Relationship between Hydrogen Absorption and Corrosion Behavior of Ti-6Al-4V Alloy Immersed in Acidic Fluoride Solutions

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1 Materials Transactions, Vol. 5, No. 5 (29) pp to 1189 #29 The Japan Institute of Metals Relationship between Hydrogen Absorption and Corrosion Behavior of Ti-6Al-4V Alloy Immersed in Acidic Fluoride Solutions Atsushi Fujita 1, Toshio Ogawa 1, Ken ichi Yokoyama 2; * and Jun ichi Sakai 1;3 1 Department of Materials Science and Engineering, Waseda University, Tokyo , Japan 2 Department of Materials Science and Engineering, Kyushu Institute of Technology, Kitakyushu , Japan 3 Faculty of Science and Engineering, Waseda University, Tokyo , Japan The relationship between hydrogen absorption and the corrosion behavior of Ti-6Al-4V alloy has been examined by immersing the alloy in acidulated phosphate fluoride (APF) solution with various concentrations. Upon immersion in.1 mass% APF solution, no hydrogen absorption is observed despite the occurrence of general corrosion. In.2% APF solution, slight hydrogen absorption occurs soon after immersion, and then the surface of the specimen becomes uniformly covered with a crystalline corrosion product (Na 3 AlF 6 ), thereby inhibiting further hydrogen absorption. In APF solutions with concentrations higher than.4%, the amount of absorbed hydrogen increases with increasing concentration of APF solution and immersion time. The type and morphology of corrosion products sensitively depend on the concentration of APF solution. Upon immersion in.4% APF solution, crystalline and massive Na 3 AlF 6 are observed on the surface of the specimen. In 1.% and solutions, Na 3 AlF 6 with a foldlike shape and granular Na 3 AlF 6 and Na 3 TiF 6 are observed. In 2.% APF solution, only granular Na 3 TiF 6 is observed. The corrosion potentials and anodic polarization curves are analogous in all APF solutions except the.2% and.4% APF solutions. In contrast, the current density of cathodic polarization curves increases with the concentration of APF solution. The results of the present study suggest that the corrosion products play an important role in the hydrogen absorption behavior of Ti-6Al-4V alloy. [doi:1.232/matertrans.mra28481] (Received December 22, 28; Accepted February 26, 29; Published April 8, 29) Keywords: Ti-6Al-4V alloy, biomaterials, hydrogen embrittlement, corrosion 1. Introduction *Corresponding author, yokken@post.matsc.kyutech.ac.jp Titanium and its alloys are used extensively in biomedical applications such as dental implants and dentures. A problem of using titanium alloys in the oral environment is the degradation of mechanical properties associated with the absorption of hydrogen, that is, hydrogen embrittlement, in fluoride solutions including prophylactic agents for caries prevention. 1 3) The amount of hydrogen absorbed by Ti-6Al- 4V alloy 3) tends to be smaller than those absorbed by commercial pure titanium 2,4) and beta titanium (Ti-11.3Mo- 6.6Zr-4.3Sn) alloy 1,5) upon immersion in acidulated phosphate fluoride (APF) solution for the same time. For example, in.2% APF solution, corresponding to the fluoride concentration of commercial toothpastes, Ti-6Al-4V alloy 3) only absorbs a small amount of hydrogen, whereas commercial pure titanium 4) and beta titanium alloy 5) absorb substantial amounts of hydrogen. Ti-6Al-4V alloy appears to have a high resistance to hydrogen absorption in APF solution. However, in 2.% APF solution, Ti-6Al-4V alloy 3) absorbs substantial amounts of hydrogen, similar to the amount absorbed by other titanium alloys. 4,5) The hydrogen absorption behavior of Ti-6Al-4V alloy may depend strongly on the concentration of APF solution. 3) To improve the resistance of titanium alloys to hydrogen absorption in APF solution, the hydrogen absorption behavior of Ti-6Al-4V alloy should be studied. The analysis of corrosion behavior may elucidate mechanisms underlying the high resistance of Ti-6Al-4V alloy to hydrogen absorption. The corrosion behavior (e.g., in the form of electrochemical potential and polarization curves) of titanium alloys in fluoride solutions has been reported by several researchers. 6 14) However, information on the relationship between hydrogen absorption and corrosion behavior in fluoride solutions is limited. For commercial pure titanium immersed in neutral NaF solution, the hydrogen absorption behavior appears to be partially interpreted as electrochemical behavior. 15) In contrast, for Ti-6Al-4V alloy immersed in neutral NaF solution, the hydrogen absorption behavior may be related to the surface conditions rather than an electrochemical factor. 16) Therefore, it is necessary to confirm experimentally the extent to which the hydrogen absorption behavior of Ti-6Al-4V alloy is related to its electrochemical behavior in APF solution. Furthermore, few studies have been carried out on the corrosion morphologies of Ti-6Al-4V alloy in fluoride solutions. The type or morphology of corrosion products on the surface of titanium alloys depends on the concentration of APF solution. 1 5) The role that corrosion products on the surface of titanium alloys play in the hydrogen absorption and corrosion behavior may be worth considering. If a corrosion product inhibits hydrogen absorption, it will be the first such observation for titanium alloys in fluoride solutions, and such a product can be used for surface modification. The purpose of the present study is to systematically investigate the relationship between the hydrogen absorption and corrosion behavior of Ti-6Al-4V alloy in various concentrations of APF solution. The findings will be essential for further improving the reliability of titanium alloys. 2. Experimental Procedure Commercial Ti-6Al-4V alloy wire (described previously 3) ) of.5 mm diameter was cut into specimens of 5 mm length. The nominal chemical composition of the wire is given in Table 1. Percentages in this paper refer to mass percent, unless otherwise stated. The specimens were care-

2 1184 A. Fujita, T. Ogawa, K. Yokoyama and J. Sakai Table 1 fully finished with 6-grit SiC paper and ultrasonically washed in acetone for 5 min. The specimens were immersed separately in 5 ml aqueous solutions of 2.% APF (.48 mol/l NaF +.15 mol/l H 3 PO 4 ) without applied stress at ph 5. at room temperature (25 2 C). To evaluate the effect of the solution concentration, APF solutions of various concentrations were prepared by the dilution of 2.% APF solution. The amount of desorbed hydrogen was measured by hydrogen thermal desorption analysis (TDA) for the immersed specimens. The immersed specimens were cut at both ends and were dried in ambient air and then subjected to TDA, which was started 3 min after the removal of specimens from the APF solution. A quadrupole mass spectrometer (ULVAC, Kanagawa, Japan) was used for hydrogen detection. Sampling was conducted at 3 s intervals at a heating rate of 1 C/h. The corrosion potentials and polarization curves of the specimens in 3 ml APF solution were measured at room temperature under aerated conditions. The counter and reference electrodes used were a platinum electrode and a saturated calomel electrode (SCE), respectively. The corrosion potentials were measured after immersion in APF solution for 1 s. Some specimens were measured for 6 h. The polarization curves were measured from the corrosion potential in the anodic or cathodic direction with a scan rate of 2 mv/min after immersion for 1 min. In addition, the anodic polarization curves were measured after immersion for 24 h. Each measurement was repeated at least three times. The side surface of the immersed specimens was observed by scanning electron microscopy (SEM). The corrosion products on the surface of the immersed specimens were examined by X-ray diffraction (XRD) measurement. The mass ratio of corrosion products on the surface of the immersed specimens was analyzed by energy-dispersive X-ray spectrometry (EDX). The size distributions of the corrosion products were measured from SEM images of 1 4 samples. 3. Results Chemical composition of Ti-6Al-4V alloy (mass%). Ti Al V Fe C N O H Balance The amounts of desorbed hydrogen obtained from TDA are shown in Fig. 1 for the specimens immersed in.1% to 2.% APF solutions under aerated conditions as functions of immersion time. The amounts of desorbed hydrogen for specimens immersed in.2% and 2.% APF solutions from 24 to 6 h are reproduced from our previous article. 3) The amount of hydrogen absorbed during immersion tests was calculated by subtracting the predissolved hydrogen content (96 mass ppm) from the amount of desorbed hydrogen. Upon immersion in.1% APF solution, no increase in the amount of desorbed hydrogen was observed even after 6 h. In.2% APF solution, the amount of absorbed hydrogen saturated at approximately 3 5 mass ppm in the early stage of the Desorbed hydrogen, C / mass ppm Desorbed hydrogen, C / mass ppm % APF.2% APF; Ref. 3).4% APF 2.% APF; Ref. 3) Immersion time, t / h.2% APF Immersion time, t / h Fig. 1 Amounts of desorbed hydrogen obtained from TDA of specimens immersed in various APF solutions as a function of immersion time up to 6 h and.2% APF solution up to 24 h. immersion. 3) As shown in Fig. 1, the hydrogen absorption in.2% APF solution occurred up to 6 h and then saturated. When the concentration of APF solution was higher than.4%, the amount of absorbed hydrogen increased with increasing immersion time and concentration of APF solution. For example, the amounts of hydrogen absorbed upon immersion in.4%, 1.%, 1.5% and 2.% APF solutions for 6 h were approximately 57, 72, 3 and 9 3) mass ppm, respectively. The shifts of the representative corrosion potentials of the specimens immersed in APF solutions under aerated conditions are shown in Fig. 2. In.1% APF solution, the corrosion potential was stable at approximately 1: V. In.2% APF solution, the corrosion potential shifted to the noble direction after 5 6 h with the deposition of a corrosion product, and then reached :5 V. In.4% APF solution, the corrosion potential shifted abruptly to the noble direction immediately after immersion, then gradually shifted to the less noble direction and reached approximately 1: V. The corrosion potentials of the specimens immersed in solutions with concentrations of 1.% and above were stable at approximately 1: V even after 6 h. Figure 3 shows the polarization curves of specimens immersed in various APF solutions under aerated conditions after 1 min. The anodic polarization curves only slightly depended on the concentration of APF solution. The current density exceeded 2 2 ma/cm 2, indicating active dis-

3 Relationship between Hydrogen Absorption and Corrosion Behavior of Ti-6Al-4V Alloy Immersed in Acidic Fluoride Solutions 1185 Corrosion potential, E / V vs. SCE % APF.4% APF.2% APF 2.% APF Immersion time, t / h Fig. 2 Changes in corrosion potentials of specimens in various APF solutions. solution. In the cathodic polarization curves, the current density increased with the concentration of APF solution, although it was the almost the same at concentrations of 1.5% and 2.%. The anodic polarization curves of specimens after immersion in various APF solutions under aerated conditions for 24 h are shown in Fig. 3. The current density for specimens in.2% and.4% APF solutions decreased to 3 and 1 ma/cm 2, respectively. The anodic polarization curves of specimens immersed in the other APF solutions after 24 h were analogous to those after 1 min. On the side surface of the nonimmersed specimen, scratches due to SiC paper polishing were observed, as shown in the SEM image in Fig. 4. For the specimen immersed in.1% APF solution for 24 h (Fig. 4), general corrosion was observed on the side surface; the scratches due to paper polishing almost disappeared. For the specimen immersed in.2% APF solution for 24 h (Fig. 4(c)), a crystalline corrosion product was observed uniformly on the entire surface of the specimen. The corrosion product was confirmed to form after 5 6 h. Magnified views and the size distribution of the corrosion product on the surface of the specimen immersed in.2% APF solution are shown in Figs. 5 and, respectively. The corrosion product was identified as Na 3 AlF 6 (monoclinic; a ¼ :7769 nm, b ¼ :5593 nm, c ¼ :544 nm, ¼ 9:18 ) by XRD measurement and EDX analysis (results not shown), as similar to that reported previously. 3) The corrosion products formed upon immersion in.4% APF solution (Fig. 4(d)) were classified into two types. One type of corrosion product spread over the entire specimen was crystalline Na 3 AlF 6 (Fig. 5(c)), and similar to that obtained upon immersion in.2% APF solution. The average size of this crystalline corrosion product after immersion in.4% APF solution (Fig. 5(d)) was smaller than that obtained after immersion in.2% APF solution (Fig. 5). The other type was a massive corrosion product (Na 3 AlF 6 ), as shown in Fig. 5(e), distributed locally on the surface of the specimen. The surfaces of the specimens Potential, E / V vs. SCE Potential, E / V vs. SCE Current density, i / µa cm % APF.2% APF.4% APF.2% APF.4% APF.1% APF 2.% APF Current density, i / µa cm -2 2.% APF Fig. 3 Polarization curves of specimens in various APF solutions after immersion for 1 min and anodic polarization curves of specimens in various APF solutions after immersion for 24 h. immersed in 1.% and solutions are shown in Figs. 4(e) and (f), respectively. The foldlike-shaped and granular corrosion products were observed on the entire surface of both specimens. In these APF solutions, two types of corrosion products, i.e., Na 3 AlF 6 and Na 3 TiF 6 (monoclinic; a ¼ :5543 nm, b ¼ :5748 nm, c ¼ :82 nm, ¼ 9:29 ), were identified by XRD measurement of the surface of the specimens. From EDX analysis, Na, Al and F were the elements mainly detected in the foldlike product, indicating the formation Na 3 AlF 6. The average size of the foldlike product for the specimen immersed in solution was larger than that for the specimen immersed in solution, as shown in Fig. 6. On the other hand, because the morphology of granular Na 3 AlF 6 is similar to that of granular Na 3 TiF 6, the composition of the granular corrosion product could not be distinguished without EDX analysis, as shown in Fig. 7. In 2.% APF solution (Fig. 5(g)), only Na 3 TiF 6 was detected by XRD measurement, similar to in a previous report. 3) With increasing

4 1186 A. Fujita, T. Ogawa, K. Yokoyama and J. Sakai general corrosion (c) (d) covered with Na 3 AlF 6 covered uniformly with Na 3 AlF 6 massive Na 3 AlF 6 (e) (f) foldlike Na 3 AlF 6 Na 3 TiF 6 foldlike Na 3 AlF 6 Na 3 TiF 6 (g) Na 3 TiF 6 1 µm Fig. 4 SEM images of typical side surface of nonimmersed specimen, and specimens immersed in.1%, (c).2%, (d).4%, (e) 1.%, (f) 1.5% and (g) 2.% APF solutions for 24 h. concentration of APF solution, the amounts of the crystalline corrosion product (Na 3 AlF 6 ) and the corrosion product with the foldlike shape decreased, whereas the amount of Na 3 TiF 6 increased. 4. Discussion The results of the present study indicate that there is no simple relationship between the hydrogen absorption and

5 Relationship between Hydrogen Absorption and Corrosion Behavior of Ti-6Al-4V Alloy Immersed in Acidic Fluoride Solutions 1187 crystalline Na 3 AlF 6 Percentage (%) (c) 2 µm crystalline Na 3 AlF 6 Percentage (%) Size of Na 3 AlF 2 6, s / µm (d) (e) 2 µm Size of Na 3 AlF 6, s / µm 2 massive Na 3 AlF 6 2 µm Fig. 5 Magnified SEM images of side surface of specimens immersed in.2%, and (c) and (e).4% APF solutions. Size distribution of crystalline Na 3 AlF 6 on side surface of specimens immersed in.2% and (d).4% APF solutions. Percentage (%) granular Na 3 TiF 6 granular Na 3 AlF Size of foldlike product, s / µm 2 2 µm Fig. 6 Size distribution of foldlike Na 3 AlF 6 on the side surface of specimens immersed in 1.% and solutions. Fig. 7 SEM image of granular corrosion products on side surface of specimen immersed in solution for 24 h.

6 1188 A. Fujita, T. Ogawa, K. Yokoyama and J. Sakai corrosion behavior of Ti-6Al-4V alloy in APF solution. As shown in Figs. 2 and 3, the corrosion potential and anodic polarization curves for the.1% APF solution were similar to those for the 1.% to 2.% APF solutions, although the cathodic polarization curve depended on the concentration of APF solution. However, no hydrogen absorption occurred in.1% APF solution, whereas the amount of absorbed hydrogen increased with the concentration of APF solution higher than.4%. In the neutral 2.% NaF solution without applied potential reported previously, 17) the corrosion potential is stable at approximately :3 V and general corrosion was observed; however, Ti-6Al-4V alloy does not absorb hydrogen. These results suggest that for Ti-6Al-4V alloy, corrosion does not necessarily lead to hydrogen absorption in fluoride solution, although for commercial pure titanium, corrosion leads to hydrogen absorption. 17) In aqueous Na 2 SO 4 solutions with ph ranging from 3. to 7., as reported by Haruna et al., 18) hydrogen-induced environment-assisted cracking of Ti-6Al-4V alloy does not occur even under a cathodic potential of 2: V. In addition, we have recently demonstrated that the hydrogen absorption of Ti-6Al-4V alloy occurs below the cathodic potential of 1:9 V in neutral 2.% NaF solution. 16) In the present study, however, Ti-6Al-4V alloy absorbed substantial amounts of hydrogen in APF solutions with concentration of.4% and higher under a corrosion potential of 1: V. Furthermore, although electrochemical behavior was not significantly different between 1.5% and 2.% APF solutions, the amount of absorbed hydrogen depended on the concentration of APF solution. Thus, it appears to be difficult to predict hydrogen absorption behavior based on only electrochemical behavior. The effects of corrosion behavior including corrosion products and corrosion morphologies on hydrogen absorption behavior should be investigated in each environment. The type of corrosion product is often changed by the composition of the titanium alloy and/or the concentration of APF solution. Upon immersion in 2.% APF solution, the corrosion product of Na 3 TiF 6 is observed on the surface of not only Ti-6Al-4V alloy 3) but also commercial pure titanium, 2,4) Ti-.2Pd alloy 19,2) and Ti-11.3Mo-6.6Zr-4.3Sn alloy. 5) Another corrosion product of Na 5 Ti 3 F 14 is also observed in the case of Ti-11.3Mo-6.6Zr-4.3Sn alloy. 1,5) On the other hand, upon immersion in.2% APF solution, the corrosion products depend on the titanium alloy. For example, the corrosion products of commercial pure titanium 4) and Ti-11.3Mo-6.6Zr-4.3Sn alloy are TiF 2 and TiF 3, 5) respectively. In the case of Ti-6Al-4V alloy immersed in.2% APF solution, the surface of the specimen is uniformly covered with the crystalline corrosion product of Na 3 AlF 6, as shown in Fig. 5. In this case, the major characteristic of the corrosion products for Ti-6Al-4V alloy seems to be the absence of Ti element. Upon increasing the concentration of APF solution, the surface of Ti-6Al-4V alloy became inhomogeneously covered with Na 3 AlF 6 with various morphologies, and Na 3 TiF 6 was also observed, as shown in Fig. 4. In.1% APF solution, no corrosion products were observed by SEM and XRD measurement. However, in.1% NaF-containing artificial saliva adjusted to ph 5 by lactic acid, Na 2 TiF 6 is detected on the Ti-6Al-4V alloy surface polished with 1 mm alumina powder using an X-ray photoelectron spectrometer, as reported by Huang. 21) The type and morphology of the corrosion product may depend on the composition of the fluoride solution as well as its concentration, although the effects of dissolved oxygen in the solution and/or the surface conditions of the specimen on corrosion behavior should not be excluded. In.1% APF solution, a possible reason for the lack of hydrogen absorption is that the amount of hydrogen evolved on the surface of the specimen was small, as inferred by the current density of cathodic polarization curve (Fig. 3) and the morphology of the surface subjected to corrosion (Fig. 4). In neutral 2.% NaF solution, when small amounts of hydrogen are evolved, no hydrogen absorption occurs, as reported previously. 16) In.2% APF solution, Ti-6Al-4V alloy absorbs a small amount of hydrogen (3 5 mass ppm), 3) upon which its mechanical properties hardly degrade, whereas commercial pure titanium 4) and Ti-11.3Mo-6.6Zr-4.3Sn alloy 5) absorb large amounts of hydrogen, upon which their mechanical properties degrade markedly. For Ti-6Al-4V alloy, the saturation of hydrogen absorption (Fig. 1) coincides with the shift to the noble direction of the corrosion potential (Fig. 2) with the deposition of the crystalline corrosion product (Na 3 AlF 6 ) on the specimen in.2% APF solution. Moreover, in the case of Ti-6Al-4V alloy immersed in.2% APF solution for 24 h, i.e., the surface of the specimen covered uniformly with crystalline Na 3 AlF 6 shown in Fig. 4(c), the corrosion resistance increased as shown by the anodic polarization behavior in Fig. 3. In separate experiments, we have confirmed that the specimen coated with crystalline Na 3 AlF 6 does not absorb hydrogen even in 2.% APF solution for 24 h. Accordingly, the crystalline Na 3 AlF 6 inhibits the hydrogen absorption of Ti-6Al-4V alloy in APF solutions. This is the first ever report of the inhibition of hydrogen absorption by a corrosion product. This finding may be applied to inhibit the hydrogen absorption and corrosion of titanium alloys. It has also been reported that hydrides formed at the surface layer of alpha titanium serve as a barrier to preventing further hydrogen absorption ) Under the sustained tensile-loading test in.2% APF solution in our previous study, 3) Ti-6Al-4V alloy fractures at high applied stress, although the fracture does not occur within 1 h at low applied stress. At high applied stress, the peeling off of Na 3 AlF 6 from the surface of the specimen probably resulted in further hydrogen absorption. This is supported by the fact that the morphology of the side surface of the specimen subjected to a sustained tensile-loading test is not always the same as that of the present specimen immersed without applied stress (Fig. 4(c)). It appears that Na 3 AlF 6 is chemically stable, but it is not effective for preventing hydrogen absorption under high applied stress. In APF solutions with concentration higher than.4%, since Ti- 6Al-4V alloy continuously absorbs hydrogen, the fracture associated with hydrogen absorption probably occurs even at low applied stress. Actually, in 2.% APF solution, fracture occurs at low applied stress, although the time to fracture increases with decreasing applied stress. 3) In.4% APF solution, the abrupt shift to the noble direction of the corrosion potential immediately after immersion (Fig. 2) and the decrease in the current density after immersion for 24 h (Fig. 3) may be related to the

7 Relationship between Hydrogen Absorption and Corrosion Behavior of Ti-6Al-4V Alloy Immersed in Acidic Fluoride Solutions 1189 critical conditions for inhibiting hydrogen absorption. When the concentration of APF solution was higher than.4%, the complete inhibition of hydrogen absorption by Na 3 AlF 6 was not recognized. However, because Na 3 AlF 6 existed on part of the surface of the specimen, hydrogen absorption appeared to be somewhat inhibited depending on the amount of Na 3 AlF 6. In addition, the inhomogeneous deposition and morphology of Na 3 AlF 6 may affect the inhibition of hydrogen absorption. Further study is needed regarding this point. 5. Conclusions We have demonstrated that the hydrogen absorption behavior of Ti-6Al-4V alloy is not necessarily consistent with the electrochemical behavior of the alloy upon immersion in APF solutions. In APF solutions with concentration higher than.4%, the amount of absorbed hydrogen increases with the concentration of APF solution and immersion time. The crystalline corrosion product (Na 3 AlF 6 ) on the surface of the specimen inhibits the hydrogen absorption of Ti-6Al-4V alloy in APF solution. The high resistance to the hydrogen absorption of Ti-6Al-4V alloy in APF solution can be explained to some extent in terms of the corrosion product formed. Consequently, the hydrogen absorption behavior should be investigated in each environment without estimating it from only the electrochemical behavior. Acknowledgments This study was supported in part by the Light Metal Educational Foundation and a Grant-in-Aid for Scientific Research (C) (185672) from the Ministry of Education, Culture, Sports, Science and Technology, Japan. REFERENCES 1) K. Kaneko, K. Yokoyama, K. Moriyama, K. Asaoka, J. Sakai and M. Nagumo: Biomaterials 24 (23) ) K. Yokoyama, K. Kaneko, Y. Miyamoto, K. Asaoka, J. Sakai and M. Nagumo: J. Biomed. Mater. Res. A 68A (24) ) K. Yokoyama, T. Ogawa, K. Asaoka and J. Sakai: Corros. Sci. 47 (25) ) K. Yokoyama, T. Ogawa, K. Asaoka and J. Sakai: Mater. Sci. Eng. A 384 (24) ) T. Ogawa, K. Yokoyama, K. Asaoka and J. Sakai: Biomaterials 25 (24) ) H. Mimura and Y. Miyagawa: Jpn. J. Dent. Mater. Dev. 15 (1996) ) Y. Oda, E. Kawada, M. Yoshinari, K. Hasegawa and T. Okabe: Jpn. J. Dent. Mater. Dev. 15 (1996) ) L. Reclaru and J.-M. Meyer: Biomaterials 19 (1998) ) M. Nakagawa, S. Matsuya, T. Shiraishi and M. Ohta: J. Dent. Res. 78 (1999) ) H. H. Huang: Biomaterials 23 (22) ) N. Schiff, B. Grosgogeat, M. Lissac and F. Dalard: Biomaterials 23 (22) ) H. M. Shim, K. T. Oh, J. Y. Woo, C. J. Hwang and K. N. Kim: J. Biomed. Mater. Res. B 73B (25) ) Y. Matono, M. Nakagawa, S. Matsuya, K. Ishikawa and Y. Terada: Dent. Mater. J. 25 (26) ) B. Lindholm-Sethson and B. I. Ardlin: J. Biomed. Mater. Res. A 86A (28) ) K. Takashima, K. Yokoyama, K. Asaoka and J. Sakai: J. Alloy. Compd. 431 (27) ) K. Yokoyama, K. Takashima and J. Sakai: Mater. Trans. 49 (28) ) K. Yokoyama, T. Ogawa, K. Asaoka and J. Sakai: J. Biomed. Mater. Res. B 78B (26) ) T. Haruna, M. Hamasaki and T. Shibata: Mater. Trans. 46 (25) ) K. Yokoyama, T. Ogawa, K. Asaoka and J. Sakai: J. Alloy. Compd. 4 (25) ) K. Yokoyama, T. Ogawa, K. Asaoka and J. Sakai: Mater. Sci. Eng. A 419 (26) ) H. H. Huang: Biomaterials 24 (23) ) I. I. Phillips, P. Poole and L. L. Shreir: Corros. Sci. 12 (1972) ) I. I. Phillips, P. Poole and L. L. Shreir: Corros. Sci. 14 (1974) ) Z. F. Wang, C. L. Briant and K. S. Kumar: Corrosion 54 (1998) ) Z. F. Wang, C. L. Briant and K. S. Kumar: Corrosion 55 (1999) ) T. Ogawa, K. Yokoyama, K. Asaoka and J. Sakai: J. Alloy. Compd. 396 (25)

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