記反応溶液を１５０〜３２０℃に保って反応させる反応過程とを含む、ＳｍＣｏ系磁性微粒子の製造方法によって解決された。

The above-described problem has been solved by the method for producing SmCo-based magnetic fine particles according to claim 1.
That is, a process of making a reaction solution by dissolving a samarium salt composed of samarium acetylacetonate hydrate and a cobalt salt composed of cobalt acetylacetonate in glycols, and a stirring process for sufficiently stirring the reaction solution; The present invention has been solved by a method for producing SmCo-based magnetic fine particles, which comprises a reaction process in which the reaction solution sufficiently stirred is reacted at 150 to 320 ° C.

ここで、好ましくは、サマリウムアセチルアセトナート水和物とコバルトアセチルアセトナートとをテトラエチレングリコールに溶解して反応溶液を作る過程と、上記反応溶液を十分に攪拌する攪拌過程と、上記十分に攪拌された反応溶液を１５０〜３２０℃、好ましくは２５０〜２８０℃に保って反応させる反応過程と、上記反応過程が終わった反応溶液から溶媒を除去し、反応物を固体粉末として取り出す過程を含む、ＳｍＣｏ系磁性微粒子の製造方法によって解決された。さらに、得られた磁性微粒子を安定に分散するためには、ＰＶＰのような保護剤を加えることが好ましい。   Here, preferably, a process of preparing a reaction solution by dissolving samarium acetylacetonate hydrate and cobalt acetylacetonate in tetraethylene glycol, a stirring process of sufficiently stirring the reaction solution, and the sufficient stirring A reaction process in which the reaction solution is reacted at 150 to 320 ° C., preferably 250 to 280 ° C., and a process of removing the solvent from the reaction solution after the reaction process and taking out the reaction product as a solid powder. This has been solved by a method for producing SmCo magnetic fine particles. Further, in order to stably disperse the obtained magnetic fine particles, it is preferable to add a protective agent such as PVP.

上記した本発明に係るＳｍＣｏ系磁性微粒子の製造方法によれば、従来技術においては使われていた、毒性があるコバルトカルボニルＣｏ2（ＣＯ）8を使うことなく、ナノサイズのＳｍＣｏ系磁性微粒子を、化学的方法で作ることができる。 According to the above-described method for producing SmCo magnetic fine particles according to the present invention, nano-sized SmCo magnetic fine particles can be obtained without using toxic cobalt carbonyl Co 2 (CO) 8 , which has been used in the prior art. Can be made by chemical methods.

以下、本発明に係るナノサイズのＳｍＣｏ系磁性微粒子の製造方法の好適な実施の形態を、詳細に記載する。   Hereinafter, preferred embodiments of the method for producing nano-sized SmCo magnetic fine particles according to the present invention will be described in detail.

ＳｍＣｏ系磁性微粒子の製造に使用した反応試薬のリストを、表１に示す。   Table 1 shows a list of reaction reagents used for the production of the SmCo magnetic fine particles.

Figure 0004700374
Figure 0004700374

先ず、表１に示したサマリウムアセチルアセトナート水和物（[CH3COCH=C(O-)CH3]3Sm
・xH2O）２２３．８ｍｇ（０．５ｍｍｏｌ）を、１，４ジオキサン２０ｍｌに溶解させ、第１の溶液を作る。
なお、サマリウムアセチルアセトナート水和物は、この明細書では、 Sm(acac)3・xH2Oと表記することもある。 First, samarium acetylacetonate hydrate ([CH 3 COCH = C (O-) CH 3 ] 3 Sm shown in Table 1)
XH 2 O) 223.8 mg (0.5 mmol) is dissolved in 20 ml of 1,4 dioxane to make a first solution.
In this specification, samarium acetylacetonate hydrate may be expressed as Sm (acac) 3 · xH 2 O.

次に、コバルトアセチルアセトナート（[CH3COCH=C(O-)CH3]3Co ）５３４．４ｍｇ（１．５ｍｍｏｌ）を、１，４ジオキサン２０ｍｌに溶解させ、第２の溶液を作る。
なお、コバルトアセチルアセトナートは、この明細書では、 Co(acac)3と表記することもある。 Next, 534.4 mg (1.5 mmol) of cobalt acetylacetonate ([CH 3 COCH═C (O—) CH 3 ] 3 Co) is dissolved in 20 ml of 1,4 dioxane to form a second solution.
In this specification, cobalt acetylacetonate may be expressed as Co (acac) 3 .

テトラエチレングリコール（HOCH2CH2OCH2CH2OH ）８０ｍｌに、ＰＶＰを１１１０．０ｍｇ（１０．０ｍｍｏｌ）溶解させ、第３の溶液を作る。
ここにおいて、ＰＶＰとは、ポリ（Ｎ−ビニル−２−ピロリドン）、すなわち、（C6H9 ON)nである。なお、ＰＶＰに代えて、他の親水性高分子（例えば、ポリアクリル酸、ポリマレイン酸、ポリグルタミン酸、およびそれらの塩、ビニルアルコール、ポリエチレングリコール、ポリプロピレングリコール、ポリアクリルアミド、ポリビニルアミン、ポリエチレンイミン、あるいはこれらの誘導体および共重合体）を使うことも可能である。 1110.0 mg (10.0 mmol) of PVP is dissolved in 80 ml of tetraethylene glycol (HOCH 2 CH 2 OCH 2 CH 2 OH) to make a third solution.
Here, PVP is poly (N-vinyl-2-pyrrolidone), that is, (C 6 H 9 ON) n . In place of PVP, other hydrophilic polymers (for example, polyacrylic acid, polymaleic acid, polyglutamic acid and salts thereof, vinyl alcohol, polyethylene glycol, polypropylene glycol, polyacrylamide, polyvinylamine, polyethyleneimine, or These derivatives and copolymers) can also be used.

続いて、上記第１の溶液と第２の溶液を、上記第３の溶液に添加して混合し、反応溶液を作る。この際、好ましくは、上記第１の溶液と第２の溶液を、テトラエチレングリコール（例えば１００ｍｌのうちの２０ｍｌ）で洗い流しながら、３口フラスコに流し込んで第３の溶液に添加する。   Subsequently, the first solution and the second solution are added to and mixed with the third solution to make a reaction solution. At this time, preferably, the first solution and the second solution are poured into a three-necked flask while being washed with tetraethylene glycol (for example, 20 ml of 100 ml) and added to the third solution.

ここで重要な点は、サマリウムアセチルアセトナート水和物と、コバルトアセチルアセトナートと、テトラエチレングリコールを混合し、反応溶液を作ることである。
そのため、上記第１の溶液と第２の溶液における第１と第２の溶媒１，４ジオキサンの量はこの例における量である必要はない。ＰＶＰの量も同様に、ここに開示された量でなくてもよい。場合によっては、溶媒の１，４ジオキサンとＰＶＰの量をゼロにすることも可能である。すなわち、サマリウムアセチルアセトナート水和物と、コバルトアセチルアセトナートと、テトラエチレングリコールとを直接的に混合して反応溶液を作ることも可能である。しかし、この実施の形態のように、第１と第２と第３の溶液を先ず作って、これらを混合すると、反応溶液を早く確実に作ることができるという利点がある。 The important point here is that samarium acetylacetonate hydrate, cobalt acetylacetonate and tetraethylene glycol are mixed to form a reaction solution.
Therefore, the amount of the first and second solvents 1,4 dioxane in the first solution and the second solution need not be the amount in this example. Similarly, the amount of PVP may not be the amount disclosed herein. In some cases, the amount of solvent 1,4 dioxane and PVP can be made zero. That is, it is possible to directly mix samarium acetylacetonate hydrate, cobalt acetylacetonate, and tetraethylene glycol to make a reaction solution. However, as in this embodiment, when the first, second and third solutions are first prepared and then mixed, there is an advantage that the reaction solution can be prepared quickly and reliably.

得られた反応溶液を十分に攪拌する。この実施の形態では、メカニカルスターラーを使用し、約１２時間混合した。   The obtained reaction solution is sufficiently stirred. In this embodiment, a mechanical stirrer was used and mixed for about 12 hours.

反応溶液には、水が含まれている可能性があるため、水を除去するため、不活性気体（例えば、窒素、アルゴン）気流下で、油浴を１１０℃に保ち約４０分間維持することが好ましい。   Since the reaction solution may contain water, to remove the water, keep the oil bath at 110 ° C. for about 40 minutes under a stream of inert gas (eg, nitrogen, argon). Is preferred.

続いて、不活性気体（例えば、窒素、アルゴン）気流下で、油浴またはマントルヒータを用いて反応溶液を１５０〜３２０℃、好ましくは２５０〜２８０℃に保ち、約３時間加熱還流し、化学反応を起させる。   Subsequently, the reaction solution is kept at 150 to 320 ° C., preferably 250 to 280 ° C. using an oil bath or a mantle heater under an inert gas (for example, nitrogen, argon) stream, and heated to reflux for about 3 hours. Start the reaction.

これによって、ＳｍＣｏ系磁性微粒子が生成される。反応が終わった後、溶液から溶媒を除き、固体粉末として生成物を得ることもできる。   As a result, SmCo-based magnetic fine particles are generated. After the reaction is complete, the solvent can be removed from the solution to give the product as a solid powder.

固体粉末として生成物を得ることは、例えば、化学反応が終わった後、室温になるまで放置し、その後、ウルトラフィルターを用いて脱水エタノール等で溶液変換と粒子の洗浄を行い、さらに、エバポレータを用いて溶媒を留去し、最後に、１０時間以上かけて４０℃で真空乾燥させることにより、実現できる。   To obtain the product as a solid powder, for example, after the chemical reaction is completed, the product is allowed to stand until it reaches room temperature, and then the solution is converted with dehydrated ethanol using an ultrafilter and the particles are washed. It can be realized by distilling off the solvent and finally vacuum drying at 40 ° C. over 10 hours.

得られた固体粉末の一例について、誘導結合プラズマ発光分析（この明細書では、ＩＣＰ分析とも表記する。）を行った。
その結果は、Ｃｏは２．２７４１ｐｐｍで、Ｓｍは１．００４３ｐｐｍであった。すなわち、この試料の場合、Ｓｍ：Ｃｏの比率はほぼ１： ５．６であり、バルク状態で良好な磁気的性質を持つ物質として知られている、ＳｍＣｏ5に近い物質が生成されたと考えられる。 An example of the obtained solid powder was subjected to inductively coupled plasma emission analysis (also referred to as ICP analysis in this specification).
As a result, Co was 2.2741 ppm and Sm was 1.0043 ppm. That is, in the case of this sample, the ratio of Sm: Co is approximately 1: 5.6, and it is considered that a substance close to SmCo 5 , which is known as a substance having a good magnetic property in a bulk state, was produced. .

なお、上記結果は一例に過ぎず、ＳｍとＣｏの材料物質の仕込み量を変えることにより、種々の比率のＳｍとＣｏの合金を製造することができる。   Note that the above result is merely an example, and various ratios of Sm and Co alloys can be produced by changing the amount of Sm and Co material materials charged.

図１は、得られた固体粉末の一例についての透過電子顕微鏡写真であり、図２は、図１の結果に基づいて求めた粒度分布図である。
図２から分るように、粒径は３から７ｎｍに分布しており、平均粒径４．５ｎｍ、標準偏差０．７８ｎｍと比較的均一なものであった。このように、１０ナノメータ以下の粒径のナノ粒子が生成されることが分った。 FIG. 1 is a transmission electron micrograph of an example of the obtained solid powder, and FIG. 2 is a particle size distribution diagram obtained based on the results of FIG.
As can be seen from FIG. 2, the particle size was distributed from 3 to 7 nm, and was relatively uniform with an average particle size of 4.5 nm and a standard deviation of 0.78 nm. Thus, it was found that nanoparticles having a particle size of 10 nanometers or less were generated.

また、図３は、得られたＳｍＣｏ合金ナノ粒子をＳＱＵＩＤを用いて、磁場（単位Ｏｅ）の関数として磁化（単位ｅｍｕ／ｇ）を測定した磁化曲線である。
この図から分るように、３００Ｋにおける飽和磁化は１００ｅｍｕ／ｇ、保磁力は５００Ｏｅであった。化学的直接合成法による１０ナノメータ以下のＳｍＣｏ系ナノ粒子で、常温においてこのような保磁力を示した報告例はまだない。 FIG. 3 is a magnetization curve obtained by measuring the magnetization (unit emu / g) of the obtained SmCo alloy nanoparticles as a function of the magnetic field (unit Oe) using SQUID.
As can be seen from this figure, the saturation magnetization at 300 K was 100 emu / g, and the coercive force was 500 Oe. There is no report yet showing such a coercive force at room temperature with SmCo nanoparticles of 10 nanometers or less by a chemical direct synthesis method.

以上、本発明に係るＳｍＣｏ系磁性微粒子の製造方法の好適な実施の形態を説明したが、本発明は、何ら既述の実施の形態に限定されず、特許請求の範囲に記載した本発明の技術的思想の範囲内において、種々の変形及び変更が可能であることは当然である。   The preferred embodiments of the method for producing SmCo-based magnetic fine particles according to the present invention have been described above. However, the present invention is not limited to the above-described embodiments, and the present invention described in the claims is not limited thereto. It goes without saying that various modifications and changes are possible within the scope of the technical idea.

例えば、上記反応で親水性高分子ＰＶＰに代えて、あるいは上記親水性高分子と共に、アルキル基やアリル基の付いたアミン類、カルボン酸類、フォスフィン類、フォスフィンオキシド類、アミド類、チオール類などの、低分子量配位子を用いることも可能である。 なお、これらの高分子や低分子量配位子は、反応前に添加しても、あるいは、反応後に添加しても構わない。   For example, amines, carboxylic acids, phosphine, phosphine oxides, amides, thiols, etc. having an alkyl group or an allyl group instead of the hydrophilic polymer PVP in the above reaction or together with the hydrophilic polymer It is also possible to use a low molecular weight ligand. These polymers and low molecular weight ligands may be added before the reaction or after the reaction.

低分子量の配位子、例えば、オレイン酸１ｍｍｏｌとオレイルアミン１ｍｍｏｌを用いて、同様に反応処理し、ウルトラフィルターの代わりに、メタノールやエタノールで再沈処理により分離すると、固体粉末としてＳｍＣｏ合金ナノ粒子を得ることができる。
このときの粒子径は３０ｎｍであり、保磁力は５００Ｏｅであった。 Using a low molecular weight ligand, for example, 1 mmol of oleic acid and 1 mmol of oleylamine, the same reaction treatment is carried out, and when separated by reprecipitation treatment with methanol or ethanol instead of an ultrafilter, SmCo alloy nanoparticles are obtained as solid powder. Obtainable.
The particle diameter at this time was 30 nm, and the coercive force was 500 Oe.

また、上記反応で、オレイン酸１ｍｍｏｌとオレイルアミン１ｍｍｏｌの代わりに、トリブチルフォスフィン１ｍｍｏｌとドデシルアミン１ｍｍｏｌを用いて処理すると、粒子径１２ｎｍのＳｍＣｏ合金ナノ粒子を得ることができた。このときの保磁力は１５０Ｏｅであった。   Further, in the above reaction, when treated with 1 mmol of tributylphosphine and 1 mmol of dodecylamine instead of 1 mmol of oleic acid and 1 mmol of oleylamine, SmCo alloy nanoparticles having a particle diameter of 12 nm could be obtained. The coercive force at this time was 150 Oe.

得られたＳｍＣｏ合金ナノ粒子の固体粉末の透過電子顕微鏡写真である。It is the transmission electron micrograph of the solid powder of the obtained SmCo alloy nanoparticle. 図１の結果に基づいて求めたＳｍＣｏ合金ナノ粒子の粒度分布図である。FIG. 2 is a particle size distribution diagram of SmCo alloy nanoparticles obtained based on the results of FIG. 1. 得られたＳｍＣｏ合金ナノ粒子をＳＱＵＩＤを用いて、磁場（単位Ｏｅ）の関数として磁化（単位ｅｍｕ／ｇ）を測定した磁化曲線である。It is the magnetization curve which measured magnetization (unit emu / g) as a function of a magnetic field (unit Oe) using the SQUID obtained SmCo alloy nanoparticle.

Claims (9)

サマリウムアセチルアセトナート水和物からなるサマリウム塩と、コバルトアセチルアセトナートからなるコバルト塩とをグリコール類に溶解して反応溶液を作る過程と、上記反応溶液を十分に攪拌する攪拌過程と、十分に攪拌された上記反応溶液を１５０〜３２０℃に保って反応させる反応過程とを含むことを特徴とする、ＳｍＣｏ系磁性微粒子の製造方法。 A process of making a reaction solution by dissolving a samarium salt composed of samarium acetylacetonate hydrate and a cobalt salt composed of cobalt acetylacetonate in glycols, a stirring process for sufficiently stirring the reaction solution, And a reaction process of reacting the stirred reaction solution at 150 to 320 ° C. 上記反応溶液を作る過程が、サマリウム塩を第１の溶媒に溶解させて第１の溶液を作る過程と、コバルト塩を第２の溶媒に溶解させて第２の溶液を作る過程と、第３の溶媒に、親水性高分子を溶解させて第３の溶液を作る過程と、上記第１の溶液と第２の溶液を第３の溶液に添加し混合して上記反応溶液を作る過程とを含むことを特徴とする、請求項１記載のＳｍＣｏ系磁性微粒子の製造方法。   The process of preparing the reaction solution includes a process of dissolving the samarium salt in the first solvent to make the first solution, a process of dissolving the cobalt salt in the second solvent to make the second solution, and a third process. A step of dissolving the hydrophilic polymer in the solvent to make a third solution, and a step of adding the first solution and the second solution to the third solution and mixing to make the reaction solution. The method for producing SmCo-based magnetic fine particles according to claim 1, comprising: 上記第１、２、３の溶媒のいずれかが、エチレングリコール、ジエチレングリコール、トリエチレングリコール、テトラエチレングリコール、ペンタエチレングリコール、１, ３−プロパンジオール、１，２−へキサンジオール、２−メチル−２，４−ペンタンジオールなどのグリコール類であることを特徴とする、請求項２記載のＳｍＣｏ系磁性微粒子の製造方法。Any of the first, second and third solvents is ethylene glycol, diethylene glycol, triethylene glycol, tetraethylene glycol, pentaethylene glycol, 1,3-propanediol, 1,2-hexanediol, 2-methyl- The method for producing SmCo-based magnetic fine particles according to claim 2, which is a glycol such as 2,4-pentanediol. 上記第１、２、３の溶媒のいずれかが、１，４−ジオキサン、フェニルエーテル、オクチルエーテルなどの比較的高沸点のエーテル類を含むことを特徴とする、請求項３記載のＳｍＣｏ系磁性微粒子の製造方法。4. The SmCo-based magnetism according to claim 3, wherein any one of the first, second, and third solvents contains a relatively high boiling point ether such as 1,4-dioxane, phenyl ether, octyl ether, or the like. A method for producing fine particles. 上記親水性高分子が、ポリビニルピロリドン（ＰＶＰ）、ポリアクリル酸、ポリマレイン酸、ポリグルタミン酸、およびそれらの塩、ビニルアルコール、ポリエチレングリコール、ポリプロピレングリコール、ポリアクリルアミド、ポリビニルアミン、ポリエチレンイミン、あるいはこれらの誘導体および共重合体、のいずれかであることを特徴とする、請求項２記載のＳｍＣｏ系磁性微粒子の製造方法。The hydrophilic polymer is polyvinyl pyrrolidone (PVP), polyacrylic acid, polymaleic acid, polyglutamic acid, and salts thereof, vinyl alcohol, polyethylene glycol, polypropylene glycol, polyacrylamide, polyvinylamine, polyethyleneimine, or derivatives thereof. The method for producing SmCo-based magnetic fine particles according to claim 2, wherein: 上記親水性高分子の代わりに、あるいは上記親水性高分子と共に、アルキル基やアリル基の付いたアミン類、カルボン酸類、フォスフィン類、フォスフィンオキシド類、アミド類、チオール類などの、低分子量配位子を用いることを特徴とする、請求項２記載のＳｍＣｏ系磁性微粒子の製造方法。Low molecular weight distribution of amines, carboxylic acids, phosphines, phosphine oxides, amides, thiols, etc. with an alkyl group or allyl group instead of or together with the hydrophilic polymer. A method for producing SmCo-based magnetic fine particles according to claim 2, wherein a ligand is used. 上記攪拌過程と上記反応過程の中間に、上記反応溶液を１１０℃程度に保持し、水分を除去する水分除去過程を含むことを特徴とする、請求項１または２記載のＳｍＣｏ系磁性微粒子の製造方法。The production of SmCo-based magnetic fine particles according to claim 1 or 2, comprising a water removal step of holding the reaction solution at about 110 ° C and removing water between the stirring step and the reaction step. Method. 上記反応過程が終わった上記反応溶液から溶媒を除去し、生成物を固体粉末として取り出すことを特徴とする、請求項１または２記載のＳｍＣｏ系磁性微粒子の製造方法。The method for producing SmCo-based magnetic fine particles according to claim 1 or 2, wherein the solvent is removed from the reaction solution after the reaction process and the product is taken out as a solid powder. 上記反応過程が終わった後、室温になるまで放置し、その後、ウルトラフィルターを用い脱水エタノール等で溶液変換と粒子の洗浄を行い、さらに、エバポレータを用いて溶媒を留去し、最後に、真空乾燥させることにより、生成物を固体粉末として取り出すことを特徴とする、請求項１または２記載のＳｍＣｏ系磁性微粒子の製造方法。After completion of the above reaction process, leave it to room temperature, then perform solution conversion and washing of particles with dehydrated ethanol etc. using an ultra filter, further evaporate the solvent using an evaporator, and finally vacuum 3. The method for producing SmCo magnetic fine particles according to claim 1, wherein the product is taken out as a solid powder by drying.
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104439283A (en) * 2014-11-26 2015-03-25 吉林吉恩镍业股份有限公司 Method for preparing nanometer cobalt powder

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* Cited by examiner, † Cited by third party
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JP2010212501A (en) * 2009-03-11 2010-09-24 Tdk Corp Exchange spring magnetic powder
CN103413644A (en) * 2013-07-25 2013-11-27 中国石油大学(华东) Method for preparing samarium cobalt magnetic powder
CN105070497B (en) * 2015-08-25 2017-08-25 广西大学 Cobalt-based single molecular magnetses synthetic method

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2002062509A1 (en) * 2001-02-08 2002-08-15 Hitachi Maxell, Ltd. Metal alloy fine particles and method for production thereof
JP2003277803A (en) * 2002-03-27 2003-10-02 Kazuyuki Taji Metal magnetic particle and manufacturing method
JP2004043287A (en) * 2002-04-17 2004-02-12 Internatl Business Mach Corp <Ibm> Synthesis of magnetite nanoparticle and method of forming nanomaterial using iron as base
JP2006131960A (en) * 2004-11-05 2006-05-25 Fuji Photo Film Co Ltd Method for producing magnetic nanoparticle, magnetic nanoparticle obtained thereby and magnetic recording medium

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CA2499318A1 (en) * 2002-09-18 2004-04-22 Angela M. Belcher Peptide mediated synthesis of metallic and magnetic materials

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2002062509A1 (en) * 2001-02-08 2002-08-15 Hitachi Maxell, Ltd. Metal alloy fine particles and method for production thereof
JP2003277803A (en) * 2002-03-27 2003-10-02 Kazuyuki Taji Metal magnetic particle and manufacturing method
JP2004043287A (en) * 2002-04-17 2004-02-12 Internatl Business Mach Corp <Ibm> Synthesis of magnetite nanoparticle and method of forming nanomaterial using iron as base
JP2006131960A (en) * 2004-11-05 2006-05-25 Fuji Photo Film Co Ltd Method for producing magnetic nanoparticle, magnetic nanoparticle obtained thereby and magnetic recording medium

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104439283A (en) * 2014-11-26 2015-03-25 吉林吉恩镍业股份有限公司 Method for preparing nanometer cobalt powder

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