Rokosz Krzysztof, Hryniewicz Tadeusz, Kacalak Wojciech, Tandecka Katarzyna, Raaen Steinar, Gaiaschi Sofia, Chapon Patrick, Malorny Winfried, Matýsek Dalibor, Pietrzak Kornel, Dudek Łukasz
Department of Engineering and Informatics Systems, Faculty of Mechanical Engineering, Koszalin University of Technology, 75620 Koszalin, Poland.
Department of Physics, Norwegian University of Science and Technology (NTNU), 7491 Trondheim, Norway.
Materials (Basel). 2020 Mar 13;13(6):1295. doi: 10.3390/ma13061295.
The present paper covers the possible ways to fabricate advanced porous coatings that are enriched in copper on a titanium substrate through Direct Current Plasma Electrolytic Oxidation (DC-PEO) with voltage control, in electrolytes made of concentrated orthophosphoric acid with the addition of copper(II) nitrate(V) trihydrate. In these studies, solutions containing from 0 to 650 g salt per 1 dm of acid and anodic voltages from 450 V up to 650 V were used. The obtained coatings featuring variable porosity could be best defined by the three-dimensional (3D) parameter , which lies in the range 9.72 to 45.18 μm. The use of copper(II) nitrate(V) trihydrate in the electrolyte, resulted, for all cases, in the incorporation of the two oxidation forms, i.e., Cu and Cu into the coatings. Detailed X-Ray Photoelectron Spectroscopy (XPS) studies layers allowed for stating that the percentage of copper in the surface layer of the obtained coatings was in the range of 0.24 at% to 2.59 at%. The X-Ray Diffraction (XRD) studies showed the presence of copper (α-CuPO, and Cu(PO)) and titanium (TiO-anatase, TiO, TiPO, and TiO) compounds in coatings. From Energy-Dispersive X-Ray Spectroscopy (EDS) and XPS studies, it was found that the Cu/P ratio increases with the increase of voltage and the amount of salt in the electrolyte. The depth profile analysis by Glow-Discharge Optical Emission Spectroscopy (GDOES) method showed that a three-layer model consisting of a top porous layer, a semi-porous layer, and a transient/barrier layer might describe the fabricated coatings.
本文涵盖了通过直流等离子体电解氧化（DC - PEO）在电压控制下，在含有浓磷酸并添加三水合硝酸铜（II）的电解液中，在钛基体上制备富含铜的先进多孔涂层的可能方法。在这些研究中，使用了每1立方分米酸中含有0至650克盐的溶液以及450 V至650 V的阳极电压。所获得的具有可变孔隙率的涂层可以通过三维（3D）参数 最好地定义，该参数范围为9.72至45.18μm。在电解液中使用三水合硝酸铜（II），在所有情况下都导致两种氧化形式，即Cu和Cu掺入涂层中。详细的X射线光电子能谱（XPS）研究层表明，所获得涂层表面层中铜的百分比在0.24原子％至2.59原子％的范围内。X射线衍射（XRD）研究表明涂层中存在铜（α - CuPO和Cu(PO)）和钛（TiO - 锐钛矿、TiO、TiPO和TiO）化合物。通过能量色散X射线光谱（EDS）和XPS研究发现，Cu/P比随着电压和电解液中盐量的增加而增加。辉光放电光发射光谱（GDOES）方法的深度剖面分析表明，由顶部多孔层、半多孔层和瞬态/阻挡层组成的三层模型可能描述所制备的涂层。
