本研究利用準穩態動電位掃瞄法、電化學交流阻抗法研究電鍍銅鈷多層膜的電化學特性，並利用X光繞射儀和掃瞄式電子顯微鏡研究鍍層的結晶結構和形態。 經由交流阻抗和電子顯微鏡的結果可以知道，定電位電鍍銅在高電位時會有CuCl產生使鍍層表面變粗糙；鍍鈷時電位愈大所得的晶粒愈小。在銅鈷合金方面，利用Vegard式可以得到直流電鍍的銅鈷鍍層所形成的固溶體(solid solution)，組成在89~96%之間，且由X光繞射得知鈷鍍層為面心立方的結構。在銅鈷多層膜方面，由X光繞射可以得知並沒有明顯的伴峰(satellite peak)出現，而從電子顯微鏡的結果可以知道當鍍銅在較大的電位時會有大的顆粒產生，在鍍鈷電位較大時則會有因為氫氧析出而產生的孔洞，而多層膜的截面則因為樣品製備的因素所以沒有明顯的層狀結構。 Electrochemical properties of electrodeposited Cu/Co multilayers were investigated by potentiodynamic curve and electrochemical impedance spectroscope. X-ray diffraction (XRD) and scanning electron microscopy were used to study the sample structure and morphology. It was revealed that CuCl may cover the electrode surface at the higher Cu deposition potential, it makes the electrode surface rough. The higher the Co deposition potential, the smaller the grain size. Using Vegard’s law to calculate the composition of the direct current plated Cu-Co solid solution was 89~96%. According to the result of XRD, the structure of Cu-Co alloy is mainly face-centered cubic phase. The result of XRD of the multilayers did not have obvious satellite peak. At higher Cu deposition potential, there are many grains on the surface of multilayers. At the higher Co deposition potential, there are holes on the multilayers surface resulted from the evolution of H2. Finally, the cross-section of the multilayers did not show obvious layered structure, because the preparation of the sample is difficult.