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  1. Epitaxial electrodeposition of Co, Cu and Ru is compared and contrasted. The seed layer for electrodeposition of all three metals was an epitaxial Ru(0001) film that was deposited at an elevated temperature onto a sapphire(0001) substrate and annealed post deposition. The epitaxial orientation relationship of the electrodeposited film and the seed layer, the epitaxial misfit strain, the role of symmetry of the seed layer versus the electrodepositing layer is addressed. In addition, the impact of underpotential deposition on film nucleation, and the growth morphology of the films is discussed. It is shown that epitaxial electrodeposition of metallic films to thicknesses of tens of nanometers is readily achievable.

    This paper 1189 was presented during the 241st Meeting of the Electrochemical Society, May 29–June 2, 2022.

     
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  2. The electrodeposition of Ru was investigated from solutions of ruthenium(III) nitrosyl sulfate and ruthenium(III) chloride onto seed layers of epitaxial and polycrystalline Ru and epitaxial Au. Using both galvanostatic and potentiostatic deposition modes, metallic Ru was found to electrodeposit as a porous layer comprised of (0001) oriented Ru crystallites, the presence of which was discovered and confirmed by X-ray and scanning transmission and transmission electron microscope (S/TEM) analyses. This finding was independent of the Ru salt and seed layer used. Using X-ray reflectivity (XRR), the average film densityρeffof the porous electrodeposited Ru layer was measured as less than the density of bulk RuρRu,bulk(14.414 g cm−3). Increasing the magnitude of the applied current density from −100μA cm−2to −10 mA cm−2in solutions of Ru nitrosyl sulfate increased theρefffrom 7.4 g cm−3to 9.7 g cm−2while the current efficiency decreased from 9.4% to 4.3%.

     
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  3. Co electrodeposition was performed onto single crystal Ru(0001) and polycrystalline Ru films to study the influence of such seed layers on the growth of epitaxial Co(0001). The effect of misfit strain on the electrodeposited Co(0001) films was studied using 60 and 10 nm-thick Ru(0001) seed layers, where the misfit strains of the Co layer on the two Ru(0001) seed layers are 7.9% and 9.6%, respectively. Despite a large misfit strain of 7.9%, the planar growth of Co(0001) was achieved up to a thickness of 42 nm before a transition to island growth was observed. Epitaxial Co films electrodeposited onto 10 nm Ru(0001) showed increased roughness when compared with Co electrodeposited onto the 60 nm seed layer. Co electrodeposition onto polycrystalline Ru resulted in a rough, polycrystalline film with faceted growth. Electrochemical experiments and simulations were used to study the influence of [Co2+] and solution pH on the throughput of the electrodeposition process. By increasing [Co2+] from 1 to 20 mM, the deposition rate of Co(0001) increased from 0.23 nm min−1to 0.88 nm min−1at an applied current density of −80μA cm−2.

     
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