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Materials Science & Engineering A 586 (2013) 86 92

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Microstructural and mechanical characterization of radial friction welded supermartensitic stainless steel joints
C.A. Della Rovere n, C.R. Ribeiro, R. Silva, L.F.S. Baroni, N.G. Alcntara, S.E. Kuri
Department of Materials Engineering, Federal University of So Carlos, Rodovia Washington Luis, Km 235, 13565-905 So Carlos, SP, Brazil

art ic l e i nf o
Article history: Received 21 May 2013 Received in revised form 27 July 2013 Accepted 5 August 2013 Available online 17 August 2013 Keywords: Supermartensitic stainless steel Radial friction welding Microstructural characterization Hardness measurement Mechanical properties

a b s t r a c t
This paper reports on an investigation of the microstructural aspects and mechanical properties of radial friction (RF) welded supermartensitic stainless steel (SMSS) joints in the as-welded condition. RF SMSS welds were produced with a matching consumable ring (CR). A detailed microstructural analysis of the weld region was carried out by optical microscopy (OM) and X-ray diffraction (XRD) allied to microhardness measurements. Conventional tensile and micro-tensile tests were also conducted to evaluate the global and local mechanical properties of the welded joints. The results of these analyses allowed that the local microstructureproperty relationship was established. The formation of a ne structure consisting of a mixture of virgin martensite and some stable austenite retained in the CR region was observed. On the other hand, the presence of virgin martensite plus -ferrite was found in the microstructures of the heat affected zone (HAZ) and themo-mechanically affected zone (TMAZ). The microhardness proles measured along the as-welded HAZ, TMAZ and CR regions of the RF welded SMSS joints indicated that they fell within the maximum hardness limit of 350 HV for application requirements. The results of the tensile and micro-tensile tests revealed higher weld region strength than that of the base material (overmatching), without presenting a signicant loss in weld zone ductility, which is directly linked with the ne transformed microstructure observed in the weld region. & 2013 Elsevier B.V. All rights reserved.

1. Introduction In recent years, supermartensitic stainless steels (SMSSs) have attracted substantial attention from the oil and gas industry due to their superior combinations of properties compared to those of conventional martensitic stainless steels, such as high strength and good low-temperature toughness, improved weldability and acceptable corrosion resistance in environments containing chlorides plus CO2 and some H2S [15]. In addition, this relatively new class of martensitic stainless steels requires only simple heat treatments and can provide certain economic advantages such as allowing for lower gauge, weight and costs. Because of these advantages, SMSSs have increasingly replaced more expensive duplex stainless steels in many onshore and offshore applications. They have been employed to produce oil country tubular goods (OCTG), which include especially seamless pipes for drilling, casing, and tubing for application in oil and gas wells with moderate corrosive conditions [2,68]. The main metallurgical changes in relation to conventional martensitic stainless steels are that SMSSs contain up to 3% more

Corresponding author. Tel.: 55 16 33518507; fax: 55 16 33518258. E-mail addresses:, (C.A. Della Rovere). 0921-5093/$ - see front matter & 2013 Elsevier B.V. All rights reserved.

molybdenum (Mo) and up to 6% more nickel (Ni). Mo is added to improve the steel's corrosion resistance, while Ni is added to stabilize austenite () at high temperatures, preventing the formation of -ferrite. Levels of carbon (C) content have been reduced to as little as 0.01 wt% to improve weldability. In addition, some microalloying with titanium (Ti) and/or niobium (Nb) has been employed to stabilize residual C and nitrogen (N) and prevent the precipitation of Cr-rich carbonitrides, which impairs the steel's corrosion resistance, and to produce a ner microstructure with superior mechanical properties [912]. Today, the major challenges of SMSSs have to do with their weldability and the resulting mechanical and corrosion performance of the welded material, as well as the development of fast, reliable, economic welding processes that minimize or even dispense with expensive and time-consuming post-weld heat treatments (PWHTs). In this context, some new and advanced processes have been investigated as alternatives to conventional welding process for SMSSs, such as laser and electron beam welding, and a novel process known as radial friction (RF) welding [1316]. This is a variant of the friction welding process which has been developed by TWI as a oneshot joining technique for pipelines, offering signicant advantages over conventional welding process, e.g. an extremely fast welding time of less than 30 s, no skilled operator requirement, high weld quality, high reproducibility and the possibility of joining dissimilar materials. In addition, many of the metallurgical problems associated

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with fusion welding processes can be avoided, since the RF welding is a solid state joining process [1721]. The RF welding process is done by butting together two beveled pipes that are held in clamps to prevent any additional rotation or axial movement. A consumable ring of the same material as that of the pipes, machined to include a sharper beveled internal prole, is located between the two pipe ends, as illustrated in Fig. 1(a). This consumable ring is then rotated and compressed radially to produce frictional heat between the rubbing ring and the stationary pipe surfaces, which in turn will generate the thermomechanical conditions necessary for weld formation (Fig. 1(b)). To keep the pipe ends radially aligned and to react against the external radial welding pressure, a heat resistant mandrel is simultaneously expanded inside the pipe bore at the weld site. This mandrel prevents collapse and ash ingress into the bore so that a smooth internal prole of the weld is formed. After a given period of time and a controlled level of metal displacement (called burnoff), rotation is stopped and the radial pressure is maintained or increased to consolidate the weld [1720]. Despite the above cited advantages and its excellent potential for joining pipes offshore, this solid-state welding process has not yet been widely applied. In addition, the current literature contains very few detailed studies about the structures and properties of RF welded joints, so further studies are of vital importance to further develop and to expand the industrial application of this relatively new welding process. Therefore, the purpose of this study was to investigate the microstructural aspects and mechanical properties of RF welded SMSS joints, particularly those of the consumable ring and the weld interface regions. General and local mechanical properties of these regions were evaluated using conventional tensile and micro-tensile tests, and hardness measurements. The resulting microstructures were characterized based on optical microscopy and X-ray diffraction analyses.

14.3 mm thick seamless pipes with 168.3 mm of outer diameter. RF welding was carried out using a matching composition SMSS consumable ring with an outer width of about 27 mm machined from a seamless pipe with 197.6 mm outer diameter and 30 mm wall thickness. The chemical compositions of the base material (BM) and consumable ring (CR) are given in Table 1 and the welding parameters in Table 2. It is worth noting that three sets of RF welds were prepared to obtain the RF welding parameters presented in Table 2. The initial choice of parameters was based on the experience of applying RF welding to other materials. These sets of RF welds were evaluated by nondestructive testing (visual inspection, ultrasonic and liquid penetrant tests), destructive testing (root and face bend tests) and macrographic evaluation. After selecting the best parameters, the nal RF SMSS welded joints studied here were produced. Moreover, the RF SMSS welded joints were not subjected to PWHT and all the analyses were done in the as-welded condition. Cross-sectional specimens of the RF welded joints were cut and embedded in bakelite to analyze their microstructures and microhardness values. For microstructural analysis, the specimens were polished mechanically to a mirror nish (alumina 1.0 mm) and etched according to the ASTM E407 standard, using either a Villela reagent [composed of 95 ml of ethanol, 5 ml of hydrochloric acid (HCl) and 1 g of picric acid (C6H3N3O7)] or an electrolytic etchant containing 10% (w/v) oxalic acid (H2C2O4.2H2O) solution at 6 V for 15 s. As depicted in Fig. 2(a), the Vickers microhardness proles
Table 2 RF welding parameters used. Parameters Rotation speed (rpm) Friction pressure (MPa) Friction time (s) Burn-off length (mm) Brake time (s) Forging pressure (MPa) Forging time (s) Conditions 200 4 24 7.5 1 4 4

2. Experimental procedure The RF welded joints were produced using SMSS (UNS S41426) pipe segments in quenched and tempered condition. These were

Fig. 1. Schematic views of the RF welding process.

Table 1 Chemical composition (wt%) of the materials. Material Element (wt%) C Base material Consumable ring 0.01 0.01 Si 0.17 0.14 Mn 0.47 0.42 P 0.012 0.010 S 0.001 0.001 Cr 12.01 11.94 Ni 6.40 6.36 Mo 2.42 2.42 Ti 0.10 0.07 Cu 0.02 0.02


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across the RF welded joints were recorded along three horizontal lines parallel to the surface: (1) at the top (outer diameter 2 mm), (2) at mid-thickness of the wall, and (3) at the bottom (inner diameter 2 mm). The Vickers microhardness measurements were taken according to the ASTM E384 standard, applying a load of 500 g for 10 s at a distance of 0.5 mm between indentations. To ascertain the presence of any retained austenite in the distinct regions of the RF welded joints, the BM, CR, and weld interface were analyzed separately by X-ray diffraction (XRD) (Fig. 2(a)). Rietveld renement was used to analyze the XRD patterns and determine the phases and their relative amounts, using Maud software [22]. Standard tensile specimens were machined from the BM (in the longitudinal direction) and from the welded joint (Fig. 2(b)) and tested to ascertain the inuence of RF welding on the global mechanical behavior of the SMSS joint. To determine changes in the local mechanical property along the weldment, micro-tensile specimens from the distinct regions of RF welded joints were also extracted in the middle region of the pipe wall by wire cut EDM, as

illustrated in Fig. 3. The tensile and micro-tensile tests were carried out at room temperature in air, using crosshead speeds of 1 mm/min and 0.2 mm/min, respectively. Two sets of measurements of each specimen were taken and an average value was considered.

3. Results and discussion 3.1. Microstructural aspects Fig. 4(a) shows a typical cross section macrograph of an RF welded SMSS joint. Note the formation of a sound welded joint without pores, inclusions or cracks along the weld interface, characterized by ash collars appearing at its outside diameter adjacent to the CR. These ash collars are formed naturally by the extrusion of the original (contaminated) surface material from the weld line, which has a benecial effect on the quality of the welded joint. Because any impurities or oxide lm at the frictional interface are broken and extruded, resulting in a clean surface between the BM and CR, the formation of ash collars has a selfcleaning effect on RF welded joints. It should be mentioned that in the case of actual service joints, the weld prole must be machined to blend evenly with the outer diameter and, if necessary, with the inner diameter of connected pipes. The heat and deformation generated during the RF welding process produce distinct microstructural zones across the welded joint (Fig. 4(b)). The outermost portions of the weld (those not directly involved in the friction process) are modied mainly by the thermal eld of the welding process, although this region has also undergone some degree of deformation. This region is called the heat affected zone (HAZ) and is similar to the HAZs observed in welds prepared by more conventional fusion welding processes. The thermo-mechanically affected zone (TMAZ) is located at the weld interface and its surroundings, where the material underwent high plastic deformation due to the compressive pressure applied to consolidate the metallic bond, in addition to the heatinduced microstructural changes. Fig. 5 presents a typical optical microscopy (OM) image of the BM region. The unaffected BM is composed mainly of tempered

Fig. 2. Schematic diagrams: (a) sites from which the samples for optical microscopy and XDR analyses were extracted (dashed black circles) and where the Vickers micro-hardness proles were taken (dashed red lines) and (b) extraction mode of conventional tensile specimens. (For interpretation of the references to color in this gure legend, the reader is referred to the web version of this article.)

Fig. 3. Schematic view of the extraction mode and dimensions of micro-tensile specimens.

Fig. 4. (a) Cross-sectional overview of an RF welded SMSS joint and (b) RF welding zone features.

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Fig. 5. Typical microstructure in the region of the base material.

Fig. 6. X-ray diffraction pattern of the distinct regions of the RF welded SMSS joint.

martensite with no evidence of -ferrite and some apparent titanium carbonitride particles. Rietveld renement of the XRD patterns (Fig. 6) also indicates that the BM contains a substantial amount of retained austenite (12.2 vol%). According to the literature [6,2327], this austenite is nely dispersed throughout the matrix (in the form of small grains located at martensite lath boundaries) and is detectable only by electron microscopy. It has been demonstrated that is possible to attain up to 2030% vol% of stable retained austenite in SMSSs with 46 wt% Ni when tempering treatment is carried out just above the austenite formation start temperature (Ac1). The thermal stability of this phase has been related with a Ni enrichment mechanism [6,23,25,26]. In addition, it was previously reported that the presence of stable retained austenite particles strongly enhances the impact toughness of these steels by means of a localized transformationinduced plasticity (TRIP) effect [2426]. Fig. 7 depicts OM images of the RF weld region, showing both the HAZ and TMAZ. The literature has demonstrated that the structural changes occurring in the solid state within the BM in response to a single weld pass in SMSS can be interpreted based on the ternary Fe NiCr phase diagram and subdivided into different regions (each one characterized by its own microstructure), which are distinguishable as a function of the peak temperature attained with the relative position

within the HAZ during the welding process [2830]. Considering this approach, it seems that the portions of the HAZ located beside the TMAZ were heated to sufciently high temperatures to reach the biphasic eld, becoming partially ferritized. Upon subsequent cooling, the reverse transformation (-) took place; however, as depicted in Fig. 7(a) and (b), this reversion was incomplete and some -ferrite was trapped along the previous austenite grain boundaries, indicating that high cooling rates are associated with the RF welding process. According to the literature [31,32], the retention of -ferrite in the microstructure of the HAZ of SMSSs is associated with the high level of enrichment of Cr and Mo into -ferrite during heating and to their incomplete back diffusion into austenite during the reverse transformation (-) when subjected to extremely rapid cooling. Thus, this region is composed predominantly of virgin martensite and some ferrite stringers that remained around prior austenite grains. In addition, it can also be noted that the microstructures of the portions of HAZ closer to TMAZ also show signicant grain renement, which is probably the result of the thermal cycle plus some deformation that took place in these regions. The peak temperatures of the HAZ decrease at greater distances from the weld interface, just reaching temperatures at which the steel's miscrostructure transforms completely or partially into austenite in response to the welding heat. Depending on the extent of solute enrichment, this austenite may transform back into virgin martensite or remain stable upon cooling. In addition, some additional tempering can also occur in the HAZ portion that consisted of mixed austenite and tempered martensite at the peak temperature. On the other hand, the severe plastic deformation and high temperatures to which the TMAZ was subjected during the friction and forging stages resulted in dynamic recrystallization of the deformed metallic matrix and subsequent grain growth, which in turn led to coarse grains slightly elongated towards the extrusion weld line. The coarsening of recrystallized microstructure observed in the TMAZ is a consequence of the longer time spent at the high temperatures generated in this zone compared to the adjacent ne recrystallized microstructure of the HAZ, and also to the higher available strain energy in the former (TMAZ). During the welding process, the TMAZ attained peak temperatures inside the -ferrite single phase eld and became fully ferritized. Upon cooling, the -ferrite decomposed into different austenite morphologies (allotriomorphic, intragranular and Widmansttten austenite), However, as indicated in Fig. 7(c), this decomposition was incomplete and a small amount of -ferrite was also retained when the material reached room temperature. Fig. 7(d) presents a more detailed OM of the TMAZ, showing residual -ferrite stringers that remained trapped within the previous Widmansttten austenite (W) structure. According to the literature [31,33,34], W is composed of parallel plates that nucleate at -ferrite grain boundaries or of pre-existing allotriomorphic austenite growing along well-dened planes of the matrix. Earlier studies [33,34] have found similar phase morphology in austenitic stainless steels solidifying as -ferrite at low cooling rates. In addition, as depicted in Fig. 6, below the martensite formation start temperature (Ms), all the austenite transformed to martensite [29,31,35]. The nal microstructure of the TMAZ consisted of virgin martensite with a very small fraction of -ferrite. As mentioned earlier, the formation of stable austenite in SMSS (which is retained when the alloy is cooled at ambient temperature) takes place during tempering at around AC1 by means of a Ni enrichment mechanism; therefore, very little, if any, austenite is retained in SMSS microstructures after heating to temperatures inside the -ferrite single phase eld, which explains the absence of austenite at the weld interface [6,23,25,26,29,31]. Fig. 8 shows an OM image of the central portion of the CR region. This portion of the CR was fully transformed into austenite


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Fig. 7. Microstructure of the (a) RF weld region; (b) HAZ; (c, d) TMAZ.

Fig. 8. Typical microstructure in the region of the consumable ring.

during the welding process, with the concomitant dissolution of some of the carbides initially present in the CR parent material, leading to a weaker etching response than that of the BM (Figs. 4 and 5). As indicated in Fig. 6, the ne-grained microstructure of this CR portion consisted mainly of virgin martensite and stable retained austenite (12.1 vol%), which probably remained from the microstructure of the original parent steel [29,30,36]. 3.2. Hardness The microhardness proles obtained from the top, middle and bottom of the RF welded joint covering all the four regions (BM, CR, HAZ and TMAZ) are illustrated in Fig. 9. Note that the BM region ( 25 to 18 mm) exhibits the lowest hardness, with values ranging from 282 to 313 HV0.5. On the other hand, the hardness values for HAZ/TMAZ ( 18 to 8 mm) and CR regions

exceed the level of the BM by about 20 and 40 HV0.5, respectively. This indicates a higher level of strength in these regions compared to that of the BM. The changes in the hardness proles can be ascribed to modications in the microstructures observed in the distinct zones across the RF welded joint. It is well known that the hardness of martensite is controlled primarily by its carbon content (or carbon plus nitrogen content), and secondarily by prior austenite grain size. Therefore, the hardness of martensite increases with increasing carbon plus nitrogen content and decreasing grain size of prior austenite. In addition, any retention of -ferrite in the microstructure will tend to lower its hardness [2729,35]. Thus, the higher hardness values of the CR region seem to be directly associated with the formation of a ne-grained structure consisting of a mixture of virgin martensite and some stable austenite, and to the absence of -ferrite. A further possible explanation is carbon and nitrogen enrichment of some of the martensite, as a result of carbon and nitrogen partitioning between stable and unstable austenite during heating. This hypothesis is supported by the work of Woollin and Carrouge [36], who reported that higher hardness values are measured in simulated HAZ microstructures of SMSSs when some retained austenite is present rather than in fully martensitic structures. On the other hand, the somewhat lower hardness values in the HAZ/ TMAZ region compared to that of the CR are most likely due to a grain size effect and/or the presence of -ferrite. Fig. 9(a) also reveals that the hardness values of the proles taken at the top, at the mid-thickness and at the bottom were very similar, indicating that the hardness throughout the thickness of the RF welded joint is quite uniform. These hardness results can be attributed to the fact that the RF welding process is a one-shot joining technique that differs considerably from those described by Grifths et al. [37], who observed the presence of high hardness zones in the capping layers or at the root of the weld region of girth-welded SMSS pipe sections produced by multi-pass gas tungsten arc (GTA) welding with a matching ller or a super-duplex stainless steel ller without PWHT, respectively. This variation in the hardness of GTA SMSS welds is due to the

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Fig. 9. Microhardness proles across the RF welded SMSS joint.

Table 3 Tensile test results (average values). Material BM RF welded joint BM CR HAZ/TMAZ

Condition As received As-welded As-welded As-welded As-welded

Test Longitudinal tensile Cross-weld tensile Micro-tensilea Micro-tensilea Micro-tensilea

Rp0.2 (MPa) 647.67 710.26 686.90 803.10 762.36

Rm (MPa) 850.72 845.96 812.54 929.35 877.18

Micro-tensile specimens were extracted as illustrated in Fig. 3.

post-weld tempering effect associated with subsequent weld passes. Therefore, to attain more uniform hardness values, the authors [37] subjected these welds to PWHTs at 650 1C for 5 min, followed by air cooling. In addition, the literature reports that in SMSS welds produced by conventional welding processes such as SMAW, GMAW, SAW, and GTAW with matching consumables, and even those produced by high energy density welding processes such as autogenous laser welding, it is difcult to limit the hardness of as-welded SMSS weldments to around 350 HV (which is considered to be the cold crack threshold). In some cases, even after a medium PWHT (30 min at 630 or 650 1C), this application requirement is not easily met [38,39]. On the other hand, the aswelded hardness proles of the RF welded SMSS joints indicate that this maximum hardness limit was satised, and that it was not necessary to reduce the hardness by means of PWHT. 3.3. Tensile properties The overall tensile properties [yielding point (Rp0.2) and ultimate tensile strength (Rm)] of the RF welded joints were assessed by testing conventional at cross-weld tensile specimens at room temperature. The results are summarized in Table 3, which also includes the BM tensile properties (in the longitudinal direction) and the results of the micro-tensile specimens. Note that the strength values of the unaffected BM determined by micro-tensile specimens (Rp0.2 686.90 and Rm 812.54) and by conventional tensile specimens (Rp0.2 647.67 and Rm 850.72) vary slightly, and are therefore consistent with each other. In addition, the micro-tensile results of the CR and HAZ/TMAZ regions in the aswelded condition clearly show an overmatching weld zone strength condition, with a strength mismatch factor (M) of 1.17 and 1.11 (M Rp0.2welded joint region /Rp0.2BM), respectively. According to the literature [40,41], a strength mismatch factor of this order protects the weld zone from deformations and should also diminish the risk of the welded joint undergoing brittle fracture. In addition, Table 3 shows that the Rp0.2 and Rm of the cross-weld tensile specimens are similar to the values of the BM in the as-received condition, and due

Fig. 10. Typical stressstrain curves of the micro-tensile specimens.

to the strength overmatch of the weld zone, all the cross-weld tensile specimens failed away from the weld zone, with necking and strain concentration occurring in the lower strength BM region. This is also in good agreement with the results of the cross-section microhardness proles (Fig. 9), which exhibit the lowest microhardness values in this region. Micro-tensile specimens were tested to determine the local mechanical characteristics through the welded joint. The typical stressstrain curves measured in the three different regions of the welded joint (BM, CR, HAZ/TMAZ) are illustrated in Fig. 10. The proles of Rp0.2, Rm and elongation at rupture (r) of the welded joint are plotted in Fig. 11. Note that the local tensile behavior is consistent with the microhardness results, indicating that the lowest Rp0.2 and Rm values are measured in the BM and that there is an increase in strength levels towards the weld center. This is probably linked directly to the following microstructural aspects found in the RF welded SMSS joint: (1) the presence of virgin martensite plus -ferrite in the HAZ and TMAZ microstructures, and (2) the formation of a ne-grained virgin martensite with some stable retained austenite in the CR region that was affected by the weld thermal cycle. Across the RF welded joint, the Rp0.2 increased from 686 MPa in the BM to around 823 MPa in the CR. The Rm increased from 812 MPa to around 950 MPa. On the other hand, the micro-tensile results also indicate that the increase in strength did not lead to a signicant decrease in weld zone ductility. As can be seen in Fig. 11, the r values are lower in the welded CR (about 10%) than in the unaffected BM (around 15%).


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Fig. 11. Tensile property proles (Rp0.2, Rm and r) obtained from micro-tensile specimens of the RF welded SMSS joint. Each point on the curves represents the average results of one micro-tensile specimen.

4. Conclusions The microstructures and mechanical properties of an RF welded SMSS joint were characterized based on OM and XRD analyses, microhardness measurements, and tensile and microtensile tests, leading to the following conclusions: 1. The RF welding process can be applied to SMSS joints and high quality SMSS (defect-free) welds can be reproducibly made with properties closely matching those of the BM, without requiring PWHT or tempering. 2. The microstructural characterization of the weld region showed the formation of a ne structure consisting of a mixture of virgin martensite and some stable retained austenite in the CR region, while the microstructures of the HAZ and TMAZ showed the presence of virgin martensite plus -ferrite. 3. The microhardness proles of the as-welded HAZ, TMAZ and CR regions of the RF welded SMSS joint fell within the hardness limit of 350 HV, which is considered to be the cold crack threshold. 4. The RF welds produced with matching CR exhibited excellent mechanical properties, not only achieving the minimum requirements of strength (Rp0.2 600 MPa and Rm 800 MPa) for a highly alloyed SMSS in the as-welded condition but also exhibiting higher strength levels in the HAZ, TMAZ and CR regions (overmatching) than that of the BM, without presenting signicant losses in weld zone ductility.

Acknowledgments The authors gratefully acknowledge FAPESP (So Paulo Research Foundation Grant no. 12/16113-6), PPGCEM/UFSCar (Postgraduate Program in Materials Science and Engineering of the Federal University of So Carlos) and the Brazilian Research Funding Agency CNPq (National Council for Scientic and Technological Development) for their nancial support of this work. The authors are also indebted to Mr. Carlos Eduardo Della Rovere for his invaluable assistance with the illustrations.