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成果報告書詳細
管理番号20180000000103
タイトル*平成29年度中間年報 エネルギー・環境新技術先導プログラム/ナノ結晶クラスター組織からなる革新的磁性材料の創製
公開日2018/12/27
報告書年度2017 - 2017
委託先名国立大学法人東北大学 大陽日酸株式会社 関東電化工業株式会社
プロジェクト番号P14004
部署名イノベーション推進部
和文要約1. 研究開発の内容及び成果等
研究項目A.高性能ガス反応装置の設計・製作
(担当:大陽日酸株式会社、東北大学)
Fe-Coナノ粒子にC、Nを目標量導入できる装置を完成させた。

研究項目B.Coを含む酸化鉄ナノ粒子の合成技術の確立
(担当:関東電化工業株式会社)
酸化鉄のFeの一部をCoで30 %まで置換したナノ粒子の合成に成功し目標を達成した。

研究項目C.Fe-Coナノクラスター組織の制御
(担当:東北大学)
ナノクラスター組織を形成させることには成功したが最終的な保磁力Hcと結晶子径の関係は必ずしも一義的な結果となっておらず、今後詳しい検証とさらなる結晶子の大きさの低減に向けた実験を行うことにしている。

研究項目D.ガス反応条件の確立
(担当:東北大学、大陽日酸株式会社)
Fe-Coに第三元素が入り込むことが確認できた。
引き続き電子回折や光電子分光法を駆使して各元素の存在形態についても解析を進めていく。

研究項目E.規則度制御条件の確立
(担当:東北大学)
本プロジェクトで高感度X線回折装置を導入し規則度の評価を可能にした。
今回合成したFe-Co-C-Nナノ粒子におけるNの規則度は、完全に規則化している場合の70 %程度であり、Nの規則度が減少していることがわかった。今後、種々の合成条件と規則度の関係を評価しN配位のメカニズムを追求するとともに、Hcとの関係を明らかにし、軟磁性を導出する。
英文要約A. Design and production of the high performance gas reaction equipment
The high performance gas reaction equipment which enables the introduction of C and N to Fe-Co nanoparticles by gas phase solid phase contact reaction was designed and constructed. Automatic shutoff system by the gas leak detection, emergency gas substitution system, prevention of backfire valve, and pressure release valve etc., were equipped for safety. Temperature control during gas reaction was enabled in the range of ±1 degrees Celsius for setting temperature. Furthermore, oxygen concentration in the atmosphere in the tubular furnace was lower than 10 ppm was realized. Target value of C concentration introduced into Fe-Co nanoparticles was achieved by this high performance gas reaction equipment.
B. Establishment of the synthetic method of iron oxide nanoparticles including Co
Synthetic method of the nanoparticles which replaced a part of the Fe of iron oxide with Co was examined. Iron oxides which Co concentration for Fe varied from 2 % to 30 % were synthesized to examine magnetic properties changes by Co addition. These were confirmed that Co was distributed uniformly in the iron oxides, and quantity of Co was adjusted near to the targeted value. We succeeded in the synthesis of the nanoparticles which replaced a part of the Fe of the iron oxides with Co up to 30 %.
C. Control of the Fe-Co nano cluster microstructure
Crystallite size of Fe-Co nanoparticles around a number of 10 nm was realized by gas reaction treatment, and it was revealed that the crystallite size grew large a little when Co was included. We succeeded in forming a nanocluster structure. But it has not been clear that the relationship between coercive force Hc and crystallite size. Further investigation will be necessary.
D. Establishment of gas reaction conditions
The gas reaction conditions to synthesize Fe-Co-C-N nanoparticles which show soft magnetic properties were investigated. Saturation magnetic induction Bs increased at the same time as Hc decreased by introducing C and N into Fe-Co nanoparticles. Bs more than 2.0 T, and Hc under 100 Oe were achieved. Target values of Bs and Hc for first 1 year of this research and development project were almost all achieved. In general, Bs and Hc show the tendency of the trade-off, but this Fe-Co-C-N alloy indicates the possibility that having low Hc with high Bs at the same time. Microstructure of Fe-Co-C-N nanoparticles resemble metallographic structure called martensite of bulk steel materials, We will aim at the soft magnetic characteristic improvement by the examination of further gas reaction conditions.
E. Control of the degree of order
In order to evaluate the degree of order of N, we introduced a high sensitive X-ray diffractometer by this project. The degree of order of N in Fe-Co-C-N nanoparticles was estimated around 70 % compared to perfect of the degree of order. Investigation to clarify the relationship between Hc and the degree of order of N will be continued to active soft magnetic properties.
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