JP2010138468A - Method for manufacturing cobalt nanoparticle - Google Patents
Method for manufacturing cobalt nanoparticle Download PDFInfo
- Publication number
- JP2010138468A JP2010138468A JP2008318132A JP2008318132A JP2010138468A JP 2010138468 A JP2010138468 A JP 2010138468A JP 2008318132 A JP2008318132 A JP 2008318132A JP 2008318132 A JP2008318132 A JP 2008318132A JP 2010138468 A JP2010138468 A JP 2010138468A
- Authority
- JP
- Japan
- Prior art keywords
- cobalt
- nanoparticles
- precursor
- serving
- cobalt nanoparticles
- 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
Images
Abstract
Description
本発明は、ナノサイズの粒径を有し、単分散であるコバルトナノ粒子の製造方法に関する。 The present invention relates to a method for producing monodispersed cobalt nanoparticles having a nano-sized particle size.
従来、磁性金属などからなるナノメータ（ｎｍ）サイズの金属粒子が知られている。その製造方法として液相合成法がある。液相合成法とは、金属塩、有機金属化合物などを液中に溶解させ、還元又は分解等により、金属微粒子を析出させる方法である。公知の液相合成法として、共沈法、アルコール還元法、有機金属化合物の熱分解法、逆ミセル法、超音波法、エレクトライド還元法などがある。各手法により合成された金属微粒子の形状及び粒径の均一性、収量、取り扱いの難易を考慮すると、金属微粒子は、アルコール還元法又は有機金属化合物の熱分解により得る方法が適している。 Conventionally, metal particles of nanometer (nm) size made of magnetic metal or the like are known. As a manufacturing method thereof, there is a liquid phase synthesis method. The liquid phase synthesis method is a method in which a metal salt, an organometallic compound, or the like is dissolved in a liquid and metal fine particles are precipitated by reduction or decomposition. Known liquid phase synthesis methods include a coprecipitation method, an alcohol reduction method, a thermal decomposition method of an organometallic compound, a reverse micelle method, an ultrasonic method, and an electride reduction method. Considering the uniformity of the shape and particle size of the metal fine particles synthesized by each method, the yield, and the difficulty of handling, the metal fine particles are suitably obtained by alcohol reduction or thermal decomposition of an organometallic compound.
下記特許文献１には、エーテル溶媒中で塩化コバルトをＣｏ前駆体として、オレイン酸とトリオクチルホスフィン（ＴＯＰ）を保護配位子として、スーバーヒドリドを還元剤として用いて、不活性雰囲気下、２００℃で反応させることにより、２〜６ｎｍのＣｏナノ粒子を生成することが開示されている。 In Patent Document 1 below, cobalt chloride is used as a Co precursor in an ether solvent, oleic acid and trioctylphosphine (TOP) are used as protective ligands, and superhydride is used as a reducing agent under an inert atmosphere. It is disclosed to produce 2-6 nm Co nanoparticles by reacting at 0 ° C.
しかし、特許文献１で得られるＣｏナノ粒子は、単分散性に欠けるという問題があった。
又、下記非特許文献１に開示された既存の手法では、粒径が大きく、多分散な粒子が生成してしまうという問題があった。
However, the Co nanoparticles obtained in Patent Document 1 have a problem of lacking monodispersity.
In addition, the existing method disclosed in the following Non-Patent Document 1 has a problem that the particle size is large and polydispersed particles are generated.
本発明は、粒径が小さく、且つより単分散なコバルトナノ粒子を製造することを目的とする。 The object of the present invention is to produce cobalt nanoparticles having a smaller particle size and more monodisperse.
本発明者は、特定の、コバルト前駆体を用いることで、上記課題が解決されることを見出し、本発明に到達した。
即ち、本発明は、コバルトナノ粒子の製造方法の発明であり、ジオクチルエーテル溶媒中で、コバルト前駆体である安息香酸コバルトと、保護配位子であるオレイン酸及びトリオクチルホスフィンと、還元剤であるスーパーヒドリドとを、不活性雰囲気下、２００℃以上で反応させることを特徴とする。
The present inventor has found that the above problem can be solved by using a specific cobalt precursor, and has reached the present invention.
That is, the present invention is an invention of a method for producing cobalt nanoparticles, and in a dioctyl ether solvent, cobalt benzoate as a cobalt precursor, oleic acid and trioctylphosphine as protective ligands, and a reducing agent. It is characterized by reacting with a certain superhydride at 200 ° C. or higher in an inert atmosphere.
本発明により、粒径が小さく、且つ従来のコバルトナノ粒子より単分散であるコバルトナノ粒子を製造することができる。 According to the present invention, cobalt nanoparticles having a small particle size and monodispersed from conventional cobalt nanoparticles can be produced.
以下、実施例および比較例によって本発明をさらに詳細に説明する。
［実施例］
図１に示す、コバルトナノ粒子の製造スキームに従って、コバルトナノ粒子を製造した。ここで、コバルト前駆体として安息香酸コバルトを用い、保護配位子としてオレイン酸（ＯＡｃ）及びトリオクチルホスフィン（ＴＯＰ）を用い、還元剤であるスーパーヒドリドとしてＬｉＢＥｔ３Ｈを用いた。
Hereinafter, the present invention will be described in more detail with reference to Examples and Comparative Examples.
[Example]
Cobalt nanoparticles were produced according to the cobalt nanoparticle production scheme shown in FIG. Here, cobalt benzoate was used as a cobalt precursor, oleic acid (OAc) and trioctylphosphine (TOP) were used as protective ligands, and LiBEt 3 H was used as a superhydride as a reducing agent.
図２に、得られたコバルトナノ粒子の電子顕微鏡写真を示す。３〜５ｎｍの単分散コバルトナノ粒子が生成していることが確認された。 FIG. 2 shows an electron micrograph of the obtained cobalt nanoparticles. It was confirmed that 3 to 5 nm monodispersed cobalt nanoparticles were generated.
［比較例１］
コバルト前駆体として酢酸コバルトを用いたほかは、実施例と同様にして、コバルトナノ粒子を製造した。
[Comparative Example 1]
Cobalt nanoparticles were produced in the same manner as in the Examples except that cobalt acetate was used as the cobalt precursor.
図３に、得られたコバルトナノ粒子の電子顕微鏡写真を示す。４〜７ｎｍの粒子径が異なるコバルトナノ粒子が生成していることが確認された。 FIG. 3 shows an electron micrograph of the obtained cobalt nanoparticles. It was confirmed that cobalt nanoparticles having different particle diameters of 4 to 7 nm were generated.
［比較例２］
コバルト前駆体として塩化コバルトを用いたほかは、実施例と同様にして、コバルトナノ粒子を製造した。
[Comparative Example 2]
Cobalt nanoparticles were produced in the same manner as in the Examples except that cobalt chloride was used as the cobalt precursor.
図４に、得られたコバルトナノ粒子の電子顕微鏡写真を示す。実施例と比較して粒子が２〜２０ｎｍと大きく、多分散のコバルトナノ粒子が生成していることが確認された。 FIG. 4 shows an electron micrograph of the obtained cobalt nanoparticles. It was confirmed that polydispersed cobalt nanoparticles were generated with particles as large as 2 to 20 nm as compared with Examples.
上記のようなカルボキシル基を含むＣｏ前駆体ではカルボキシル基は中心Ｃｏとキレート配位を形成しており、塩化コバルトと比較して、Ｃｏ−配位子間の結合力は小さい。そのため、熱分解が容易に起こり、核形成と核成長を適切に制御できると考えられる。 In the Co precursor containing a carboxyl group as described above, the carboxyl group forms a chelate coordination with the central Co, and the binding force between the Co-ligand is smaller than that of cobalt chloride. Therefore, it is considered that thermal decomposition occurs easily, and nucleation and growth can be appropriately controlled.
コバルト前駆体として安息香酸コバルトを用いることにより、粒径が小さく、且つ従来のコバルトナノ粒子より単分散であるコバルトナノ粒子を製造することができる。 By using cobalt benzoate as a cobalt precursor, cobalt nanoparticles having a small particle size and monodispersed than conventional cobalt nanoparticles can be produced.
Claims (1)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2008318132A JP2010138468A (en) | 2008-12-15 | 2008-12-15 | Method for manufacturing cobalt nanoparticle |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2008318132A JP2010138468A (en) | 2008-12-15 | 2008-12-15 | Method for manufacturing cobalt nanoparticle |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JP2010138468A true JP2010138468A (en) | 2010-06-24 |
Family
ID=42348838
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2008318132A Pending JP2010138468A (en) | 2008-12-15 | 2008-12-15 | Method for manufacturing cobalt nanoparticle |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2010138468A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106077691A (en) * | 2016-05-30 | 2016-11-09 | 湖州师范学院 | A kind of metallic cobalt microsphere |
| CN106077692A (en) * | 2016-05-30 | 2016-11-09 | 湖州师范学院 | A kind of preparation method of metallic cobalt microsphere |
| CN114905049A (en) * | 2022-05-11 | 2022-08-16 | 江南大学 | Chiral cobalt super particle and preparation method thereof |
-
2008
- 2008-12-15 JP JP2008318132A patent/JP2010138468A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106077691A (en) * | 2016-05-30 | 2016-11-09 | 湖州师范学院 | A kind of metallic cobalt microsphere |
| CN106077692A (en) * | 2016-05-30 | 2016-11-09 | 湖州师范学院 | A kind of preparation method of metallic cobalt microsphere |
| CN114905049A (en) * | 2022-05-11 | 2022-08-16 | 江南大学 | Chiral cobalt super particle and preparation method thereof |
| CN114905049B (en) * | 2022-05-11 | 2023-06-02 | 江南大学 | Chiral cobalt super-particle and preparation method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Fiévet et al. | The polyol process: a unique method for easy access to metal nanoparticles with tailored sizes, shapes and compositions | |
| Seo et al. | Polyvinylpyrrolidone (PVP) effects on iron oxide nanoparticle formation | |
| Lignier et al. | Scalable strategies for the synthesis of well-defined copper metal and oxide nanocrystals | |
| Wang et al. | Shape-control and characterization of magnetite prepared via a one-step solvothermal route | |
| Li et al. | Synthesis of hexagonal and triangular Fe 3 O 4 nanosheets via seed-mediated solvothermal growth | |
| KR100869026B1 (en) | Spherical assembly particle composition of cuprous oxide and preparation method thereof | |
| Fereshteh et al. | Effect of ligand on particle size and morphology of nanostructures synthesized by thermal decomposition of coordination compounds | |
| CN103537293B (en) | For the preparation of Catalysts and its preparation method and the application of chiral selectivity and the selective SWCN of electric conductivity | |
| JP5558826B2 (en) | Method for producing iron or iron oxide nanopowder particles | |
| Ma et al. | Novel synthesis and characterization of bismuth nano/microcrystals with sodium hypophosphite as reductant | |
| Wang et al. | Tailored synthesis of various Au nanoarchitectures with branched shapes | |
| JP2005336530A (en) | Flock of nanoparticles of magnetic metal, and manufacturing method therefor | |
| Wang et al. | Solution synthesis of triangular and hexagonal nickel nanosheets with the aid of tungsten hexacarbonyl | |
| JP5448673B2 (en) | Method for producing composite oxide nanoparticles | |
| Logutenko et al. | Characterization and growth mechanism of nickel nanowires resulting from reduction of nickel formate in polyol medium | |
| US20220241857A1 (en) | Synthetic method for preparing small palladium nanocubes | |
| Sadeghi et al. | Nanoplates controlled synthesis and catalytic activities of silver nanocrystals | |
| JP2010138468A (en) | Method for manufacturing cobalt nanoparticle | |
| JP2013524021A (en) | Mass production method of silver nanoparticles having uniform size | |
| JP2009097038A (en) | PRODUCTION METHOD OF FePt NANOPARTICLE | |
| JP2009215583A (en) | Sm-Co-BASED ALLOY NANOPARTICLE, AND METHOD FOR PRODUCING THE SAME | |
| JP2011184725A (en) | Method for synthesizing cobalt nanoparticle by hydrothermal reduction process | |
| Chen et al. | Template-free synthesis and characterization of dendritic cobalt microstructures by hydrazine reduction route | |
| JP2008188573A (en) | Fine particle manufacturing method | |
| Murugesan et al. | An Overview on synthesis of metal oxide nanoparticles |