P. CHAKRABORTY et al.

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EFFECT OF MAGNETIC FIELD ON THE CORROSION

BEHAVIOR OF INDIAN RAFMS IN LIQUID Pb-Li

P. Chakraborty a,*, V. Singh

a, P. Trivedi

b, S. Malhotra

b, K. Singh

a, V. Kain

c and R. Tewari

a

a Material Science Division,

b Accelerator Control Division,

c Materials Processing and Corrosion Engineering

Division,

Bhabha Atomic Research Centre, Mumbai 400085, India

*poulamic@barc.gov.in

Abstract

In the present study, the effect of magnetic field on the corrosion of Indian Reduced Activation Ferritic Martensitic Steel

(IN RAFMS) in flowing lead lthium eutectic (Pb-Li) has been studied in an electromagnetic pump driven loop (EMPPIL-M). The

loop was operated for 2,800 h at an average flow velocity of 1.5 m/s with a 0.5 KG (T) magnetic field introduced over the IN

RAFMS samples. The corrosion rate in the presence of magnetic field at temperature of 773 K has been found to be 1.3 times

higher than that observed in the absence of magnetic field. The exposed samples have been charachterized by various techniques

like stereomicroscopy, optical profilometry, optical and secondary electron microscopy and energy dispersive spectroscopy. The

surface of the sample located inside the magnetic field showed non uniform corroison and formation of distinct surface features.

Pb-Li attack in the presence of magnetic field was not only confined to the prior austenite and martensitic lath boundaries as in

the absence of magnetic field; but also happened in the intra-lath regions causing formation of subgrains. The change in Pb-Li

flow profile due to magneto-hydrodynamic effect is expected to play a major role in the formation of surface features, non

uniformity in surface attack and increased corrosion rate in the presence of magnetic field. On the other hand, an increase in the

depletion of iron from the steel matrix noted inside magnetic field was a result of its direct interaction with the field parameters.

1. INTRODUCTION

Corrosion of structural materials with lead-lithium eutectic (Pb-Li) is a major area of concern while designing Pb-Li

cooled blankets for fusion reactor [1-2]. Along with high temperatures (~753-823 K) in these systems; the structural

materials and flowing Pb-Li come under the direct influence of magnetic field which is used for confining the fusion

plasma [3-4]. It is thus important to study the effect of magnetic field on the corrosion of these materials in Pb-Li

and also understand the underlying corrosion mechanism [5-7]. Some studies have been earlier conducted on the

effect of magnetic field over the corrosion behavior of EUROFER and modified 9Cr-1Mo steel (P91) in flowing Pb-

Li [8-10]. Both these materials showed non uniform corrosion in the presence of magnetic field leading to the

formation of wavy lines on their surface [8-9]. Through various theoretical analyses on the Pb-Li exposure data of

EUROFER samples, R. Morreu et al. predicted that the key phenomenon behind corrosion inside magnetic field was

the dissolution of iron into Pb-Li [11]. However, not much experimental proof of this phenomenon has been

obtained or detailed investigation of the microstructural aspect of Pb-Li attack inside magnetic field has been carried

out. To explore this issue, a forced circulation Pb-Li loop coupled to a permanent magnet (EMPPIL-M) was

installed at BARC, Mumbai. Samples of Indian Reduced Activation Ferritic Martensitic Steel (IN RAFMS) were

exposed in Pb-Li, flowing transverse to the magnetic field and at a temperature of 773 K. The experiment was

conducted for a continuous run of 2,800 h. The exposed samples were then investigated in detail to study their

corrosion behavior.

2. EXPERIMENTAL

An electromagnetic pump driven Pb-Li loop (EMPPIL) had been already installed at BARC for conducting

corrosion experiments in flowing Pb-Li [12]. In order to conduct preliminary Pb-Li corrosion experiments in the

presence of magnetic field, the existing EMPPIL facility was modified and coupled with a 0.5 T Dipole (permanent)

magnet to form a new loop called EMPPIL-M. The schematic diagram of EMPPIL-M fabricated out of SS316L

material is shown in Figure 1. A dipole magnet (0.5 KG or 0.5 T) was installed over a support base such that a part

of the vertically mounted sample holder comes in between the pole of the magnetic field. As shown in Figure 2, the

sample holder had a length of 300 mm and an inner diameter of 15.7 mm. For the present study, the sample holder

contained of six samples (A, B, C, D, E and F) of IN RAFMS material (Fe-9%Cr-1.4%W-0.06%Ta). Each sample

had a size of 40 mm x10 mm x 2 mm making the total length of sample stack to be 240 mm. Flat and rectangular

samples were specifically chosen for this loop in order to have a uniform magnetic field over the sample surface. All

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these samples have been metallographically polished up to diamond finish and weighed before loading into sample

holder. Moreover, the roughness profile and roughness parameters over the surface of these samples were recorded

with the help of an optical profilometer. The samples were placed in such a way so as to have the face having the

largest surface area located in a direction perpendicular to the magnetic field. Since the vertical length of the

magnetic pole was 50 mm, it was possible to place only one sample completely under the influence of uniform

magnetic field. It may be noted that the magnetic field in the space between the magnetic poles was mapped with the

help of a high resolution Guassmeter. A field uniformity of 95 % was observed within the magnetic poles over an

active volume of 35 mm x 50 mm x 50 mm and the results are shown in Figure 3. The dipole magnet was integrated

with the sample holder in such a manner that the last sample starting from the direction of flow (Sample F) faced the

magnetic field. Thus, the samples A to D were present completely outside the magnetic field while sample F was

located completely inside the magnetic field. On the other hand, Sample E was located partially inside the magnetic

field. It had been earlier observed in EMPPIL that local fluctuations in velocities are created when the flowing liquid

first impinges on the sample stack [12]. It was also observed that the flow takes a certain distance (~100 mm) to

reduce its fluctuations to a minimum. Thus in the present case (EMPPIL-M), the samples A to D actually allowed

the flow to stabilize before entering the magnetic field region and the flow is supposed to be completely stabilized as

it reaches the fourth sample D.

FIG 1 Schematic of Pb-Li loop with magnetic field (EMPPIL-M)

After integrating the sample holder along with the IN RAFMS samples with the main loop, the system was

evacuated through the expansion tank and then flushed with high purity argon to remove any adhered gasses. The

entire loop was initially heated to 623 K (350 ˚C) and molten Pb-Li through from dump tank was filled into the loop

through argon gas pressurization. The coil type heaters used for heating the entire loop length were by passed around

the part of the sample holder within the magnetic poles. This was to have maximum interaction of the magnetic field

with the test sample.

Afterwards, Pb-Li circulation was established through the rotation of electromagnetic pump and the average velocity

of Pb-Li flow was fixed at 1.5 m/s (measured through electromagnetic flow meter). On the other hand, the

temperature of the test section was maintained at 773 K (500˚C) and then the EMPPIL-M system was operated for

2,800 h continuously. Later, molten Pb-Li was drained back into the melt tank and the IN RAFMS samples were

taken out of the loop. For preliminary investigation of the effect of magnetic field, two representative samples were

chosen. These were “Sample D” which was completely outside the magnetic field and “Sample F” which was

completely inside the magnetic field (Figure 2). Out of the four samples (A, B, C and D) outside magnetic field,

Sample D was specifically chosen because it was expected that some disturbance of flow would occur at the

beginning of the sample stack (i.e. near sample A) [12]. Both the exposed samples (D and F) were cleaned off the

adherent Pb-Li by repeatedly exposing them to a mixture of acetic acid, acetone and hydrogen peroxide in the ratio

1:1:1. The weight of the cleaned samples was noted in order to measure the weight loss due to Pb-Li exposure and

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corrosion rate. Thereafter, the surface roughness profile of these exposed samples was measured with the help of

optical profilometer. Afterwards, their surface and the cross-section were examined with the help of Optical

Microscopy (OM) and Secondary Electron Microscopy- Energy Dispersive Spectroscopy (SEM-EDS).

FIG 2: Schematic diagram of sample holder in EMPPIL-M indicating the location of the samples and magnetic field.

FIG 3: Magnetic field mapping at z= 0 (55 mm from edge) within the magnetic poles with 0.5T magnetic field.

3. RESULTS AND DISCUSSION

Table 1 shows the weight loss of Sample D (outside magnetic field) and Sample F (inside the magnetic field) after

exposure to Pb-Li in EMPPIL-M. Sample F clearly showed a greater weight loss than Sample D. The greater

corrosion attack in the presence of magnetic field was possibly associated with the change in velocity profile of liquid

Pb-Li due to Magneto-Hydrodynamic effects (MHD) [4].

Figure 4 (a) and (b) shows the optical micrographs of the surface of the IN RAFMS samples after Pb-Li exposure in

the presence and absence of magnetic field. The distinct wavy pattern observed on the surface of P91 and EUROFER

samples after exposure to Pb-Li in the presence of a high magnetic field of ~1.7 T [8-9] was not noted in the present

case i.e. at 0.5 T field. However, the formation of distinct surface patterns could be noted over the present IN RAFMS

samples in the presence of magnetic field. These were possibly due to the difference in extent of attack at various

locations inside the field. However, these surface patterns did not bear any directional similarity with the Pb-Li flow

as observed for EUROFER and P91 earlier [8-9].

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TABLE 1: CORROSION RATE OF IN RAFMS IN FLOWING Pb-Li AT 773 K FOR 2800 h WITH 0.5 T MAGNETIC FIELD

Sample Weight Loss Corrosion Rate (µg/cm2.h) Corrosion Rate (µm/y)

Inside Magnetic Field 0.1084 5.0086 56.224

Outside Magnetic Field 0.0828 3.8089 42.71

For further understanding, the roughness parameters of the area denoted by the optical images shown in Figure 4

were studied and compared with that of an as-received sample with 3-D Optical Profilometer. Figure 5 (a), (b) and

(c) shows the 2-D surface roughness profile of the IN RAFMS samples before exposure, after exposure without

magnetic field and after exposure with magnetic field respectively. The general increase in roughness after exposure

to Pb-Li could be clearly noted in Figure 5 (b) and (c). The maximum difference in surface elevation for the exposed

samples both in the presence and absence of magnetic field were almost the same (~40 µm). However, the fraction

of area with maximum elevation was much higher in the presence of magnetic field signifying localized corrosion

taking place. This means a certain part of the surface remained completely un-attacked while the other parts were

getting heavily attacked (Figure 5(c)). On the hand, only a few points on the surface were found to have the highest

elevation in the absence of magnetic field signifying the absence of gross localized corrosion (Figure 5(b)). The

greater difference in surface roughness has been also recorded for EUROFER samples exposed to Pb-Li in the

presence of magnetic field [10].

FIG 4: Optical image of the IN RAFMS samples exposed to Pb-Li at 773 K (a) with and (b) without the presence of magnetic

field; at 20 X magnification.

FIG 5: 2-D Surface roughness profiles of the IN RAFMS samples (a) before exposure, (b) after exposure without magnetic field

and (c) after exposure with magnetic field.

Figure 6 (a) and (b) shows the 3-D surface roughness profile of the IN RAFMS samples after exposure to Pb-Li in

the presence and absence of magnetic field respectively. The greater fraction of the un-attacked or less attacked

areas was clearly seen for the sample placed under magnetic field. It was also noted that the maximum elevation was

slightly lesser within the magnetic field although the corrosion rate of this sample was higher than that outside the

field (Table 1). This was because of the fact the regions with maximum elevation in both the samples were not un-

attacked but actually less attacked. Due to corrosion / dissolution in Pb-Li, the original surface may not be present

after 2,800 h of exposure. Thus it would not be correct to correlate the maximum elevation with corrosion rate. For

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this reason, another parameter (Sa) was used to quantify the surface roughness. „Sa‟ can be appropriately expressed

by Equation 1 which gives an absolute value of the difference in height of each point compared to the arithmetical

mean of the surface.

Sa = 1

𝐴 𝑍 𝑥, 𝑦 𝑑𝑥. 𝑑𝑦

𝐴 (1)

Where A is the surface area and Z (x,y) is the difference of each pint with the arithmetic mean surface plane.

FIG 6: 3-D surface roughness profile of the IN RAFMS samples exposed to Pb-Li at 773 K (a) with and (b) without the presence

of magnetic field.

Table 2 gives the surface roughness parameter of the IN RAFMS samples before and after exposure calculated through

Optical Profilometer as per standard ISO 25178 procedures. The change in „Sa‟ after Pb-Li exposure were in good

agreement with the surface profiling results and the maximum roughness in the presence of magnetic field matched

well with the higher value of corrosion rate in this region (Table 1). Similar results were also observed for P91 samples

exposed to Pb-Li in the presence of magnetic field [9]

TABLE 2: SURFACE ROUGHNESS OF IN RAFMS SAMPLES BEFORE AND AFTER EXPOSURE TO Pb-Li AT 773 K

Sample Surface Roughness (Sa) (µm)

Before Exposure 0.03

After Exposure (With magnetic Field) 7.79

After Exposure (Without magnetic Field) 5.23

The difference in surface features observed over the surface of the exposed samples was prominantly revealed through

SEM –EDS analysis. The SEM image of the IN RAFMS samples exposed in the presence and absence of magnetic

field are shown in Figure 7 (a) and (b) respectively The non uniform Pb-Li attack over the surface of sample exposed

within magnetic field is clearly visible in Figure 7 (a). Moreover, the difference in microstructure of the regions facing

various extent of attack inside magneic field is also revealed (Figure 7 (a)). In Figure 7 (a), the region with lesser

attack i.e. highest elevation has been indicated by “1” while the one with higher attack i.e lowest elevation is marked

by “2”. On the other hand, the sample outside magnetic field (Figure 7 (b)) showed a clear evidence of grain boundary

attack all over it‟s surface revealing the martensite lath structure. When EUROFER samples had been exposed to Pb-

Li, it was observed that corrosion took place predominantly via the grain boundaries in the absence of magnetic field

[10]. However when a magnetic field was applied, the corrosion mechanism changed and the bulk of the steel matrix

also started dissolving in Pb-Li [10]. These results were in agreement with the present results on IN RAFMS (Figure

7) where a distinct diffrence in the nature of attack is found in the presence and absence of magnetic field.

Figure 8(a) shows SEM image of the surface of the IN RAFMS sample under as-recieved condition at a magnification

of ~ 4.5 kx [13]. Along with the typical tempered martensite structure and grain boundary carbides (Cr23C6 ), the prior

austenite grain size was found lie within 8 – 15 µm [13]. The surface of IN RAFMS after exposure to Pb-Li in the

absence of magnetic field (Mag ~ 4.5 kx) is shown in Figure 8(b). As observed earlier in Figure 7(b), Pb-Li attack

outside magnetic field was confined along the lath boundaries and grain boundaries which resulted in the lath matrix

protruding outwards (Figure 8(b). The carbides found in the as-received sample could not be noted as well, indicating

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carbide dropping due to grain boundary dissolution/ attack [14]. A number of pits are also noted over the surface

mostly over the lath boundaries.These were possibly the Pb-Li channels penetrating the lath boundaries perpendicular

to the plane of the paper. However the pits may also be a result of dropping of the larger carbides. Formation of

surface pits have also been observed in the case of JLF 1 steel when exposed to Pb-Li at 823 K [15].

Fig 7: SEM images of the IN RAFMS surface after exposure to Pb-Li in (a) the presence of magnetic field and (b) the absence of

magnetic field.

FIG 8 : SEM image of the surface of IN RAFMS (a) before exposure, (b) after exposure in the absence of magnetic field, (c) less

attacked areas after Pb-Li exposure in the presence of magnetic field [Region 1 in Figure 7(c)] and (d) highly attacked areas after

Pb-Li exposure in the presence of magnetic field [Region 2 in Figure 7(c)].

Figure 8(c) and (d) shows the magnified images (Mag ~ 4.5 kx) of the diffrently attacked regions over the surface of the

sample exposed to Pb-Li in the presence of magetic field which were indicated by 1 and 2 in Figure 7 (a) respectively.

As discussed earlier, Region 1 shows the area with lesser attack and Region 2 shows the area with higher attack. This

means that the Region 1 indicated the microstructure developed in the initial stages of Pb-Li attack inside magnetic

field. As observed in Figure 8 (c), the attack in Region 1 was not only confined to lath boundries but also took place in

the intra-lath regions. In fact, some of the regions seemed to have been broken into very tiny subgrains which may have

been formed due to fragmentation of the laths during intra lath attack. Such an area has been enclosed by a box in

Figure 8 (c). A strong fragmentation of the martensite phase over the exposed surface under the combined action of Pb-

Li and magnetic field has been also recorded for EUROFER samples when exposed under a field of 1.8 T for 1,000 h

[10]. The authors have confirmed that the corrosion process in the magnetic field was more intensive and involved

matrix dissolution resulting in the formation of sub-structures. In that case, the sub-structural size was of 1-3 µm [10].

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In Region 2 (Figure 8 (d)), the parent microstructure in IN RAFMS was revealed with prior austenite grain size similar

to the as-received structure shown in Figure 8 (a). The density of grain boundary carbides was less as compared to an

unexposed sample which indicated initiation of grain boundary attack. It was possible that this part of the surface had

been freshly exposed after the top surface layers above it (containing fragmented grains as observed in Region 1) were

washed away by flowing Pb-Li.

In order to know whether the formation of various surface structures were also associated with any composition

changes created through Pb-Li attack, the average compositions of the regions shown in Figure 8 were recorded through

EDS. Table 3 lists the contents of major elements detected in EDS analysis for the IN RAFMS samples placed inside

and outside magnetic field and also includes the composition of as-received sample for reference. It was observed that

depletion of Fe was predominant in the presence of magnetic field while depletion in chromium content took place

outside it. It has been reported that due to the slower diffusivity of chromium in the steel matrix and higher diffusion of

the same in Pb-Li, a chromium depleted zone is genrally formed below the exposed surface of RAFM steels [14,16].

This condition of chromium depletion was reflected for the sample ouside magnetic field in the present case. However,

the enrichment in chromium inside magnetic field was possibly due to a comparitively greater decrease in iron content

since the EDS ananlysis takes normalized values into account.

Since the content of Ni in IN RAFMS was negligible, it is expected that the source of this Ni lies in the corrosion of the

SS 316L tube walls [12]. However, the greater deposition of Ni over the sample surface in the presence of magnetic

field was possibly due to the higher corroion of SS316 L tube walls in this location due to increase in local flow

velocities. On the other hand, greater depletion of Fe in the presence of magnetic field might also be associated with its

extensive ferro-magnetic charachteristics. Nevertheless, no major variation of composition was found over the

differently attacked regions of the sample (Region 1 and 2 in Figure 7 (a)) exposed to Pb-Li inside the magnetic field.

This indicated that the non uniform Pb-Li attack inside magnetic field was predominantly associated with the higher

local flow velocities and not with any change in the dissolution rate of alloying elements. It was however true that the

overall Pb-Li attack was more intense inside magnetic field resulting in both inter and intra lath corrosion on IN

RAFMS. Moreover, the extent of attack was different at different regions which can faster detachment of the regions

facing higher attack (due to higher flow) into the flowing Pb-Li. The detachment of weaker surface layers after attack

can lead to exposure of fresh surfaces and further attack. Therefore, a continous proscess could be established and the

non uniform attack could sustain over the entire period of exposure. It was highly possible that under higher magnetic

fields like 1.7 T, this phenomenon could give rise to wave like structures as observed in the case of P91 and EUROFER

[8-9].

TABLE 3 : CONTENT OF MAJOR ELEMENTS OVER THE SURFACE OF THE IN RAFMS SAMPLES BEFOERE AND

AFTER EXPOSURE TO Pb-Li AT 773 K FOR 2,800 h

Locations/

Elements

(wt%)

As received

(Fig 8 (a))

Outside

Magnetic field

(Fig 8 (b))

Inside magnetic field

(less attacked) (Region1 in Fig

8 (c))

Inside magnetic field

(more attacked)

(Region 2 in Fig 8 (d))

Fe 87.9 87 75.1 74.5

Cr 9.5 5.8 11.1 10.6

W 1.5 1.9 1.9 1.7

Ni 0.1 2.7 8.5 10.3

On the other hand, Pb-Li attck inside magnetic field was also associated with a greater dissolution of iron. It has been

also reported that iron dissolution is the rate controlling step for Pb-Li attack in case of ferritic/martensitic steels [16].

Therefore, the greater depletion of iron in the presence of magnetic field could clearly lead to a higher corrosion rate of

IN RAFMS. However, the actual reason for higher iron dissolution in magnetic field may involve in-depth analysis of

the Magnetohydrodynamic (MHD) effects as well as the interaction of iron with magnetic field [4-5]. Neverthesless, a

possible indication has been given earlier by R. Moreau based on the experimental results of the EUROFER samples

exposed to Pb-17Li in the forced circulation loop at IPUL, Latvia under a magnetic field of 1.8 T [11]. The

corresponding paper [11] reported that an electric current is developed in the samples in the presence of magnetic field

which contributes to corrosion by a mechanism called electro-dissolution. They also predicted that the change in

velocity due to the effect of magnetic field will affect the general dissolution flux (of elements into Pb-Li) while the

magnitude of the applied magnetic field will affect the electro-dissolution leading to a high corrosion rate [11]. It is

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obvious that due to its highly ferromagnetic nature, iron will be the most affected element in the electro-dissolution

process. This fact has been theoretically predicted by R Morreu et al. [11] and experimentally proved by the present

study on the corrosion of IN RAFMS in Pb-Li under magnetic field.

4. CONCLUSIONS

i. An electromagnetic pump driven loop named EMPPIL-M have been installed to study the corrosion of

structural material in flowing Pb-Li in the presence of magnetic field.

ii. The corrosion of IN RAFMS material in the flowing Pb-Li has been studied in the presence of 0.5 T

magnetic field at 773 K for 2,800 h of exposure. The value of corrosion rate was found to be 1.3 times

higher in the presence of the magnetic field.

iii. The sample surface inside the magnetic field showed non uniform corroison along with the formation of

distinct regions having different surface morphology.

iv. The Pb-Li attack in the presence of magnetic field was not only confined to the prior austenite and lath

boundaries as in the absence of magnetic field but also took place in the intra-lath regions causing

formation of subgrains.

v. Dissolution of iron and chromium was found to be responsible for the corrosion of IN RAFMS. However

the dissolution of iron was found to much higher in the presence of magnetic field.

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