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1 2012; 31(2): Effects of argon gas flow rate on laser-welding Yasuko TAKAYAMA 1, Rie NOMOTO 2, Hiroyuki NAKAJIMA 3 and Chikahiro OHKUBO 1 1 Department of Removable Prosthodontics, Tsurumi University School of Dental Medicine, Tsurumi, Tsurumi-ku, Yokohama , Japan 2 Department of Dental Engineering, Tsurumi University School of Dental Medicine, Tsurumi, Tsurumi-ku, Yokohama , Japan 3 Dental Laboratory Fandarium, Naka-Rokugo, Ota-ku, Tokyo , Japan Corresponding author, Yasuko TAKAYAMA; takayama-y@tsurumi-u.ac.jp The purpose of this study was to evaluate the effects of the rate of argon gas flow on joint strength in the laser-welding of cast metal plates and to measure the porosity. Two cast plates (Ti and Co-Cr alloy) of the same metal were abutted and welded together. The rates of argon gas flow were 0, 5 and 10 L/min for the Co-Cr alloy, and 5 and 10 L/min for the Ti. There was a significant difference in the ratio of porosity according to the rate of argon gas flow in the welded area. Argon shielding had no significant effect on the tensile strength of Co-Cr alloy. The 5 L/min specimens showed greater tensile strength than the 10 L/min specimens for Ti. Laser welding of the Co-Cr alloy was influenced very little by argon shielding. When the rate of argon gas flow was high, joint strength decreased for Ti. Keywords: Argon gas shielding, Laser-welding, Joint strength, Micro-CT, 3D image INTRODUCTION Titanium (Ti) is considered to be highly biocompatible. It has a low density, and superior anti-corrosion and antiabrasion properties 1,2). Due to its favorable characteristics, Ti has a wide range of applications in dentistry from implants to crowns and denture bases. Wang and Welsch 3) suggested that the following factors that affect Ti joining should be considered: joint design, adequate energy delivery to areas to be joined, method of energy delivery, cooling rate, and amount of contamination during the joining procedure. The wave length, peak pulse power, pulse energy, output energy, pulse duration, pulse frequency and spot diameter of the laser affect the mechanical strength of joints 4-6). NaBadalung and Nicholls 7) suggested that a successful laser weld was formed from a succession of overlapping weld spots and the operating range of this process is determined by a combination of beam power, welding speed, shielding gas, and plasma gas control. Although commercially pure (CP) Ti and Ti alloy are appropriate metals for laser-welding, oxygen contamination is a problem that must be managed in order to produce a successful weld. Oxygen, nitrogen and hydrogen might cause titanium to become brittle, and contamination by these elements during the Ti joining process might result in an alteration of the crystal slip behavior 8-10). Because of the great affinity of Ti for oxygen and its rapid reaction rate at high temperatures, embrittlement of the weld by oxygen absorption easily occurs 11,12). Yamagishi et al. 4) reported a significant relationship between bending strength and the irradiation atmosphere; the irradiation intensity and the combination of atmosphere and intensity. Therefore, it is important to control the atmosphere in the chamber of the laser-welding machine. If the shield is defective, TiO 2 on the surface of Ti may prevent the efficient generation of thermal energy efficiently. In many Japanese dental laboratories, welding procedures have been performed as follows to ensure weld strength and accuracy of laser welding: edge preparation (a groove) is designed in the laser welded alloy joints, the position is determined by penetrationwelding, and the weld area is filled with filler metal under an argon atmosphere. The rate of argon gas flow clinically used during the laser welding procedure for all metals is 5 L/min. A few studies in the past have investigated tensile and bending strengths using argon shielding in laser-welding 4,13), but studies of the specimens produced by this welding procedure used clinically are rare 14-19). The purpose of this study was to compare the effects of argon gas flow rates in laser-welding on the joint strength of cobalt-chromium (Co-Cr) alloy and Ti welded specimens using clinical conditions. In addition, this study evaluated the porosity of specimens welded under various argon gas shielding conditions non-destructively using X-ray micro-focus computerized tomography (micro-ct). MATERIALS AND METHODS Preparation of welded specimens Two metals, Co-Cr alloy and Ti, and two joining metals (filler metals) for welding were chosen for this study (Table 1). Rectangular metal plates were prepared using the lost-wax casting method. Two different sizes of acrylic resin (ShinkoLite; Mitsubishi Rayon Co., Ltd., Tokyo, Japan) patterns were invested in casting rings with an investment material for the subsequent joint strength test. One was mm for the laser-welded specimens and the other was mm for non-welded specimens as a control. An investment material (Multi-Vest; Dentsply Intl. Inc., York, Pa) was used for the Co-Cr alloy and Ti plates before they were cast using Received Jul 22, 2011: Accepted Dec 28, 2011 doi: /dmj JOI JST.JSTAGE/dmj/

2 317 Table 1 Cast metal plate Chemical compositions of the tested alloys Material Code Manufacturer Composition (%) Lasernium EX Co-Cr Ruby Co., Ltd., Osaka, Japan Co(61.2), Cr(30.0), Mo(4.1), Fe(0.7), Mn(0.5), Si(2.0), W(1.0),Ti(0.5) Filler Metal Cast metal plate Lasernium Wire Ti ingot JS2 * Co-Cr Ruby Co., Ltd., Osaka, Japan Co(68.0), Cr(25.0), Mo(5.0), Fe, Si, Al Ti Selec Co., Ltd., Osaka, Japan Ti(99.485), H(0.015), O(0.20), N(0.05), Fe(0.25) Rolled plate Flat bars Ti Nippon Stainless Steel KOZAI Co.Ltd., Niigata, Japan Ti(99.485), H(0.0027), O(0.08), N(0.01), Fe(0.05) Filler Metal Laser Wire Ti * Japanese Industrial Standards (JIS) class2 commercially pure Ti Ti Selec Co., Ltd., Osaka, Japan Ti(99.605), H(0.015), O(0.15), N(0.03), Fe(0.20) a centrifugal casting machine (Co-Cr alloy: Supertron-II; Unique Co., Ltd., Saitama, Japan; Ti: Selecast Super R; Selec Co., Ltd., Osaka, Japan). All the cast plates were removed from the molds, and the sprues of the cast plates were cut off from the cast plates. The cast Co-Cr alloy plates were polished using an electro-polisher (Elepika, Shofu Inc., Kyoto, Japan) at 2 A, 8 C in the electrolyte solution (H 2SO 4 10%) (Shofu Inc., Kyoto, Japan) for 2 min, and the Ti cast plates were immersed in acid solution (Titaclean, Reburn Ohara, Osaka, Japan) at room temperature for 2 min. After electro-polishing or acid immersion, each cast specimen was abraded using silicon points (Shofu Inc., Kyoto, Japan). To prevent generation of heat as much as possible, grinding of the specimen surface was performed at a slow speed with occasional cooling using a spray of water. About 0.3 mm groove was made with a cutting disk in the part to be laser-welded (Fig. 1) and then airborne-particle abraded with 50 µm alumina particles (4.0 kg/cm 2, 20 s) (Fujilundum A80; Fuji Manufacturing Co., Ltd., Tokyo, Japan). Non-welded specimens were prepared as the controls for all experimental conditions. In addition, the CP Ti rolled plates (laser-welded: mm and non-welded: mm) with Japanese Industrial Standards (JIS) class 2 equivalence were prepared. The same about 0.3 mm groove was made in the CP Ti rolled plates as in the specimens for casting. The non-welded specimens were taken as the controls for all experimental conditions. One dental technician with 10 years experience in laser welding fabricated the specimens, since operator dexterity has a significant influence upon laser-welding quality 20). The cast plates and CP Ti rolled plates were matched (Co-Cr alloy to Co-Cr alloy or Ti to Ti) to make welded specimens of similar metals. Each pair of plates was butted longitudinally using a jig and weld-bonded using a Nd:YAG laser welding machine (ALP-50; Alpha-Laser GmbH, Puchheim, Germany). The Co-Cr alloy specimens were welded at a constant voltage of 210 V, pulse duration of 5.4 ms, and spot diameter of 0.7 mm. Ti specimens were welded at a constant voltage of 172 V, Fig. 1 Diagram of the welding specimen. pulse duration of 10.0 ms, and spot diameter of 0.6 mm. Spot welding was initially conducted at three points, namely, the center and one-fourth of the distance bilaterally as a pre-welding procedure. One-spot welding was conducted initially for the CP Ti rolled plates only. These spot welds were penetration-welding, that is, the weld penetration depth exceeded the thickness of the specimens. After the pre-welding procedure, the edge preparation areas in the welded areas were filled with filler metals from both sides. Ti and Co-Cr alloy filler metals (diameter: 0.5 mm) were used for welding. The rate of overlap was approximately 90%. The laser welding was performed with argon gas shielding, in which a flow of argon gas was directed near the surface of the welded area from a nozzle set at an angle of 45 above the specimens. The diameter of the nozzle was 6 mm. The distance between the spot to be welded and the nozzle was approximately 10 mm. The rate of the argon gas flow was controlled by a flow meter on the gas canister. The rates of argon gas flow were 0 L/min, 5 L/ min and 10 L/min for the Co-Cr alloy, and 5 L/min and 10 L/min for Ti. It is understood that argon shielding is definitely necessary for Ti, so the argon gas flow at a rate of 0 L/min was not included in the experimental conditions 4,16). Five welded specimens were produced for each experimental condition along with five non-welded specimens for each metal as controls. Non-destructive analysis The area ( mm) including the welded area of the

3 318 cast specimens was observed and analyzed using a micro-ct device (MCT-CB 100MF, Hitachi Medico, Tokyo, Japan) before tensile testing. The tube voltage and current of the X-ray generator were 80 kv (Co-Cr alloy), 65 kv (Ti) and 100 µa, respectively. X-ray image acquisition was performed with the CCD camera supplied in the micro-ct. Two hundred and one sliced images of the specimens were obtained horizontally along the length of the specimens. The thickness of each slice was mm. These images were reconstructed three-dimensionally (3D) using image analysis software (TRI/3D-Bon; Ratoc Engineering, Tokyo, Japan). The sizes, numbers and total volume ratios of the bubbles present in the specimens were also determined using this software. Fig. 2 Measurement part of microhardness. (a) the CP Ti rolled plates and the Ti cast specimens, (b) the Ti cast specimens Elemental analysis The element analysis of the surface of the welded area of the cast specimens was conducted using an electron probe X-ray microanalyzer (EPMA) (JXA-8900R, JEOL, Tokyo, Japan). The analytical conditions were: magnification 300; accelerating voltage 20.0 kv; dwell time 15.0 ms; and probe current A. The distribution of oxygen at the welded surface of the specimens was examined by mapping analysis. Microhardness test Vickers microhardness measurements were carried out with a hardness tester (MVK-E, Akashi Co., Kanagawa, Japan). Microhardness tests were performed on polished welded areas of the Ti specimens (the CP Ti rolled plates and cast specimens) with a 200 g load for 25 s at 0.0, 0.5, 1.0, 1.5, 2.0 and 5.0 mm distances from the center of welded specimen (Fig. 2a). Moreover, microhardness measurements within a range of 1.7 mm from the center of welded area were taken at three points (A: 0.5 mm from left end of specimen, B: center of specimen, C: 0.5 mm from right end of specimen) in the Ti cast specimens (Fig. 2b). Tensile test The efficiency of the welded joint was measured by tensile testing conducted with a universal testing machine (AG-20 kn; Shimadzu Co, Kyoto, Japan) at a crosshead speed of 1 mm/min and gauge length of 10 mm. The maximum load (N) was recorded and the tensile strengths (MPa) and their means and standard deviations were calculated. The elongation at the maximum load and elastic modulus were calculated from the stress-strain curve of the tensile test. After the tensile test, the fractured surfaces were observed using a scanning electron microscope (SEM) (JSM-5600LV, JEOL, Tokyo, Japan). Statistical analysis Statistical analyses of the group means were made using a one-way analysis of variance and Bonferroni s multiple comparison, Mann-Whitney U test and the Student s t-test ( =0.05). A regression analysis was performed to evaluate the relationship between the porosity and the joint strength. All statistical analysis was performed using software (SPSS for Windows Ver.12.0, SPSS Japan Inc., Tokyo, Japan). RESULTS Figure 3 shows 3D images of the welded areas of the cast specimens. The porous areas were found mostly at the center of the welded area in the Co-Cr alloy specimens, while more porosity was found in the entire welded area of the 5 L/min Ti cast specimens but there was almost none in the 10 L/min Ti cast specimens. Table 2 shows the amounts of porosity in the welded areas of the cast specimens. All the Co-Cr alloy and Ti cast specimens had porosity in the welded area. There were significant differences in porosity for each rate of argon gas flow. There were significant differences between the 5 L/min cast specimens and the 10 L/min cast specimens for both metals. The porosity tended to decrease in Ti although it tended to increase in Co-Cr alloy as the rate of the argon gas flow increased. Moreover, there was a significant difference between the 10 L/min Co-Cr alloy specimens and the 10 L/min Ti cast specimens. Figure 4 shows the microhardness profiles for distances up to 5.0 mm from the center of the welded areas for the Ti specimens. The 5 L/min and 10 L/min cast specimens exhibited almost the same microhardness near the center of the specimen (points 0.0 and 0.5 mm). At 1.0 mm from the specimen center, the mean microhardness was 257 Hv for the 5 L/min cast specimen and 204 Hv for the 10 L/min cast specimen, and at this distance from the specimen center no major variations were found from point to point. The mean microhardness of the CP Ti rolled plates was similar to that of the cast specimens in the center of the welded areas, but became lower at distances of 2.0 mm or more from the center. At more than 1.0 mm, the microhardness decreased gradually with distance from the center, regardless of the rate of argon gas flow for the CP Ti rolled plates and the cast specimens. Figure 5 shows the microhardness profiles within 1.7 mm from the center of welded areas on the Ti cast

4 319 a b c d e Fig. 3 Representative 3D images of the welded areas of the cast specimens. (a) Co-Cr alloy (0 L/min), (b) Co-Cr alloy (5 L/min), (c) Co-Cr alloy (10 L/min), (d) Ti (5 L/ min), (e) Ti (10 L/min)

5 320 Table 2 Porosity in the welded area Welded metal Argon gas Amount of volume of porosity (mm 3 ) Porosity (%) (L/min) Mean (SD) Mean (SD) Co-Cr alloy (0.009) 0.18 (0.06) A (0.017) 0.30 (0.10) A,B (0.007) 0.47 (0.05) Ti (0.041) 0.36 (0.28) B (0.003) 0.03 (0.02) The same letters in Bonferroni group do not differ significantly different at p=0.05. Fig. 4 Profile of Vickers hardness of the Ti specimens (CP Ti rolled plates and Ti cast specimens) within 5.0 mm from the center of welded areas. specimens. The mean microhardness values at the centers of welded areas ( mm) were, for point A: Hv, B: Hv, and C: Hv in the 5 L/min Ti cast specimens. In the 10 L/min Ti cast specimens, the mean microhardnesses within the same area were A: Hv, B: Hv and C: Hv. There was not a large difference in microhardness between the 5 L/min cast specimens and the 10 L/min cast specimens at B. However, a tendency was revealed for the microhardness of the end of specimens to be larger than the microhardness of the center of specimens. The results of tensile testing are shown in Fig. 6. The tensile strengths of the 0 L/min, 5 L/min and 10 L/ min Co-Cr alloy specimens were 719 MPa, 741 MPa and 737 MPa, respectively. The tensile strength of the controls was significantly greater than that of the 0 L/ min Co-Cr alloy specimens. However, no significant difference was found among the three argon shielding conditions. There was a greater significant difference in the tensile strength of the control Ti cast specimens compared to that of the CP Ti rolled plates (control: 435 MPa; 5 L/min: 394 MPa; 10 L/min: 400 MPa). As for the tensile strength of the Ti cast specimens, the controls had the maximum value (504 MPa), followed by the 5 L/ min cast specimens (440 MPa) and the 10 L/min cast specimens (353 MPa). Although the tensile strength of the 10 L/min cast specimens was considerably lower, Fig. 5 Profile of Vickers hardness at the welded areas of the Ti cast specimens. (a) 0.5 mm from left end of specimen (Fig. 2b-A), (b) center of specimen (Fig. 2b-B), (c) 0.5 mm from right end of specimen (Fig. 2b-C).

6 321 Fig. 6 Results of tensile test. Asterisk indicates significant difference (*: p<0.05, **: p<0.01) among the pairs. Fig. 7 Results of elongation (%). Asterisk indicates significant difference (**: p<0.01) among the CP Ti rolled plates and the Ti cast specimens for the same argon gas flow rate. Fig. 8 Results of elastic modulus (GPa). Asterisk indicates significant difference (**: p<0.01) among the CP Ti rolled plates and the Ti cast specimens for the same argon gas flow rate. there were no significant differences among those specimens. When the argon gas flow rates 5L/min and 10L/min were compared, there was no significant difference in the tensile strength of the CP Ti rolled plates and the cast specimens. The tensile strength had no relationship with the porosity in the welded area (Pearson s product moment correlation coefficient; Co-Cr alloy, correlation coefficient 0.442, p=0.099, Ti, correlation coefficient 0.481, p=0.160). Figures 7 and 8 show the elongation at the maximum load and elastic modulus. For the elongation of the Co-Cr alloy and Ti specimens, no significant difference was found due to argon gas flow rate. However, significant differences were found between the CP Ti rolled plates

7 322 Fig. 9 The fractured Ti cast specimens and SEM images of a fracture cross section in the welded area. (a) 5 L/min, (b)10 L/min and the Ti cast specimens among the elongation of the 5 L/min and the 10 L/min argon gas flow rates. For elastic modulus, a significant difference was found between the CP Ti rolled plates and the Ti cast specimens at the control and the 5 L/min argon gas flow rate. As a result of the tensile test, all of the Co-Cr alloy specimens fractured in the parent materials. All of the 10 L/min Ti cast specimens fractured in the welded area. For the 5 L/min Ti cast specimens, 3 out of 5 specimens demonstrated a ductile fracture in the parent metal; a crack occurred at the end of the interface of the welded surface and developed into the parent metal in a ductile fashion. All of the CP Ti rolled plates were fractured by the ductility of the parent metal. Figure 9 shows SEM micrographs of the fractured surfaces of the welded areas of the Ti cast specimens after tensile testing. Some ductile fracture was evident on the fractured surfaces. Figure 10 shows the results of EPMA map analysis for the welded areas on the Ti cast specimens. No difference in the distribution of oxygen in the Ti cast specimens was detected as a result of the rate of argon gas flow. DISCUSSION Edge preparation, penetration-welding, two-sided welding and overlapped welding in an argon atmosphere are now common procedures used in welding of dental prostheses. The laser welding conditions, such as the current, pulse duration and spot diameter, used for prosthodontic repair were similar to those in this study. Miura et al. 21) measured the cross-sectional microhardness of the CP Ti cast plates at the depths of mm from the as-cast surface. They found that the mean microhardness at the depth of mm was 545 Hv, and decreased to 274 Hv at the depth of 0.1 mm 21). However, for depths of mm, the microhardness was almost constant 21). In the present study, the mean microhardness of the cast specimens at 5.0 mm from the center was 225 Hv for an argon flow rate of 5 L/min and 269 Hv for 10 L/min. Comparing these results with those of Miura et al., it seemed that about 0.1 mm of the as-cast surface region had been removed from the specimens. Miura et al. 21) also carried out a qualitative analysis using EPMA for Ti polished using two different methods to produce a mirror surface and a rougher inner surface (such as for the inside of clasps). It was found that although Ti, O, N, C, Si and Al were detected from both surfaces, P was also detected from the inner surface 21). In the present study, P was not detected from the surface although mirror polishing was not performed on the Ti cast specimens. suggested there was no contamination due to the investment materials. For Ti, it is believed that the state of the cast plates influences laser welding. The cast specimens used in the present study were similar to the cast plates currently used in clinical procedures. study reports the results of a novel approach to quantify porosity in welded areas by micro-ct. The micro-ct system used in this study provided highresolution images (0.014 mm). A limitation of the method was that bubbles less than mm in diameter were

8 is (a) (b) Fig. 10 EPMA map analysis of the welded area of the Ti cast specimen. (a) 5 L/min: COMPO, O, Ti, (b) 10 L/min: COMPO, O, Ti. 323

9 324 difficult to visualize. Micro-CT made it possible to visually record air bubbles in 3D images of specimens (Fig. 3). It was confirmed that porosity existed in the center of the welded area in Co-Cr alloy. part was the area where the two cast plates were butted and penetration-welding. In contrast, the porosity was distributed throughout the entire welded area in Ti. The penetration depth by the laser differed among the specimens because the rate of laser beam absorption, the thermal conductivity, and the melting point are different for each metal 20). Togaya 22) and Watanabe et al. 23) reported that this difference in laser penetration occurs because the rates of laser beam absorption and thermal conductivity are different in these metals. Watanabe and Topham 16) suggested that oxidation of Ti took place over the entire melted area, whereas the oxidation of Co-Cr alloy was limited to the surface, which increased the penetration of the laser into the alloy. The influence of the laser irradiation on Ti might be thought to be greater than that on Co-Cr alloy. Therefore, wesurmise that the influence of the laser irradiation is concentrated in the vicinity where the penetration-welding was performed in Co-Cr alloy, while it influenced the entire filler metal in Ti. The ratio of porosity tended to decrease as the flow rate of argon gas increased in Ti. Berg et al. 24) suggested that weld porosity may be the most significant factor affecting the strength of welded Ti, although Taylor et al. 14) reported that the presence of porosity on the fractured surfaces was infrequent and did not correlate with the tensile properties measured. Nomoto et al. 25) reported that joint strength was not related to porosity in the welded area. In this study, low porosity did not necessarily result in high tensile strength; joint strength had no relationship with porosity in the welded area. finding suggested that the porosity caused by the laser-welding procedures does not affect joint strength. NaBadalung and Nicholls 7) reported that fracture loads for laser-welded joints were lower than those in as-cast specimens; the failure occurred immediately adjacent to the weld beads, and this suggested that there were microstructural changes. In this study, there was a significant difference in the tensile strength between the control and 0 L/min specimens for Co-Cr alloy. All of the welded specimens fractured in the parent metal for Co-Cr alloy. It has been reported that the hardness of a welded area is higher than that of the parent metal 4,26,27). Roggensack et al. 26) suggested that the increased hardness of the welded area might be due to interstitial impurities (oxygen or other elements) as well as changes in grain size and structure, which may be the reason why the specimens did not fracture at the interface but in the parent metal. The tensile strength values of the 0 L/min Co-Cr alloy specimens were minimal. However there were no significant differences among the other welded specimens of Co-Cr alloy. Watanabe and Topham 16) found that argon shielding was detrimental to the effective welding of Co-Cr alloy. NaBadalung and Nicholls 7) suggested that a shielding gas is necessary in the laser welding process to protect against atmospheric contamination, and that porosity and fusion defects can be minimized by controlling the oxidizing potential of the shielding gas. In the present study, it seemed that argon shielding was effective in welding Co-Cr alloy. Yamagishi et al. 4) reported that the increase in hardness was less for test pieces welded in an argon atmosphere than for those irradiated in ambient air. Liu and Welsch 8) reported that oxygen incorporation altered the mechanical properties of Ti; the tensile strength increased and elongation decreased. Barrett et al. 28) reported that an increase in the tensile strength associated with oxygen incorporation may have been overridden by a decrease in tensile strength associated with coarsening of the microstructure. Tanaka et al. 17) reported that the structure of the welded metal was independent of the argon gas flow rate. Moreover, they found that the 5 L/min Ti specimens had the highest quantities of oxygen and nitrogen, and that the oxygen and nitrogen concentrations in the melted metal decreased as the argon gas flow rate increased 17). In addition, the microhardness and tensile strength of the welded metal were found to increase with oxygen and nitrogen concentrations, whereas the elongation decreased 17). There might be an optimum flow rate for laser-welding. In the present study, the tensile strength of the 5 L/min Ti cast specimens was stronger than that of the 10 L/min Ti cast specimens although the microhardness profile traversing the welded joints of the 10 L/min Ti cast specimens was similar to that of the 5 L/ min Ti cast specimens. The microhardness was harder around the welded region than in the parent metal. Oxidation of alloy surfaces is known to increase the rate of laser energy absorption 29). These findings might explain why the 10 L/min Ti cast specimens fractured at the interface although the microhardness values of 5 L/ min and 10 L/min Ti cast specimens were similar in the present study; the measured microhardness was the surface hardness. In the present study, the elongation of the 5 L/min Ti cast specimens was large (Fig. 7) since 3 out of 5 specimens demonstrated a ductile fracture in the parent metal. On the other hand, the elongation of the 10 L/min Ti cast specimens was small since all of the specimens demonstrated interface fractures. However, the distribution of oxygen in 5 L/min and 10 L/min Ti cast specimens was similar regardless of the flow rate of argon gas by the map analysis (Fig. 10). Detection of the difference between the 5 L/min and 10 L/min Ti cast specimens oxygen distributions using EPMA might be difficult since only several µm depth from the surface can be analyzed using EPMA. Watanabe and Topham 16) reported that argonshielded laser-welded CP Ti and Ti-6Al-7Nb specimens had higher failure loads compared with non-shielded specimens because ambient oxygen was incorporated into these alloys during the melting/solidification process of laser-welding. Wang and Welsch 3) wrote that the question remains as to what level of oxygen contamination would be clinically acceptable when joining Ti prostheses. Such contamination has been understood to decrease the joint strength although a rate of argon gas flow in laser

10 325 welding of 10 L/min prevents such oxidation. As shown in Fig. 6, for the CP Ti rolled plates, the 5 L/min and 10 L/min rolled plates exhibited almost the same tensile strength. For the Ti cast specimens, the 10 L/min cast specimen exhibited a slightly lower tensile strength than the 5 L/min cast specimen, although there was no significant difference between them. During laser welding of Ti, when regions of the surface are not fully shielded from air by the argon gas flow, those regions react with oxygen or nitrogen 17). Kikuchi et al. 18) studied the effects of nozzle positions and gas flow rates on the oxygen concentration on a Ti surface during laserwelding. The results indicated that the region with an oxygen concentration of 0 vol% is narrow, so optimization of the nozzle position and the argon gas flow rate is important 18). A further study by Kikuchi et al. 19) found that for an argon gas flow rate of m 3 /min, the area with an oxygen concentration of 0 vol% is larger than that for m 3 /min. In each of these studies, Kikuchi et al. 18,19) performed one-time laser irradiation of a Ti plate. Since the region with an oxygen concentration of 0 vol% was narrow 18), it was assumed that the influence of the welded area was immense. In the present study, the size of the cast specimens was large compared to the CP Ti rolled plates. Three-spot welding was conducted initially for the cast specimens, compared with one-spot welding for the CP Ti rolled plates. We consider that for the CP Ti rolled plates in the present study the effect of the shielding from air was similar to that in the study of Kikuchi et al. 19). In the cast specimens, it was thought that the difference in the shielding from air with different argon gas flow rates occurred because the welded area was large. Thus, it can be assumed that the influence of oxidation will be more significant as the melted depth and the size of the melted region increase. When a welded area is large, such as when repairing a framework, the inside of the welded area may show some variation. There was a tendency for the microhardness at the ends of welded cast specimens to be larger than that in the center (Fig. 5). It was also found that the microhardness at the specimen ends exhibited a large amount of variation. Kikuchi et al. 19) reported that the oxygen distribution varied with both the nozzle position and the argon gas flow rate. Fracture of the specimens might begin from such regions of non-uniform microhardness. Since it is likely that the shielding provided by the argon gas is also non-uniform, care must be taken in choosing the position of the nozzle and the welding technique used, so that the welded area is as large as possible. CONCLUSION 3D images of the welded areas of the specimens showed that the porosity was close to the center of the welded area in Co-Cr alloy, but was distributed throughout the entire welded area in Ti. Laser welding of Co-Cr alloy was influenced very little by argon shielding. In contrast, for Ti, the joint strength of the welded specimens was affected by the rate of argon flow. It was suggested that there is a possibility of decreased welding strength, although an excessive flow of argon gas prevented oxidation. REFERENCES 1) Lautenschlager EP, Monaghan P. Titanium and titanium alloys as dental materials. Int Dent J 1993; 43: ) Könönen M, Rintanen J, Waltimo A, Kempainen P. Titanium framework removable partial denture used for patient allergic to other metals: a clinical report and literature review. J Prosthet Dent 1995; 73: ) Wang RR, Welsch GE. Joining titanium materials with tungsten inert gas welding, laser welding and infrared brazing. 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