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Surface oxide analysis of lead‐free solder particles

Xin Luo (Key Laboratory of New Displays and System Integration, SMIT Center, Shanghai University, Shanghai, People's Republic of China and BioNano Systems Laboratory, Department of Microtechnology and Nanoscience (MC2), Chalmers University of Technology, Göteborg, Sweden)
Wenhui Du (Chalmers University of Technology, Göteborg, Sweden)
Xiuzhen Lu (Chalmers University of Technology, Göteborg, Sweden)
Toshikazu Yamaguchi (Henkel Limited, Kanagawa, Japan)
Gavin Jackson (Henkel Limited, Hemel Hempstead, UK)
Li lei Ye (SHT Smart High Tech AB, Göteborg, Sweden)
Johan Liu (Key Laboratory of New Displays and System Integration, SMIT Center, Shanghai University, Shanghai, People's Republic of China and BioNano Systems Laboratory, Department of Microtechnology and Nanoscience (MC2), Chalmers University of Technology, Göteborg, Sweden)

Soldering & Surface Mount Technology

ISSN: 0954-0911

Article publication date: 1 February 2013

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Abstract

Purpose

The composition and thickness of surface oxide of solder particles is extremely important to the quality of interconnect and reliability of packaged system. The purpose of this paper is to develop an observable measurement to research the issue.

Design/methodology/approach

AES (Auger electron spectroscopy), XPS (X‐ray photoelectron spectroscopy), TEM (transmission electron microscopy) and STEM (scanning transmission electron microscopy) were employed to examine the oxide layer on microscale solder powders. Conventional techniques and FIB (Focus Ion Beam) were employed for the TEM sample preparation. High angle annular dark field (HAADF) pattern was applied to distinguish the oxide layer and the solder matrix by the contrast of average atomic number. The results were confirmed by AES and XPS measurement.

Findings

The solder powders were exposed to air (70% relative humidity) at 150°C for 0, 120 and 240 h for the accelerated growth of oxide. The surface oxide thickness was 6 nm and 50 nm measured by TEM for 0 h and 120 h samples, respectively. It was found that the increase in surface oxide thickness of solder particles is proportional to the rooting of time. The elemental distribution along the oxide was quantified by line scanning using STEM and the atomic ratio of Sn to O in the oxide layer nearer to the outer, the middle, and the inner (adjacent to the solder matrix) was found to be 1:2, 2:3 and 1:1, respectively. The result was validated using XPS which gave Sn to O ratio of 1:2 at 5 nm depth of surface oxide.

Originality/value

This is the first time FIB technology has been used to prepare TEM specimens for solder particles and TEM pictures shown of their surface oxide layer. Though requiring more care in sample preparation, the measurements by TEM and STEM are believed to be more direct and precise.

Keywords

Citation

Luo, X., Du, W., Lu, X., Yamaguchi, T., Jackson, G., lei Ye, L. and Liu, J. (2013), "Surface oxide analysis of lead‐free solder particles", Soldering & Surface Mount Technology, Vol. 25 No. 1, pp. 39-44. https://doi.org/10.1108/09540911311294588

Publisher

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Emerald Group Publishing Limited

Copyright © 2013, Emerald Group Publishing Limited