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    Doi - 10.1016 - J.msea.2007.02.113 - Leitor Avançado Da Elsevier

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    Almerindo Junior

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    Materials Science and Engincer we A 464 (2007) 157-169 -worcleeviercomocateinsea Mitigation of sensitisation effects in unstabilised 12%Cr ferritic stainless steel welds Martin van Warmelo, David Nolan *, John Norrish Faculty of Engineering, University of Wollongong, NSW 2522, Australia Received 16 November 06; receive in revised form 25 Janey 2007: accep 25 Febnsary 2007 Abstract Senstisation inthe heatuffected zones of feritic stainless steel welds i typically prevented by stabilisation ofthe parent material with Ganium ‘or niobium, and suitable design of the overall composition to produce suitably high ferite factor. However, such alloy mexification has proven tobe economically unviable for thick gauge (>10 mm) plate products and therefore unstabilsed 12%Cr (ACR2) material is sill curently being used for heavy gauge structural applications ia many pars ofthe world. The aim of the current work was to review the mechanisms responsible for ‘ion in these unstabilised ferrite stainless steels, and to characterise the sensitisation efTeets arising Irom multipass welding procedures. ‘The objective was to determine the influence of Welding parameters and thereby to recommend mitigating tategies, TWo particular sensitisation ‘modes were found fo occur in the current Work, although only one Was predominant and considered problematic from a practial perspective. It ‘was found that with proper positioning of weld capping runs and control of weld overlap, iti possible to ensure that sensitising isotherms remain ‘buried beneath the parent surface, and so reduce harmiul corrosion effects © 2007 Ekevier BV. All rights reserved [Keywonds: Semsitsation; 126Cr stock: Welling: Ferric stainless see! 1. Introduction In recent years, sensitisation in 12%Cr (3CRI2) steels has, been the subject of intensive investigation in Australia after sev- eral corrosion failures were reported in welds on coal wagons. was subsequently determined that sensitisation could occur as a result of a number of different mechanisms, manifesting after different heat treatments and at different positions in the heat-affected zone (HAZ). The main conclusion of the work was that sensitisation could only be totally eliminated by effective stabilisation by titanium or niobium additions, and by suitable ccontrol ofthe ferrite factor. While simple in theory. this presents some problems for the steel manufacturer. Since titanium is a very strong ferrite stabiliser, the presence of titanium needs 10 be offset by appropriate amounts of -y stabilisers, but the two ‘most potent candidates (carbon and nitrogen) are undesirable. ‘This leaves manganese and nickel as suitable candidates and these elements are typically added in concentrations of appro ‘mately 2 and 1%, respectively. With these concentrations a fully * Corresponding shoe Tel: ¥t 2.42218849; fax: 461 24221 3112 Email address: doolan@ ow. (D. Noles, (0921-50035 se fron mater © 2007 Elev BL. Allright sscrve hit 0.10165. se. 2007.02.13 martensitic high-temperature HAZ (HTHAZ) can be achieved ‘which has the additional advantage of having increased tough- ness, since the presence of coarse 8 ferrite is eliminated. This does, however, present a major challenge to the steel maker because both these elements depress the Acy temperature and inerease the tempering resistance ofthe ste! [1]- High Aci tem- peratures are advantageous because they allow higher anneating temperatures, which decreases the required holding time and inereases throughput, resulting in lower cost, Steels with low ‘Ac temperatures require batch annealing which isa slower pro- ess compared to continuous line annealing, which is possible ‘with higher Acy temperatures “These measures, however donot provide a solution in all cit- cumstances. In comparison to fully ferrite grades like 409 and 430, 3CRI2 is considered to have good weldability and HAZ toughness in thick as well as thinner gauges, and itis supplied in thicknesses up to 30mm [2]. Material 10mm and greater is ‘most commonly supplied as shear plate and nots coil thas, the final at strip is eu drwetly tothe desired length after hot rolling ‘without being coiled. With the relatively high cooling ates expe- rienced during the cutting process, complete uansformation to ‘martensite will take place, respective ofthe Ae} and chemical composition, Annealing is therefore required, but an equivalent 158 Man Warmelo eal. Materials Science and Eineering A 464 (2007) 157-169 of batch annealing for stacks of cut plate becomes impractical and expensive. As a result titanium stabilised material in gauges above 8mm is generally not available. and unstabilised material is sill being imported into Australia, Unstablised thick gauge material is theoretically highly prone to sensitisation. The work by Williams and Barbaro [3] tnd Matthews etal. [4.5] showed that intersecting isotherms ean lead to sensitisation, and thick gauge materia, which requires ‘multiple passes forthe simplest joints, will naturally have several overlapping weld beads with intersecting isotherms. However it is not a foregone conclusion that eritical sensitisation will take place, since the postion of the beads, and the degree of overlap, will determine whether any particular HAZ. is sen- sitised by subsequent weld beads. The work by Matthews et al. [4] also showed to what extent the degree of overlap influ- ‘enced the presence of sensitisation and IGC. A significant factor also whether the sensitised region reaches the surface of the plate or whether it remains within the interior where it is The current investigation was initiated in an attempt to determine the extent to which thick gauge 3CRI2 material ‘was susceptible to sensitisation, to characterise its occurence in multiple pass welds, and to determine to what extent it could be minimised by appropriate control of the welding parameters, 2. Background Sensitisation in stainless steel can be defined as susceptibil- ity to intergranular corrosion (IGC), which occurs due to the presence of chromium-depleted zones at the grain boundaries. ‘This depletion of chromium is generally associated with the pre- cipitation of chromium carbides on the grain boundaries, which remove chromium from the matrix and thereby locally reduce the corrosion resistance along the grain boundaries. In their sim- plest form, the carbides would be CrasCs or CrxC3, and they consume a large quantity of chromium on formation due to the high stoichiometric ratio. Predicting the sensitisation behaviour of 3CR12 during weld, thermal eycles is complicated by the presence of the so-called gamma loop in the typical Fe-Cr phase diagram, illustrated in Fig. 1. In high purity Fe-Crsystems, the gamma loop extends as farasabout 13.5%Cr[I]-after which the structure is fully ferriti at all temperatures, Due to its otherwise low alloying content, 3CRI2 lies in the dual phase region, and the structure will there- fore consist of a mixture of delta ferrite (untransformed), alpha ferrite (transformed from austenite on cooling) and martensite, depending on the cooling rate. ‘The phase diagram naturally does not provide a good indi cation of the structure which will be found in the HAZ of a weld, but in conjunction with the typical continuous cooling transformation (CCT) diagram shown in Fig. 2 [6]. the typi cal features of the HAZ expected in 3CRI2 type steels can be explained. Unlike the HAZ for plain carbon steels, the HAZ zone for 3CRI2 has two visually distinct zones: the high-temperature (or coarse grained) HAZ (HTHAZ) and the low temperature HAZ (LTHAZ). Material heated close to the liquidus (above the (a) 6-<0.01% 1900 1400 1900 200 100 +000 Temperature in °C 8 hh 1 as (Chromium in 9% 3 eS 70 Fig. 1, Typical Fe-Cr phase gram illsatng the gamma loop (alter Derma up. As) transforms completely to 8 ferrite and rapid grain growth ‘occurs. On cooling, the amount of reversion to y will be deter- mined by the CCT diagram and therefore the HTHAZ. frequently consists of coarse-grained 8 ferrite, with islands of martensite at the grain boundaries. The CCT diagram indicates that if the ‘material temperature reaches 1050 °C within 1-2, no reversion to y will occur and the 8 ferrite structure will be maintained to room temperature. However, material which has been heated above the Ae) but below the Aes will contain significant frac- tions of y which will transform to martensite, resulting ina tough fine-grained structure Extensive work by Williams and Barbaro [3] has shown that, the origin of sensitisation in 3CRI2, that is, the creation of chromium-depleted zones, can be ascribed to four different pro- cesses oF modes. These modes distinguish between where and how the chromium-depleted zone will be formed and the thermal conditions required {6 ereate the chromium depletion 2.1. Mode 1 sensitisation ‘This mode of sensitisation is linked tothe presence of untem- pered martensite in the steel before itis exposed tothe sensitising temperature. This means that as a result of a single weld pass, lee gro] 38 J Me ‘ : 7 fe) ME ay Mt Fol t 10° 0 10" 10° Contin Fig. 2. Proposed continuous cooling transformation diagram forthe wansfrms tion offerte to in the hih-temperatare HAZ. dirng weld thermal eles (pte fom Pistorian andl van Rooyen [6 1M. van Warmelo eal. / Materials Seience and Engincering A 464 (2007) 157-169 19 Fig. 3. Macrossctionsillstrating the inflacnesof weld geometry and welding sequence on mode 2 sestston (after Wiliams and Barbro [SD, sensitisation can ovcur parallel to the weld bead wherever the ‘material reached the critical sensitising temperature. In practice, the presence of substantial amounts of untempered martensite in 3CR12 sheet will only occur if the material was incorrectly annealed (that is the Acy temperature was exceeded during annealing or any other form of heat treatment before process- ing). Mode 1 is potentially the most severe manifestation of sensitisation in these steels, principally because itis likely 10 extend over a large area, Ifa plate or edge of a coil is over- heated during the final annealing stage. it renders the entire area susceptible to sensitisation if itis Welded. The sensitised region can therefore be very widespread and extend along the entire length of a weld bead. However, commercially available material should not contain any untempered martensite since the material is not deliberately heated above the Ac} during annealing. 2.2, Mode 2 sensitisation Fundamentally, the mechanism for mode 2 is identical 10 mode 1, but the difference lies in how the untempered martensite in the material is created. Mode 2 assumes at least two welding ppasses where the first pass created untempered martensite in the HAZ and the critical sensitising isotherm from the second pass ccauses carbide precipitation in the first HAZ. Essentially, both modes require two exposures to high temperature but the man- ifestation will be different. In mode 1, the intergranular attack will be associated directly with the weld bead that caused the precipitation, while in mode 2, corrosive attack will be asso ated with weld | while the precipitation was effectively caused by weld 2. Depending on the weld geometry and dimensions, ‘mode 2 sensitisation can manifest itself on the opposite side of a plate from where the weld was positioned, as illustrated in Fig. 3. I has been shown by Williams and Barbaro [3] and Matthews, etal, [5] thatthe joint configuration and positioning of the weld beads can significantly affect whether sensitisation occurs. If the sensitising isotherm from the second weld only intersects with the filler metal or unaffected base metal, sensitisation is avoided, 2.3. Mode 3 sensitisation Mode 3 sensitisation occurs in the HTHAZ. (ie. the coarse rained region adjacent to the fusion line) in material where the HTHAZis predominantly feritic. Since the material close to the fusion zone is heated well above the Acs temperature, this moxie is independent of any previous heat treatment and material condition. Unlike mode 2 sensitisation, mode 3 ‘occurs afier a single exposure to high temperatures above the Acs temperature and has been shown to oecur even in titanium stabilised steels with higher ferrite factors Although not well understood, recent work has shown that mode 3 is caused by extremely rapid cooling rates generally associated with very low heat input welds [7] and by shallow ‘Weld toe eusps and are strikes [3]. As ean be seen from the CCT. diagram for 12%Cr steels [6]. very rapid cooling from above 1350 °C will result in a fully & ferrite structure, Atthese elevated temperatures, even TiC and TIN can dissolve to release carbon and nitrogen back into the 8 matrix. Ifthe + transformation is suppressed during cooling, there will be a strong tendeney for carbides to precipitate at the grain boundaries as the material passes through the critical temperature range. It appears that reformation of Ti(C. N) precipitates is kinetically unfavourable ‘under these conditions, and preventing sensitisation is therefore achieved by the presence of sutficient -y during cooling which absorbs and traps the carbon and nitrogen rejected by the 8 ferrite uring cooling. In the recent work by Greet and Du Toit [7] it ‘was shown that for equal heat input levels, material with higher ‘ypotential had a lower propensity for sensitisation than material with lower y potential. It was also shown that increasing the heat input resulted in reduced sensitisation due to lower cooling rates, which in turn resulted in more 8 reverting toy. This work confirms previous reports by Gooch etal. [8] that the degree of dom the phase of sensitisation sensitisation in single pass welds would de} balance of the material Itis therefore desirable to increase the level of austenite ref- ‘ormation during cooling in order to maximise the volume of martensite in the HAZ. Gooch and Ginn [9] suggested that pre- heating in the region of 300°C would result in slower cooling ‘with a subsequent inerease in the volume of y formed on cooling, but also commented that very little success had been achieved experimentally. Even if moderate success had been observed, this would not necessarily represent a practical solution because it negates the benefits that the utility Ferritics were designed to deliver. specifically ease of fabrication, similar to that of carbon steels. 24. Mode 4 sensitisation Mode 4 sensitisation is only associated with steels which have a relatively high Aci temperature, where the Aci for common 160 M. vam Warmelo ea / Matera Science and Engineving A 464 (2007) 157-109 Table | ‘Chemical analysis of 3CRI2 mstaril (all vlues in weight percent) MucialiD_€ s > Ma St Ni Ge Moi N CG ar 0016 0957 OMT oai6 Ras 0.003 00080 - a oor pon 0280 OSs 22D ou ouo7s = = a 0030 0.00% 0028 ID O60 KD 002 003300012 0m 1204Cr steels ranges between 760 and 840°C. The mechanism for mode 4 has not been confirmed but it is believed that car- bides start to dissolve in the region just below the Aci and then precipitate as chromium carbides on cooling. The model proposed by Williams and Barbaro [3] suggests that elements. such as boron and vanadium are involved. It is suggested that ‘chromium borides and vanadium carbides dissolve at temper atures around 800°C and then chromium carbides precipi ‘on cooling. In their review on stabilisation and potential carbide forming elements, Gordon and van Bennekom [10] report that vanadium is unsuitable because of sluggish precipitation, and ecause VE dissolves close to 800°C, which correlates with the hypothesis by Williams. Vanadium was present as a resi ual in all the materials showing mode 4 in the work done by Williams and Barbaro [3] and, if the resulting sensitisation is ‘due (© VC dissolution, this would explain the observation that the severity of mode 4 sensitisation is generally low. Williams also suggests that some dissolution of carbornitrides can start ‘occurring from temperatures above 790°C since the solubility limit of carbon at this temperature can be as high as 0.03% [11]. In steels with low Ac) temperatures, any dissolved carbon oF nitrogen will be absorbed by the austenite formed when the Aci temperature is exceeded. The severity of mode 4 is there- fore strongly dependent on the amount of earbon and nitrogen released into solution and the temperature range between the dissolution temperature and the Aci. The severity of mode 4 ‘would be expected to increase with higher heat input and resul- lant inereased time at the dissolution temperature. Conversely, very low heat input and fast travel speeds have been shown to be instrumental in causing mode 3 sensitisation [7], and there- fore the heat input needs to be controlled within an optimal range. ‘Mode 4 can occur after a single heat cycle and is not depen- dent on martensite being present or created by previous heat cycles. A third zone has therefore been identified in the HAZ, and is generally referred to as the subcritical HAZ [5]. This are \was previously considered as being unaffected by welding c since no phase transformations occur, but with the isolation of mode 4 sensitisation, this region becomes highly significant. ate 3. Experimental methods 31, Materials ‘The main aim of the work carried out was to determine the ‘extent fo which multiple weld passes and varying heat input influences the degree of sensitisation in thick gauge 3CRI2 ‘The experimental work was carried out in two parts, involving bead on plate (BOP) welds and straight butt welds. “The material fr the investigation was supplied by Atlas Spe ity Metals, who import the stel from various suppliers around the world. Material from two different manufacturers was pro- Vided and plats from two different batches were provided by supplier A. The nominal chemical analysis for each material, as shown on the material test certificates, is given in Table 1. ‘These analysis values have been used t0 ealeulate the various material characteristics, as given in Table 2. As expected, the Kaltenhauser Ferrite Factor (KFF) value [13] is higher than the Bluescope Steel Ferrite factor (FFgs.) for each material and, aeconding to the criteria given by Williams and Barbaro (3], only material A2 should be immune from mode 3 sensitisation, ‘even though the difference between the analyses of Al and A2 is typical of the variation between production casts from the same manufacturer. While the prediction for the martensite start transformation temperature is fairly consistent for the formulas used by Smith and Tarboton [12] and Gooch et al. [8]. the same ‘cannot be said forthe Aes temperatures. Given that all the steels are unstabilised, the Acy temperature is an important factor in determining susceptibility to mode 4 sensitisation, The values calculated by Smith and Tarboton [12] are determined from an ‘empirical model based on dilatometry results of several hundred analyses and was specifically developed for 12-14%Cr steels. ‘The Folkhard equation [11] is based on more limited data and, 4s such, the results given by Smith etal. re more likely to be more accurate Asset of preliminary trials were required inorder to optimise ‘experimental welding conditions and ensure weld quality. As rateral availabilty from supplier C was limited, the initial wil ‘work was undertaken using material AI. Once the experimental mater Tole? Material characteristics ofthe 3CR2 materials (srmperatres in degrees elit) MacialiD—KFFUIS]—FFpsu 5] Aci Folkhand [1] Ae (Smithand AZM (Mathows __-Me(Smiihand Ms Gooch Tarbocon (12) etal (5) Tatoton) 12] etal (8) al 942 870 ory 7650 78 357 65 a xo X16 S19 W519 sos 4043 952 ci 40 921 m7 8264 ms 4817 ass 1M. van Warmelo eal. / Materials Seience and Engincering A 464 (2007) 157-169 161 difficulties had been overcome, material from both suppliers was ‘welded and tested to obtain comparative results between the two variants. Since the available AT material was consumed for the -sperimentation, direct comparisons have only been erial AZ and C1. In any ease, the variation in the analyses of AL and A2 is typical of the level of variation expected in commercial production, 3.2, Welding procedures But welds were produced between two 10 mm thick flat bars, ‘which had a double sided 60° V weld preparation witha 1.5mm landing (as per the manufacturer's recommended practice [2]. ‘The samples were tack welded at either end so that a 2mm gap ‘was let at the bottom of the V-notch. The tacked sample was clamped to prevent bowing but a 10mm gap was left etween the sample and the base plate. As per the manufacturer's rec- ommended welding practice, the filler metal used was 0.9 mm diameter solid austenitic wire G309L), and the shielding gas used was StainShield Lite (argon, 1%0.). Shielding gascontain- ing carbon dioxide is not recommended, due to the possibility of carburisaton. The interpass temperature was controlled 10 below 60°C and the plate was allowed to cool naturally with- cout forced air or water quenching between passes. The welding torch was clamped to a Bug-O system trolley which ran along 4 rail mounted parallel to the base plate, For the preliminary experiments on material Al, no backing bar was used for the root pass and the back side of the root pass was ground out before the backing pass was laid down, Root penetration was not ‘ery good on these initial weld runs and thorough back grind- ing was done before the back pass was laid down, A ceramic backing strip was used on the later welds using material A2 and CI. Better control of the root pass could be achieved and root penetration was significantly better on these welds. Back nding was still done on all samples, but it was less extensive than for material Al. The welds were cleaned with a stain- less wire brush between passes but grinding was only done fon the root run, The back pass was always done as the very last pass Transverse samples were cut across the welds for metallo- graphical analysis and sensitisation tests. The samples were cut using a hand saw so as to prevent any local overheating ofthe surface and then ground 10 1200 grit finish and polished to a wm finish. Etching with acidified FeCls solution or Kallings No. 2 revealed the coarse primary ferrite in the CGHAZ and the martensite/ferrite HAZ and matrix. Electrolytic etching in 10% oxalic acid clearly revealed the regions of fresh un pered martensite where effectively no carbide precipitation had ‘occurred, and severely attacked the grain boundaries where pre- cipitation had occurred. 3. Modified Strauss test ‘The modified Strauss test isa variation on ASTM A. 763-98, Practice Z [14] for detecting susceptibility to sensitisation in ferritic stainless steels, Samples are placed in a copper Sulphate solution (60 g CuSOs in lof water) which is aeiiied by adding 0.5% sulphuric acid @ mL HyS04 in TI water). layer of copper shot is placed on the ottom of the vessel and the samples are placed in the solution in such a way as to prevent direct contact ‘with the welded region. The solution is then boiled for 20h. During the test, chromium-depleted regions will undergo anodic dissolution and copper will be deposited on the corrod- ing regions. This generally highlights the areas where IGC is ‘occurring but sometimes this ean be masked by other corrosion products. Copper will deposit anywhere that corrosion is occur ring and if any pitting or crevice corrosion takes place. copper deposition will be seen. It should also be noted that position- ing of the samples can also influence the test results, in that test surfaces positioned horizontally tend to show more copper deposition than those positioned vertically. This may be due 10 a settling effect, and subsequent enhancement of corrosion via 2 erevice corrosion mechanism. An example of this effect is shown in Fig. 4 where the sample in Fig. 4(a) was positioned horizontally while the sample shown in Fis. 4(b) was positioned vertically during testing, and the decrease in copper deposition in the case of vertical positioning is clear. ‘The samples which had been analysed metallographically ‘were tested by this method, as well as two additional samples from every weld. The polished specimens were placed in the vessel so that the polished surface was horizontal and facing up while the other specimens were placed so thatthe weld bead ‘was parallel withthe base ofthe vessel, i. the eut surfaces were vertical. After the samples were removed from the test solution, llsurfaces were scrubbed with a soft brush o remove any excess copper and other surface accumulation ) Fig. 4. Cross-scton showing more copper deposition on (a te boriontlly psioned sample. compucd to () the vertically positioned sample. 182 M. vam Warmelo ea / Matera Science and Engineving A 464 (2007) 157-109 ‘Tle Welding parameters used for preliminary but welds on material AT Sample 1D Heat input (ina) ‘Cureat [AT Potent [V] “Travel speed mua) Wire feed ate (ania) BWaoT 68 20 eI BWA bas 250 60 BWA.S 035 20 62 BWA 04 040 20 250 63 BWA 037 300 63 BWA 06 ost 20 6s BWAOT O68 200 2 BWA 08, 039 300 60 BWA 09" 03 2x0 62 BWA 10 as 270 6s ‘Constant parameters forall samples ‘Gas ow rate 15 Limin Contact ip to work distances [Sm Filler material: 19mm 309, Tntcpass empertire<80°C If metallographical analysis was required after the samples, hhad been tested, the samples were cleaned in nitric acid to remove the copper and then polished lightly. Results 4.1. Preliminary welding trials: material A} A satisfactory root run could be obtained when a dip transfer mode was set on the welding machine and so this mode was used forthe root run and the two eapping runs on all welds. The remainder of the passes were generally done using spray transfer mode settings. The heat input and welding parameters are given in Table 3. From literature [15] the are efficiency for GMA welding isin the region of 60-75% and a factor of 75% was used inthe calculation for heat input. The heat input value given inthe table represents the average ofall the passes excluding the root passes done using the dip transfer parameters. The heat input was varied by adjusting the travel speed and the wie feed rate, and the arc eurrent and potential were determined by the welding machine, The values given in Table 4 for these {wo parameters are the final values displayed by the welding machine after welding had been completed. Given thatthe recommended heat input range for 3CRI2 type materials js 04-10 kV/mm, these values ae all onthe lower side othe range. Nevertheless, the material deposition rate proved more than adequate to fill dhe V-notch, and atthe higher heat input values, eight passes were not required to complete the weld Consistency in the weld bead positioning created the majority o the variation between the welds. In many cases, the weld bead tended to ride up on one side of the V, leaving a very sharp notch atthe base on the opposite side. Fusion defects were frequently noted at this position. The weld bead also frequently tended to wander and this created very uneven and lopsided welds, specifically with the last cover passes. This also created a situation where subsequent beads overlapped a great deal more than would be expected in an expertly welded joint. As was shovsn in literature [4], the degree of overlap plays a significant role in whether sensitisation will occur. Examples ofthis will be shown in later sections, Samples for metallographical examination were cut fom each test piece, which were then polished and eiched in oxalic acid. Ie was apparent that the precpitate-free untempered iartensite was essentially unattacked, However, in some cases it could clearly be seen where intersecting isotherms had reached Tables Welding parameters fr comparative tals on materials A2 and CL Sample 1D eat inp in Corea AT Potcatial IV] Travel peed ln) Wir feed te [ovnia) BWA 201 059 11 = 20 os Wa 202 040 us as x20 6s BWA 208, on m2 26 200 18 BWA 204 oa? 2 240 6s BWC 101 037 20 6s BWC 102 039 x20 6s BWC 103 04s 240 6s BWC 10d 07 20 75 Constant parameters forall samples ‘Gas ow rate 5 Lnin ‘Contact ip to work distance: 1S mm Ceramic hacking strip on root pass Filler material: 0.9m 3001. Inecpas temperature

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