本研究為利用脈衝電鍍法由硫酸銅溶液中製備奈米雙晶銅，改變脈衝電鍍的電流密度以及頻率兩種參數，再利用EBSD(Electron Backscatter Diffraction Pattern)和XRD分析，探討參數的改變對於鍍層微結構，如優選取向、晶粒尺寸和晶界性質的影響。以及比較EBSD、XRD和TEM三種分析方法來決定晶粒尺寸之優劣。
實驗結果發現晶粒的尺寸會隨著電流密度的增大和頻率的降低而減小。增加電流密度可以提高成核速率且產生較細緻的晶粒；然而當頻率增加時，脈衝電鍍機制中的吸附離子解離和亞銅離子的不對稱性反應的發生會導致晶粒粗大。由XDR、EBSD以及TEM來決定純銅鍍層的平均晶粒大小分別為82.9nm、1.035μm和0.5~1.0μm。銅鍍層是由生長雙晶以及具有{110}優選取向的不規則形狀晶粒所組成。
XRD是根據Scherrer’s equation來決定晶粒大小，但Scherrer’s equation用來決定具有織構材料的晶粒大小卻有其限制。TEM比EBSD具有更高的空間解析度，但是EBSD的觀察範圍可比TEM高數個數量級，這代表EBSD所得到的OIM影像涵蓋更多的晶粒，較具有統計學上的代表性。因此，決定晶粒大小最適合的方式為EBSD。

In this study nano-twin coppers were synthesized by using a pulsed electrodeposition technique from an electrolyte of CuSO4, in which the current density and frequency were experiment parameters. Electron back-scattering diffractioin (EBSD) and XRD were carried on characterizing microstructure features of preferred orientation, grain size and boundary character.
It was observed that the grain size decreases with increasing the current density and with decreasing the frequency. Increasing a current density leads to enhance a nucleation rate, resulting in a fine-grain microstructure. However, as a frequency increases, a disproportionation reation of cuprous ions and a dissolution reaction of copper adatoms into bulk solution, resulting in a coarse-grain microstructure. The average grain size of as-deposited coppers determined from XRD, EBSD and TEM are 82.9nm, 1.035μm and for 0.5μm to 1.0μm, respectively. The as-deposited Cu samples consisted of growth twins and irregular-shaped grains with a {110} preferred orientation.
Scherrer’s equation is not able to determine a correct grain size of preferred orientation materials. The determination of grain size using XRD is limited due to the application of Scherrer’s equation. TEM images show a higher spatial resolution of microstructures than EBSD, but the observed area of EBSD could be several orders larger than that of TEM. This means that an orientation image map obtained from EBSD provides a higher accuracy in statistics than a microstructure from TEM.

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