The purpose of this study was to analyze surface chemical species deposited on various implant materials immersed in simulated body fluid (SBF). The investigated materials including pure titanium, two beta titanium alloys and stainless steel (316L) were formed into discs using cold pressing and sintering. The samples were examined using SEM and mid-IR microscopes. All the sample discs exhibited nucleation and growth of calcium phosphates, precipitated from the SBF solution containing calcium, phosphate and other ions. The results have shown that the nucleation and growth of phosphates depend on the alloy composition and become more intensive in the case of the titanium alloy with the niobium additio

J. Kolmas

J. Mystkowska

J. R. Dabrowski

P. Deptula

English

Journal of Vibroengineering

 519. SURFACE ACTIVITY OF TITANIUM ALLOYS CONTACTED WITH THE SIMULATED BODY FLUID. 
J. MYSTKOWSKA1,A, P. DEPTUŁA1,B, J. KOLMAS2,A, J. R. DĄBROWSKI1,C 
 
 
 VIBROMECHANIKA. JOURNAL OF VIBROENGINEERING.   DECEMBER 2009. VOLUME 11, ISSUE 4. ISSN 1392-8716 
725 
519. Surface activity of titanium alloys contacted with 
        the simulated body fluid  
 
 
J. Mystkowska1,a, P. Deptuła1,b, J. Kolmas2,a, J. R. Dąbrowski1,c 
1
 Bialystok Technical University, Wiejska 45C, 15-351 Bialystok, Poland  
e-mail:  1a j.mystkowska@pb.edu.pl, 1b piotrdep@o2.pl, 1c jrd@pb.edu.pl 
Phone: +48857469251; Fax: +48857469248 
2 Medical University of Warsaw, Department of Inorganic and Analytical Chemistry, Banacha 1,  
02-097 Warsaw, Poland 
e-mail: 2a joanna.kolmas@wum.edu.pl 
Phone: +48225720755; Fax: +48225720784 
 
(Received  2 June 2009;  accepted 27 November 2009) 
 
 
Abstract. The purpose of this study was to analyze surface chemical species deposited on 
various implant materials immersed in simulated body fluid (SBF). The investigated materials 
including pure titanium, two beta titanium alloys and stainless steel (316L) were formed into 
discs using cold pressing and sintering. The samples were examined using SEM and mid-IR 
microscopes. All the sample discs exhibited nucleation and growth of calcium phosphates, 
precipitated from the SBF solution containing calcium, phosphate and other ions. The results 
have shown that the nucleation and growth of phosphates depend on the alloy composition and 
become more intensive in the case of the titanium alloy with the niobium addition.  
 
Keywords: titanium alloy, simulated body fluid (SBF), calcium phosphate, bioactive surfaces 
 
 
Introduction 
 
Pure titanium, titanium alloys and stainless steel grade 316L have been widely used in the 
manufacturing of dental and orthopedic implants owing to their superior mechanical properties 
and high corrosion resistance [1]. On the other hand, the bioactivity of metal surfaces is not 
sufficient to induce growth and fixation of bone tissues [2]. An ideal biomaterial for medical 
applications should exhibit excellent biocompatibility with no adverse cytotoxity, excellent 
corrosion resistance, and a good combination of mechanical properties such as high strength and 
fatigue resistance, low modulus, and good wear resistance [3, 4]. Thus, intensive and thorough 
investigations are needed to obtain materials with properties similar to the replaced tissues. One 
of the prospective research directions is the application of porous metallic materials for 
osteointegration processes. Application of materials with appropriate porosity allows one to 
accomplish mechanical fixation of implants without using a bone cement. This successful result 
can be achieved because of spontaneous bone growth into the implants’ porous structure [5]. 
Modern technologies, such as powder metallurgy, offer new possibilities of producing original 
porous alloys and composite materials. 
On account of the relevance of titanium alloys for orthopedic applications, both nucleation and 
growth of calcium phosphates have been investigated. A simulated body fluid (SBF) with ion 
concentrations nearly equal to those of human blood plasma, can be used in tests of the 
bioactivity of investigated materials [6]. Apatite depositions on the surface of materials 
immersed in SBF solution have been widely used for the in-vitro assessment of the bioactivity of 
bone and dental implant materials [2].   
 
 519. SURFACE ACTIVITY OF TITANIUM ALLOYS CONTACTED WITH THE SIMULATED BODY FLUID. 
J. MYSTKOWSKA1,A, P. DEPTUŁA1,B, J. KOLMAS2,A, J. R. DĄBROWSKI1,C 
 
 
 VIBROMECHANIKA. JOURNAL OF VIBROENGINEERING.   DECEMBER 2009. VOLUME 11, ISSUE 4. ISSN 1392-8716 
726 
The aim of the present study was to investigate the bioactivity (surface composition) of 
the titanium alloys immersed in SBF solution. Also, the titanium surface structure using SEM 
was examined. The chemical analysis of the surface layer was conducted using the FTIR method 
[7-10].  
 
Materials and methods 
 
Pure titanium, two beta titanium alloys and steel 316L were investigated. Metal discs, 
7.0 mm in diameter and 1.5 mm thick, were produced of those materials using the powder 
metallurgy method. Two titanium alloys, Ti-15Mo-2.8Nb and Ti-7.5Mo-2Fe were prepared 
using commercial pure titanium powder of the particle size below 150µm, pure molybdenum 
powder of the particle size 3-7 µm, pure niobium powder of the particle size 1-5 µm and pure 
iron powder of the particle size below 10 µm. The steel disc was prepared using the 316L 
powder of the particle size 125 - 250µm. 
The technological process involved cold pressing under the pressure of  
500 MPa, followed by sintering. The sintering process was carried out in vacuum for 3h at 
1230ºC. Thus formed discs were cooled down naturally to ambient temperature inside a furnace. 
Before immersing all the samples into the SBF solution consisting of KCl, NaCl, HCl, 
MgCl2·6H2O, CaCl2, Na2SO4, NaHCO3, KH2PO4·3H2O and TRIS (hydroxymethyl 
aminomethane) [6], the surface of the discs was mechanically polished and analyzed using 
HITACHI S-3000N electron microscope with attachment for X-ray microanalysis. The samples 
were immersed for 56 days in the SBF solution (pH 7.2, 37ºC) specified above and afterwards 
the precipitation of calcium phosphates was investigated. 
The FTIR method was used to analyze chemical composition of the coating produced after 
immersion of the metal discs into the SBF solution. The middle-range infrared spectra were 
collected using a PerkinElmer Autoimage infrared microscope equipped with a digital camera 
and operating in the reflection mode. The background was recorded prior to the measurement of 
coated surfaces by reflection from an untreated surface of each studied alloy and it was 
automatically subtracted. All the spectra were acquired in the same conditions (aperture size 
100/100 µm2, number of scans 500, resolution 1 cm-1). The spectra did not show any derivative-
like features, typical of specular reflectance, hence neither Kramers-Kronig nor Kubelka-Munk 
transformations were required. The spectra were processed with the GRAMS/AI 8.0 software 
(Thermo Scientific), which was also used for deconvolution of selected spectral regions and 
curve-fitting of overlapping bands. 
 
Results 
 
The surfaces of the tested titanium, titanium alloys and steel 316L were studied using SEM 
before and after immersing them for 56 days in the SBF solution (Fig. 1).   
                      a)                 b)                           c)      d) 
 
 
 
 
 
 
 
Fig. 1. SEM micrographs of the sample surfaces after the SBF treatment: a) pure titanium,  
b) Ti-7,5Mo-2Fe, c) Ti-15Mo-2,8Nb, d) steel 316L 
 
 519. SURFACE ACTIVITY OF TITANIUM ALLOYS CONTACTED WITH THE SIMULATED BODY FLUID. 
J. MYSTKOWSKA1,A, P. DEPTUŁA1,B, J. KOLMAS2,A, J. R. DĄBROWSKI1,C 
 
 
 VIBROMECHANIKA. JOURNAL OF VIBROENGINEERING.   DECEMBER 2009. VOLUME 11, ISSUE 4. ISSN 1392-8716 
727 
Figure 1 indicates that apatite crystallites were formed on each of the sample surfaces. 
The SEM images showed deposition of dendrite-like particles which habit is typical of apatite 
crystallites. The crystallites have been further analyzed using the FTIR microscopy. Figure 2 
shows a representative infrared reflectance spectrum of the studied coatings obtained for the 
316L steel sample. The spectral assignment was done using IR frequencies from the literature 
[Thomas S. Enhanced IR-Wizard. Available from URL: http://www.chem.uni-potsdam.de 
/~thomas/index.php (follow the link to Wizards)]. All the acquired spectra are similar and 
contain bands originated from the SBF components. The peaks at 1658, 1561 and 1296 cm-1 
come from the organic component (TRIS). The intensive, well resolved band at 662 cm-1 
originates from sulphates. Carbonate bands were detected in the 1450-1400 cm-1 region and 
at 873 cm-1. 
 
 
Fig. 2.  The representative infrared spectrum of the analyzed coatings (steel 316L) 
 
 
 
Fig. 3. Deconvolution of the 1200-900 cm-1 IR region (steel 316L) 
 
 519. SURFACE ACTIVITY OF TITANIUM ALLOYS CONTACTED WITH THE SIMULATED BODY FLUID. 
J. MYSTKOWSKA1,A, P. DEPTUŁA1,B, J. KOLMAS2,A, J. R. DĄBROWSKI1,C 
 
 
 VIBROMECHANIKA. JOURNAL OF VIBROENGINEERING.   DECEMBER 2009. VOLUME 11, ISSUE 4. ISSN 1392-8716 
728 
The broad, complex peak in the 1200-900 cm-1 region comprises overlapped acidic 
phosphate (HPO42-), sulphate (SO42-) and phosphate (PO43-) bands (Fig. 3). The presence of the 
bands at 1053 cm-1 and 1036 cm-1 indicates that the coatings contain crystalline calcium 
phosphate. The bands in the 600-550 cm-1 spectral range confirm the presence of apatite 
phosphates. It may be noticed that the apatitic deposits are poorly crystalline, because the band 
at 630 cm-1 characteristic of structural hydroxyl groups is not detectable. The carbonate bands 
indicate that PO43- groups from apatite crystals are partially substituted by CO32- groups (B-type 
substitution).  
 
Conclusions 
 
Bioactivity of pure titanium, two beta titanium alloys and steel 316L was investigated using the 
SEM and IR microscopic methods in this work. Considering the results of the investigations, the 
following conclusions may be formulated: 
• Bioactive precipitations were formed on the surface of each sample; 
• The SEM micrographs show dendrite-like crystallites that are typical of apatite 
phosphates; 
• The FTIR spectra confirm the presence of poorly crystalline carbonatoapatite in the 
deposited surface layer; 
• The FTIR spectra indicate that the carbonatoapatite is of type B (PO43- groups are 
partially replaced by CO32- groups in the crystal lattice). 
 
Acknowledgments 
This work was supported by the Polish Ministry of Science and Higher Education, grant number:  
R1503402. 
 
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Surface activity of titanium alloys contacted with the simulated body fluid

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Surface activity of titanium alloys contacted with the simulated body fluid

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