液态Al氧化的环境透射电镜观察

蔡俊; 凌国平; 陈长安; 张桂凯

doi:10.3724/SP.J.1037.2013.00165

金属学报 >

2013 , Vol. 49 >Issue 8: 953 - 958

DOI: https://doi.org/10.3724/SP.J.1037.2013.00165

论文

液态Al氧化的环境透射电镜观察

蔡俊 ,
凌国平 ,
陈长安 ,
张桂凯

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1)浙江大学材料科学与工程学系, 杭州 310027
2)中国工程物理研究院表面物理与化学国家重点实验室, 绵阳 621907

蔡俊, 男, 1986年生, 博士生

收稿日期: 2013-03-24

修回日期: 2013-06-13

网络出版日期: 2013-08-11

基金资助

中国工程物理研究院表面物理与化学国家重点实验室开放基金资助项目SPC201101

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OBSERVATION ON THE OXIDATION OF LIQUID Al BY ENVIRONMENTAL TRANSMISSION ELECTRON MICROSCOPE

CAI Jun ,
LING Guoping ,
CHEN Changan ,
ZHANG Guikai

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1)Department of Materials Science and Engineering, Zhejiang University, Hangzhou 310027
2)State Key Laboratory of Surface Physics and Chemistry, China Academy of Engineering Physics, Mianyang 621907

Received date: 2013-03-24

Revised date: 2013-06-13

Online published: 2013-08-11

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摘要

为研究液态Al初期氧化产物的相组成及其氧化机理,采用环境透射电镜(E-TEM)对纳米Al粉末在720℃时的氧化进行了原位观察.差热分析(DTA)和TEM形貌观察结果表明, 纳米Al粉末表面存在5—6 nm厚的非晶Al₂O₃膜,该非晶膜在350—550℃间转变为γ-Al₂O₃.纳米Al粉末在10^-4 Pa高真空下熔化后冷却, 可以得到无氧化膜的固态Al.再次熔化后的Al在720℃, 10^-2 Pa氧分压下氧化, 直接形成棒状的纳米α-Al₂O₃.同时, XRD检测结果表明, 熔融的块状金属Al在720℃, 10^-2 Pa氧分压下氧化,也得到α-Al₂O₃. 液态Al的这种特殊氧化结果与其液态结构以及液态Al蒸发成气体再氧化有关.

关键词： 液态Al; 氧化; α-Al₂O₃; 环境透射电子显微镜

本文引用格式

蔡俊 , 凌国平 , 陈长安 , 张桂凯 . 液态Al氧化的环境透射电镜观察[J]. 金属学报, 2013 , 49(8) : 953 -958 . DOI: 10.3724/SP.J.1037.2013.00165

Abstract

The study of liquid metal oxidation is of particular importance since some liquid metals are highly reactive with oxygen even under ultrahigh vacuum. The investigation of the oxidation behavior of liquid aluminum is strongly demanded due to its wide applications but relatively low melting point. However, it is still ambiguous about the products at the initial oxidation stage of liquid aluminum through the researches done in the past several decades. In order to investigate the initial oxidation products together with the oxidation mechanism of liquid aluminum, in-situ oxidation of nano aluminum powder was carried out at 720℃ in the environmental TEM (E-TEM). Prior to the oxidation, the nano aluminum powder was visualized and analyzed by E-TEM and DTA respectively.The results show that there is an amorphous Al₂O₃ film of 5—6 nm thick on the surface of the aluminum powder, which transforms toγ-Al₂O₃ at a temperature range of 350—550℃. By melting the nano powder to liquid followed by cooling under a total pressure of 10^-4 Pa in E-TEM, oxide-free solid aluminum is obtained. Re-melting of the solid aluminum at 720℃ yields oxide-free liquid aluminum. After oxidation of the oxide-free liquid aluminum under an oxygen partial pressure of 10^-2 Pa in E-TEM, α-Al₂O₃ nano wires appear on the liquid aluminum surface, demonstrating that the initialoxidation product of liquid aluminum isα-Al₂O₃. Moreover,the oxidation of liquid aluminum prepared from oxide-free bulk aluminum at 720℃ under an oxygen partial pressure of 10^-2 Pa was also studied. The XRD analysis of the products confirms that the oxide is constituted of singleα-Al₂O₃. Additionally, this particular oxidation result of liquid aluminum is attributed to its liquid structure and vapor oxidation process.

Key words： liquid Al; oxidation; α-Al₂O₃; environmental transmission electron microscope

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