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Available online at www.worldscientificnews.com

( Received 27 February 2018; Accepted 13 March 2018; Date of Publication 14 March 2018 )

WSN 95 (2018) 246-259 EISSN 2392-2192

SEM and EDS analysis of enriched in phosphorus and copper coatings fabricated by AC-PEO

treatment

Krzysztof Rokosza, Tadeusz Hryniewiczb, Kornel Pietrzakc, Łukasz Dudekd

Division of BioEngineering and Surface Electrochemistry, Department of Engineering and Informatics Systems, Faculty of Mechanical Engineering, Koszalin University of Technology,

Racławicka 15-17, PL 75-620 Koszalin, Poland

a-dE-mail address: [email protected] , [email protected] ,

[email protected] , [email protected]

ABSTRACT

In the present paper, SEM and EDS studies of coatings obtained on CP Titanium Grade 2 under

sinusoidal alternating voltage (AC) with frequency 50 Hz in Plasma Electrolytic Oxidation (PEO)

process at voltages of 200 Vpp, 250 Vpp and 300 Vpp during 3-minute treatments, are displayed. Based

on SEM micrographs it may be stated that the porous surfaces, which are needed for biomedical and

catalysis application, are obtained only for samples fabricated at 200 Vpp. It was found out that thickest

and most morphologically developed surfaces were obtained at 200 Vpp, too. The surfaces obtained at

250 Vpp and 300 Vpp are cracked and had low concentration of copper, i.e. 0.9 at% and 1.1 at%,

respectively, while that one obtained at 200 Vpp was porous and had 8.6 at% copper.

Keywords: Plasma Electrolytic Oxidation (PEO), Micro Arc Oxidation (MAO), CP Titanium Grade 2,

copper nitrate Cu(NO3)2∙3H2O

1. INTRODUCTION

Metal surface treatments by electrochemical processing have been steadily developed

since many decades. Standard electropolishing (EP) [1-5], considered as a surface finishing

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World Scientific News 95 (2018) 246-259

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performed on a plateau current density level has been recently modified by extending the

treatment conditions to the high-current-density electropolishing (HCEP) [6-8] or high-

voltage electropolishing (HVEP) [9], with the improved results concerning nano-films or

nano-coatings. Another electrochemical surface technique acquires a magnetic field [10] with

the process named magnetoelectropolishing (MEP) [10-24] in which, apart from improving

surface finishing [13-25], nanohardness [12], corrosion resistance [13-16, 70, 71], biological

response [26], and fundamental about 90-percent de-hydrogenation is obtained [27, 28].

On the other hand, Plasma Electrolytic Oxidation (PEO) [29] also known as Micro Arc

Oxidation (MAO) has been developed to form micro-coatings on metals and alloys [30-66].

These coatings are usually porous and may be enriched with chemical elements, such as

phosphorus and calcium to form the hydroxyapatite-like structure [40-48]. Moreover, another

elements, such as bactericidal copper [49-58], magnesium, which may accelerate the healing

of wounds [43, 60, 61] as well as zinc with antibacterial properties [42, 62-65], capable for

improving osteogenic characteristics and bone regenerating capacity [66-69], may be

introduced into the porous coatings.

The aim of this work is to characterize coatings obtained during AC-PEO process on CP

Titanium Grade 2 obtained during Plasma Oxidation Process enriched with antibacterial

copper analyzed by SEM and EDS techniques.

2. METHOD

The CP Titanium Grade 2 samples with dimensions of 10 mm × 10 mm × 2 mm by

plasma electrolytic oxidation (PEO) process were treated. The process was performed at

voltages of 200 Vpp, 250 Vpp and 300 Vpp by using 50 Hz AC power transformer. The

electrolyte composition was the following: 1 L of 85% H3PO4 with 500 g Cu(NO3)2∙3H2O.

For each run, the electrolytic cell made of glass was used, containing up to 500 ml of the

electrolyte.

For studies, the scanning electron microscope Quanta 250 FEI with Low Vacuum and

Environmental Scanning Electron Microscope (ESEM) mode and a field emission cathode as

well as the Energy-Dispersive X-ray Spectroscopy (EDS) system in a Noran System Six with

nitrogen-free silicon drift detector, were employed.

3. RESULTS AND DISCUSSION

In Figures 1, 2 and 3, the SEM images of coating formed on CP Titanium Grade 2 after

PEO process at 200 Vpp in the electrolyte containing of 500 g Cu(NO3)2∙3H2O in 1 L H3PO4,

are presented. It can be observed that irregular surface with well-developed porous

morphology was obtained. In Table 1, results of EDS measurements are presented. The EDS

data show the presence of copper (8.6 at%), phosphorus (48.8 at%) and titanium (42.6 at %)

which signal comes partly from metallic matrix. Based on these results, copper-to-phosphorus

ratio Cu/P was calculated and equal 0.18.


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Fig. 1. SEM pictures with magnification 1000 times of coating formed on Titanium after PEO

treatment for 3 min at 200 Vpp in electrolyte containing of 500 g Cu(NO3)2∙3H2O

in 1 L H3PO4



in 1 L H3PO4


-249-

Fig. 3. SEM pictures with magnification 10000 times of coating formed on Titanium after

PEO treatment for 3 min at 200 Vpp in electrolyte containing of 500 g Cu(NO3)2∙3H2O

in 1 L H3PO4

Table 1. EDS results of coatings formed on Titanium after PEO treatment for 3 min at 200

Vpp in electrolyte containing of 500 g Cu(NO3)2∙3H2O in 1 L H3PO4

Atomic concentration [%] Ratio

Cu P Ti Cu/P

8.6 48.8 42.6 0.18

In Figures 4-6, the SEM images of coating formed on CP Titanium Grade 2 after PEO

process at 250 Vpp in the electrolyte containing of 500 g Cu(NO3)2∙3H2O in 1 L H3PO4, are

presented. The obtained surfaces are generally non-porous, displaying island-like structure

with visible cracks. In Table 2, results of EDS measurements are presented. The EDS data

show the presence of copper (1.1 at%), phosphorus (7.1 at%) and titanium (91.8 at %) which

signal comes partly from the metallic matrix. Based on these results, copper-to-phosphorus

ratio Cu/P was calculated and equal 0.15.


-250-



in 1 L H3PO4



in 1 L H3PO4


-251-



in 1 L H3PO4

Table 3. EDS results of coatings formed on Titanium after PEO treatment for 3 min at 250



Cu P Ti Cu/P

1.1 7.1 91.8 0.15

In Figures 7- 9, the SEM images of coating formed on CP Titanium Grade 2 after PEO

process at 300 Vpp in the electrolyte containing of 500 g Cu(NO3)2∙3H2O in 1 L H3PO4, are

displayed. The obtained surfaces are generally non-porous, of island-like structures with

visible cracks. In Table 3, results of EDS measurements are presented. The EDS data show

the presence of copper (0.9 at%), phosphorus (12.9 at%) and titanium (86.2 at%) which signal

comes partly from the metallic matrix. Based on these results, copper-to-phosphorus ratio

Cu/P was calculated and equal 0.07.


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in 1 L H3PO4



in 1 L H3PO4


-253-



in 1 L H3PO4

Table 3. EDS results for coatings formed on Titanium after PEO treatment for 3 min at 300



Cu P Ti Cu/P

0.9 12.9 86.2 0.07

4. CONCLUSIONS

The studies carried out on porous coatings on titanium, fabricated by AC-PEO treatment

allowed to formulate the following conclusions:

It is possible to obtain coatings on titanium with the use of AC-PEO method

The applied voltage higher than 200 Vpp may result in island-like and cracked

surfaces.

The coatings obtained at 200 Vpp contain more copper (8.6 at%) than coatings

obtained at 250 Vpp (1.1 at%) and 300 Vpp (0.9 at%).


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Acknowledgements

This work was supported by subsidizing by Grant OPUS 11 of National Science Centre, Poland, with

registration number 2016/21/B/ST8/01952, titled "Development of models of new porous coatings obtained on

titanium by Plasma Electrolytic Oxidation in electrolytes containing phosphoric acid with addition of calcium,

magnesium, copper and zinc nitrates".

Prof. Winfried Malorny from Hochschule Wismar-University of Applied Sciences Technology, Business and

Design, Faculty of Engineering, DE 23966 Wismar, Germany, is given thanks for providing access to the

SEM/EDS apparatus allowing to perform the studies.

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sem and eds analysis of enriched in phosphorus and copper …€¦ · of wounds [43, 60, 61] as...

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