The Development for In-situ Observation of Chemical Reaction between Solid and Solid

固体与固体间化学反应原位观测研究进展

• 批准号: 17560656
• 负责人: ISHIKAWA Nobuhiro
• 金额: $ 2.16万
• 依托单位: National Institute for Materials Science
• 依托单位国家: 日本
• 项目类别: Grant-in-Aid for Scientific Research (C)
• 财政年份: 2005
• 资助国家: 日本
• 起止时间: 2005 至 2007
• 项目状态: 已结题
• 来源: https://kaken.nii.ac.jp/grant/KAKENHI-PROJECT-17560656/
• 关键词: TEM; In-situ observation; Wustite; Iime; alumina; Boundary; 酸化アルミニウム; 二酸化ケイ素; 炭素蒸着; 酸化カルシウム; ヘマタイト; 固体接触技術; その場解析; 化学反応; 酸化鉄; 試料作製技術

The reduction of iron oxides has been one of the most frequently studied topics in iron smelting. Transmission electron microscope (TEM) was used for in-situ observation of microscopic analysis. But the applications were mainly focused on the gas-solid reaction such as using CO or H as reductant. The coke i.e. solid state carbon is used in iron industry and the solid state carbon is also important reductant. The aim of this study is to realize in-situ observation of the chemical reaction between solid and slid such as carbon and iron-oxides in TEM. We used wustite as an iron-oxide and carbon-deposition was applied to get solid/solid boundary between carbon and wustite. The fracture surface was applied to get the clean surface of wustite. The carbon was deposited on the fracture surface to contact with wustite. The preparation of the specimen was done with the size of thin foil of TEM sample. In-situ observation was performed at elevated temperature. The precipitates were generated at the boundary of wustite and carbon and grew into the carbon layer at the higher temperature about over 873K. The energy dispersive X-ray spectroscopy (EDS) showed that the precipitates were pure iron. The effect of lime and alumina as impurities were also investigated. The increase of the concentration of impurities caused suppress the precipitation and growth of Fe even up to 1073K. These results indicated that the Ca and Al played as barriers to the reduction of FeO.

氧化铁的还原一直是铁冶炼中最常研究的课题之一。采用透射电镜（TEM）进行现场观察。但其应用主要集中在以CO或H为还原剂的气固反应中。焦炭即固态碳用于炼铁工业，固态碳也是重要的还原剂。本研究的目的是在TEM中实现固体与碳、铁等氧化物之间化学反应的原位观察。我们以浮氏体作为铁氧化物，用沉积碳的方法得到了碳与浮氏体的固/固边界。对断口表面进行了处理，得到了清洁的浮氏体表面。碳沉积在断口表面，与浮氏体接触。样品的制备是根据TEM样品的薄片大小来完成的。在高温下进行原位观察。析出相产生于浮氏体与碳的边界，并在873K以上的高温下生长到碳层中。能谱分析（EDS）表明析出物为纯铁。还考察了石灰和氧化铝作为杂质的影响。杂质浓度的增加抑制了Fe的析出和生长，最高可达1073K。这些结果表明Ca和Al是FeO还原的障碍。

项目成果

固体炭素による酸化鉄還元TEM内その場観察

使用固体碳还原氧化铁的 TEM 原位观察

• 发表时间: 2006
• 期刊: 鉄と鋼 192
• 作者: T. Inami.;et. al.;N.Ishikawa;N.Ishikawa;T.Kimura;石川 信博
• 通讯作者: 石川 信博

The Structural Analysis of the Immersed-Au between a Sn-Zn Based Lead Free Solder and a Substrate

Sn-Zn基无铅焊料与基材之间浸金结构分析

• 发表时间: 2006
• 作者: 石川 信博;他;N.Ishikawa;石川 信博;M.Song;N.Ishikawa;N. Ishikawa;N. Ishikawa;N. Ishikawa;M. Song;N. Ishikawa;Kwang-Jin Lee;N.Ishikawa;N.Ishikawa;石川 信博;光岡 那由多;K. wang-Jin. Lee;N. Ishikawa
• 通讯作者: N. Ishikawa

The in-situ observation of the reaction at the boundary of Iron oxides and Carbon in TEM

TEM原位观察铁氧化物和碳界面的反应

• 发表时间: 2005
• 作者: 石川 信博;他;N.Ishikawa;石川 信博;M.Song;N.Ishikawa;N. Ishikawa;N. Ishikawa;N. Ishikawa;M. Song;N. Ishikawa;Kwang-Jin Lee;N.Ishikawa;N.Ishikawa;石川 信博;光岡 那由多;K. wang-Jin. Lee;N. Ishikawa;N. Ishikawa;N. Mitsuoka;石川 信博;N. Ishikawa
• 通讯作者: N. Ishikawa

Growth Manner of Intermetallic Compounds at the Weld Interface of Steel/Aluminum Alloy Lap Joint Fabricated by a Defocused Laser Beam

• DOI: 10.2320/matertrans.l-mra2007838
• 发表时间: 2007-06
• 期刊: Materials Transactions
• 影响因子: 1.2
• 作者: Kwang-jin Lee;S. Kumai;Naonori Kawamura;N. Ishikawa;K. Furuya

Surface Modification of Gamma-Titanum Aluminides with L12-type Tri-Aluminides by Pack Cementation

L12型三铝化物包埋法表面改性γ-钛铝化物

• 发表时间: 2005
• 期刊: Mat.Trans. 46
• 作者: T. Inami.;et. al.;N.Ishikawa;N.Ishikawa;T.Kimura;石川 信博;N. Ishikawa;N. Ishikawa;T. Kimura;N. Ishikawa;N.Ishikawa;N.Ishikawa;石川 信博;Kwant-Jin Lee;T.Kimura
• 通讯作者: T.Kimura