Electrodeposition of Au-Cu Alloys and the Micro-Mechanical Properties
Authors: Chang Tso-Fu Mark , Tang Haochun , Chen Chun-Yi , Yamane Daisuke , Ito Hiroyuki , Machida Katsuyuki , Masu Kazuya , Sone Masato 
Published: May 2020

Electrodeposited gold is used in movable micro-components of micro-electro-mechanical systems (MEMS) devices to allow further enhancement in the sensitivity and miniaturization of the device [1]. Mechanical strengths of gold are low among materials commonly used as structure materials in electronic devices. Electrodeposition method is advantageous in strengthening metallic materials because of the ability to refine the average grain size to nano-scale, which the mechanical strength increases along with a reduction in the grain size based on the grain boundary strengthening mechanism or the Hall-Petch relationship. Alloying of metallic materials is also an effective strategy to achieve the strengthening according to the solid solution strengthening mechanism.
On the other hand, mechanical properties of metallic materials exhibit the sample size effect when dimensions of the specimen are reduced to micro or sub-micro scale. Therefore, mechanical property characterization of materials for MEMS applications should be conducted using specimens having dimensions in micro-scale. Various micro-mechanical testing methods have been developed in our group to characterize micro-specimens, such as micro-compression test [2,3], micro-tensile test [4], and micro-bending test [5]. Among them, micro-bending test is suggested to be the most suitable method to evaluate materials for applications in MEMS when compared with micro-compression and micro-tensile tests since cantilever-like structures are often applied in MEMS components, such as the micro-spring in a MEMS accelerometer.
In this study, Au-Cu alloys are prepared by electrodeposition, and micro-mechanical properties of the electrodeposited Au-Cu alloys are characterized by a micro-bending test. Young’s modulus is an important information in design of movable micro-components. A non-destructive Young’s modulus evaluation method, resonance frequency measurement, is conducted using the Au-Cu alloy micro-cantilevers. Also, long-term vibration tests are conducted to reveal structure stability of the Au-Cu alloy micro-cantilevers.
The Au-Cu electrolyte used in this work was a commercially available electrolyte provided by MATEX Co. Japan, which contained 17.3 g/L of X3Au(SO3)2 (X = Na, K), 1.26 g/L of CuSO4, and ethylenediaminetetraacetic acid as the additive with pH at 7.5. The electrodeposition was carried out at 50 °C, and the current density was varied from 0.1 to 8 mA/cm2. Specimens used in the micro-bending test were micro-cantilevers fabricated from the Au-Cu alloy films by focused ion beam. Dimensions of the micro-cantilevers fabricated were 10 µm × 10 µm × 50 µm. The micro-bending tests were conducted using a test machine equipped with a spherical diamond indenter at a constant displacement rate of 0.05 µm/s.
For the Young’s modulus and long-term structure stability evaluations, the micro-cantilevers were prepared by electrodeposition combined with lithography process. The long-term vibration test was carried out under conditions of the cycle number in a range from 103 to 106, the frequency of 10.0 Hz, and the acceleration of 1.0 G (1 G = 9.8 m/s2). The structure stability was determined by evaluating height profiles of top surface of the micro-cantilevers before and after the vibration test by a 3D optical microscope.
The Au-Cu alloy film electrodeposited at 5 mA/cm2 had the finest average grain size among films prepared in this work, which the grain size was 4.76 nm. Bending test of a micro-cantilever prepared from this film shows a high yield stress at 1826 MPa. Gold, copper, and Au-Cu alloys are known to be ductile materials, but brittle fracture was observed during the bending test when the current density used in prepared the film was higher than 5 mA/cm2.
From the resonance frequency method, Young’s moduli of the Au-Cu alloy micro-cantilevers were ranged from 68.0 to 79.5 GPa, which were similar to the value of bulk-size specimens and indicated no sample size effect on the Young’s modulus. Regarding the long-term structure stability, after 106 cycles of the vibration test, all the micro-cantilever were still intact, and the height profiles did not change much after the vibration. Results obtained in this study confirmed high mechanical strength and structure stability in the electroplated Au-Cu alloys and demonstrated the advantage in applications as movable components in MEMS devices.
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