The Physical and Biological Properties of Alkali –Heat Treated Titanium Implant Material

International Journal of Engineering & Technology IJET-IJENS Vol:13 No:04 59

137504-3838-IJET-IJENS © August 2013 IJENS I J E N S

Abstract- Recent studies on the surface modification by alkali and heat treatments in Titanium metal are reviewed. Previous laboratory studies investigated the effects of different alkali and heat treatments on properties of Ti implant material. It seems hopeful that this type of treatments is a suitable technique for dental implants. In the present study, heat treatments applied above700co that may seem hopeful to apply change in the limit of temperature range that all previous researches decide. Apply physical studies to correlate with other properties for development of high bioactive materials.

Index Term- Alkali and heat treatments - crystallite size and lattice distortions– indentation hardness – Ph value- Electrochemical measurements

I. INTRODUCTION

The demand for titanium and its synthetic rutile (which is the most common for TiO2) implant materials are greatly increasing because of the rapid growth of the population ratio of the aged people in the representative countries (1,2) .Chosa et al(3) have been indicated that the apatite was bone – like and accelerated the osteogenic differentiation of human osteoblast – like SaOS- 2cells , suggesting that alkaline –heat treatment might facilitate better integration of titanium implants with bone.Later it was also found that the titanium metal with a titanium oxide layer formed on its surface showed a high apatite –forming ability in a stimulated body fluid when the treatment temperature was in the range 500ᵒc-700oc,(4).The nature of selection of titanium for implantation is determined by a combination of most favorable characteristics including immunity to corrosion , biocomptability, strength, low modulus and density and the capacity for joining with bone(osseointegration) and other tissue. The purpose of this study using X-ray diffraction

analysis is to correlate the structure with other physical and biophysical properties of alkaline –heat treated titanium and the degree of biocomptability of bone. So there is a lack of quantitative experimental data describing the physical and mechanical behviour.Ti-implants have been used for many years as a popular prosthetic restoration for the missing teeth(5). An attempt is made to solve this proplem in this paper with respect to the data needed for evaluating the strengthening contribution in the alkaline –heat treated titanium metal.

II. MATERIALS AND METHODS

Alkali-heat Treatment of Ti Commercially pure (c.p.) Ti plates (10 x 10 x 1 mm for surface analyses (Ti > 99.8%, Kobe Steel, Kobe, Japan) were mechanically polished with 100-, 180-, and 320-grit sand paper, successively, and ultrasonically washed in acetone and distilled water. In our study we have twelve samples from Ti plates they classified according to the condition of the process into two groups, the first group (6 samples) soaked in 5M NaoH at 60oc for 2 days, followed by gentle washing in distilled water and drying in an oven at 37°C for (5 min). A-TI plates were subsequently heated to 800ᵒc, 882oc and 900oc at a rate of 5°C/min in an electrical furnace, kept for2 hr, three of them quenched rapidly in ice, and the other allowed to cool in the furnace (AH-TI).The second group (6 sample) soaked in 5M NaoH at 60 oc for 4 days, followed by gentle washing in distilled water and drying in an oven at 37°C for (5 min). A-TI plates were subsequently heated to 800cᵒ,882coand 900co at a rate of 5°c /min in an electrical furnace, kept for2 hr ,three of them quenched rapidly in ice , and the other allowed to cool in the furnace (AH-TI).

The Physical and Biological Properties of Alkali –Heat Treated Titanium Implant Material

Mustafa Kamal, Raghda .Abogabil* . Metal Physics Lab, Physics Department, Faculty of Science, Mansoura University, Egypt.

Essam E.Al- Wakeel, Dental Biomaterials,Faculty of Dentistry,Mansoura University.

Abd El –Rahman.M.M Oral biology depatement, Faculty of Dentistry,Mansoura University.

K.Shalabi Chemistry Department, Faculty of Science , Mansoura University.

Kamal42200274@yahoo.com raghda9@hotmail.com

*corresponding author, M. sc student, Mansura Urology and Nephrology Center

III. ELECTROCHEMICAL FREQUENCY MODULATION (EFM) FOR CORROSION MONITORING

Electrochemical measurements were made at 37ᵒC using a cell containing naturally aerated simulated body fluid (SBF) as electrolyte the working electrode was pure Titanium (Ti), the reference electrode is a saturated calomel electrode (SCE), and all potentials are referred to this electrode. A large-area platinum electrode was used as the counter electrode. The specimen was connected to a copper wire and then imbedded into an epoxy resin. Before measurements were taken, electrode was polished with emery paper, and then washed thoroughly with doubly distilled water. Finally the electrodes were cleaned ultrasonically for 10 minutes in ethanol, and then it is immersed in the test solution.EFM experiments were performed with applying potential perturbation signal with amplitude 10 mV with two sine waves of 2 and 5 Hz. The choice for the frequencies of 2 and 5Hz was based on three arguments [6]. The larger peaks were used to calculate the corrosion current density (icorr), the Tafel slopes (βc and βa) and the causality factors CF2 and CF3 (7). All electrochemical experiments were carried out using Gamry instrument PCI300/4 Potentiostat/Galvanostat/Zra analyzer, DC105 corrosion software, EIS300 electrochemical impedance spectroscopy software, EFM140 electrochemical frequency modulation software and Echem Analyst 5.5 for results plotting, graphing, data fitting and calculating. Titanium sample and surgical procedure This study was carried out using 10 pure square titanium disks measuring 3*3mm with thickness 1 mm. The samples were modified by soaking in alkaline medium for 4 days and then divided into 2groups (5discs heated to 600ᵒc(gp1) and the other 5 heated to 800ᵒc(gb2)).10 male guineapigs animals weighting 400-500 gm were used in this study and divided into 2 groups (5animals for( gp1)and 5 animals for(gp2).The animals were anaesthiesized with intraperitoneal injection of 10% chloral hydrate,0.4 ml/100mgin addition to 0.1 lidocaine with 1: 100,000 epinepherine was infilterated for local anaesthesia and hemostatsis.The chin of the animal was shaved. A small vertical skin incision was made down to the bone of the mandible and the labial surface of chin area was exposed. Standardized 3*3 bone cavity with depth 1mm (that compatible with disk size) was created on the labial surface of the chin area just adjacent to the madline at the right side. The titanium disks were inserted into the prepared disk bed .The flab was repositioned and the skin closed with non resorable silk 3-0(8). All animals were submitted for 4 weeks in the Medical Research center- Faculty of medicine, Mansoura University. Animals were killed 4 weeks postsurgery by an overdose of general anaesthesia .Samples were taken and kept in 4% buffered formaldehyde solution for 24 hours, Then decalcified with 10%nitric acid and prepared for histological examination(9).

IV. RESULTS AND DISCUSSION

a) Structural analysis 1) Phase identification

A typical X-ray diffraction obtained from the alkaline –heat treated titanium metal is shown in the figure [1, 2]. The experimentally observed interplanar spacing of the strong and weak reflections are tabulated in the table. The pattern can be indexd in terms of the existence of tetragonl TiO2 "rutile "It can be seen from table I, the position of the rutile TiO2 phase peaks are similarly to those observed by earlier workers(3,4)

Table I hkl

d(Aᵒ)

110 100 3.247 101 50 2.487 200 8 2.297 111 25 2.188 210 10 2.054 211 60 1.6874 220 20 1.6237 002 10 1.4797

0 20 40 60 80-500

10001500200025003000

0 20 40 60 80-500

10001500200025003000

0 20 40 60 80-500

10001500200025003000

2 days alkaline thenheat treated 900c

2 days alkaline then heat treated 882c

2days alkaline then heat treated 800c

0 20 40 60 80-500

100015002000250030003500

0 20 40 60 80-500

100015002000250030003500

0 20 40 60 80-500

100015002000250030003500

(2theta)

2days alkaline then heat treated 900cthen water quenched

(2theta)

Fig. 1. X ray diffraction analysis of Ti immersed in NaOH 2 days then heat

treated.

0 20 40 60 80

10001500200025003000

0 20 40 60 80

10001500200025003000

0 20 40 60 80

10001500200025003000

(2theta)

4days alkaline thenheat treated 900c then water quenched

(2theta)

0 20 40 60 80

10001500200025003000

0 20 40 60 80

10001500200025003000

0 20 40 60 80

10001500200025003000

(2theta)

Fig. 2. X ray diffraction analysis of Ti immersed in NaOH 4 days then heat

treated.

2) Crystallite size and lattice disorders A polycrystalline metallic material with no lattice strain and consisting of crystallites larger than 500nm .shows sharp peaks in X ray diffractometer .Defects in the structure of the crystallites consisting the sample cause a broadening of the diffraction peaks, as does lattice strain. Large crystallites give rise to sharp peaks, as the domain size reduces, the peak width increases and the intensity decreases (10). Line widths B, both FWHM and integral were used in a Willamson –Hall plot (11, 12, 13) as illustrated in the fig [3, 4].

0.15 0.20 0.25 0.30 0.35 0.400.0

sin ((θ/λ))

sin ((θ/λ)) 900c)

sin ((θ/λ))

800c (w.q)

sin ((θ/λ)) 882(w.q))

sin ((θ/λ))

900c(w.q)

sin ((θ/λ))

Fig. 3. illustrate the lattice distoration of Ti immersed in NaOH for 2 days.

0.15 0.20 0.25 0.30 0.35 0.400.0

sin (q/l)

sin (q/l) 900c)

sin (θ/λ)

800c (w.q)

sin (q/l) 882(w.q)

sin (q/l)

900c(w.q))

sin (θ/λ)

Fig. 4. illustrates the lattice distortion of Ti immersed in NaOH for 4 days.

To derive information about the size of coherent zones (crystallite size Deff ) and local strain < Ƹ2 > in all phases:

The 1/Deff and <�2>½ parameters are given in table II

Table II

illustrate the result of 1/Deff and <�2>½ parameters.

1/Deff (A-

conditions

0.065102

0.168344

2daysalkaline 800cᵒ

0.076542

0.194599

4days alkaline 800cᵒ

0.068721

0.180319

2days alkaline 800cᵒ (water quenching)

0.071232 0.147368

0.057847

0.088248

0.072247

0.166765

0.07203

0.174212

2daysalkaline 882cᵒ (water quenching)

0.079853

0.19346

0.091509

0.2168

2daysalkaline900cᵒ

0.08733

0.211561

4daysalkaline900cᵒ

0.064076

0.153374

2daysalkaline900cᵒ (water quenching)

0.071768

0.182738

For the conditions 2 days alkaline 882Co, 1/Deff is measured, hinting to a good crystallization state .Lattice distortions for all samples are lower for 2 days alkaline 882 Co .This supports the optimum formation of the rutile phase close to valence electron concentration e/a=3.2.This condition is more ordered than the others supporting the stacking faults in segregation origin of the rutile lattice. Stacking faults in tetragonal lattice cause specific shifts and line width variations. Therefore, we

must calculate that the concentration of stacking faults in the condition 2 days alkaline 882 Co is low enough to be concealed by the low –angle diffractometric aberrations causing line shifts. So the changes in line profile with the alkaline treatment have been correlated with the changes in the intensity and it s show that some lattice defects must be present in the alkali treated state. Table III shows the lattice parameters a, c and c/a of the tetragonal rutile. The axial ratio, measured at all conditions, was shown to decrease slightly from 0.770 to 0.584 when the conditions varied. Observations about changes in lattice parameters with different conditions; it is found in a non linear way .The c/a ratio varied from 0.7770 to 0.584 .This behaviour is similar to hexagonal close packed structure. As there is no reason to suppose that atoms in these crystals are not in contact ,it follows that they must be ellipsoidal in shape rather than spherical .It should be noted that the effect of temperature on the thermal vibrations of the atoms of a crystal does not cause any broadening of the diffraction lines ; they remain sharp ,but their maximum intensity gradually decreases .It is also worth noting that the mean amplitude of the atomic vibrations is not a function of the temperature alone but depends on the elastic constants .

Table III shows the lattice parameters a, c and c/a of the tetragonal rutile.

C/a C (A0) a (A0)

conditions

.584 2.684 4.595 2daysalkaline 800cᵒ

.644 2.96 4.595 4days alkaline 800cᵒ

.632 2.91 4.594 2days alkaline 800cᵒ (water quenching)

.741 3.208 4.328 4days alkaline 800cᵒ (water quenching)

.648 2.97 4.58 2daysalkaline 882cᵒ

.795 3.44 4.3272 4daysalkaline 882cᵒ

.644 2.961 4.593 2daysalkaline 882cᵒ (water quenching)

.644 2.962 4.5929 4daysalkaline 882cᵒ (water quenching)

.77 3.33 4.32 2daysalkaline900cᵒ

.648 2.97 4.582 4daysalkaline900cᵒ

.646 2.97 4.594 2daysalkaline900cᵒ (water quenching)

.64 2.95 4.59 4daysalkaline900cᵒ (water quenching)

3) Determination of the number of atoms in a unit cell The next step after establishing the phase identification and lattice distortions is to find the number of atoms in that cell .To find this number we use the fact that the volume of the unit cell, calculated from the lattice parameters by means of the following equation which gives the volume of the tetragonal unit cell, V=a2c, multiplied by the measured density of the substance equals the weight of all the atoms in the cell, so from the followings equation we have (14):

ƩA is the sum of the atomic weights of the atoms in the unit cell ρ is the density (gm/cm3) V is the volume of the unit cell (A˚3) and, n is the number of atoms per unit cell Table IV indicated the number of molecules per unit cell. When the number of atoms determined in this way, the number of atoms per cell is always an integer, within experimental error, expect for a few substance which have defect structures.

Table IV indicated the number of molecules atoms per unit cell.

Number of atoms per unit cell

conditions

1.9 2daysalkaline 800cᵒ 1.8 4days alkaline 800cᵒ 1.9 2days alkaline 800cᵒ

(water quenching) 1.8 4days alkaline 800cᵒ

(water quenching) 1.9 2daysalkaline 882cᵒ 2.1 4daysalkaline 882cᵒ 1.9 2daysalkaline 882cᵒ

(water quenching) 2.1 4daysalkaline 882cᵒ

(water quenching) 1.9 2daysalkaline900cᵒ 1.95 4daysalkaline900cᵒ 2.1 2daysalkaline900cᵒ

(water quenching) 1.95 4daysalkaline900cᵒ

(water quenching) In these substances which treated in this work, atoms are simply missing from a certain fraction of those lattice sites which they would be expected to occupy, and the result is a non integral number of atoms per cells. It is found in the primitive cell of TiO2 in the rutile structure which shown in fig [5].

Fig. 5. primitive cell of TiO2 in the rutile structure.

Primitive unit cell in the rutile structure; the red and yellow spheres represent the Ti and O atoms, respectively.In this study it is also investigated that any distortion of the unit cell which decreases its symmetry, in the sense of introducing additional variable parameters, will increase the number of

lines on the diffraction pattern. If the hexagonal cell of the titanium metal is distorted along its two axis, then it becomes tetragonal , its symmetry increases , and less diffraction lines are formed .The decrease in the number of lines is caused by uniform distortion without introduction of new plane spacing. (b)Mechanical properties 1) Elastic moduli In general, Polycrystalline solids comprised of randomly oriented crystallites exhibit quasi-isotropic elastic behaviour. The magnitude of defect free material s is only a function of the magnitude of the stiffness of the atomic bonds. In real polycrystalline materials, other factors, such as porosity, texture, concentrations of impurities and alloying elements, intergranular phases, etc may influence the magnitude of the elastic constants (15).Dynamic techniques provide an advantage over static technique because of ease of specimen preparation, wide variety of specimen shapes and sizes, great precision and measurement over a wide temperature range.Elastic moduli are lists in the table V it can be seen that the dynamic Elastic moduli as a function of both the time and temperature decreases and then increased to the value of 73.6 GPa .But in the case of water quenching, it was found that the Young's modulus increased gradually to the value 131GPa. It is well known that Young's modulus, one of the intrinsic natures of materials, is determined by the bonding force among atoms. This bonding force is not only related to the crystal structure but also to the distances among atoms, and it can be effected by alkali heat treatment. So Young' modulus is not sensitive to grain size and the structure of materials for the present studied sample in this work, the elastic moduli mainly depends on the lattice disorder.Elastic materials have characteristic sets of natural acoustical resonance frequencies, which are determined by the elastic moduli. The specific density and the dimensions of the body, Thus it is evident to use these frequencies (16) as a tool to determine the elastic moduli . Results of the measured Elastic moduli values are lists in the table V using the following equations:

Where the density of the sample ρ , l is the length of the sample, fo is the resonance frequency of the sample, k is the thickness of the sample.

Table V listed Elastic moduli.

conditions

58.75 28.69 74.03 2daysalkaline 800cᵒ 43.33 21.2 54.6 4days alkaline 800cᵒ 73.88 36.36 93.1 2days alkaline 800cᵒ

(water quenching) 20.13 40.91 51.55 4days alkaline 800cᵒ

(water quenching) 2daysalkaline 882cᵒ 39.36 19.4 49.6 4daysalkaline 882cᵒ 55.5 27.131 70 2daysalkaline 882cᵒ

(water quenching) 45.625 22.4 57.488 4daysalkaline 882cᵒ

(water quenching) 28.57 14.1 36 2daysalkaline900cᵒ 58.42 28.7 73.62 4daysalkaline900cᵒ 33.62 68.25 86 2daysalkaline900cᵒ

(water quenching) 50.77 103.9 131 4daysalkaline900cᵒ

(water quenching)

V. 2) VICKERS MICROMECHANICAL INDENTATION OF

CRYSTALS

Many investigation have been undertaken to correlate the indentation hardness with other physical properties .Hardness testing provide useful information concerning the mechanical behaviour of solids (17).Hardness data provide a good general impression of surface preparation and anisotropy of elastic and plastic properties. March (18,19), therefore treated the indentation process as analogous to the expansion of a spherical cavity in an elastic boy and derived the equation:

And υ is the poisson's ratio , E the young's modulus , �y the yield stress and H the hardness (defined as load divided by projected area of indentation) . The early theoretical attempts to correlate the hardness to tensile parameters have used the slip line field .Hence simplified correlations of the form H=K�y with k as proportionality constants have been successfully used for specific metals over a limited range of plastic deformation

response. This relation H=K�y is explained in details by Jaramillo et al (20)who confirmed its validity for metals with high ratio , �y /E . For example, for metallic materials, it is commonly observed that H=3�y (21)

Theoretical justification for this approximation has been derived by Hill, based on slip –plane field analysis (22). The measured hardness values are listed in table VI along with corresponding yield stress; the hardness values represent average 12 to 20 reading.

Table VI

listed the measured hardness values

Hv/ �y Hv(M Pa) �y conditions 1870.036 5.18 2.77* 2daysalkaline 800cᵒ

1386.957 4.466

3.22* 4days alkaline 800cᵒ

2337.591 6.405 2.74* 2days alkaline 800cᵒ

(water quenching)

1322.069 3.834 2.9* 4days alkaline 800cᵒ

(water quenching) 1244.828 3.61 2.9* 2daysalkaline 882cᵒ 1304.59 3.979 3.05* 4daysalkaline 882cᵒ

1797.241 5.212 2.9* 2daysalkaline 882cᵒ

(water quenching)

1502.606 4.613 3.07* 4daysalkaline 882cᵒ

(water quenching) 906.8293 3.718 4.1* 2daysalkaline900cᵒ 1893.75 6.06 3.2* 4daysalkaline900cᵒ

2190 5.913 2.7* 2daysalkaline900cᵒ

(water quenching)

2000 3.60 1.08* 4daysalkaline900cᵒ

(water quenching) 3) Hardness Yield stress and the maximum shear stress. The maximum shear stress that is created by a locally applied pressure occurs on the central axis below the pressurized region (23).The maximum shear stress will be Tm=½Hv

And using υ=0.28 this gives Ƭm =0 .333 Hv It shows hardness measurements can be used to obtain yield stresses for these materials and to estimate impact Yield stress (24,25).The results are shown table VII.

Table VII shown result of Vickers hardness and yield stress.

Tm (M Pa) Hv(M Pa) conditions

1.72 5.18 2daysalkaline 800cᵒ 1.487 4.466

4days alkaline 800cᵒ

2.13 6.405 2days alkaline 800cᵒ (water quenching)

1.276 3.834 4days alkaline 800cᵒ (water quenching)

1.202 3.61 2daysalkaline 882cᵒ 1.32 3.979 4daysalkaline 882cᵒ 1.735 5.212 2daysalkaline 882cᵒ

(water quenching) 1.536 4.613 4daysalkaline 882cᵒ

(water quenching) 1.23 3.718 2daysalkaline900cᵒ 2.017 6.06 4daysalkaline900cᵒ 1.969 5.913 2daysalkaline900cᵒ

(water quenching) 1.1918 3.60 4daysalkaline900cᵒ

(water quenching)

(c)Ph value The data in table VIII came in coordination with those obtained by Kim et al. (1997) (26), Gil et al. (2002) (27) and Jonasova et al.(2004) (28)as they all agreed that the ionic movement in the soaking solution (SBF) leads to increase in its PH. It was found that the sodium titanate at the surface releases Na+ ions via exchange with H3O+ ions in the simulated body fluid (SBF) to form many Ti–OH groups on the surface. As a result, the surface is negatively charged and reacts with the positively charged Ca2+ ions in the SBF to form calcium titanate. As the Ca2+ ions accumulate, the surface becomes positively charged and reacts with negatively charged phosphate ions to form metastable phase from Calcium Phosphate. This calcium phosphate is metastable and hence eventually transforms into stable crystalline bonelike apatite.

Table VIII

values of PH value Ph value

conditions

control

8.2 2daysalkaline 800cᵒ 8.37 4days alkaline 800cᵒ 8.2 2days alkaline 800cᵒ

(water quenching) 8.2 4days alkaline 800cᵒ

(water quenching) 8.1 2daysalkaline 882cᵒ 8.32 4daysalkaline 882cᵒ 8.22 2daysalkaline 882cᵒ

(water quenching) 8.34 4daysalkaline 882cᵒ

(water quenching) 8.25 2daysalkaline900cᵒ 8.2 4daysalkaline900cᵒ 8.41 2daysalkaline900cᵒ

(water quenching) 8.28 4daysalkaline900cᵒ

(water quenching) (d)Electrochemical frequency modulation, EFM The EFM is a nondestructive corrosion measurement technique that can directly give values of the corrosion current without prior knowledge of Tafel constants. Like EIS, it is a small ac signal. Intermodulation spectra obtained from EFM measurements are presented in Figures [6, 7, 8, 9] are examples of Ti soaked that classified according to the condition of the process into two groups, The first group (6 sample) soaked in 5M NaoH at 60 ᵒc for 2 days, followed by gentle washing in distilled water and drying in an oven at 37°C for (5 min). A-TI plates were subsequently heated to 800 cᵒ,882oc and 900oc at a rate of 5°C/min in an electrical furnace, kept for2 hr ,three of them quenched rapidly in ice , and the other allowed to cool in the furnace (AH-TI).The second

group(6 sample) soaked in 5M NaoH at 60 ᵒc for 4 days, followed by gentle washing in distilled water and drying in an oven at 37°C for (5 min ). A-TI plates were subsequently heated to 800 ᵒc, 882oc and 900oc at a rate of 5°C/min in an electrical furnace, kept for2 hr, three of them quenched rapidly in ice, and the other allowed to cool in the furnace (AH-TI). Each spectrum is a current response as a function of frequency. The two large peaks are the response to the 2 Hz and 5Hz excitation frequencies. These peaks are used by the EFM140 software package to calculate the corrosion current and Tafel constants. The calculated corrosion kinetic parameters at different treatment of Ti (icorr, βa, βc, CF-2, CF-3) are given in the table IX

Table IX Electrochemical kinetic parameters obtained by EFM technique for Ti subjected for different treatment.

conditions icorr.

µAcm-2

Βa x10-3 mV dec-

Βc x10-3 mV dec-1

CF2 CF3

control 4.005 113.8 135.4 1.3 1.1 2daysalkaline 800cᵒ .7313 42.69 49.98 1.95 2.99 4days alkaline 800cᵒ .4757 49.55 52.37 1.90 3.01

2.664 46.23 47.49 1.98 2.90

2.667 46.49 47.49 1.95 2.95

2daysalkaline 882cᵒ .8291 80.91 89.12 2.01 3.03 4daysalkaline 882cᵒ .908 96.51 130.2 1.95 2.99 2daysalkaline 882cᵒ (water quenching)

1.948 100.2 120.4 1.90 3.01

2.881 104.2 124.6 1.98 2.90

2daysalkaline900cᵒ .8009 81.67 89.42 1.95 2.95 4daysalkaline900cᵒ .4726 14.32 14.93 2.01 3.03 2daysalkaline900cᵒ (water quenching)

1.781 61.04 73.9 1.3 1.7

1.982 65.07 75.6 1.3 1.7

0.0 0.5 1.0 1.5 2.0 2.51E-10

Frequency (Hz)

control

Frequency (Hz)

Fig. 6. 2days soaked in alkaline medium and heat treated .

0.0 0.5 1.0 1.5 2.0 2.5

frequency (Hz)

control

frequency (Hz)

Fig. 7. 2days soaked in alkaline medium and heat treated then water

quenching.

0.0 0.5 1.0 1.5 2.0 2.5

frequency (Hz)

control

frequency (Hz)

Fig. 8. 4days soaked in alkaline medium and heat treated..

0.0 0.5 1.0 1.5 2.0 2.5

Frequency (Hz)

control

Frequency (Hz)

Fig. 9. 4days soaked in alkaline medium and heat treated then water

quenching.

Histological Results:

Fig 10: photomicrograph of group (1) showing the interface area occupied by interconnected network of bony trabculae radiating from old bone periphery with large bone marrow cavities. Oesteoblastic activity could be seen at the

periphery of the trabeculae(H&E stain,400X).

Fig. 11. photomicrographog group (2) showing the area of interface between

bone and titanium plates with formation of new bone sheet with lage oeteocytes dispersed within it . Oesteoblastic activity is seen at the periphery of newly formed sheet. Line of demarcation is apparent between old and new

bone (H&E stain, 400X).

The Hematoxylin and Eosin stain and disscusion The histological sections of (gp2) revealed the formation of new bone sheet with large osteocytes dispersed within the bone. This bone occupying the interface area between old bone and the titanium disc. Osteoblastic activity could be seen along the periphery of newly formed bone. As for (gp1), a network of bony trabeculae is formed with large marrow spaces intervening between them. The bone that was formed with (gp2) was homogenous and appear as one piece than bone formed with (gp1). The clinical success of dental implant is related to early osseointegration which defined as a direct structural and functional connection between ordered living bone and the surface of load carrying implant (29). The important goal of implantology is still to achieve a faster and stronger bone to implant integration for early loading (30). According to our histological result (gp2) appeared to provide a faster and strong connection with titanium disc, This appeared from the shape and organization of the newly formed bone than formed with (gp1)with its network form. This means bone formed with (gp2) was ahead than (gp1).Several modifications have been performed using new treatment methods based on implantation with carbon oxygen (CO) ions (31). Other modifications by producing porous titanium and

titanium alloy implant including the CAD/CAM procedures sintering of particles or plasma spraying of the powder onto implant surface (32). Such modifications were directed to modify the surface composition and topography of dental implant(33) thus facilitate the attachment and differentiation of osteoblasts(34), This come in accordance with the results obtained by Helal and his colleagues(5), they studied the effect of different titanium laser surface treatments on osseointergaration. As a result of this modifications they found that in vitro effect of laser of high power setting increased surface roughness leading to improve osseointegration through using the benefit of the absorptive capacity of Ti toward Nd:YAG.

CONCLUSION Elevated PH values of simulated body fluid (SBF) after immersion of the treated specimen so can be surely linked to the ionic movement that took place between titanium surface and the surrounding solution. In simulated body fluid, the oxide film on treated titanium exhibits high corrosion resistance and a long-term stability than control. Treated Ti subjected to water quenching after treatment is less corrosion resistance than the others as the oxide film responsible for passivity effected by rapid water quenching. Ti treated in 4 days alkaline medium is more favored than 2 days as it show more corrosion resistance. Heating till a800oc leads to better formation and integration with bone than heating to 600oc. So our present experimental data could establish the suitable condition to obtain rutile in a good bone – bonding ability and better integration of titanium implants with bone.

Future Work Future work , according to our experimental data of titanium implants with bone, a porous titanium metal modified with a titanium oxide on its pore will be showed high apatite forming ability in simulated body fluid (SBF), resulting high osteoconductivity as well as osteoinductivity. If detailed mechanisms are revealed in future, new bioactive material could be developed. Scope of this research Our present results could establish the conditions required for the biophysical and alkaline-heat treatments to obtain a rutile TiO2 that could induce high osteogenic differentiation of human osteoblast. In the future work titanium alloys used in a nano scale in orthopedic and dental evaluated in vitro.

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