阳极氧化铝膜中间层阻挡元素扩散研究<sup>*</sup>

doi:10.11900/0412.1961.2015.00385

金属学报

2016, Vol. 52

Issue (3): 341-348 DOI: 10.11900/0412.1961.2015.00385

论文

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阳极氧化铝膜中间层阻挡元素扩散研究^*

黄祖江¹,周敏^1,²,杨阳¹,陈泉志¹,唐仕光¹,李伟洲¹(

)

1 广西大学材料科学与工程学院, 南宁 530004
2 富士康科技集团, 深圳 518109

STUDY OF ANODIC ALUMINUM OXIDE FILM AS AN INTERLAYER TO SUPPRESS ELEMENT DIFFUSION

Zujiang HUANG¹,Min ZHOU^1,²,Yang YANG¹,Quanzhi CHEN¹,Shiguang TANG¹,Weizhou LI¹(

)

1 School of Materials Science and Engineering, Guangxi University, Nanning 530004, China
2 Foxconn Technology Group, Shenzhen 518109, China

引用本文:

黄祖江, 周敏, 杨阳, 陈泉志, 唐仕光, 李伟洲. 阳极氧化铝膜中间层阻挡元素扩散研究^*[J]. 金属学报, 2016, 52(3): 341-348.
Zujiang HUANG, Min ZHOU, Yang YANG, Quanzhi CHEN, Shiguang TANG, Weizhou LI. STUDY OF ANODIC ALUMINUM OXIDE FILM AS AN INTERLAYER TO SUPPRESS ELEMENT DIFFUSION[J]. Acta Metall Sin, 2016, 52(3): 341-348.

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摘要:

对铌合金C103基体上真空蒸镀的Al膜进行阳极氧化处理获得阳极氧化铝(AAO)膜, 利用电镀技术在AAO膜上制备Ni表层, 通过高温处理研究元素通过AAO膜的扩散行为. 结果表明: 没有中间层的Ni/C103及以纯Al膜作为中间层的Ni/Al/C103样品, 涂层和基体间的元素扩散严重; 而以AAO膜为中间层的Ni/AAO/C103样品, 涂层和基体间的元素扩散受到明显抑制. 经900 ℃热处理后, Ni/C103, Ni/Al/C103及Ni/AAO/C103样品其外层中Nb含量分别为7.05%, 5.08%和3.55%; 基体中的Ni含量分别为6.84%, 3.62%和2.85%; AAO膜作为中间层有较强的元素扩散阻挡能力. 在900 ℃退火后, Ni/C103和Ni/Al/C103样品表面均生成了NbNi₃相, 而Ni/AAO/C103样品并未出现Nb和Ni的反应生成物. 通过Fick定律计算得知, 900 ℃时Ni在AAO膜的扩散系数为3.28×10^-14 m²/s, Nb为2.16×10^-14 m²/s; 1000 ℃时Ni的扩散系数上升至1.03×10^-13 m²/s, Nb为3.58×10^-14 m²/s.

关键词 ：阳极氧化铝(AAO)膜, 扩散阻挡层, 多孔结构, Fick定律, 扩散系数

Abstract：

Element interdiffusion will accelerate failure of surface coating systems after a long time service at high temperature. To extend service life of the coatings, developing a diffusion barrier between the coating and the substrate is considered as an efficient way. Many research results showed that a diffusion barrier with single function such as metallic or ceramic one can not meet requirements for strong barrier ability and strong interfacial strength of the coatings onto the substrate at the same time. Anodic aluminum oxide (AAO) film with porous surface structure, which has an effective role for element diffusion so as to strengthen the interfacial adhesion rapidly, and a dense Al₂O₃ sublayer to suppress the interdiffusion was effectively used as diffusion barrier in this work and interdiffusion barrier ability was investigated. The AAO film was obtained by anodizing Al film deposited on C103 niobium alloy by vacuum evaporation technology, and an electroplating Ni plating was prepared as an overlayer. Vacuum heat treatment was applied to promote element diffusion. The results indicated that substantial diffusion occurred in the Ni/C103 specimen without an interlayer and in the Ni/Al/C103 specimen with Al film as an interlayer. In the Ni/AAO/C103 specimen, hardly any interdiffusion was observed. After 4 h vacuum annealing at 900 ℃, NbNi₃ phase was detected on the Ni/C103 and Ni/Al/C103 specimens, which could not be found in the Ni/AAO/C103 specimen. Nb content in the Ni overlayer of Ni/C103, Ni/Al/C103 and Ni/AAO/C103 specimens was 7.05%, 5.08% and 3.55%, respectively. Ni content in the substrate of Ni/C103, Ni/Al/C103 and Ni/AAO/C103 specimens diffusing from the overlayer was 6.84%, 3.62% and 2.85%, respectively. Thus, AAO film exhibited strong barrier ability in suppressing element diffusion. From calculation of the Fick's law, it was found that diffusion coefficient of Ni and Nb in the AAO film at 900 ℃ was 3.28×10^-14m²/s and 2.16×10^-14 m²/s, respectively, and it was raised to 1.03×10^-13 m²/s and 3.58×10^-14 m²/s at 1000 ℃, respectively.

Key words： anodic aluminum oxide (AAO) film diffusion barrier porous structure Fick's law diffusion coefficient

收稿日期: 2015-07-13

基金资助:* 国家自然科学基金项目51371059, 51361003和51001032, 广西自然科学基金项目2014GXNSFCA118013, 广西高等学校高水平创新团队项目(第二批), 以及广西自然科学基金创新研究团队项目2011GXNSFF018001资助

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图1 阳极氧化铝(AAO)膜中间层EDS取点示意图

图2 经过真空蒸镀,阳极氧化和电镀Ni后沉积态涂层表面的SEM像

图3 含或不含中间层样品的沉积态涂层XRD谱

图4 900和1000 ℃保温4 h后退火态涂层的表面SEM像

图5 900和1000 ℃保温4 h后退火态涂层的XRD谱

图6 900 ℃热处理4 h 后的试样扩散截面SEM像及EDS分析选区

表1 图6 中扩散截面不同区域的EDS分析结果

图7 Ni/AAO/C103 样品的沉积态及900 和1000 ℃退火后的扩散截面不同距离的Ni 和Nb原子分数

表2 Ni/AAO/C103 样品900 和1000 ℃退火后中间层的Ni 和Nb元素扩散系数

图8 Ni/AAO/C103 样品900 和1000 ℃退火后中间层Ni 和Nb元素的Z拟合

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