Microstructure of TiCuO Films on Copper Ion Release and Endothelial Cell Behavior

doi:10.15541/jim20180004

Abstract

Abstract:

TiCuO films with different microstructures and Cu contents were prepared on Si and 316L SS substrates using DC magnetron sputtering. The microstructure and chemical composition of the films were analyzed by X-ray diffraction (XRD), transmission electron microscopy (TEM), X-ray energy dispersive spectroscopy (EDS), and X-ray photoelectron spectroscopy (XPS). Corrosion behavior and Cu ions release properties of the films were evaluated by electrochemical corrosion and simulated body-fluid immersion tests, respectively. Endothelial cell (EC) viability on the films was evaluated by CCK-8 assay in vitro. Un-doped TiO₂ films exhibit rutile phases. After Cu incorporation, the TiCuO films consist of nano-crystalline grains of Cu₂O on their amorphous matrix. The films with higher Cu contents are more susceptible to corrosion and release more Cu ions. The Cu-rich phases of the films result in corrosion. EC viability is enhanced by a certain concentration of Cu ions released from TiCuO films. All above results demonstrated that microstructures and Cu contents of TiCuO films play an important role in controlling copper ions release behaviors, and therefore affect the EC viability.

Key words: TiCuO films, magnetron sputtering, Cu ions release, ECs viability

CLC Number:

TG178
R318

CHENG Dan, HUANG Bin, CHEN Tao, JING Feng-Juan, XIE Dong, LENG Yong-Xiang, HUANG Nan. Microstructure of TiCuO Films on Copper Ion Release and Endothelial Cell Behavior[J]. Journal of Inorganic Materials, 2018, 33(10): 1089-1096.

Figures/Tables 11

Table 1 Atomic concentration of TiCuO films evaluated by EDS

Sample	Cu/at%	Ti/at%	O/at%
TiCuO-1	12.4	12.3	75.3
TiCuO-2	23.1	6.7	70.2

Fig. 1 XRD patterns of TiO2 and TiCuO samples

Fig. 2 TEM image (a), Cu contents evaluated by EDS (b), the selected area electron diffraction results of A region (c) and B region (d), and their corresponding HRTEM images (e, f), respectively, of the TiCuO-1 sample

Fig. 3 TEM image(a), corresponding line-scanning of Cu, O, Ti elements (b) across a selected area (yellow line in (a)), the selected area electron diffraction results of A region (c) and B region (d), and their corresponding HRTEM images (e, f) respectively of the TiCuO-2 sample

Fig. 4 Cu2p (a) and Ti2p (b) XPS spectra of TiCuO-1 and TiCuO-2 films

Table 2 The area percentages of Ti4 +, Ti3 + and Ti2 + in the Ti2p spectra and the area percentage of Cu2 + and Cu + in Cu2p spectra of TiO2, TiCuO-1 and TiCuO-2 samples

Sample	Ti2p			Cu2p
Sample	Ti⁴⁺	Ti²⁺	Ti³⁺	Cu²⁺	Cu⁺
TiCuO-2	47at%	53at%	0	30.2at%	69.8at%
TiCuO-1	39at%	43at%	18at%	6.2at%	93.8at%
TiO₂	32at%	34at%	34at%	-	-

Table 3 Corrosion potential (Ecorr) and current densities (Icorr) of SS, TiO2 and TiCuO films derived from potentiodynamic polarization curves

Sample	SS	TiO₂	TiCuO-1	TiCuO-2
E_corr/V(vs.SCE)	-0.13	-0.06	-0.16	-0.17
I_corr/(μA·cm^-2)	0.49	0.03	0.62	3.89

Fig. 5 Electrochemical corrosion polarization curves of TiO2, TiCuO and 316 L SS samples (A) and morphology of the TiCuO-2 sample with its EDS results of the four different corroded areas labeled with a, b, c and d (B)

Fig. 6 Accumulated Cu ions concentration (a) and release rate (b) of Cu ions released from TiCuO-1 and TiCuO-2 samples

Fig. 7 ECs viability detected by CCK-8 assay (a) and fluorescence microscopic images stained by rhodamine (b) after being cultured on the samples of TiO2 and TiCuO

Fig. 8 ECs viability detected by CCK-8 assay (a) and fluorescence microscopic images stained by rhodamine (b) after being cultured under condition medium with CuCl2 solution at different concentration

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