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Electron Beam Welding of Superduplex Stainless Steel S32750

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<strong>Electron</strong> <strong>Beam</strong> <strong>Welding</strong> <strong>of</strong> <strong>Superduplex</strong><br />

<strong>Stainless</strong> <strong>Steel</strong> <strong>S32750</strong><br />

Presenter:<br />

Parvan Chavdarov<br />

Academic Education and Degrees<br />

Post-graduate student – “Weldability <strong>of</strong> duplex stainless steels”<br />

– Technical University <strong>of</strong> S<strong>of</strong>ia<br />

2001 Master degree on technology <strong>of</strong> metals, Technical<br />

University <strong>of</strong> S<strong>of</strong>ia, Bulgaria<br />

Present pr<strong>of</strong>essional position:<br />

Expert in Industrial Services in TUV Rheinland Bulgaria<br />

Originally presented at the <strong>Stainless</strong> <strong>Steel</strong> World 2007 Conference, Maastricht, the Netherlands


<strong>Electron</strong> <strong>Beam</strong> <strong>Welding</strong> <strong>of</strong> <strong>Superduplex</strong><br />

<strong>Stainless</strong> <strong>Steel</strong> <strong>S32750</strong><br />

Authors: Read.Dr Serafim Serafimov – Technical University <strong>of</strong> S<strong>of</strong>ia<br />

Dipl.eng.Parvan Chavdarov – post-graduate student – TUV Rheinland S<strong>of</strong>ia<br />

Adress: Zona B-19, “Dr Kalinkov” str.18, app.10, S<strong>of</strong>ia, Bulgaria<br />

Post Code 1309, tel. +359 898529051<br />

e-mail: P_Chavdarov@mail.bg<br />

Keywords: duplex stainless steel, welding parameters, ferrite content, microstructure,<br />

intermetallic phases, metallographic analysis<br />

Abstract:<br />

The aim <strong>of</strong> this paper is to present the influence <strong>of</strong> the welding parameters upon the<br />

shape <strong>of</strong> the weld, the microstructure and respectively the precipitation <strong>of</strong> second<br />

phases in superduplex stainless steel <strong>S32750</strong>. Plates with 10mm thickness have been<br />

butt welded with electron beam without filler by altering the heat input. Metallographic<br />

sections have been prepared and the ferrite content in the weld metal has been<br />

measured. The availability <strong>of</strong> intermetallic phases is examined.<br />

Originally presented at the <strong>Stainless</strong> <strong>Steel</strong> World 2007 Conference, Maastricht, the Netherlands


1. Introduction<br />

Duplex stainless steels are a family <strong>of</strong> grades combining good corrosion resistance<br />

with high strength and ease <strong>of</strong> fabrication. Their physical properties are between those<br />

<strong>of</strong> the austenitic and ferritic stainless steels and tend to be closer to those <strong>of</strong> the ferritic<br />

and to carbon steel. These steels are very attractive for various applications because<br />

<strong>of</strong> their advantages:<br />

• Very high corrosion resistance especially against pitting and crevice corrosion in<br />

aggressive media containing chlorides and fluorides;<br />

• Higher mechanical properties (because <strong>of</strong> the ferrite phase) than the austenite<br />

stainless steels which are predominantly used in practice;<br />

• Higher ductility (because <strong>of</strong> the austenitic phase) than the ferrite stainless steels<br />

which reflects on the weldability.<br />

• Better compatibility to C-Mn structural steels, because the coefficients <strong>of</strong> heat<br />

expansion are comparatively close, which results in lower thermal stresses.<br />

All these advantages result in extremely wider usage <strong>of</strong> duplex alloys in many industry<br />

branches like petrochemical, chemical, pulp and paper, <strong>of</strong>f-shore, energy, gas fuel,<br />

mining, shipbuilding, power generations, marine transportations, food manufactures,<br />

etc.<br />

A balanced austenite/ferrite ratio <strong>of</strong> 50/50% is crucial for their high performance.<br />

Compared with normal austenitic steels, duplex steels contain less nickel which<br />

increases its cost-effectiveness considerably. The desire structure is obtained by heat<br />

treatment at approximately 1050 to 1100˚C (solution annealing). The optimum ratio<br />

between both phases can be influenced by the welding processes.<br />

2. Metallurgy <strong>of</strong> duplex stainless steels<br />

2.1 General<br />

Modern duplex stainless steels are characterized by a two phase structure, which<br />

consists <strong>of</strong> a mixture <strong>of</strong> about 50% volume austenite in ferrite grains. Both cast and<br />

wrought products have roughly equivalent volume fractions <strong>of</strong> ferrite and austenite,<br />

which in the case <strong>of</strong> wrought components, contain a rolling texture obtained by hot<br />

working, followed by a solution annealing and quench. The optimum phase balance for<br />

modern wrought products varies between manufacturers, but overall a range <strong>of</strong><br />

between 45% and 60% austenite may be expected.<br />

Fig.1 shows a schematic section <strong>of</strong> the Fe-Cr-Ni diagram at the 70%Fe level. The<br />

phase proportions and their respective compositions are indicated for a given alloy<br />

analysis and annealing temperature, with the high temperature stability <strong>of</strong> the duplex<br />

structure being influenced more by nitrogen content, than by Cr or Mo. The addition <strong>of</strong><br />

0,25%N to a 25%Cr alloy produces a ferrite volume fraction <strong>of</strong> about 50% at 1250˚C,<br />

compared to nearly 80% ferrite with 0,18%N. Nevertheless, it is difficult to predict the<br />

microstructure <strong>of</strong> a duplex alloy from simplified diagrams, due to the effects <strong>of</strong> other<br />

alloy elements, which modify the phase fields.<br />

Originally presented at the <strong>Stainless</strong> <strong>Steel</strong> World 2007 Conference, Maastricht, the Netherlands


Fig.1: Concentration pr<strong>of</strong>iles in<br />

the ternary Fe-Cr-Ni constitution<br />

diagram at 70% and 60%Fe. The<br />

effect <strong>of</strong> nitrogen additions is<br />

shown in the first figure.<br />

2.2 Heat treatment<br />

Numerous structural changes can occur in the duplex stainless steels during<br />

isothermal and anisothermal heat treatments. Most <strong>of</strong> these transformations are<br />

concerned with the ferrite, as element diffusion rates are approximately 100 times<br />

faster than in austenite. This is principally a consequence <strong>of</strong> the less compact lattice <strong>of</strong><br />

the BCC crystal structure. Moreover, the ferrite is enriched in Cr and Mo, which<br />

promote the formation <strong>of</strong> Intermetallic phases. Besides, element solubility in the ferrite<br />

falls with a decrease in temperature, increasing the possibility <strong>of</strong> precipitation during<br />

heat treatment.<br />

Wrought and heat-treated products are considered to be segregation free, but in case<br />

<strong>of</strong> castings and welded joints the element segregation during cooling will affect<br />

precipitation kinetics and the stability <strong>of</strong> phases formed [1].<br />

2.2.1 Temperatures above 1050˚C<br />

Duplex stainless steels solidify completely in the ferrite field for standard grades and<br />

normal cooling rates. This is followed by solid state transformation to austenite (fig.1),<br />

which is naturally reversible, so that any large increase in temperature, for example<br />

from 1050˚C to 1300˚C, leads to an increase in ferrite content. Further, as he<br />

temperature increases, there is a reduction in the portioning <strong>of</strong> substantial elements<br />

between the phases. In addition, the ferrite becomes enriched in interstitial elements<br />

such as carbon and nitrogen.<br />

Heat treatment in the temperature range 1100-1200˚C can have a dramatic influence<br />

on the microstructure <strong>of</strong> a wrought product. The grains can be made equiaxed by<br />

prolonged treatment at high temperature or can be rendered acicular, with a<br />

Widmannstaetten type structure by cooling an intermediate rate. A dual structure,<br />

consisting <strong>of</strong> both coarse and fine austenite grains, can be obtained by step<br />

quenching, with or without simultaneous mechanical strain. These acicular structures<br />

are also encountered in weld deposits.<br />

2.2.2 The 600-1050˚C nose<br />

Originally presented at the <strong>Stainless</strong> <strong>Steel</strong> World 2007 Conference, Maastricht, the Netherlands


The alloy lean grades are the least prone to Intermetallic phase precipitation and<br />

requires exposure <strong>of</strong> at least 10 to 20 hours to initiate formation at temperatures below<br />

900˚C. For that reason, a solution annealing temperature below 1000˚C can be chosen<br />

for this material.<br />

More alloyed grades are more sensitive to precipitation due to the molybdenum<br />

content. This element not only increases the rate <strong>of</strong> Intermetallic precipitation, but also<br />

extents the stability range to higher temperatures. That is why higher solution<br />

annealing temperatures are needed – above 1000˚C.<br />

The superduplex alloys show the greatest propensity for precipitations, due to their<br />

higher Cr, Mo and W contents. However, it should be emphasized that the precipitation<br />

kinetics in these high alloy grades are, at worst, equivalent to the superaustenitic or<br />

superferritic stainless steels [2]. And still, by taking precautions during heat treatment,<br />

including rapid removal from the furnace followed by water quenching, the superduplex<br />

alloys can be used satisfactory in industrial applications. However, especial care is<br />

required for heavy section components during all stages <strong>of</strong> production.<br />

Precipitates re-dissolve during a solution anneal, which for the superduplex grades<br />

must be performed at 1050˚C or above. A few minutes at 1050-1070˚C are sufficient<br />

for grade <strong>S32750</strong>. Similar high temperatures are necessary for welds as consumables<br />

tend to contain higher Ni, Si and Mn contents than base materials. The higher Nicontent<br />

encourages high austenite contents when annealed and results in enrichment<br />

<strong>of</strong> Cr and Mo in the remaining ferrite. This fact, combined with higher Si and Mn levels,<br />

increases the stability <strong>of</strong> Intermetallic phases. And yet, lower annealing temperatures<br />

(1040˚C compared to 1100˚C) can be used for weldments made with matching<br />

consumables [3].<br />

2.2.3 The 300-600˚C nose<br />

The alloy lean grades are the least sensitive to hardening in this temperature range,<br />

and a significant effect is not recorded until about 3 hours exposure to 400˚C. A much<br />

shorter incubation time is found for more alloyed grades, containing molybdenum,<br />

which would appear to accelerate hardening [1]. The 25%Cr and superduplex alloys<br />

show the widest temperature range for hardening and shorter incubation times<br />

accordingly. This is the result <strong>of</strong> both the higher Cr and Mo contents and, if present,<br />

copper additions.<br />

2.2.4 Continuous cooling diagrams<br />

At temperatures near the solvus, the nucleation <strong>of</strong> precipitates is slow and their growth<br />

is fast, whereas the opposite is true at lower temperatures, near the “nose” <strong>of</strong> the<br />

transformation curve. Therefore, it is difficult to avoid phase transformations, such as σ<br />

precipitation, during the reheating <strong>of</strong> heavy section products (for example ingots,<br />

castings, thick plate, etc.), and so a solution treatment should be performed at a<br />

sufficiently high temperature to re-dissolve any such phases. On the other hand, during<br />

cooling, the slow nucleation rate at high temperature and the sluggish growth rate at<br />

lower temperatures make it relatively easy to avoid the formation <strong>of</strong> σ phase, even in<br />

the case <strong>of</strong> air cooling <strong>of</strong> certain castings <strong>of</strong> heavy plate.<br />

2.3 Characteristics and morphology <strong>of</strong> precipitates<br />

Originally presented at the <strong>Stainless</strong> <strong>Steel</strong> World 2007 Conference, Maastricht, the Netherlands


In welds <strong>of</strong> duplex stainless steels some detrimental second phases can occur in the<br />

temperature range <strong>of</strong> 300-1100˚C. The tendency to precipitation depends mainly on<br />

the content <strong>of</strong> alloying elements and therefore, it differs for the different duplex grades.<br />

The precipitation <strong>of</strong> phases is much more typical during heat treatment or welding <strong>of</strong><br />

superduplex steels because <strong>of</strong> the higher content <strong>of</strong> such elements [4]. The following<br />

paragraphs describe the various phases which have been observed in duplex alloys.<br />

Their character and morphology <strong>of</strong> these phases vary considerably, as do the time for<br />

them to form and their influence over the properties.<br />

On fig.2 is given the diagram for the precipitation <strong>of</strong> the various phases for grade<br />

<strong>S32750</strong>. It can be easily seen what is the incubation time for the formation <strong>of</strong> a certain<br />

phase. Details for each phase can be observed in table1<br />

Fig.2: Time-temperature<br />

transformation diagram for alloy<br />

<strong>S32750</strong>.<br />

Particle Chemical formula Cr Ni Mo Formation range, ˚C Lattice type<br />

σ Fe-Cr-Mo 30 4 7 600-1000 tetragonal<br />

χ Fe 36 Cr 12 Mo 10 25 3 14 700-900 BCC- αMn<br />

α’ 65 2,5 13 300-525 BCC<br />

R Fe 2 Mo 25 6 35 550-650 trigonal<br />

π Fe 7 Mo 13 N 4 35 3 34 550-600 cubic<br />

τ 550-650 orthorhombic<br />

ε Cu-rich Not defined<br />

Type 1 same as ferrite ≤ 650<br />

γ 2 Type 2 24,3 11 3,4 650-800 FCC<br />

Type 3 700-900<br />

Cr 2 N 72 6 15 700-950<br />

CrN<br />

cubic<br />

M 7 C 3 950-1050<br />

M 23 C 6 58 2,5 12 650-950 FCC<br />

Table 1: Crystallographic characteristics <strong>of</strong> particles observed in duplex stainless<br />

steels<br />

2.3.1 Intermetallic phases<br />

• Sigma (σ)<br />

Originally presented at the <strong>Stainless</strong> <strong>Steel</strong> World 2007 Conference, Maastricht, the Netherlands


The deleterious Cr, Mo rich σ-phase is a hard embrittling precipitate, which forms<br />

between 650 and 1000˚C, <strong>of</strong>ten associated with a reduction in both impact properties<br />

and corrosion resistance. At the peak temperature <strong>of</strong> around 900˚C, ferrite<br />

decomposition to sigma takes as little as two minutes in superduplex alloys. According<br />

to some authors, the formation <strong>of</strong> sigma phase should be concerned with the<br />

requirement for pre-existing M 23 C 6 particles [5]. Certainly, this phase has been found to<br />

nucleate at temperatures above 750˚C in association with such particles with the<br />

following order <strong>of</strong> preference: δ/γ phase boundaries, austenitised δ/δ sub-grain<br />

boundaries and high energy δ/δ grain boundaries (table 1). These nuclei can grow into<br />

coarse plates, lamellar eutectoid σ + γ 2 (fig.3), or σ + δ lamellar aggregates. In the last<br />

case, the interlamellar ferritic region has a high dislocation density attributed to the<br />

volumetric expansion from δ to σ. Further, in the case <strong>of</strong> phase boundaries, for<br />

instance when δ transforms to γ or γ 2 , the remaining δ becomes enriched in Cr and<br />

Mo, and denuded in Ni, enhancing σ-formation and, for the same reason, growth<br />

progresses into the destabilized ferrite.<br />

Fig.3: SEM micrograph <strong>of</strong> σ + γ 2<br />

eutectoid. <strong>Steel</strong> <strong>S32750</strong> after 72<br />

hours at 700˚C.<br />

The formation <strong>of</strong> sigma is encouraged by the presence <strong>of</strong> Cr, Mo, Si and Mn. Ni is also<br />

found to enhance σ-formation, but reduce the equilibrium volume fraction [6]. This<br />

occurs as Ni induces γ-formation and so concentrates the σ-promoting elements in the<br />

remaining ferrite.<br />

• Chi (χ) phase<br />

Like σ-phase, χ-phase forms between 700 and 900˚C, although in much smaller<br />

quantities. However, enrichment <strong>of</strong> ferrite with intermetallic forming elements during a<br />

long exposure to relatively low temperatures, i.e. 700˚C, favors the precipitation <strong>of</strong> χ-<br />

phase (фиг.2). Like sigma, χ-phase <strong>of</strong>ten forms on the δ/γ boundary and grows into<br />

the ferrite. The cube-cube orientation relationship (table 1) ensures continuity between<br />

χ and the δ-matrix. This phase has similar influence on corrosion and toughness<br />

properties as sigma, but, as both phases <strong>of</strong>ten co-exist, it is difficult to study their<br />

effects individually.<br />

• Alpha prime (α’)<br />

The lowest temperature decomposition within duplex steel is that <strong>of</strong> alpha prime (α’),<br />

which occurs between 300 and 525˚C, and is the main cause <strong>of</strong> hardening and “475<br />

embrittlement” in ferritic stainless steels. It is suggested that α’-formation is a<br />

consequence <strong>of</strong> the miscibility gap in the Fe-Cr system, whereby ferrite undergoes<br />

spinodal decomposition into Fe-rich δ-ferrite (table 1) and a Cr-rich α, or, just outside<br />

the spinodal but still within the gap, classical nucleation and growth <strong>of</strong> α’ occurs. Alpha<br />

prime is <strong>of</strong>ten associated with the co-precipitation <strong>of</strong> Cr 2 N in the form <strong>of</strong> sub-grain<br />

networks <strong>of</strong> Cr 2 N needles interspersed within a film <strong>of</strong> α’.<br />

Originally presented at the <strong>Stainless</strong> <strong>Steel</strong> World 2007 Conference, Maastricht, the Netherlands


• R, π, и τ phases<br />

R phase, also known as Laves, (Fe 2 Mo) precipitate in small quantities between 550<br />

and 650˚C after several hours exposure (table 1) [1]. They form at both intra- and<br />

intergranular sites, are molybdenum-rich and reduce pitting corrosion resistance.<br />

However, as those that precipitate at intergranular sites contain slightly more Mo (40%<br />

compared to 35%Mo), their influence on pitting resistance is more considerable.<br />

The π-nitride has been identified at intragranular sites in duplex weld metal after<br />

isothermal heat treatment at 600 ˚C for several hours [7]. It is Cr Mo rich and so has<br />

been previously confused with σ-phase.<br />

Heat treatment for several hours in the temperature range 550 to 650˚C (table 1) can<br />

lead to the formation <strong>of</strong> the heavily faulted needle-like τ-phase on δ/δ boundaries [8].<br />

• Cu-rich epsilon (ε) phase<br />

In alloys containing copper and/or tungsten, other hardening mechanisms can occur.<br />

In the case <strong>of</strong> Cu, the super saturation <strong>of</strong> the ferrite due to the decrease in solubility at<br />

lower temperature leads to the precipitation <strong>of</strong> extremely fine Cu-rich ε-phase particles<br />

after 100 hours at 500˚C, which significantly extend the low temperature hardening<br />

range <strong>of</strong> the duplex grades. Although the reported temperature range for their<br />

formation varies, it would seem that they all form in the same temperature regime as<br />

γ 2 .<br />

2.3.2 Secondary austenite (γ 2 )<br />

Secondary austenite can form relatively quickly and by various mechanisms depending<br />

on the temperature (table 1). About 650˚C, γ 2 has similar composition as the<br />

surrounding ferrite, suggesting a diffusionless transformation, with characteristics<br />

similar to martensite formation [9].<br />

At temperature range 650 and 800˚C where diffusion is faster, many Widmanstaetten<br />

austenite forms can precipitate (fig.4). In this range, γ 2 obeys the Kurdjumov-Sachs<br />

relationship, its formation involves diffusion as it is enriched in Ni compared to the<br />

ferrite matrix (table 1). Even though there is some enrichment <strong>of</strong> N in γ 2 compared to<br />

the matrix, both Cr and N contents <strong>of</strong> γ 2 are substantially below that <strong>of</strong> primary<br />

austenite.<br />

Fig.4: Optical micrograph <strong>of</strong> γ 2 in<br />

superduplex welds, x1000. Etch:<br />

electrolytic sulphuric acid.<br />

Originally presented at the <strong>Stainless</strong> <strong>Steel</strong> World 2007 Conference, Maastricht, the Netherlands


In the 700-900˚C range, a eutectoid <strong>of</strong> γ 2 + σ can form (fig.3), as γ 2 absorbs and<br />

rejects Cr and Mo, encouraging Cr, Mo-rich precipitates, such as sigma phase.<br />

Similarly, one form <strong>of</strong> γ 2 which forms at δ/γ boundaries is found to be depleted in Cr.<br />

Either <strong>of</strong> these diffusion controlled reactions can render the area susceptible to pitting<br />

corrosion.<br />

2.3.3 Carbides M 23 C 6 and M 7 C 3<br />

M 7 C 3 forms between 950 and 1050˚C (fig.2) at the δ/γ grain boundaries. However, as<br />

its formation takes 10 minutes, it can be avoided by normal quenching techniques.<br />

Further, as modern duplex grades contain less that 0,02%C, carbides are rarely if ever<br />

seen [10].<br />

In duplex grades with moderately high carbon levels, like <strong>S32750</strong>, <strong>of</strong> about 0,03%, the<br />

carbide M 23 C 6 rapidly precipitates between 650 and 950˚C (fig.2), requiring less that 1<br />

minute to form at 800˚C. Precipitation predominantly occurs at δ/γ boundaries, where<br />

Cr-rich ferrite intersects with carbon rich austenite. This type <strong>of</strong> carbide can be found<br />

also at the δ/δ and γ/γ boundaries and to a lesser degree inside he ferrite and<br />

austenite grains. Several precipitate morphologies have been recorded including<br />

cuboidal and aciculat particles, as well as a cellular form, although each type will have<br />

an associated Cr depleted zone in its vicinity.<br />

2.3.4 Nitrides Cr 2 N and CrN<br />

Nitrogen is added to duplex alloys to stabilize the austenite, and to improve strength<br />

and pitting resistance. The solubility <strong>of</strong> N is considerably higher in austenite than in<br />

ferrite, and has been shown to partition to the former phase. Above the solution<br />

annealing temperature (about 1040˚C), the volume fraction <strong>of</strong> ferrite increases, until<br />

just below the solidus a completely ferritic microstructure can be present, though in the<br />

in the higher alloy grades some austenite may remain. At these temperatures, the N<br />

stability in ferrite is high, but on cooling the solubility drops and the ferrite becomes<br />

supersaturated in N, leading to the intragranular precipitation <strong>of</strong> needle-like Cr 2 N. In a<br />

similar manner, Cr 2 N is most likely to form after higher solution heat treatment<br />

temperatures and forms rapidly even if quenched from such temperatures [11].<br />

<strong>Welding</strong> process favors the formation <strong>of</strong> another nitride in the heat-affected zone: the<br />

cubic CrN, table.1.<br />

Isothermal exposure to the 750-900˚C temperature range (fig.2), produces<br />

intergranular Cr 2 N at δ/δ grain boundaries as thin plates on sub-grain boundaries,<br />

triple points and inclusions. The latter form <strong>of</strong> Cr 2 N has been stated to affect pitting<br />

corrosion [10].<br />

2.4 <strong>Electron</strong> beam welding <strong>of</strong> duplex steels<br />

Normally duplex steels are weldable using welding procedures generally used for high<br />

alloyed steels. The experience with such comparatively new welding method like<br />

electron beam welding is still limited. However, there have been a few successful<br />

Originally presented at the <strong>Stainless</strong> <strong>Steel</strong> World 2007 Conference, Maastricht, the Netherlands


applications and there is every reason to expect that procedures will be developed<br />

more fully. <strong>Electron</strong> beam welding is especially suited to produce joints <strong>of</strong> heavy<br />

section materials in one or two passes. Unfortunately, it tends to produce rapid cooling<br />

rates and therefore highly ferrite in the melt zone, particularly in thin sections [12].<br />

Nevertheless, the toughness remains high which can be attributed to the very low<br />

oxygen content in the weld. Still the qualification <strong>of</strong> the procedure must be alert to the<br />

possibility <strong>of</strong> excessive ferrite in the HAZ and even in the weld when the high speed<br />

welding capabilities <strong>of</strong> these methods are considered.<br />

Special feature <strong>of</strong> this welding method is the formation <strong>of</strong> the welding pool and bead.<br />

Because <strong>of</strong> the high temperature and concentration <strong>of</strong> energy, peculiar gas-steam<br />

channel in the welded metal is created. The electron beam continues to penetrate<br />

through this channel to bigger depth and thus it is possible thicknesses up to 200 mm<br />

to be fully penetrated with minimum width <strong>of</strong> the weld. This is a prerequisite for the<br />

formation <strong>of</strong> the so called “dagger” form <strong>of</strong> the weld (fig.5)<br />

Fig. 5: Formation <strong>of</strong> “dagger” form <strong>of</strong> the bead.<br />

In this case the ration between the penetration<br />

depth and the weld width is 3,6:1 (10:2,75), but it can<br />

much bigger (50:1).<br />

3. Experimental results<br />

3.1 <strong>Welding</strong> machine<br />

Installation LEYBOLD-HERAEUS EWS-1560 has been used for the welding. The<br />

sketch <strong>of</strong> the experimental configuration is shown on fig.6<br />

Fig.6<br />

1 – Devices for computer driven control;<br />

2 – <strong>Electron</strong> gun;<br />

3 – Source for acceleration;<br />

4 – Cathode feed;<br />

5, 6, 7 – Deflection/focus coils;<br />

8 – Leading;<br />

9 – Vacuum chamber.<br />

Originally presented at the <strong>Stainless</strong> <strong>Steel</strong> World 2007 Conference, Maastricht, the Netherlands


This electron beam machine is a conventional one. It is composed <strong>of</strong> an electron beam<br />

gun, a power supply, control system, motion equipment and vacuum welding chamber.<br />

The fusion <strong>of</strong> the base metals eliminates the need for filler material. Besides, the<br />

vacuum requirement for operation <strong>of</strong> the electron beam equipment eliminates the need<br />

for shielding gases and fluxes.<br />

The electron beam gun has a tungsten filament which is heated, freeing electrons. The<br />

electrons are accelerated from the source with high voltage potential between a<br />

cathode and anode. The stream <strong>of</strong> electrons then pass through a hole in the anode.<br />

The beam is directed by magnetic forces <strong>of</strong> focusing and deflecting coils. This beam is<br />

directed out <strong>of</strong> the gun column and strikes the workpiece.<br />

The potential energy <strong>of</strong> the electrons is transferred to heat upon impact <strong>of</strong> the<br />

workpiece and cuts a perfect hole at the weld joint. Molten metal fills in behind the<br />

beam, creating a deep finished weld.<br />

The electron beam stream and workpiece are manipulated by means <strong>of</strong> precise,<br />

computer driven controls, within a vacuum welding chamber <strong>of</strong> 0,5m 3 , and thus<br />

eliminating oxidation and contamination.<br />

3.2 <strong>Welding</strong> details<br />

Plates from superduplex stainless steel <strong>S32750</strong> with thickness <strong>of</strong> 10mm have been<br />

butt welded with electron beam without filler material and in one pass. As a result, six<br />

welds are accomplished and for each <strong>of</strong> them the heat input is different. For the first<br />

three welds the parameter which values are being changed is the welding speed<br />

(mm/s) in order to observe its influence over the weld shape and the percentage <strong>of</strong> the<br />

ferrite phase in the weld and the heat-affected zone. On the contrary, the other plates<br />

are welded with one and the same welding speed, but with different current. The idea<br />

is to be found out what is the minimum value <strong>of</strong> the welding current that secures full<br />

penetration. The welding regimes are given in table 2.<br />

Weld No Voltage, kV <strong>Welding</strong> Current, mA <strong>Welding</strong> Speed, mm/s Heat Input, kJ/mm<br />

1 53 45 10 0,24<br />

2 53 45 15 0,16<br />

3 53 45 25 0,10<br />

4 53 52 15 0,18<br />

5 53 65 15 0,23<br />

6 53 75 15 0,27<br />

Table 2: <strong>Welding</strong> parameters<br />

3.3 Influence <strong>of</strong> the welding parameters over the shape <strong>of</strong><br />

the welds<br />

For each weld macroscopic analysis has been done in order to be studied he influence<br />

<strong>of</strong> the welding parameters over the shape <strong>of</strong> the welds (penetration depth,<br />

Originally presented at the <strong>Stainless</strong> <strong>Steel</strong> World 2007 Conference, Maastricht, the Netherlands


einforcement height and the weld width). The etching is done by a mixture <strong>of</strong> 10 ml<br />

HNO 3 , 20 ml HCl and 30 ml H 2 O for 3-4 minutes depending on the temperature <strong>of</strong> the<br />

solution.<br />

Оn fig.7 is shown how the width <strong>of</strong> the weld (B) changes with the increase/decrease <strong>of</strong><br />

the welding speed (V w ) and the current (I) accordingly with constant voltage (U=const)<br />

in both cases.<br />

U=const, I=const<br />

B(mm)<br />

V w(mm/s)<br />

1,1 25<br />

1,55 15<br />

2,75 10<br />

B(mm)<br />

3.0<br />

2.8<br />

2.6<br />

2.4<br />

2.2<br />

2.0<br />

1.8<br />

1.6<br />

1.4<br />

1.2<br />

1.0<br />

8 10 12 14 16 18 20 22 24 26<br />

V(mm/s)<br />

Fig.7: Influence <strong>of</strong> V w on the weld width<br />

U=const, V w=const<br />

B(mm)<br />

I(mA)<br />

1.75 52<br />

1,8 65<br />

2,0 75<br />

B (m m )<br />

2.5<br />

2.4<br />

2.3<br />

2.2<br />

2.1<br />

2.0<br />

1.9<br />

1.8<br />

1.7<br />

1.6<br />

50 55 60 65 70 75<br />

I(mA)<br />

Fig.8: Influence <strong>of</strong> I on the weld width<br />

In the same way, the effect <strong>of</strong> changing the welding speed (V w ) and current (I) over the<br />

reinforcement height (H r ) and the penetration depth (H pen ) is studied and depicted on<br />

the following four fig.9-fig.12. The voltage again is constant – U=53 kV.<br />

U=const, I=const<br />

H r (mm)<br />

V w(mm/s)<br />

1.2 25<br />

1,3 15<br />

1,8 10<br />

Originally presented at the <strong>Stainless</strong> <strong>Steel</strong> World 2007 Conference, Maastricht, the Netherlands


Hус(mm)<br />

1.8<br />

1.7<br />

1.6<br />

1.5<br />

1.4<br />

1.3<br />

1.2<br />

8 10 12 14 16 18 20 22 24 26<br />

Vз(mm/s)<br />

Fig.9: Influence <strong>of</strong> V w on the reinforcement height<br />

U=const, V w=const<br />

H r (mm)<br />

I(mA)<br />

1,45 52<br />

1,65 65<br />

1,70 75<br />

Hус(mm)<br />

1.70<br />

1.65<br />

1.60<br />

1.55<br />

1.50<br />

1.45<br />

50 55 60 65 70 75<br />

Iз(mA)<br />

Fig.10: Influence <strong>of</strong> I on the reinforcement height<br />

U=const, I=const<br />

H pen (mm)<br />

V w(mm/s)<br />

5,1 25<br />

6,3 15<br />

10,0 10<br />

Hпр(mm)<br />

10<br />

9<br />

8<br />

7<br />

6<br />

5<br />

8 10 12 14 16 18 20 22 24 26<br />

Vз(mm/s)<br />

Fig.11: Influence <strong>of</strong> V w on the penetration depth<br />

U=const, V w=const<br />

H pen (mm) I(mA)<br />

7,15 52<br />

7,60 65<br />

Originally presented at the <strong>Stainless</strong> <strong>Steel</strong> World 2007 Conference, Maastricht, the Netherlands<br />

8,45 75


Hпр(mm)<br />

8.6<br />

8.4<br />

8.2<br />

8.0<br />

7.8<br />

7.6<br />

7.4<br />

7.2<br />

7.0<br />

50 55 60 65 70 75<br />

Iз(mA)<br />

Fig.12: Influence <strong>of</strong> I on the penetration depth<br />

The experiments have proved something which is known for a long time, namely that<br />

with the increase <strong>of</strong> the welding speed (it varies from 10 to 25 mm/s) under constant<br />

other circumstances, the values <strong>of</strong> all parameters pertaining to the shape <strong>of</strong> the weld<br />

diminish. The biggest influence has been exerted on the width <strong>of</strong> the weld – from<br />

2,75mm to 1,1mm. Certainly this is not a surprise, because the higher the speed is, the<br />

less the heat input is. At the same time the penetration depth also becomes much<br />

smaller – from full penetration to 5,1mm, i.e. two times decrease. The smallest<br />

modification refers to the reinforcement height – 40%.<br />

The effect <strong>of</strong> growing the welding current on the shape <strong>of</strong> the weld is just the opposite<br />

from what was said for the welding speed. With the increase <strong>of</strong> the current (from 52 to<br />

75mA), all above mentioned parameters grow bigger, as the ratio is almost the same<br />

for all <strong>of</strong> them.<br />

3.3 Ferrite content in the weld and the base metal<br />

It is well known that the duplex stainless steels solidify as ferrite and some <strong>of</strong> them<br />

transforms to austenite as the temperature falls to about 1000˚C depending on alloy<br />

composition. There is little further change in the ferrite-austenite balance at lower<br />

temperatures. In case <strong>of</strong> welding the metallurgical processes are less equilibrium than<br />

during heat treatment, because the heating, respectively the cooling rate are very high<br />

and there is no enough time for the diffusion to make the composition uniform<br />

throughout the whole volume.<br />

Bearing in mind how decisive the ferrite content is for the mechanical and corrosion<br />

properties <strong>of</strong> the duplex grades, it was measured for all six welds. Conclusions are<br />

made about the influence <strong>of</strong> the welding regime (welding parameters) over this<br />

criterion, therefore over the properties <strong>of</strong> the steels in question.<br />

For the measurement <strong>of</strong> the ferrite content a ferritoscope ‘Foerster-1.053’ has been<br />

used. An additional graduation is made in order to be increased the measuring scope<br />

<strong>of</strong> the apparatus. After changing the distance between the measuring inductive drill<br />

and the surface <strong>of</strong> the examined sample by means <strong>of</strong> a non-metallic folio with 0,5mm<br />

thickness, the power <strong>of</strong> the measured signal has been altered and the possibility for<br />

Originally presented at the <strong>Stainless</strong> <strong>Steel</strong> World 2007 Conference, Maastricht, the Netherlands


the measurement <strong>of</strong> the ferrite content has been increased to 100%. Thus the scope is<br />

raised, but the sensibility <strong>of</strong> the apparatus becomes smaller.<br />

The results from the measurements <strong>of</strong> the ferrite phase in the welds are ordered in<br />

table 3.<br />

Weld No<br />

Ferrite content in the welds, %<br />

Measurement results<br />

Mean value<br />

1 63, 65, 57, 60 63,75<br />

2 65, 60, 66, 62 63,25<br />

3 50, 55 52,50<br />

4 58, 60, 58, 53 57,25<br />

5 57, 55, 60, 58 57,50<br />

6 58, 50 54,00<br />

Table 3: Ferrite content in the welds<br />

The ferrite content at the fusion boundaries is given in table 4.<br />

Fusion boundary Ferrite content at the fusion boundaries, %<br />

for Weld No Measurement results Mean value<br />

1 43, 48, 47, 45, 46, 48, 43, 45, 44 45,44<br />

2 45, 44, 46, 48, 43, 45, 44, 43, 38 44,00<br />

3 50, 48, 50, 53, 49, 48, 45 49,00<br />

4 47, 47, 43, 45, 43, 45, 48, 48, 44 45,55<br />

5 44, 44, 38, 45, 46, 53, 45, 45 45,00<br />

6 44, 47, 46 45,67<br />

Table 4: Ferrite content at the fusion boundaries<br />

The relevant values <strong>of</strong> this phase in the base metal are presented in the following table<br />

5.<br />

Ferrite content in the base metal, %<br />

Measurement results<br />

Mean value<br />

38, 37, 40, 45, 42, 44, 38, 41 40,63<br />

Table 5: Ferrite content in the base metal<br />

The difference in the ferrite content pertaining to the welds, the fusion lines and the<br />

base metal is obvious. It is most in the welds, because the cooling rate is highest in<br />

these zones and the transformation from ferrite to austenite is impeded at low<br />

temperatures. As a result, more quantities <strong>of</strong> high-temperature ferrite can be observed<br />

in the structure. On the other hand the initial balance between both phases is disrupted<br />

also in the heat affected zones (which for the electron beam welding are very thin<br />

zones, like a line), but not to this extent like in the welds. That is why the mean value <strong>of</strong><br />

the ferrite content in the HAZ is smaller than in the weld, but still is bigger in<br />

comparison with the base metal.<br />

Originally presented at the <strong>Stainless</strong> <strong>Steel</strong> World 2007 Conference, Maastricht, the Netherlands


3.4 Metallographic analysis<br />

Metallographic analysis on preliminary prepared five sections from duplex steel<br />

<strong>S32750</strong> has been performed. For that purpose an optical microscope Leica DM6000M<br />

which allows optical magnification x2000 has been used. The sections are prepared<br />

(coarse and fine grinding with subsequent polishing) with Struers. The testing has<br />

been done in accordance with BDS EN 3690 (Visual-optical Methods) and BS EN<br />

1321 (Normal and Special Metallographic Analysis).<br />

Object <strong>of</strong> analysis for every section has been the weld, the fusion boundary and the<br />

base metal.<br />

3.4.1 Microstructures<br />

• Weld 1<br />

a b c<br />

d<br />

e<br />

Fig.13: Microstructure in the weld under different magnifications: a-c) x200; d) x500; e)<br />

x1000<br />

a<br />

b<br />

Originally presented at the <strong>Stainless</strong> <strong>Steel</strong> World 2007 Conference, Maastricht, the Netherlands


Fig.14: Microstructure at the boundary between the weld and the base metal under<br />

different magnifications: a) x200; b) x500<br />

• Weld 2<br />

a<br />

b<br />

Fig.15: Microstructure in the weld under different magnifications: a-c) x200; b) x1000;<br />

c) x1500<br />

a b c<br />

Fig.16: Microstructure at the boundary between the weld and the base metal under<br />

different magnifications: a) x500; b-c) x1000<br />

Fig.17: Microstructure in the base metal x1000<br />

• Weld 3<br />

Originally presented at the <strong>Stainless</strong> <strong>Steel</strong> World 2007 Conference, Maastricht, the Netherlands


a b c<br />

Fig.18: Microstructure in the weld under different magnifications: a) x750; b) x1000; c)<br />

x2000<br />

a b c<br />

Fig.19: Microstructure at the boundary between the weld and the base metal under<br />

different magnifications: a) x200; b) x1000; c) x2000<br />

Fig.20: Microstructure in the base metal x200<br />

• Weld 4<br />

a b c<br />

Fig.21: Microstructure in the weld under different magnifications: a) x200; b) x1000; c)<br />

x2000<br />

Originally presented at the <strong>Stainless</strong> <strong>Steel</strong> World 2007 Conference, Maastricht, the Netherlands


a b c<br />

Fig.22: Microstructure at the boundary between the weld and the base metal under<br />

different magnifications: a) x750; b) x1000; c) x2000<br />

Fig.23: Microstructure in the base metal x200<br />

• Weld 5<br />

a b c<br />

Fig.24: Microstructure in the weld under different magnifications: a) x200; b) x1000; c)<br />

x2000<br />

a b c<br />

Originally presented at the <strong>Stainless</strong> <strong>Steel</strong> World 2007 Conference, Maastricht, the Netherlands


Fig.25: Microstructure at the boundary between the weld and the base metal under<br />

different magnifications: a) x500; b) x750; c) x1000<br />

• Weld 6<br />

a b c<br />

Fig.26: Microstructure in the weld under different magnifications: a) x500; b-c) x1000<br />

a b c<br />

Fig.27: Microstructure at the boundary between the weld and the base metal under<br />

different magnifications: a) x200; b) x1000; c) x2000<br />

3.4.2 Results<br />

• For all probes (welded with different regimes <strong>of</strong> electron beam welding) a typical<br />

structure with five distinguished zones can be observed (fig.28):<br />

Zone1<br />

1<br />

Zone2 Zone3 Zone4 Zone5<br />

- Zone 1 – coarse grains in the middle<br />

part <strong>of</strong> the weld;<br />

- Zone 2 – strongly prolonged through<br />

the front <strong>of</strong> the grains;<br />

- Zone 3 – dispersive structure at the<br />

boundary with the base metal;<br />

- Zone 4 – fusion boundary;<br />

- Zone 5 – base metal.<br />

Originally presented at the <strong>Stainless</strong> <strong>Steel</strong> World 2007 Conference, Maastricht, the Netherlands<br />

Fig.28: Microstructure at the<br />

boundary weld – base metal, х200


• The base metal has ferrite-austenite structure with ratio between both phases close<br />

to 50%-50% and with a texture <strong>of</strong> the grains (fig.29). Non-metallic inclusions are<br />

not outlined in the section field.<br />

a<br />

b<br />

Fig.29: Microstructure <strong>of</strong> base metal: a) x200 (weld 3); b) х1000 (weld 4)<br />

• The weld structure is non-equal and consists <strong>of</strong> grains with different sizes, which is<br />

a result <strong>of</strong> the different speed <strong>of</strong> heat-conduction in the material. In all welds the<br />

formation <strong>of</strong> skeleton-like structure can be seen (fig.30). Under big metallographic<br />

magnifications (х1000, х2000) the structures which set up this skeleton are clearly<br />

discernable. On the periphery <strong>of</strong> the grains (1) white zones can be observed (2)<br />

and at the boundaries – needle-shaped precipitations (3).<br />

1<br />

2<br />

3<br />

а<br />

b<br />

1<br />

2<br />

3<br />

c<br />

d<br />

Fig.30: Microstructure in weld, х1000:<br />

Originally presented at the <strong>Stainless</strong> <strong>Steel</strong> World 2007 Conference, Maastricht, the Netherlands


а) weld 5; b) weld 4; c), d) weld 1<br />

Main phase component in the welds is δ-ferrite. Inside the δ-ferrite grains<br />

precipitations <strong>of</strong> γ 2 are registered and at the boundaries – austenite, which has<br />

particularly a Widmannstaeten structure. Intermetallic phases like σ-type are not<br />

registered upon using metallographic analysis.<br />

• The formed heat affected zone (zone 4) is very thin (10-35µm) and is visible as a<br />

boundary between the weld and the base metal. The microstructure in this zone is<br />

identical as the one in the base metal. Intermetallic phases are not registered.<br />

• In most <strong>of</strong> the welds some typical for electron beam welding imperfections in the<br />

root are visible – porosity, non-uniform surface, etc.<br />

Originally presented at the <strong>Stainless</strong> <strong>Steel</strong> World 2007 Conference, Maastricht, the Netherlands


4. Conclusions<br />

• With the increase <strong>of</strong> the welding speed all parameters which pertain to the<br />

shape <strong>of</strong> the weld, namely penetration depth, weld width and reinforcement<br />

height, become smaller because <strong>of</strong> the low heat input. This speed should be<br />

chosen very carefully, because there is a risk <strong>of</strong> lack <strong>of</strong> penetration if it is too<br />

high.<br />

• The influence <strong>of</strong> the welding current over the shape <strong>of</strong> the weld is the following<br />

– the higher the current is, the bigger are the geometrical dimensions <strong>of</strong> the<br />

weld.<br />

• The ferrite content in the weld is bigger that the relevant one in the heataffected<br />

zone and the base metal, because the structure is not equilibrium in<br />

the weld. In comparison with the heat treatment, the welding processes are<br />

faster, the cooling rate is higher and the time for diffusion is shorter. As a<br />

result <strong>of</strong> this, high-temperature condition is fixed at lower temperatures.<br />

• The ferrite content in the weld is more when the heat input is less, for example<br />

when the welding speed is higher or the current is lower than some initial<br />

values.<br />

• The heat-affected zone in the materials, which are welded with electron beam<br />

is very thin, <strong>of</strong> the order <strong>of</strong> some µm. This is an advantage for this welding<br />

method, because very small part <strong>of</strong> the base metal is affected by the welding<br />

process.<br />

• The measurement <strong>of</strong> the ferrite in the base metal has shown that the volume<br />

<strong>of</strong> this phase is the range which is given in the literature – between 40% and<br />

60% in annealed and quenched condition.<br />

• The initial position <strong>of</strong> the plates is annealed to 1050˚C and quenched in order<br />

to be re-dissolved all second phases in the structure. In comparison with the<br />

ferritic stainless steels, duplex alloys are famous with the slower diffusion rate,<br />

i.e. the incubation time for the phase precipitation is longer. This means that<br />

the “nose” <strong>of</strong> the curve is translated to the right.<br />

• The review <strong>of</strong> the metallographic photos has not shown the precipitation <strong>of</strong><br />

intermetallic phases. The explanation <strong>of</strong> this fact can be found in the timetemperature<br />

transformation diagram. According to this diagram the incubation<br />

time is enough long to secure that no phases will precipitate. Therefore<br />

electron beam welding is proper for welding <strong>of</strong> duplex stainless steel <strong>S32750</strong><br />

for the lack <strong>of</strong> second phases in the microstructure which could affect<br />

embrittlement and reduction in the corrosion resistance.<br />

• The more alloyed is one duplex grade, the more susceptible it is to the<br />

precipitation <strong>of</strong> second phases. That is to say the standard duplex stainless<br />

grades are more susceptible to the precipitation than the lean ones. The<br />

chance these phases to form in the high alloyed grades are much bigger than<br />

in the standard steels. The superduplex alloys show the greatest propensity<br />

for precipitations, due to their higher Cr, Mo and W contents.<br />

Originally presented at the <strong>Stainless</strong> <strong>Steel</strong> World 2007 Conference, Maastricht, the Netherlands


5. References<br />

[1] Charles J: Proc conf Duplex <strong>Stainless</strong> <strong>Steel</strong>s ’91, Beaune, 1991, Vol.1, 3-48.<br />

[2] Mancia F, Barteri M, Sasseth L, Tamba A, Lannaioli A: York ’87, vide ref.11,<br />

160-167.<br />

[3] Gunn R: Duplex <strong>Stainless</strong> <strong>Steel</strong>s, Woodhead Publishing, 2003.<br />

[4] Leif Karlson: Intermetallic Phase Precipitation in Duplex <strong>Stainless</strong> <strong>Steel</strong>s and<br />

Weld Metals. Metallurgy, Influence on Properties, <strong>Welding</strong> and Testing Aspects. Doc.<br />

IX-1920-98.<br />

[5] Goldsmith HJ: Interstitial Alloys, Plenum Press, 1967, 167.<br />

[6] Maehara Y, Ohmori Y, Murayama J, Fujino N: Metal Science 17, 1983, 541.<br />

[7] Nilsson J-O, Liu P: Mater Sci Technol 7, 1991, 853.<br />

[8] Redjaimia A, Metauer G, Gantois M: Beaune ’91, vide ref.2, Vol.1, 119-126.<br />

[9] Soulignac P, Dupoiron F: <strong>Stainless</strong> <strong>Steel</strong> Europe 2, 1990, 18-21.<br />

[10] Nilsson J-O: Materials Science and Technology 8, 1992, 685-700.<br />

[11] Herzman S, Roberts W, Lindenmo M: The Hague ’86, vide ref. 7, paper 30,<br />

257-267.<br />

[12] Bonnefois B, Charles J, Dupoiron F, Soulignac P: Proc conf Duplex <strong>Stainless</strong><br />

<strong>Steel</strong>s ’91, Beaune, France, Oct. 1991, Vol.1, 347-362;<br />

Originally presented at the <strong>Stainless</strong> <strong>Steel</strong> World 2007 Conference, Maastricht, the Netherlands

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