Effect of Articial Aging Time on the Mechanical Properties of Weldment on API 5L X-52 Line Pipe Steel

B. VARGAS-ARISTA, A. ALBITER, C. ANGELES-CHAVEZ, and J.M. HALLEN The effect of articial aging time on the microstructure and mechanical properties in the weld and base metals of an API 5L-X52 line pipe steel was studied. Articial aging was performed for 1000 hours at 250 C and was monitored every 100 hours. Vickers hardness and tensile tests were used to examine the aging effect on the mechanical properties. Scanning electron microscopy and transmission electron microscopy (TEM) studies were carried out to analyze the microstructure evolution. The Vickers hardness results showed that the weld and base metals displayed a hardening tendency up to a maximum value at 500 hours of aging. The yield strength increased with aging time while the elongation-to-fracture decreased. The maximum yield strength was found at 500 hours, which was attributed to the peak-aged condition. After 500 hours, both the Vickers hardness and yield strength were reduced while the elongation was increased due to the overaging condition. The TEM observations and fracture analysis of specimens showed that the improvement of strength was associated with the nanoparticles precipitation, while the degradation of the microstructure and mechanical properties was related to the coarsening process of iron carbide (cementite) and niobium carbide for the weld and base metals, respectively. The largest amount of precipitation in both alloys occurred at 500 hours. I. INTRODUCTION deterioration of toughness. This heat treatment is equivalent to 2-year-old naturally aged steel.[11] A third case is the weld metal of multilayer steel aged at 550 C for a time up to 30,000 hours; the thermally affected zone exhibits minimum hardness values and microstructural changes such as the agglomeration and coarsening of precipitates.[12] Another example is found in the weld metal of 308 stainless steel produced by SAW aged at 500 C for 24 hours, which resulted in a raise of susceptibility to intergranular corrosion caused by chromium carbide precipitation.[13] Additionally, a study related with the articial aging in API-5L line pipe steel is carried out at 250 C, resulting in the increase of ferrite grain size as a function of aging time and a greater susceptibility to corrosion in aqueous chloridecontaining media;[14] however, this study does not show a relationship between aging and mechanical properties. There are also reports on carbon steels, indicating that articial aging induced by heat treatment can be performed in the temperature range from 100 C to 350 C,[69] to accelerate the natural aging within the service temperature range from 25 C to 70 C for long times. Additionally, Homma and Gil[11,14] nd that low-strength steel is susceptible to aging at 250 C. Since most of the line pipe used for hydrocarbon transport is manufactured with low-strength steel and has a service life over 20 years, we decided to study the effects of accelerating natural aging by means of heating at a constant temperature of 250 C to study the long-term changes of natural aging in the microstructure and mechanical properties of the weld and base metals of an API5L X-52 line pipe steel, in order to produce further understanding of its capabilities and performance as basic metallurgical features relating microstructure and properties alike. The objective of this work is to characterize the changes on the microstructure and mechanical properties of the weld and base metals of the aforementioned steel, produced by the accelerated articial aging process at 250 C for different times. The results will permit establishment of the metallurgical bases to understand the degradation of the
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API-5L line pipe steel is commonly used for oil and natural gas transport in the petroleum industry. This type of line pipe is manufactured using microalloyed steel with elements such as Nb, Ti, and V. The thermomechanically controlled rolling process (TMCP) is used to control grain renement and subsequent precipitation strengthening during rolling, cooling, and coiling.[15] Pipe longitudinal welding is achieved through double-pass submerged arc welding. As are most alloys, line pipe steel is subjected to natural aging phenomenon that is likely to be accelerated by the service conditions, capable of producing changes in the microstructure and mechanical properties (yield strength, tensile strength, hardness, ductility, and toughness), described by the peak-aged condition associated with the highest strength and overaging condition related to the decrease in the strength by long aging times and hence probability of failure after several years of service.[69] There is some research on aging of ferrous alloys such as API-5L line pipe steel that have aimed to produce a clearer understanding of the causes and effects of aging, such as the degradation of the microstructure and mechanical properties. Some works are related to 17GS line pipe steel that transported oil, which after 30 years of service displayed signicant changes in mechanical properties (yield strength, tensile strength, and Charpy absorbed energy).[10] A second case is the JIS-SM490YB-0.17 wt pct C low-strength steel for welded structures, which shows susceptibility to aging at 250 C for 1 hour resulting in
B. VARGAS-ARISTA, Doctoral Student, and J.M. HALLEN, Professor and Research Scientist, are with the Departamento de Ingeniera Metalurgica, IPN-ESIQIE, Laboratorios Pesados de Metalurgia, UPALM Zacatenco, 07738 Mexico D.F., Mexico. Contact e-mail: bvarista26@yahoo.com.mx A. ALBITER and C. ANGELES-CHAVEZ, Research Scientists, are with the Instituto Mexicano del Petroleo, Mexico D.F. 07730. Manuscript submitted May 12, 2005.
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microstructure and mechanical properties of commercial line pipe naturally aged having more than 20 years of service, without considering the pressure work and chemical composition of the uid transport, which has a great effect in the mechanical properties. II. EXPERIMENTAL PROCEDURE

A. Test Material Specimens of the weld and base metals were obtained from an API 5L X52 line pipe steel with a product specication level (PSL 1). The dimensions of the line pipe were 9.5-mm thickness and 914-mm nominal diameter. The line pipe was welded longitudinally by double-pass SAW through an X-groove conguration, under an API 1104 welding procedure specication (WPS).[15] The chemical composition reported by the supplier and the mechanical properties given for the weld and base metals in the asreceived condition, in accordance with API 5L,[16] are listed in Tables I and II, respectively. B. Mechanical Tests and Microstructure Specimens of weld and base metals were cut according to the schematic representation shown in Figure 1(a). After, the specimens were machined according to the mechanical test type, as illustrated in Figure 1(b). For evaluation of the Vickers hardness in three different microstructures, transversal specimens having 10-mm width and 50-mm length were used. For the weld metal, Vickers hardness and tensile property measurements were made in the rst and root passes of the welding thermal cycle. The cylindrical and longitudinal specimens for tensile testing had 6-mm gage diameter and 152-mm length. Subsequently, all specimens were articially aged in a Carbolite furnace at 250 C 6 5 C[11,14] for 1000 hours, with periodic monitoring every 100 hours to follow the behavior of the aging process as completely as possible. Vickers hardness testing was performed with an microhardness tester (FM-7, Future Tech Corp., Tokyo, Japan) applying a 2.9 N load repeating 20 times every reading, according to the NRF-001-PEMEX and ASTM E-92.[17,18] Uniaxial tensile testing was carried out on a 100 kN, AG10TG Shimadzu machine under stroke (displacement) control at an average strain rate of approximately 1.6 3 104 s1, and the tensile strain was measured by a SG 50-50 extensometer (Shimadzu Co., Japan) at room temperature, in accordance with ASTM E-8M.[19] For the microstructural characterization, the specimens were ground, polished, and subsequently etched using Nital 2 vol pct solution to reveal the microstructure. The microstructural features were observed by means of a JEOL*
*JEOL is a trademark of Japan Electron Optics Ltd., Tokyo.

6300 scanning electron microscope. The morphological, structural, and chemical characterizations were achieved by means of a JEOL-2000FX-II transmission electron microscope and Tecnai G2 F30 SuperTwin, which were equipped with energy dispersion spectroscopy, operated at 200 and 300 kV, respectively. The thin foils of 3-mm diameter were prepared by grinding and jet polishing until perforation, using a twin-jet electropolisher (Model 110, E.A. Fishione Instruments Inc., Export, PA) using a 30 vol pct HNO3 1 70 vol pct CH3OH (methanol) solution, maintained at 55 C during the operation. III. EXPERIMENTAL RESULTS AND DISCUSSION

A. Mechanical Properties The yield strength, Vickers hardness, and elongation to fracture in the weld and base metals were modied with the articial aging time at 250 C. Figure 2(a) shows the variation of mean yield strength (0.2 pct offset) in both alloys, increasing with aging time at the early stages of the aging process, thereby reaching a maximum at 500 hours due to the peak-aged condition. After this time, the behavior decreased due to the overaging condition. The effect of aging was also followed by Vickers hardness testing in both alloys. These results are shown in Figure 2(b) and illustrate the variation of mean Vickers hardness as a function of elapsing time. A gradual increase was noted with aging time that reached a maximum at 500 hours. Afterward, a decrease became clearly observed. The yield strength and Vickers hardness results were consistent with the elongation-to-fracture behavior (pct in 50 mm), since the elongation had a decrease as the aging time increased at the early stages of the aging process. The minimum was also obtained at 500 hours related to peak aging (Figure 2(c)). Afterward, the elongation showed an increase due to the overaging. However, the increase in the elongation for the weld metal was insignicant compared to that in the base metal, because the weld metal showed greater strength and hardening than those of the base metal. Similar results were reported for the 17GS line pipe steel, titanium, and aluminum alloys.[10,20,21] B. Microstructure Evolution There were three signicant changes in microstructure of the weld and base metals after articial aging for different times at 250 C. These were an increase in ferrite grain size,[14] strengthening from precipitation of ne nearly rounded nanoparticles at the early stages of the aging process,[15,13,20,21] and their coarsening process for long times.[1,12,20,21] The as-rolled microstructure of the base metal was mainly formed by a ferrite phase matrix and pearlite

Table I.

Chemical Composition of the Weld and Base Metals (Weight Percent) Element (Weight Percent)

Material Condition Base metal Weld metal

C 0.080 0.046

Mn 1.06 1.14

Si 0.26 0.27

Ti 0.003 0.020

V 0.054 0.030

Nb 0.041 0.050

P 0.019 0.021

S 0.003 0.010

Al 0.039

Ni 0.019

Ceq 0.274 0.242

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colonies with a relative proportion of each constituent of about 66 and 34 vol pct, respectively. The initial alloy had an ASTM grain size number G of about 9.36. With aging time, as grain size increased, the G number was modied accordingly. The changes ensuing were followed recording grain size number measurements, according to the ASTM E-112.[22] These results are displayed in Figure 3, where the variation of mean G number with aging time is presented. It exhibited a minimum reduction as the aging time increased during the early stages. Subsequently, a signicant decrease of G, about 7 vol pct compared to that in the as-received condition, was observed between 500 and 600 hours.[14] The value obtained at 600 hours strongly affected the grain size, which could be related to the disappearance of small grains into the large grains resulting in an increase in grain size. The relative phase distribution was also modied to 74 vol pct ferrite phase and 26 vol pct pearlite. The increase in grain size brought about a decrease of the overall length of grain boundaries, resulting in lower obstacles for the plastic deformation; therefore, after 500 hours, this process favored a decrease in Vickers hardness and yield strength. The solidication microstructure of the weld metal was mainly formed by large columnar ferrite grains and acicular ferrite phase. It was not possible to measure the grain sizes in the as-received and aged weld metal due to the microstructural complexity apparently associated with the presence of large columnar ferrite grains and acicular ferrite[13,2224] (microstructures in Figure 2(a)), which did not accomplish the grain structure required by the standard to measure the grain size. The Nb-C containing nanoparticles were located among dislocations within the ferrite grains of the base metal. A typical transmission electron microscopy (TEM) image of
Table II. Mechanical Properties of the Weld and Base Metals of the API 5L-X52 Line Pipe Steel Material Condition Base metal Weld metal Vickers Hardness HV (HRC) 188.3 (8.0) 217.1 (14.6) sYS 0.2 Pct (MPa) 419 518 UTS (MPa) 514 589 Elongation (Pct) 30 22

these particles on dislocation networks is shown in Figure 4(a). The energy-dispersive X-ray (EDX) spectrum displayed the characteristic C, Nb, and Ti peaks (Figure 4(b)), which corresponded to the nearly rounded particle inserted in Figure 4(a). The structural characterization by the selected-area diffraction (SAD) pattern (Figure 4(c)) obtained from this nanoparticle showed reection points with the following interplanar distances of 0.495, 0.295, and 0.250 nm, which corresponded to the (010), (101), and (111) planes with the [101] zone axis. Therefore, this result suggested that the nanoparticles precipitated in the base metal were made up of Nb2C compound, according to JCPDS standard 77 to 0998. The interplanar distances obtained from this nanoparticle did not match those of other Nb and C compounds.[13,5] The most intense reection points, marked as (200)m and (211)m planes in the diffraction pattern, having interplanar distances of 0.141 and 0.117 nm, respectively, corresponded to the iron matrix, according to JCPDS standard 06 to 0696. Similar results were obtained in the weld metal, thus demonstrating the presence of nanoparticles among dislocations within the columnar ferrite grains (Figure 5(a)). The main difference between the particles of both alloys was the chemical composition. Those found in the weld metal were mainly Fe-C containing. The EDX spectrum obtained from this nanoparticle type is illustrated in Figure 5(b), which clearly shows the characteristic Fe and C peaks. The structural characterization of Fe-C containing nanoparticles was not possible by the SAD pattern, because the particles had quite a ne size and disorientation. The results of the structural characterization carried out by high-resolution TEM (HRTEM) image analysis are displayed in Figure 5(c). The HRTEM image showed the atomic resolution of a nanoparticle embedded in the steel matrix. The interplanar distance measured on the image was 0.302 nm. Additionally, the fast Fourier transform pattern obtained from this nanoparticle, inserted in Figure 5(c), showed other fringes with 0.309-nm interplanar distance. These interplanar distances were corresponded to the (111) and (111) planes with the [110] zone axis. Therefore, the evidence was quite clear in revealing that the nanoparticles, which had precipitated in the weld metal were a Fe3C cementite-type compound, according to JCPDS standard 76 to 1877.

Fig. 1(a) Schematic representation of the specimens obtained from the API 5L-X52 line pipe and (b) Vickers hardness and tensile specimens used in this study.
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Fig. 3ASTM grain size number vs aging time for the base metal aged at 250 C.

Fig. 2(a) Yield strength vs aging time, (b) Vickers hardness vs aging time, and (c) elongation to fracture vs aging time for the weld and base metals aged at 250 C.
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Figure 6 from TEM image analysis gives a good representation of the density and mean size of the nanoparticles formed after the exposure period for the weld and base metals aged at 250 C. Figure 6(a) shows the apparent nanoparticle density for both alloys. There was a considerable increase with aging time. A maximum was reached at 500 hours due to peak aging. Therefore, at 500 hours of aging, the effect on the microstructure of both alloys was the increase in particle numbers, i.e., precipitation of a larger amount of ne nearly rounded nanoparticles. The weld metal exhibited a cementite particle size ranging from 10 to 20 nm, while the base metal showed niobium carbide sizes from 5 to 20 nm. The increase in the number of particles was related to the precipitation generated by the aging process resulting in the precipitation strengthening described by the Orowan process.[1,3] The nanoparticles nucleated heterogeneously on the dislocation networks, originating stronger interactions, more intersects, and obstacles for the dislocation motion, thus resulting in additional strength to the nal microstructure. Therefore, this precipitation strengthening produced a maximum increment in the yield strength and Vickers hardness at 500 hours. The weld metal showed a larger increase in particle density (47 vol pct) than that of the base metal (22 vol pct) at the peak-aged compared to the as-received condition, seemingly being more susceptible to aging, which promoted a larger amount of precipitation. The base metal exhibited a lower increase in particle density due to the reduced extent of precipitation. After 500 hours of aging, the effect on the microstructure of both alloys was to cause a decrease in particle density, which was related to the coarsening of medium nearly rounded nanoparticles formed under conditions of overaging. The weld metal showed particle sizes ranging from 10 to 30 nm, while the base metal showed particle sizes from 10 to 25 nm at 900 hours of aging. Then, particle density decreased because the nanoparticles underwent coarsening,
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Fig. 4TEM bright-eld (BF) image obtained from the base metal at peak-aged condition for 500 h: (a) nanoparticles showing dislocation interactions, (b) microanalysis by EDX at Nb-C rich nanoparticles, and (c) electron diffraction pattern for niobium carbide identied.

Fig. 5TEM BF image obtained from the weld metal at peak-aged condition for 500 h: (a) nanoparticles showing dislocations interactions, (b) microanalysis by EDX at Fe-C-rich nanoparticle, and (c) HRTEM image showing the atomic resolution of a nanoparticle identied as Fe3C cementite by FFT pattern.

as illustrated in Figure 6(b), which shows the variation of mean particle size with aging time for both alloys aged at 250 C. At rst, a considerable coarsening in the particle size was not observed, because during the early aging periods, only the precipitation process seemed to have prevailed. Subsequently, after 500 hours, the coarsening of the particles was notable due to overaging, as described by the Ostwald ripening process.[1] A selective growth of the larger nanoparticles at the expense of the other smaller ones was the dominant process. The latter diminished continuously until they disappeared completely. This fact could be related to the solute
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diffusion and reduction of interfacial energy between the matrix and particle. The new medium size particles had weak interactions between dislocation networks, which represented a lesser impediment during plastic deformation. Therefore, it generated a decrease in the yield strength and Vickers hardness, while the elongation to fracture exhibited a minimum increase.[12,25] The base metal achieved higher particle coarsening (75 vol pct) than that of the weld metal (33 vol pct) after overaging for 900 hours compared to that in the as-received condition, due to the ne particles precipitated by the TMCP process,[15] contributing to the coarsening of the larger particles.
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Fig. 6(a) Nanoparticle density vs aging time and (b) nanoparticle size vs aging time for the weld and base metals aged at 250 C.

Fig. 7(a) Microvoid density vs aging time and (b) microvoid diameter vs aging time from the tensile fractured specimens for the weld and base metals aged at 250 C.

C. Fracture Additional indirect measurements of the microstructural changes involving the increase in density and size of nanoparticles were achieved by the scanning electron microscopy study of fracture surfaces obtained from the tensile fractured specimens for the weld and base metals aged for different times. The fracture surfaces exhibited a ductile failure associated with the mechanism of nucleation, growth, and coalescence of microvoids in both alloys. The void nucleation centers were promoted by the presence of nanoparticles and nonmetallic inclusions.
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The effect of articial aging on the fracture surfaces of both alloys became apparent as an increment in microvoid density (Figure 7(a)) and a reduction in the microvoids diameter[21,26] (refer to Figure 7(b)). A maximum void density and a minimum void diameter were obtained at 500 hours and related to the larger precipitation of nanoparticles as a consequence of peak aging. Afterward, the fracture surfaces exhibited a reduction in the void density and an increment in the void diameter induced by the coarsening of the particles due to overaging. These results were in good agreement with the TEM results presented in Figures 6(a) and (b).
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The fracture surfaces of the aged base metal exhibited lower void density and larger diameters than those of the weld metal, which showed less precipitation of niobium carbides and greater growth of voids. The aged weld metal showed larger void density values compared to that of the base metal, which related to a greater number of void nucleation centers due to the precipitation of cementite particles producing less growth of voids. Thus, the weld metal reached a larger void density increment (69 vol pct) than that of the base metal (37 vol pct) at the peak-aged compared to the as-received condition. In the case of the void diameter reduction, the weld metal had a greater value (36 vol pct) than that of the base metal (26 vol pct) at peak aging. This weld metal behavior was related to a larger amount of precipitation of particles generated by the articial aging process. In summary, the weld metal showed more susceptibility to articial aging than the base metal because of a larger amount of precipitation, greater hardening, and consequently higher yield strength and microvoid density. All these were related to higher precipitation strengthening from cementite nanoparticles and their density increment (47 vol pct) than those of the base metal (22 vol pct) at peak aging. Additionally, the base metal ductility was greater than that of the weld metal. This indicated that the base metal achieved a higher elongation reduction (26 vol pct) than that of the weld metal (14 vol pct) from peaking at 500 hours and greater particle coarsening (75 vol pct) than that of the weld metal (33 vol pct) from overaging after 900 hours. The property behavior was strongly dependent upon the microstructural feature differences observed among the weld metal, which showed a solidication microstructure with columnar ferrite grains, acicular ferrite, and cementite nanoparticles precipitation (Figure 2(a)), while the base metal exhibited the as-rolled microstructure with ferrite matrix, pearlite, and niobium carbide precipitation. Thus, the differences observed between both alloys were the morphology type of the ferrite grains, density, size, and chemical composition of the nanoparticles. Therefore, the alloys exhibited different mechanical properties. The main effect of articial aging at 250 C was the nanoparticle precipitation imparting the improvement of strength for short aging times, and the coarsening of these particles producing the degradation of the microstructure and mechanical properties for long aging times. The precipitation results suggested that during the natural aging process in the service temperature range from 25 C to 70 C of the commercial line pipe, the ne carbides precipitated improvement in the strength while ductility decreased, and after long service times, they started a coarsening process of medium carbides and an increase in the ferrite grain size, producing the decrease in the strength. We believe that our results are important to the pipeline community, at least to mechanical properties, which are modied by changes in the microstructure produced by natural aging.

ical properties. The strength was improved while elongation was decreased until 500 hours related to peak aging. After this time, a degradation of strength and increase in elongation started because of overaging. During the early stages of the aging process, precipitation strengthening from nanoparticles was the dominant process until 500 hours, after which followed a coarsening process of these particles, which was unfavorable to the strength. The weld metal was more susceptible to accelerated aging than the base metal due to a larger increase in carbide precipitation and their lower coarsening. The evolution of articial aging strongly depended on the microstructural features, precipitation process, mechanical properties, and chemical composition of the alloy, as shown by the differences in carbide precipitation and subsequent coarsening between both alloys.

ACKNOWLEDGMENTS The authors are grateful for the experimental support received and for the nancial support from the Program of Research and Development for pipelines of the Instituto Mexicano del Petroleo, Program of Development & Technology PEP-IPN and CONACYT.

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IV. CONCLUSIONS The weld and base metals were susceptible to articial aging at 250 C, affecting their microstructure and mechanMETALLURGICAL AND MATERIALS TRANSACTIONS A

18. Standard Test Method for Vickers Hardness of Metallic Materials, ASTM Standard E-92, ASTM, West Conshohocken, PA, 1982 (reapproved 2003), pp. 309-14. 19. Standard Test Methods for Tension Testing of Metallic Materials, ASTM Standard E-8M, ASTM, West Conshohocken, PA, 2004, pp. 153-60. 20. M. Ikeda, S.Y. Komatsu, I. Sowa, and M. Niinomi: Metall. Mater. Trans. A, 2002, vol. 33A, pp. 487-93. 21. H.R. Shakeri and Z. Wang: Metall. Mater. Trans. A, 2002, vol. 33A, pp. 1699-713.

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