Studies on metallurgical and impact toughness behavior of variably sensitized

weld metal and heat affected zone of AISI 304 L welds

Subodh Kumar, A.S. Shahi

PII: S0264-1275(15)30554-2
DOI: doi: 10.1016/j.matdes.2015.09.145
Reference: JMADE 715

To appear in:

Received date: 28 June 2015

Revised date: 18 August 2015
Accepted date: 27 September 2015

Please cite this article as: Subodh Kumar, A.S. Shahi, Studies on metallurgical and
impact toughness behavior of variably sensitized weld metal and heat affected zone of
AISI 304 L welds, (2015), doi: 10.1016/j.matdes.2015.09.145

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Studies on metallurgical and impact toughness behavior of variably sensitized weld metal

and heat affected zone of AISI 304L welds

Subodh Kumar and A. S. Shahi*

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Department of Mechanical Engineering, Sant Longowal Institute of Engineering & Technology,

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(Deemed University), Longowal, Sangrur (Punjab), India-148106

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*
Corresponding author’s email ID: [email protected]

Tel.: 91-1672-253272, Fax: 91-1672-280057

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Abstract
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Influence of sensitization on the metallurgical and impact toughness behavior of different gas

tungsten arc AISI 304L welds has been investigated. Each weld has been characterized
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individually to understand the role of welding conditions on the carbide precipitation behavior
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which influences its impact toughness performance. Weld metal subjected to sensitization
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conditions leads to carbide formation that occurs inter-dendritically along the δ-γ interface. Low
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heat input weld metal possessing lathy ferrite morphology shows relatively a low degree of
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sensitization (DOS) as compared to the high heat input weld metal possessing vermicular ferrite

morphology. Grain coarsening in the heat affected zone (HAZ) of these welds is found to

influence the DOS significantly. As welding heat input increases, HAZ grain coarsening also

increases, which results into higher DOS. An increase in the post weld thermal aging time results

into higher DOS, which significantly degrades the impact toughness of the weld metal as well as

the HAZ of these joints. Charpy V-notch (CVN) testing results under cryogenic testing

conditions of (-196 °C) show that carbide formation causes a severe degradation of the impact

toughness of these welds as examined through their scanning electron fractographs, which show

the formation of deep and wide intergranular cracks.

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Keywords: AISI 304L SS welds; Weld metal; Heat affected zone; Microstructure; Impact

toughness; Degree of sensitization

1.0 Introduction

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Stainless steels (SS) being an important class of engineering materials, besides general

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use, have been extensively used in a variety of critical applications where harsh conditions like

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high temperature and extremely corrosive environments are involved [1]. Austenitic stainless

steels (ASS) comprising of 300 series form an important part of the family of stainless steels that

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are used in a variety of applications. For instance, in the food industry, food contact stainless
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steel surfaces being a major concern, welding induced surface features play an important role on

the accumulation of the bacterial species and the welds to be used for such fabrications must be
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able to meet the food industry roughness standards [2]. In transportation industry, series of cold
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rolled plates of these grades have been used for manufacturing of light-weight railroad cars

where reliability and safety of running trains depends upon the quality of welds [3]. In the
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chemical industry, environmental compatibility is a prime requirement for reliable performance

of materials. So these grades are also widely used as construction materials for storage tanks for
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highly concentrated methanesulfonic acid (MSA) which is a strong organic acid and give rise to

highly corrosive reactions during its manufacturing [4]. In the nuclear industry these grades are

specifically used as boiling water reactors where pressurized water reactor environment leads to

corrosion failures after long time service [5].

Welding is one major fabrication technology that is used for such industrial applications,

and as such various weldability issues and concerns that arise during welding play a vital role in

deciding about the reliability and satisfactory performance of such welded fabrications. Since

welding of these materials involve temperatures in the range of 550˚C to 850˚C, these steels
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become prone to intergranular corrosion. This intergranular corrosion of austenitic stainless

steels, in general, is a conventional and serious problem during welding and high temperature

use, which makes these steels susceptible to sensitization, which is a process of chromium

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carbides formation at the grain boundaries surrounded adjacently by the chromium depleted

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zones [6]. The corrosion properties of the austenitic stainless steel welded joint are deteriorated

as its heat affected zone (HAZ) is often sensitized by formation of intergranular Cr-rich carbides

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[7]. Welding causes microstructural variations across weld zones and HAZs, which in turn,

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influences the thermodynamic and kinetics of specific corrosion processes leading to accelerated

corrosion and/or fracture of the weldment [8]. The austenitic stainless steel fabrications like
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nuclear waste containment vessels and desulphurization of crude oil in petrochemical industry

when exposed to service environments lying in a temperature range of less than 500˚C for longer
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durations become susceptible to carbide precipitation. This susceptibility towards carbide

formation affects the mechanical and corrosion properties of such critical fabrications. In other
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words, the extent of carbide precipitation occurring during welding and the post weld thermal
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conditions, both play an important and combined role in affecting the overall mechanical and
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corrosion behavior of these weldments. During such industrial applications, exposure to these

environmental conditions also results into the growth of pre-existing carbides nucleated during

welding, especially when exposure times are longer [9]. Such type of conditions where carbide

growth takes place during low temperatures for long exposure times is referred to as low

temperature sensitization (LTS) and hence becomes an important aspect of research in view of

assessing the reliability and dependability of such welded fabrications.

While considering the design and manufacturing stages of such stainless steel products,

fundamental technological aspects play a significant role in attempting to predict their service
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behavior. So in view of this, research involving determining of the most adequate welding

procedures for anticipating the functionality of welded joints becomes important [10]. Previous

work reports that changes in microchemistry and microstructure have been examined for

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studying and developing correlations among grain boundary chemistry, precipitate density and

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intergranular fracture [11]. Few studies have also been reported where the corrosion behavior of

weld metal has been compared with HAZ and it is observed that welding process has a

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detrimental effect on corrosion behavior and biocompatibility of stainless steels, especially when

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attacked preferentially in corrosion environments [12]. The roles of few phases like austenite that

are preferentially attacked under corrosive environments have also been examined [13]. Since
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welding involves localized heating and cooling, different zones of the weldments experience

variable cooling rates owing to different thermal gradients that are established during welding,
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which are directly dependent upon the process parametric combinations used. Such conditions

when met by austenitic stainless steel welds lead to microstructural as well as local
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compositional variations in various zones of their weldments, thus giving rise to

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microsegregation effects in the weld zone [14], whereas HAZ undergoes a varying degree of
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carbide precipitation. The implications of these microstructural changes that occur due to

welding may be so significant that during actual service these steels can become prone to

sensitization, which can consequentially degrade their corrosion performance, thus leading to

premature failures.

From the literature reviewed, it is observed that sensitization in AISI 304L weldments

poses serious problems during service applications. So considering the importance of

investigating the role of welding conditions as well as different sensitization conditions on the
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metallurgical and impact toughness of AISI 304L welds, the present investigations have been

carried out.

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2.0 Experimental

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2.1 Materials and welding methodology

From the hot rolled plates of AISI 304L having 6 mm thickness, base plates were cut to

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suitable sizes and the edges were machined in accordance with the butt joint configuration with a

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single-V groove design. AISI 308L SS being compatible with the base material, was selected as

the filler material with electrode diameters of 1.6 mm and 2.4 mm that were used for giving the
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root and the main weld passes respectively for accomplishing welds using gas tungsten arc

welding (GTAW) process. Table 1 shows the chemical composition of the base material and the
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filler electrode used in the present work.

Weld quality related aspects were given due consideration and it was ensured that proper
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alignment of the base plates was maintained using tack welding of the plates prior to actual

welding whereas suitable clamping arrangements were used that helped in minimizing
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distortional effects in the plates. In accordance with the welding heat input levels and the joint

design selected for accomplishing the joints, one root pass and two main weld passes were used

to fill the groove volume for each joint. Table 2 shows the details of the experimental conditions,

including three different levels of welding heat input, used for welding. Due care and caution

was exercised during welding where all necessary precautions like pre-cleaning of the groove

edges and interpass cleaning between consecutive weld passes were followed to avoid

contamination of any sort, thus ensuring defect free welds.

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2.2 Post weld thermal aging (PWTA) of the weldments

2.2.1 Low temperature sensitization thermal aging

With an aim of studying the sensitization behavior of these weldments it was important to

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expose these joints to nearly similar sensitization conditions that are expected to be encountered

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during actual service applications. Keeping in view the service conditions where LTS conditions

exist, research attempts require rationale means which should form the basis for selecting

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suitably a range of temperatures where similar LTS conditions could be created in the specimens,

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thus helping in accurately predicting the material’s behavior [15]. On such approach is that of

using Arrhenius equation for simulating the service life of such materials for the desired
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duration. In the present work, this formulated the basis of selecting three post weld aging

treatments viz. 500˚C for 1, 5 and 11 days such that the service life of AISI 304L welded
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fabrications from 10 to 100 years at 300˚C could be simulated. These PWTA treatments were
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worked out as under:-

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t2/t1 = e-Q/R {(1/T2)-(1/T1)} [1],

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where Q is the activation energy (150 kJ/mol), R=8.314 is the universal gas constant (J/mol K),
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T1 is the aging temperature (773 K or 500˚C), T2 is the temperature at which the life is being

estimated (573 K or 300˚C), t1 is expected life (10, 50 and 100 years), and t2 is the time required

to expose at T1 (in days).

Based upon the LTS treatments as calculated above, different weldments from each joint were

subjected to three post weld thermal aging treatments viz. 500˚C for 1, 5 and 11 days such that

the service life of the weldments from 10 to 100 years at 300˚C could be simulated.
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2.2.2 Classical sensitization temperature thermal aging

Samples extracted from different weld pads were also subjected to PWTA in the classical

sensitization (CS) range in order to study the effect of relatively higher temperature for shorter

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durations on the carbide precipitation behavior of these joints. In the present case, three different

post weld thermal aging treatments (CS) viz. 650˚C for 1 hour, 650˚C for 12 hours and 650˚C for

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24 hours were used.

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Various post weld thermal aging treatments used in the present work have been represented by

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LTS1 for 500˚C/1 day, LTS2 for 500˚C/5 days and LTS3 for 500˚C/11 days corresponding to the

LTS range, whereas CS1 for 650˚C/1 hour, CS2 for 650˚C/12 hours and CS3 for 650˚C/24 hours
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corresponding to the CS range.
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2.3 Impact testing and Microstructural studies

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As per the work plan, suitable numbers of different specimens (to be used for testing in

the as-welded condition as well as in the thermally aged conditions) were machined out from
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each weld pad for conducting impact testing and microstructural studies. Charpy V-notch (CVN)

impact specimens of size 55 mm×10 mm×6 mm were prepared in accordance with ASTM E23
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standards [16] as shown in Fig. 1. In order to assess the impact toughness of the weld metal and

HAZ of each joint individually, V-notch was provided at the centre of the weld zone and the

HAZ respectively. Five number of Charpy impact specimens representing each weldwere

machined and tested at room temperature and liquid nitrogen temperature (-196˚C), using a

pendulum type impact testing machine with a maximum capacity of 300 J. For determining the

impact energy absorption at -196˚C, the specimens were dipped in liquid nitrogen for a sufficient

time to lower their temperatures and thereafter impact testing was carried out within less than

five seconds of being taken out of liquid nitrogen [17]. The fracture behavior of the impact tested
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specimens corresponding to various welding and aging conditions was studied through

fractography using scanning electron microscopy (SEM) of the fractured ends of these

specimens. Electrolytic etching procedure was used for revealing the microstructures of the weld

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metal, fusion zones and HAZs of the weldments. The electrolyte comprising of 10 gms. of oxalic

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acid and 100ml of distilled water was used with the etching parameters of 6 volts as cell voltage

and 1 minute as the etching time [18]. Photomicrographs of different zones of weldments like

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weld metal (WM), heat affected zone (HAZ) and fusion boundary zone (FBZ) of different joints

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were captured using an inverted type metallurgical microscope supported with a dedicated

metallurgical software. Quantitative measurements of delta ferrite in the weld metal of the joints
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were made using Ferritescope (Make: Fischer International, Model: M30).
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2.4 DOS evaluation of the weld metal and the HAZ of the joints using DLEPR test
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Double loop electrochemical potentiokinetic reactivation (DLEPR) technique was used

for sensitization studies through DOS evaluation of the specimens comprising of weld metal as
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well as HAZs representing different weldments (as-welded as well as thermally aged) as

suggested by the previously reported studies [19-22]. The specimen sampling plan for degree of
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sensitization (DOS) studies as represented schematically through Fig. 2 shows how weld metal

and HAZ were extracted individually from each weld pad. Each specimen contained a cross-

sectional area measuring 10 mm wide x 6 mm thick, which was exposed directly to the test

solution in DLEPR test. Section X-X in Fig. 2 shows the location across which the weld metal

specimens were extracted comprising of the cross sectional area taken in the longitudinal

direction of weld. Specimen location comprising of HAZ of the weld is represented by the cut

section Y-Y and the final area meant for subjecting to DOS evaluation was taken longitudinally

to the direction of the weld. For facilitating the mounting of each specimen in the epoxy resin 10
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mm depth was taken and for each specimen an overall area of 60 mm2 was exposed to the test

solution. An austenitic stainless steel cable was used for ensuring the electrical contact for each

specimen. The surfaces of the specimens were prepared metallographically and polishing up to

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3000 grit finish was achieved. The electrolyte used comprised of a mixture of [0.5 M H2SO4

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(sulfuric acid) + 0.01 M KSCN (potassium thiocyanate)] solution prepared with pure reagents

and distilled water. The electrode combination used in the present case comprised of graphite

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counter electrode, a reference electrode of saturated calomel electrode (SCE) and the working

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electrode (test specimen). A potentiostat/galvanostat (Make: Gamry Instruments, Model:

Reference 600) supported by the dedicated software was used for conducting DLEPR tests on the
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specimens. The DLEPR testing of the aforementioned specimens was carried out at room

temperature and the procedure involved three stages viz. (a) allowing for a delay of 5 minutes at
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the open circuit voltage (OCV) (b) taking a anodic polarization scan from 50 mV below the OCV

to 300 mV (SCE) in the passive range using a scan rate of 100 mV/min, (c) taking a cathodic
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reactivation scan from 300 mV (SCE) to OCV at the same scan rate. The measurement of the
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degree of sensitization (DOS) of each sample was taken as the ratio of the reactivation current to
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the activation current multiplied by 100 [23]. The average DOS values for each specimen were

measured on the basis of taking three readings individually for each surface and between each

reading fresh test solution was used.

3.0 Results and discussion

3.1 Microstructure of the weldments

3.1.1 Weld metal microstructures (as-welded & sensitized)

In order to check the susceptibility of the weld metal to hot-fissuring tendency, ferrite

studies were carried out. It was found that in all the welds (despite of significant variations in the
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weld microstructure), the ferrite content varied (low heat input weld from 4.2 to 4.8 %, medium

heat input weld from 5.0 to 5.5 % and high heat input weld from 5.8 to 6.4 %) in the

recommended range indicating that these welds were not prone to hot fissuring/cracking [24].

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The photomicrographs of the weld metal in the as-welded condition are shown in Fig.3. Here

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Fig. 3a, c and e represent the microstructure of the weld cover pass of the low, medium and high

heat input welds respectively, where morphological changes in ferrite are clearly seen. Low heat

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input weld possesses lathy ferrite morphology which changes to vermicular/skeletal in case of

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medium and high heat input welds. Similar results have been reported by Delong [25], where it is

stated that for the common commercial welding processes like gas tungsten GTAW, GMAW,
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SAW etc., variation of welding heat input over broader ranges does not exert significant

influence on the ferrite content of welds, despite of morphological changes in ferrite. Fig 3b, d
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and f show the microstructure of the weld metal comprising of the freshly formed fusion zone as

well as the HAZweld pass (that forms within the previously deposited 1stweld pass). Such HAZs that
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form within the weld metal itself, experience a temperature range of 550˚C to 850˚C during
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welding. These conditions promote the chances of carbide precipitation along the δ-γ interface,
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which in turn makes the overall weld zone prone to sensitization during post weld thermal aging

conditions [26]. Such type of carbide precipitation that takes place along inter dendritic

interfaces in the weld metal is referred to as IDC (inter-dendritic corrosion) [26].

Some observable differences in the interpass weld area are also seen. It is observed for

the as-welded condition as well as post weld thermally aged conditions that in the weld metal

microstructure of the low heat input weld (Fig. 3b, 4b and 5b) fusion boundary zone is so small

that a clear demarcation in terms of dendrite orientation is not so prominently seen. However, the

dendrite orientation indicating the presence of interpass regions become visible in case of the
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weld metal microstructure of the medium heat input weld (Fig. 3d, 4d and 5d). Finally the effect

of welding heat input on the weld metal microstructure of the high heat input weld (Fig. 3f, 4f

and 5f) is more pronounced in terms of demarcation of the FBZ, besides which prominent

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epitaxial growth occurs along the fusion boundary.

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While examining the role of weld metal’s contribution towards sensitization, it may be

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seen that when these welds are subjected to post weld thermal aging in the LTS range, the

carbides that nucleated in the HAZweld pass as well as HAZroot pass during welding tend to grow

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along the δ-γ interface. This effect of weld metal sensitization taking place in different joints
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subjected to different LTS treatments is shown in Fig. 4b, d and f, which is attributable to carbide

growth taking place in the respective HAZweld pass of each weld. However, as shown in Fig. 4a, c,
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and e, weld metal comprising of the cover pass does not show signs of precipitation as no fresh
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precipitates are expected to nucleate here, as this portion of the weldment does not experience

the sensitization temperature range during welding.

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For understanding the sensitization behavior of the weld metal of these joints subjected to
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different treatments in the CS temperature range it may be reasoned out that carbide precipitation

expectedly occurs along the δ-γ interface regions of their respective weld metal microstructures.

Few micrographs representing such an occurrence of precipitation along the δ-γ interface in the

aforementioned regions of the weld metal of different joints are shown in Fig. 5.From this figure,

carbide precipitation is found to occur along the δ-γ interface regions, both in the weld cover

pass (Fig. 5a, c and e) as well as the HAZweld pass (Fig. 5b, d and f). Higher degree of precipitation

in these welds aged in the CS range may be attributed to the fact that in this temperature range

precipitation kinetics gets accelerated due to nucleation as well as growth of the interdendritic

carbides in different regions of the weld metal of these joints.

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3.1.2 Heat affected zone (HAZ) microstructures (as-welded & sensitized)

Fig. 6a, b and c show the HAZ microstructure in the as-welded condition for different

levels of heat input used during welding. Among these joints the variable welding heat input

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results into a varying degree of grain coarsening in their respective HAZs. Grain size

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measurements in the HAZs were carried out using interception method. It is observed that the

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HAZ of the high heat input joint undergoes a greater degree of grain coarsening (with an average

grain size of 94 µm) than the HAZ of the low heat input joint, which possesses an average grain

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size of 39 µm. This grain size variation may be attributed to different cooling rates experienced
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by the weldments corresponding to their respective heat inputs. Since higher heat input results

into lower cooling rate of the weldments, its HAZ undergoes relatively a higher degree of grain
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coarsening than found in the HAZ of the lower heat input weldment. Such a grain coarsening
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effect as observed in the HAZs of these welds is found to play a significant role in influencing

their strength as indicated by the Hall-Petch relationship i.e. finer grain size leads to higher
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strength and vice versa. This variable degree of HAZ grain coarsening in these joints in the as-

welded condition is further found to exert a significant influence on the degree of carbide
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precipitation during different post weld thermal aging treatments. Few representative

micrographs showing the grain coarsening effect on the carbide precipitation behavior of the

HAZs of different joints when subjected to LTS and CS treatments are shown in Fig. 6d to 6f

and Fig. 6g to 6i respectively. From these micrographs it is clearly seen that carbide formation

takes place intergranularly in all the HAZs which is also referred to as IGC (intergranular

corrosion) [27]. It is further seen among all the joints that HAZ of the low heat input joint by

virtue of lesser grain coarsening, exhibits relatively a lesser degree of precipitation than the HAZ

of the high heat input joint which possesses a higher degree of grain coarsening. This
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dependence of the degree of precipitation on the grain size of the HAZ may be explained on the

basis of the fact that relatively fine grained microstructure (as formed in the HAZ of the low heat

input joint) increases the grain boundary area which hinders the formation of continuous network

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of intergranular carbides. Conversely, in case of the coarse grained microstructure (as formed in

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the HAZ of the high heat input joint) lesser grain boundary area offers less hindrance to the

formation of continuous network of carbides, thus resulting into relatively a greater degree of

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precipitation [24].

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It is further observed from the photomicrographs as shown from Fig. 6d to 6i, that the

HAZs of all the joints (irrespective of welding heat input), subjected to CS treatments exhibit a
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higher degree of precipitation than found in case of the joints subjected to LTS treatments. This

may be attributed to the fact that during aging in the CS range, the temperatures encountered are
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relatively high, due to which nucleation as well as growth of the carbides in the HAZ of these

joints gets accelerated. It is worth mentioning here that this precipitation is a diffusion controlled
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process which tends to increase with an increase in temperature. However in the LTS range,
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precipitation in the HAZ occurs mainly due to the growth of the preexisting carbides that
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nucleate during welding and no fresh carbides nucleate under these conditions.

3.2 DOS studies of the weldments

3.2.1 DOS in the weld metal

DLEPR technique was used for evaluating DOS in the weldments and the results of the

DOS values measured in the weld metal of each of these joints, in the as-welded as well as

different post weld thermal aging treatments are shown in Table 3 and 4, and the corresponding

DLEPR curves are shown from Fig. 7 and 8. In the as-welded condition, the DOS values of

0.027, 0.12 and 0.34 were measured for the weld metal of low, medium and high heat input
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welds respectively. It is further observed that when these joints were subjected to post weld

thermal aging treatments in the LTS as well as the CS range, the DOS corresponding to each

joint’s weld metal showed an increasing trend of varying degree. Maximum DOS was observed

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for the weld metals subjected to LTS3 and CS3 treatments and the measured values for the low,

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medium and high heat input joints corresponding to LTS3 treatment were 5.5, 6.4 and 8.1

respectively, whereas for the CS3 treatment these values were 21.07, 23.15 and 26.42

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respectively. This significant DOS variation in the weld metal of these joints, among LTS and

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CS treatments, are attributable to the mechanism involved for carbide precipitation in these

welds. During LTS treatments the precipitation occurs due to carbide growth of the preexisting
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carbides that tend to nucleate along delta-gamma interfaces in the HAZs (HAZweld pass and

HAZroot pass) formed in the weld metal during welding. For higher degree of DOS as observed in
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the weld metal of these joints in the CS range, the mechanism of carbide precipitation is partially

similar to the LTS one i.e. besides the carbide growth of the preexisting nuclei in the HAZs of
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the weld metal, fresh carbides also tend to nucleate and grow in the weld metal along the delta-
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gamma interface. This accelerates the precipitation kinetics thus resulting into higher DOS under
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these CS range conditions.

Apart from the above DOS observations, welding heat input used during welding is also

seen to have an important influence on the DOS performance of these welds during post weld

thermal aging treatments. As seen from Table 3 and 4, low heat input weld metal shows

relatively lower DOS values than the weld metal of the high heat input weld, both for the LTS as

well as CS treatments. These variations in the DOS values among weld metal of different joints

may be attributed to a varying degree of precipitation occurring due to the microstructural

changes (especially different ferrite morphologies achieved) in the weld metal.

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3.2.2 DOS in the heat affected zone (HAZ)

The DLEPR results of the HAZ of different joints in the as-welded as well as post weld

thermally aged conditions are shown in Table 3 and 4 and the corresponding DLEPR curves are

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shown in Fig. 9 and 10. In the as-welded condition, HAZ of the low, medium and high heat input

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weld shows DOS value of 0.08, 0.24 and 0.52 respectively. The DOS performance of the HAZ

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of these joints when subjected to post weld thermal aging under LTS and CS conditions shows

an increasing trend.

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DOS of the HAZ of the low heat input joint when subjected to LTS1 and LTS2
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treatments show a slightly increasing trend of 0.15 and 0.87 respectively, which increases

considerably to 6.03 for the LTS3 treatment. HAZs of the medium and high heat input joints
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show a similar trend of DOS performance but with relatively a higher degree of increase in their
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respective DOS values corresponding to LTS1 and LTS2 treatment, which increase considerably
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to higher values of 8.53 and 12.65 respectively, when these joints are subjected to LTS3
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treatment. This trend in the DOS performance may be explained on the basis of the fact that, in
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the HAZs of these welded joints, temperatures encountered during welding cause precipitation to

occur in these zones due to nucleation of intergranular carbides which when subjected to post

weld thermal aging in the LTS range, tend to grow proportionately with the aging time.

It is further observed that the DOS values possessed by the respective HAZs of these

joints, when subjected to CS treatments show an increasing trend, which in all welds is found to

be higher than the DOS of HAZs under LTS conditions. Among all the joints, for all the aging

treatments in the CS range, a significant increase in the DOS values of the HAZs occurs when

aging time increases beyond 1 hour. The precipitation behavior of these HAZs changes in such a
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manner that their DOS values show a considerable increase that ranges between 13.45 to 21.32

for aging time of 12 hours (CS2 treatment) and 28.57 to 36.68 for aging time of 24 hours (CS3

treatment). Higher DOS values as possessed by these HAZs may be attributed to the fact that in

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this range, precipitation does not occur only due to carbide growth of the preexisting nuclei

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formed during welding, but also fresh carbides may nucleate intergranularly which may

subsequently grow, thus increasing the respective DOS values of the HAZs of these joints.

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It is also observed that among all the welded joints and for all the aging treatments, DOS

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possessed by the HAZ of the low heat input weld is found to be less as compared to the HAZ of
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the high heat input weld, thus indicating a trend that DOS of the HAZs of these joints increase as

welding heat input is increased. This increasing trend of DOS in the HAZs of these joints with
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increasing heat input may be explained on the basis of the grain size attained by the HAZ during
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welding, e.g. relatively smaller grain size is attained in the HAZ of the low heat input joint due to

lesser grain coarsening which results into an increased overall grain boundary area. This
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condition poses a hindrance in the formation of continuous network of carbides at the grain

boundaries of the HAZ, thus resulting into relatively lesser precipitation in this zone during
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thermal aging. Higher tendency of precipitation in the HAZ of the high heat input joint as shown

by its higher DOS value is due to a greater degree of grain coarsening in its HAZ, thus

decreasing the grain boundary area where continuous intergranular network of carbides is formed

with relative ease. Such a dependence of DOS on grain size has been reported previously also

where the effect of grain size on the susceptibility to corrosion has been investigated for refined

AISI 304 austenitic stainless steel and high nitrogen low nickel austenitic stainless steel, and it is

concluded that intergranular corrosion rate decreases with decreasing grain size [28].
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3.3 Impact testing of weld metal and HAZ

The Charpy V-notch (CVN) impact testing of the weldments was carried out to study the

impact toughness behavior of the weld metal and HAZ individually, both in the as-welded as

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well as post weld thermally aged conditions, at two testing temperatures i.e. room temperature as

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well as at cryogenic temperature of around -196˚C. The results of CVN testing of these welds are

shown in Fig. 11 & Fig. 12. It is seen for all the joints that under both the impact testing

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conditions, the weld zones (in the as-welded condition as well as all the thermal aging

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treatments) possess higher CVN values than their respective HAZs. These results show that

among all the welds, the weld metal (as-welded as well as thermally aged) corresponding to low
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welding heat input possesses the highest CVN value, followed by the weld metal of the medium

and high heat input weld respectively. This trend of toughness variation in the weld metal of
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these joints may be attributed to the morphological changes that take place during welding which

further account for a varying degree of interdendritic carbide (IDC) precipitation along the δ-γ
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interfaces that occurs during various post weld thermal aging treatments (PWTA).
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CVN testing results of the HAZs of different joints, both in the as-welded as well as
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different PWTA conditions, show that all the HAZs suffer relatively a greater loss in their

toughness as compared to their respective weld zones. This toughness degradation in the HAZs

may be attributed to grain coarsening that occurs during welding. It is further observed that low

heat input HAZs possess relatively higher CVN values as compared to the high heat input HAZs,

which like weld metal may be attributed to a varying degree of carbide formation occurring in

these zones. The low heat input HAZs possess fine grained microstructure as steeper thermal

gradients are encountered during welding, which when subjected to different PWTA treatments
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lead to relatively a lesser degree of precipitation which accounts for their higher toughness as

compared to the high heat input HAZs.

When the weldments are tested under the cryogenic condition of around -196˚C, it is

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observed w.r.t. the room temperature testing condition that both, the weld metal as well as the

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HAZs suffer a drastic loss in their respective CVN values. The toughness loss of these zones is

again attributable to the formation of interdendritic carbides and intergranular carbides in the

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weld metal and HAZ respectively. This serious degradation of toughness occurring at cryogenic

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testing conditions was further analyzed through the fractographic examination of the fractured

ends of the impact tested specimens using SEM and few of these are shown in Fig. 13 and Fig.
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14. As seen from these fractographs it is observed that in the as-welded condition, weld metal

and HAZ exhibit largely dimpled morphological fracture features. For the weld metal as shown
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in Fig. 13, it is observed that due to carbide precipitation the fractured regions/areas exhibiting

dimpled morphology reduce and tend to change into mixed mode where dimples coexist with
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cleavage facets. These are the signs indicating that the weld metal loses its impact toughness as
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the ratio of dimples to cleavage facets decreases, which is observed when aging conditions
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change from LTS3 to CS3 (Fig. 13d-13i).The significant loss of toughness is shown by the weld

metal of the high heat input joint subjected to CS3 treatment where higher degree of precipitation

leads to predominantly cleavage fracturing mechanism (Fig. 13i). Fractographs of the HAZs of

the CVN specimens tested cryogenically are shown in Fig. 14, which indicate that in the as-

welded condition, HAZs of the different joints show dimpled morphology along with some flat

featureless regions (Fig. 14a-14c). However, when these joints are subjected to various post weld

thermal aging treatments, the dimpled morphology changes into branched cracks that form

intergranularly. This branching of the cracks indicate the weakening effect induced in the grain
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boundaries owing to carbide precipitation, due to which the grain boundaries are not able to keep

hold with the matrix effectively. This leads to an effect called grain boundary separation (Fig.

14h & 14i), which accounts for serious degradation of impact toughness of these zones.

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4.0 Conclusions

Based upon the present work the main conclusions drawn are summarized as below:-

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1. Ferrite content in the weld metal of the AISI 304L joints when welded using heat input in the

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range of 8.7 to 14.7 kJ/cm length of the weld, does not change significantly, but its morphology

changes from lathy to vermicular as heat input is increased. During thermal aging, vermicular
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ferrite morphological features of the weld metal (as found in case of high heat input welds)

promote a high degree of carbide precipitation that occurs inter-dendritically, whereas weld
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metal with lathy ferrite morphology (as found in case of low heat input welds) shows relatively

lesser precipitation.
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2. Microstructural variations in terms of grain coarsening are observed in the HAZ of the joints
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due to welding heat input variations. Depending upon the heat input levels used it is found that
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the HAZ of the low heat input joint undergoes relatively a lesser degree of grain coarsening as

compared to the HAZ of the high heat input ones. This variable degree of HAZ grain coarsening

exerts a significant influence on the degree of carbide precipitation that occurs intergranularly,

when subjected to post weld thermal aging treatments. Less grain coarsened HAZ corresponding

to low heat input weld exhibited comparatively a lesser degree of precipitation than the more

grain coarsened HAZ of the high heat input weld.

3. DOS (degree of sensitization) of the different zones of the weldments as evaluated through

DLEPR technique show that both in the as-welded condition as well as thermally aged
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conditions, HAZs of the joints possess relatively higher DOS values than their corresponding

weld metals. It is further found that DOS in the weld metal as well as HAZ of the joints does not

depend on thermal aging alone but welding conditions used during welding also affect it

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significantly. Low heat input weldments (comprising of weld metal and HAZ) subjected to

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shorter exposure times in the post weld thermal aging range show small DOS values whereas

high heat input weldments subjected to longer exposure times during aging show relatively

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higher DOS.

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4. Carbide precipitation affects the impact toughness of the weld metal as well as the HAZ of

these joints to a significant extent. Under cryogenic testing conditions, weld metal as well as
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HAZs lose their toughness drastically. This carbide precipitation is found to induce a weakening

effect in the weld metal and the HAZ, which when fractographically examined through SEM
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show that in the extreme case, heavily precipitated grain boundaries of the HAZs create a

condition where the weaker grain boundaries get detached from the matrix, thus leading to poor
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toughness.
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Acknowledgements

The authors gratefully acknowledge the infrastructural support extended in the form of

research facilities by the Welding Metallurgy Laboratory, Mechanical Engineering

Department, Sant Longowal Institute of Engineering and Technology, Longowal, Sangrur

(Deemed University), Punjab, India.

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References

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procedures on bacterial colonization of stainless steel weldments. Journal of Food

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Engineering 1999; 42: 85-96.

[3] Liu W, Wang RJ, Han JL, Xu XY, Li Q. Microstructure and mechanical performance of

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resistance spot welded cold-rolled high strength austenitic stainless steel. Journal of

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Materials Processing Technology 2010; 210: 1956-1961.

[4] Finsgar M, Milosev I. Corrosion behavior of stainless steels in aqueous solutions of

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methanesulfonic acid. Corrosion Science 2010; 52: 2430-2438.

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[6] Bruemmer SM, Charlot LA. Development of grain boundary chromium depletion in type
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304 and 316 stainless steels. Scripta Metallurgica 1986; 20: 1019-1024.
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[7] Park SHC, Sato YS, Kokawa H, Okamoto K, Hirano S, Inagaki M. Corrosion resistance of

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[8] White WE. Observations of the influence of microstructure on corrosion of welded

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[9] Povich MJ. Low temperature sensitization of type 304 stainless steel. Corrosion 1978; 34:

60-65.
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[10] Zumelzu E, Sepulveda J, Ibarra M. Influence of microstructure on the mechanical behavior

of welded 316L SS joints. Journal of Materials Processing and Technology 1999; 94: 36-

40.

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[11] Bruemmer SM, Charlot LA, Bagchi A, Atteridge DG.Influence of grain boundary carbides

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and phosphorus segregation on the low temperature intergranular embrittlement of type 316

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[12] Dadfar M, Fathi MH, Karimzadeh F, Dadfar MR, Saatchi A. Effect of TIG welding on

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corrosion behavior of 316L stainless steel. Materials Letters 2007; 61: 2343-2346.

[13] Cui Y, Lunding CD. Austenite-preferential corrosion attack in 316 austenitic stainless steel
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weld metals. Materials and Design 2007; 28: 324-328.

[14] Cui Y, Lunding CD. Evaluation of initial corrosion location in E316 austenitic stainless
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steel weld metals. Materials letters 2005; 59: 1542-1546.

[15] Mozhi TA, Juhas MC, Wilde BE. Modeling low temperature sensitization of austenitic
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stainless steels. Scripta Metallurgica 1987; 21: 1547-1552.

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[16] ASTM International E23-11. Standard test methods for notched bar impact testing of
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metallic materials.

[17] Tseng T, Gan D, Kao P-W. The effects of grain boundary carbides on the low temperature

impact properties of type 316 stainless steel. Materials Science and Engineering 1987; 95:

73-80.

[18] ASTM International E407-07. Standard practice for microetching metals and alloys.

[19] Lopez N, Cid M, Puiggali M, Azkarate I, Pelayo A. Application of double loop

electrochemical potentiodynamic reactivation test to austenitic and duplex stainless steels.

Materials Science and Engineering A 1997; 229: 123-128.

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[20] Tiedra PD, Martin O, Lopez M. Combined effect of resistance spot welding and post-

welding sensitization on the degree of sensitization of AISI 304 stainless steel. Corrosion

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[21] Cihal V, Stefec R. On the development of the electrochemical potentiokinetic method.

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Electrochemica Acta 2001; 46: 3867–3877.

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double-loop EPR in H2SO4 containing KSCN by Taguchi method. Corrosion Science 2010;

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52: 2653-2660.

[23] Kain V, Chandra K, Adhe KN, De PK. Effect of cold work on low-temperature
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sensitization behavior of austenitic stainless steels. Journal of Nuclear Materials 2004; 334:

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[24] Khatak HS, Raj B. Corrosion of Austenitic Stainless Steels. India: Narosa Publishing

House; 2002, p. 122-128.

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[25] Delong WT. Ferrite in austenitic stainless steel weld metal. Welding Journal 1974; 53:
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273s-286s.
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[26] Gracia C, Tiedra de MP, Blanco Y, Martin O, Martin F. Intergranular corrosion of welded

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[27] Yae Kina A, Souza VM, Tavares SSM, Pardal JM, Souza JA. Microstructure and

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[28] Schino AD, Kenny JM. Effects of the grain size on the corrosion behavior of refined AISI

304 stainless steel. Journal of Materials Science Letters 2002; 21: 1631-1634.
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Figure captions
Fig. 1: Schematic illustration showing the details of the Charpy V-notch impact specimen.
Fig. 2: Schematic illustration showing the cross-section of (X-X) weld metal and (Y-Y) HAZ,
selected from each welded joint for DOS studies.

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Fig. 3: Photomicrograph (at 100X) of the weldments (in the as welded condition) showing the
weld metal (cover pass& the HAZweld pass): (a) & (b) for low heat input; (c) & (d) for medium

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heat input; (e) and (f) for high heat input.

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Fig. 4: Photomicrograph (at 100X) of the weldments (thermally aged condition at 500˚C for 11
days) showing the weld metal (cover pass & the HAZweld pass): (a) & (b) for low heat input; (c) &
(d) for medium heat input; (e) and (f) for high heat input.

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Fig. 5: Photomicrograph (at 100X) of the weldments (thermally aged condition at 650˚C for 24
hours) showing the weld metal (cover pass & the HAZweld pass): (a) & (b) for low heat input; (c) &
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(d) for medium heat input; (e) and (f) for high heat input.

Fig. 6: Photomicrograph (at 100X) of the zone comprising of HAZ (largely), FBZ and epitaxial
growth region of the weld metal(a, b & c): low, medium and high heat input welds respectively,
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in the as welded condition; (d, e, & f): low, medium and high heat input welds respectively,
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thermally aged at 500˚C for 11 days); (g, h & i): low, medium and high heat input welds
respectively, thermally aged at 650˚C for 24 hours).
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Fig. 7: DLEPR curves of the weld metal (in the as welded and under different LTS conditions):
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(a) low heat input weld (b) medium heat input weld (c) high heat input weld.

Fig. 8: DLEPR curves of the weld metal (in the as welded and under different CS conditions): (a)
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low heat input weld (b) medium heat input weld (c) high heat input weld.

Fig. 9: DLEPR curves of the HAZ (in the as welded and under different LTS conditions): (a) low
heat input weld (b) medium heat input weld (c) high heat input weld.

Fig. 10: DLEPR curves of the HAZ (in the as welded and under different CS conditions): (a) low
heat input weld (b) medium heat input weld (c) high heat input weld.

Fig. 11: CVN impact energy results of the weldments (a-weld metal and b-HAZ) showing
toughness variation of the joints welded with different heat inputs (low, medium & high),
subjected to different thermal aging conditions (in the LTS range) and tested at room temperature
(RT) and cryogenic temperature (CT) around -196˚C.

Fig. 12: CVN impact energy results of the weldments (a-weld metal and b-HAZ) showing
toughness variation of the joints welded with different heat inputs (low, medium & high),
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subjected to different thermal aging conditions (in the CS range) and tested at room temperature
(RT) and cryogenic temperature (CT) around -196˚C.

Fig. 13: SEM fractographs (weld metal at 500X) of the CVN impact tested specimens tested at
cryogenic temperature around -196˚C (a, b & c): low, medium and high heat input welds

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respectively, in the as welded condition; (d, e, & f): low, medium and high heat input welds
respectively, thermally aged at 500˚C for 11 days); (g, h & i): low, medium and high heat input
welds respectively, thermally aged at 650˚C for 24 hours). (Scale bar as shown in each

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fractograph is 50 µm).

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Fig. 14: SEM fractographs (HAZ at 500X) of the CVN impact tested specimens tested at
cryogenic temperature around -196˚C (a, b & c): low, medium and high heat input welds
respectively, in the as welded condition; (d, e, & f): low, medium and high heat input welds

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respectively, thermally aged at 500˚C for 11 days); (g, h & i): low, medium and high heat input
welds respectively, thermally aged at 650˚C for 24 hours). (Scale bar as shown in each
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fractograph is 50 µm).
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Fig. 1
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Fig. 2
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a b
Lathy Ferrite Lathy Ferrite

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HAZweld pass
FB

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c d
Skeletal Ferrite Skeletal Ferrite
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HAZweld pass
FB
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e f
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Skeletal Ferrite
Skeletal Ferrite
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HAZweld pass
FB
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Fig. 3
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a b
Lathy Ferrite Lathy Ferrite

HAZweld pass
FB

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IDC

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c d
Skeletal Ferrite
Skeletal Ferrite

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FB

IDC
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e f
Skeletal Ferrite Skeletal Ferrite
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HAZweld pass
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FB
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IDC

Fig. 4
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a b

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Lathy Ferrite Lathy Ferrite

HAZweld pass

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FB

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IDC
IDC

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c d
Skeletal Ferrite
Skeletal Ferrite
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HAZweld pass
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FB
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IDC
IDC
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e f
Skeletal Ferrite
Skeletal Ferrite
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HAZweld pass
FB
IDC

IDC

Fig. 5
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a b c

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WM
FB

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HAZbase metal HAZbase metal
HAZbase metal

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FB
FB
WM WM

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d e f
WM
WM
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FB
FB
WM
HAZbase metal FB
HAZbase metal HAZbase metal
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IGC IGC IGC

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g h i

WM
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WM WM FB
FB FB
HAZbase metal HAZbase metal HAZbase metal

IGC IGC
IGC

Fig. 6
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MA b
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Fig. 7
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b
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Fig. 8
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Fig. 9
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b
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Fig. 10
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(a) Weld metal

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(b) HAZ
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Fig. 11
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(a) Weld metal

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(b) HAZ
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Fig. 12
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a b c
Dimpled Dimpled Dimpled
morphology morphology morphology

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Dimpled

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d Dimpled e morphology f Cracks
morphology Dimpled
River like River like morphology
pattern pattern River like

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pattern

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Crack Cracks
g Dimpled h i Cracks
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morphology
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River like
pattern
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Bright
River like Facets
Flat featureless
pattern
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region

Fig. 13
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a Dimpled b Flat featureless c Dimpled

morphology region morphology

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Dimpled

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Flat featureless morphology Flat featureless
region region

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d Flat featureless e f
region Cracks
Intergranular

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Dimpled star type crack
morphology
Bright
Facets
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Cracks
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g h i
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Intergranular
Intergranular star type crack
Intergranular star type crack Grain
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Cracks separation
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Grain
separation
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Fig. 14
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Table captions

Table 1: Chemical composition of the base and filler material used (wt.%)

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Table 2: Experimental conditions showing different welding heat input combinations used in the

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present work

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Table 3: DLEPR results (DOS values of WM and HAZ in the as-welded as well as different post

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weld thermal aging conditions in the LTS range)

Table 4: DLEPR results (DOS values of WM and HAZ in the as-welded as well as different post
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weld thermal aging conditions in the CS range)
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Table 1: Chemical composition of the base and filler material used (wt.%)

Alloy element C Si Mn P S Cr Mo Ni Ti V Fe
Base 0.025 0.446 1.386 0.028 0.014 18.238 0.296 9.196 0.006 0.061 Balance
(304L SS)

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Filler 0.028 0.421 1.420 0.021 0.012 19.151 0.256 10.02 0.003 0.032 Balance
(308L SS)

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Table 2: Experimental conditions showing different welding heat input combinations used in the

present work

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Average Heat input per Average heat
Welding Welding Welding welding unit input per
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heat Type of passes current voltage speed length per weld unit
input (A) (V) (mm/s) pass length per
(kJ/cm) main weld
pass (kJ/cm)
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Root pass 100 11 1.48 5.2

Low Middle pass 120 13 1.27 8.6 8.7
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Cover pass 120 13 1.24 8.8

Root pass 100 11 1.42 5.4
Medium Middle pass 150 15 1.39 11.3 11.5
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Cover pass 150 15 1.34 11.7

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Root pass 100 11 1.45 5.3

High Middle pass 180 18 1.56 14.5 14.7
Cover pass 180 18 1.51 14.9
*Heat input per unit length, H=η (V*I)/S, where ‘η’ denotes heat transfer efficiency (taken as 0.7 in the
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present case), ‘I’ denotes welding current, ‘V’ denotes voltage and ‘S’ denotes welding speed
Secondary details: Tungsten electrode = EW-Th-2 (Thoriated tungsten) of 2.4 mm diameter, Interpass
temperature = 100˚C, Shielding gas flow rate of industrially pure Argon= 15 L/min, Electrode to work
angle = 45˚, Polarity = DC electrode negative.
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Table 3: DLEPR results (DOS values of WM and HAZ in the as-welded as well as different post
weld thermal aging conditions in the LTS range)

S. No. Weldin Degree of sensitization (DOS=(Ir/Ia)*100)

g heat Weld metal (WM) Heat affected zone (HAZ)

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input As- PWTA treatments As- PWTA treatments
welded LTS LTS LTS welded LTS LTS LTS3
condition 1 2 3 condition 1 2

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1. Low 0.029 0.09 0.48 5.44 0.07 0.18 0.86 6.03
9

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2. Medium 0.13 0.29 0.68 6.25 0.27 0.45 1.92 8.64
3. High 0.34 0.59 0.94 8.15 0.53 0.98 3.84 12.24

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Table 4: DLEPR results (DOS values of WM and HAZ in the as-welded as well as different post
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weld thermal aging conditions in the CS range)

S. No. Weldin Degree of sensitization (DOS=(Ir/Ia)*100)

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g heat Weld metal (WM) Heat affected zone (HAZ)

input As- PWTA treatments As- PWTA treatments
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welded CS1 CS2 CS3 welded CS1 CS2 CS3

condition condition
1. Low 0.029 0.41 7.35 21.5 0.07 0.73 13.3 28.7
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1 9 1
2. Medium 0.13 0.61 9.69 23.2 0.27 1.75 16.1 31.5
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1 1 0
3. High 0.34 1.17 12.9 26.3 0.53 3.42 20.1 36.7
4 3 3 4
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WM Graphical abstract

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Type of weld Microstructures DOS performance Charpy V-notch fractographs

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Low heat
WM Intergranular
input welds

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Cracks
HAZbase metal FB

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IGC

ED
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Intergranular
star type crack
WM
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High heat
FB
input welds Grain
HAZbase metal
separation
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IGC
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Highlights

 Ferrite morphologies affect the sensitization behaviour AISI 304L welds

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 Heat affected zone becomes more prone to carbide precipitation than the weld metal

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 Grain coarsening affects the sensitization behavior of the heat affected zone

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Impact toughness decreases with an increase in degree of sensitization in the welds

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