Rebecca Schaller

Q u a l i f yi n g E x a m |1

1. Introduction
Friction Stir Welding (FSW) is a solid state joining technique invented at the Welding
Institute by Wayne Thomas in 1991.[1] It was originally developed and applied to aluminum
alloys, primarily in the aerospace industry. Previous standard welding methods were insufficient
for many Al alloys due to their low melting temperatures. Some of the significant advantages of
FSW over conventional welding are its minimal effect on material properties, smaller heat
affected zones (HAZ), single pass weldability, it is less hazardous as there is no detectable
generation of harmful gasses (as in traditional welding),[2] and extra material usage is lower.
Due to these advantageous properties, the application of FSW to higher temperature materials,
such as steel and titanium, is becoming increasingly appealing.[3]
One area of interest for the application of FSW is the repair of stainless steel (SS)
components and existing welds in nuclear light water reactors (LWRs). LWRs of two types were
first developed and put into service in the 1950s, with currently 359 in operation.[4] Since
implementation, material degradation has been a major issue. For boiling water reactors (BWRs)
in the US alone, an estimated 3 billion dollars was lost due to irradiation assisted stress corrosion
cracking (IASCC).[5] A degradation in fracture toughness has been shown to correlate with
increased neutron irradiation dosage.[6] Repair and/ or replacement of these irradiated SS parts
has and will continue to involve welding. Thus far, traditional arc welding has been used for
repair of structures. Evidence has shown that these repairs have been unsuccessful, producing
large HAZ due to the high heat and multiple passes of welding.[4] These zones were both
susceptible to increased sensitization and coalescence of helium causing embrittlement of the SS.
Both conditions have led to weld cracking.[7] FSW could alleviate many of these problems since
the temperature range generated through FSW is much lower than customary welds. Thus issues
of sensitization and helium embrittlement may be diminished.
Preliminary studies of FSW for high temperature materials have uncovered some
obstacles. First, is the FSW tool strength. Traditional tools used for FSW in low temperature Al
alloys would not be suitable for their high temperature counterparts. New tool developments
with polycrystalline boron nitride (PCBN) and tungsten alloys (harder tool materials with higher
Tm) have enabled preliminary application of FSW to these high temperature materials, but tool
life expectancy is still uncertain. Another issue facing the specific application of FSW to
austenitic SS is the formation of sigma phase during welding. While this phase itself is a higher
strength, corrosion resistant material containing large amounts of Cr, it leads to corrosion
susceptibility of the weld. Since it is formed at higher temperatures and longer durations, the
temperature profile during welding is extremely important. Studies in minimizing the time spent
at high temperature through transverse weld speed or underwater FSW (UWFSW) have
displayed initial improvements in the decline of formation of the sigma phase in the welds.[8],[9]
This proposal addresses the implementation of FSW to austenitic SS in LWRs where a
great deal of attention must be paid to the effects of irradiation. Sensitization due to irradiation
of the material prior to welding and He bubble formation induced by the higher temperature
welds, resulting in a lower fracture toughness of the SS, may still be issues in FSW due to the
high stresses involved. Weld speed optimization and UWFSW are proposed here to minimize
these effects. Characterization of weld optimization through electron microscopy,
electrochemical degree of sensitization (DoS) measurements, and temperature modeling will
combine to allow for analysis of the weld quality of these FSW techniques on pre-irradiated 304
and 304L SS.

2. Austenitic Stainless Steel

The reactor parts under consideration in this study, consisting of AISI type 304 and 304L
SS, belong to the austenitic SS alloy class. As seen in the Fe-Cr phase diagram, the austenite
 Rebecca Schaller
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phase (face centered cubic) is not thermodynamically stable at room temperature. However,
Figure 1. Fe-Cr phase diagram.[10]
austenitic stainless steels contain a large weight percent
of nickel (greater than 8 wt%) so that the austenite
phase is favored at room temperatures. Ni offsets the
delta ferrite-forming tendency of the austenite and
lowers the martensitic start temperature. Large
chromium content enhances the corrosion resistance by
reacting to produce a passive film (Cr2O3) on the metal
surface, but also increases the tendency of delta ferrite
and carbide formation. Ni is employed to a sufficient
level to counteract the Cr. These steels are not heat
treatable but hardened and strengthened through cold
work. Austenitic stainless steels are chosen for use
because of their high fabricability, high corrosion
resistance, and stability at higher operating
temperatures.

3. Light Water Reactors

As mentioned, LWRs consist of two main groups of reactors; BWRs and pressurized
water reactors (PWRs). This class of reactors uses light water (H2O) instead of heavy,
deuterated water (D2O) as their coolant. In both types, many of the components within the
reactors, such as coolant pipes or pressure vessels, are constructed of 304 and 304L SS (Table 1).
In their areas of service, the
Table 1. Composition of Austenitic Stainless Steels, wt %.[11] components are subjected to
C Mn Si P S N heat, water and neutron
Alloy Fe Ni Cr
Max Max Max Max Max Max irradiation, often of fluences
8.0- 18.0-
(integrated flux over area;
304 Bal
10.5 20.0
0.08 2.0 1.0 0.03 0.045 - radiation doses) of 1020 up
to 1026 neutrons/cm2.[12] At
8.0- 18.0- 0.1-
304L Bal
12.0 20.0
0.03 2.0 1.0 0.03 0.045
0.16 higher fluences, irradiation
can greatly affect the
material through IASCC.

3.1 Corrosion Damage (Irradiation Assisted)

Due to the long lifetime of current in-service parts of LWRs, corrosion damage,
specifically irradiation-assisted corrosion (IAC), is of growing concern.[13],[14] The higher
operational temperature range, typically around 270 to 370 oC for LWRs [12],[15] spans a range
over which irradiation assisted microstructural changes become significant. The K1SCC (the stress
intensity above which stress corrosion cracking occurs) of the steel relies on a combination of
stress, corrosive environment, and irradiation.

3.1.1 He Embrittlement Conditions

Helium is generated in the inner austenitic SS components through B or Ni transmutation
processes. 304 and 304L SS contain a high wt% of Ni for austenite stabilization. The two-step
transmutation reaction is as follows:[16]
58
Ni + n →59Ni (1)
59
Ni + n →56Fe + 4He (2)

With n being a neutron.

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At higher fluences, Ni transmutation occurs and there is production of He which builds

up within the SS components. Under higher temperatures (T 0.4Tm[17]) and internal tensile
stress, He migrates to grain boundaries (gb) which then become embrittled. This is exacerbated
by increased temperature due to the T dependence of diffusion. The embrittlement reduces the
cohesive strength of the gb and with applied stress can result in brittle rupture.[18]

3.1.2 Sensitization
Another detrimental effect of the high temperature and irradiation of 304 and 304L SS is
sensitization. Sensitization is the susceptibility of a material to IGC and SCC due to depletion of
Cr from solid solution. This depletion of Cr is due to two factors, thermodynamics of carbide
formation and the Cr diffusion coefficient. At higher temperatures, chromium carbides are
thermodynamically favored. They tend to nucleate on grain boundaries, dislocations or
deformities due to the lower activation energy necessary at these high interfacial energy sites. As
nucleation occurs, they deplete their surrounding area of Cr. However, this is not believed to be
a factor in 304 or 304L SS below 400 oC.[15] This high temperature is very unlikely in standard
LWR operating conditions, but could be easily reached during welding. Another sensitization
effect is based on the differences in diffusion coefficients of Cr and C and is motivated by
irradiation. Irradiation induced defects (vacancies) stimulate the inverse Kirkendall effect by
diffusing towards the gb and promoting diffusion away from the gb of faster diffusing solutes
like Cr, leading to gb depletion of Cr. Since the energy for vacancy diffusion is from thermal
vibrations (Eav~kBT), this effect increases with increasing temperature. Even though Cr depletes
to levels around 14-16wt% (much more than the 12 wt% required to make it a “stainless steel”) it
results in a corrosion susceptible area, on average 2-4% less than the bulk Cr concentration.[19]
This leads to easier dissolution of the metal surrounding the gb (intergranular corrosion, IGC),
which is now less noble then the matrix and can encourage intergranular stress corrosion
cracking (IGSCC) if the right environment and sufficient stress are present.

4. Fracture Toughness Degradation

Fracture toughness, the resistance of a material to withstand the propagation of a crack

under an applied stress, is greatly influenced by irradiation. Michel et. al. found an irradiation
fluence of 1022 n/cm2 in 304 SS produced a large reduction in fracture toughness as compared to
the un-irradiated solution annealed state. [6] This cracking susceptibility is attributed to IASCC,
specifically irradiation induced segregation and changes to material microstructure.[20]

5. Conventional Welding Repair

Figure 2. Transmission electron
microscopy (TEM) image of He
coalescence at gb.[18]
multi-passes leading to prolonged times at elevated temperatures can induce further sensitization
The repair or replacement procedure of cracked material
currently involves welding of components through gas metal arc
welding (GMAW), gas tungsten arc welding (GTAW) or laser
welding, all of which involve temperatures above the materials’
melting temperature.[21] Welding of 304 and 304L SS with pre-
existing He concentrations can result in welds that are prone to
cracking. As the temperature of the material increases above
0.4Tm, He tends to nucleate along the gb, unites and forms
bubbles. As the material is embrittled, K1scc is lowered and IGSCC
promoted. A dimpled structure results along the crack length
indicative of the He gb bubble formation (Figure 2).
Welding of 304 and 304L SS, with high temperatures and
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of the already IAC materials. Also, low temperature sensitization can result due to the carbide
nuclei formed during high temperature welding which grow over time at the lower temperatures
within the LWRs.[11] Residual stresses from welding and/or stresses arising later from the in-
service environment can often be enough to induce IGSCC if the material is highly sensitized.
The higher temperatures and longer times of traditional welding lead to larger HAZ areas, thus a
greater area of the component is susceptible.
To alleviate some of the issues associated with sensitization, often a post weld heat
treatment (PWHT) is applied. This redistributes the Cr in solid solution and reduces Cr depleted
regions. However, this can lead to increased hardness of the weld and reduced ductility.
Oftentimes, a PWHT in situ is not physically possible.[22] Adding additional steps to the
welding process prolongs the time necessary for the reactor to be out of service and presents a
greater economic issue.[23]

6. Friction Stir Welding

FSW is a solid state form of welding. It applies a large amount of force to the weld
through the generation of friction and heat to plastically deform the weld materials. The FSW
tool consists of a pin and shoulder that rotate depending on weld optimization, with a large force
applied perpendicular to the weld direction (can also be tilted for certain optimizations). There
are two directions of motion in FSW: tool rotation (initiated prior to plunging into the material)
and transverse motion of the tool along the weld. The tool is positioned with the surface of the
weld touching the tool shoulder. Due to the rotation of the pin (and shoulder), a large amount of
friction, and consequently heat, is generated. However, the temperature stays at or below 0.8 TM
of the material being welded. The material under the tool is plastically deformed and
transported, due to the tool rotation, from the front to the back of the tool.1 The shoulder
continuously applies pressure to this area, ensuring that the weld material is captured and trapped
below it. At the end of the weld, the friction stir tool is pulled out, often leaving a hole that can
be either plugged, or eliminated by processing specifications.[1] Continued rotation of the FSW
tool during extraction is one possible solution for diminishing the size of the removal hole.
Some noteworthy regions generated by this welding process are shown in Fig 3 below. It is
important to point out that the highest temperatures in FSW of steel have been found to occur in
the advancing side (AS) of the weld.[24]
b)

a)
Figure 3. a) Schematic and b) weld section where A: Base metal, B: HAZ, C: Retreating side of stir zone, D: Weld nugget, and
E: Advancing side of stir zone, with transverse direction into the paper. [25]

6.1 FSW on 304 and 304L SS

Preliminary applications of FSW to 304 and 304L SS have been made possible by
stronger tool materials. Thus far, experiments have been promising, showing welds resulting in
a finer grain structure than the base metal. One study showed welds stronger than the base metal
(due to work hardening from the FSW tool), and exhibiting excellent ductility (ability of the

1
General motion is from front to back however; numerous studies have taken place to follow exact particle flow,
which can exhibit two paths; straight through flow or maelstrom flow. (Mishra)
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material to deform under a tensile stress) with elongation to fracture greater than 50%.[1] The
HAZ material of FSW has a lower corrosion susceptibility than the base metal but, in many
cases, the AS shows greater susceptibility to corrosion due to the formation of the sigma phase.

6.2 Sigma Phase Formation

Sigma phase is an intermetallic compound of Fe-Cr that has a tetragonal crystal structure
of thirty atoms. This phase in 304 SS (isopleth in Figure 4) is not thermodynamically favored at
standard pressure outside the temperature range of 697 to 807 oC. Also, due to kinetics (slow
substitutional diffusion of Cr and C) sigma
formation is sluggish from the austenite
phase.[27] The presence of the sigma phase
affects both the mechanical properties of the
material and the corrosion resistance. The sigma
phase is comprised of 42.7 to 48.2 wt% Cr; its
formation greatly depletes the surrounding areas
of Cr in solid solution, leading to sensitization of
the stainless steel.[28] Some studies indicated
that the means of Cr diffusion towards these
forming particles is through gb diffusion (known
Figure 4. Calculated Isopleth through 304L and to be faster because it is a less restrictive
sigma region (blue). Ni rich region is at right of structural area than the bulk). This gb depletion
diagram. [26]
has been confirmed through TEM and EDS by
Schwind et al.[28] Gb depletion, rather than a
general depletion throughout the matrix, leads to highly susceptible gbs prone to IGC.
FSW, occurring at 0.8 Tm, produces a smaller HAZ than traditional GTAW. Also, the
degree of sensitization produced in the HAZ is much lower. Finally the time the HAZ in FSW
spends in the sigma phase temperature zone is five times shorter than it is in a typical
GTAW.[29] Based on the slow kinetics of sigma formation, sigma phase would not be predicted
for these welds. However, sigma has been found in the AS of FSW. The sigma phase presence is
believed to be a result of delta ferrite formation subject to very high strains during welding. The
FSW tool introduces these high strains into the material through rotation and this leads to rapid
decomposition of the delta ferrite to sigma phase. Sorensen et. al. have proposed that the sigma
phase is actually formed through static recrystallization from the heavily strained delta ferrite in
the shear bands produced on the AS of the weld.[26]

6.2.1 Weld Speed and UWFSW

Reynolds et. al. showed the amount of banding in the advancing side of the weld is
related to the stir rpm of the tool (sigma phase was not specifically identified).[30] Park et. al.
found if heat can be dissipated more quickly from the AS, the decomposition of delta ferrite to
sigma is lessened.[31] One option to reduce the time the weld area spends at high heat, is to
increase the transverse speed of FSW. The tradeoff is at too slow of a speed, sigma formation is
great, but at too fast of a speed, the weld is insufficient and tunneling occurs (Figure 5).

a) b) c)
Figure 5. SEM of 304 SS SZ formed at transverse speeds of a) 60, b) 600, and c) 1200 mm/min.[8]
 Rebecca Schaller
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Another method to aid in the alleviation of the sigma phase is to implement underwater
friction stir welds (UWFSW). Owing to the high heat capacity of water, the heat generated from
the weld is quickly dissipated away from the surface. This helps to reduce the time at higher
temperatures, thus reducing the possibility of delta ferrite formation and subsequent
transformation to sigma.[9]

7. Proposed Plan of Research

For application of FSW to irradiated stainless steel, it is necessary to study the altered
microstructures and how they react to FSW. Optimization of weld parameters (primarily weld
speed and rotation) is crucial to achieve the desired microstructure in the weld. However, in
FSW of SS, not only is prior irradiation induced sensitization and embrittlement important, but
also the reduction of sigma phase. Dissipation of heat from the weld zone is key to reducing
sigma phase and possibly sensitization and embrittlement. Techniques involving faster weld
speeds, or UWFSW to reduce the temperature could be advantageous for this. Study of the
resulting microstructure and corrosion properties of the weld will give insight into weld quality.
Previous temperature modeling of stainless steel FSW involved optimization for both rotational
and transverse welding speeds[32],[24] , but implementation of this to include the effects of
water, and pre-irradiated microstructure would be highly beneficial.

7.1 Weld optimization

Optimization will be tested in regards to two properties, microstructure and corrosion
resistance, with the results giving an implication of how the weld material might perform in-
service with regards to fracture
Table 2. Example FSW optimization for three different toughness. Pre-irradiated 304 and 304L
fluences of pre-irradiated SS. SS will be used for optimization testing
600 mm/min 800 mm/min 1000 mm/min of FSW. Irradiation to three fluence
300 rpm 1, 2, 3, 4, 5, 6* 1, 2, 3, 4, 5, 6 1, 2, 3, 4, 5, 6
500 rpm 1, 2, 3, 4, 5, 6 1, 2, 3, 4, 5, 6 1, 2, 3, 4, 5, 6 levels is proposed to see if there is an
600 rpm 1, 2, 3, 4, 5, 6 1, 2, 3, 4, 5, 6 1, 2, 3, 4, 5, 6 effect of irradiation dosage on FSW.
* 1,4 low fluence for 304 and 304L, 2,5 mid fluence, and 3, 6 high Samples irradiated at 320 oC (average
fluence. LWR operating temperature) and to a low
fluence of 1020 n/cm2, mid of 5 x 1021 n/cm2 and high of 1023 n/cm2 will represent the weld in
different stages of in-service use and/ or regions of the LWR subject to varying fluences. [15] An
un-irradiated set of samples of each SS will be used for comparison. Multiple welds using a
range of rpm and transverse speeds with constant applied pressure will be tested using prior
knowledge of ultra-high speed weld parameters from un-irradiated SS FSW studies (Table 2).[8]
This same matrix will be repeated to look at the optimization of UWFSW of irradiated SS. If
oxidation of the weld is significantly detrimental, use of ethanol, which also has a high heat
capacity, could be substituted.
Also, weld temperature measurements will be taken of the heat dissipation during fast
FSW and UWFSW, which will be used as preliminary verification of a three-dimensional
temperature model.
 Rebecca Schaller
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Measurements will be made from

inserted thermocouples (TC) along the
weld (Figure 6) that will be inserted from
the backside of the weld up to a depth of
50% the steel thickness. TC locations
are on the edge or adjacent to the stir
zone, not along the weld line. Accurate
measurements of the weld temperature
are desired, but there is a tradeoff with
the possibility of integration/
contamination of the TCs into the weld.

Figure 6. Weld heat thermocouple locations for temperature

measurements (based on pervious study by Owen).[24]

7.2 Characterization
Microstructural characterization will evaluate the change and/or formation of phases in
the weld. Characterization of the weld can be done optically for a general view, but for a more
detailed analysis, SEM cross sections through the weld will be taken. For confirmation of
presence or non-existence of the sigma phase, sections for transmission electron microscopy
(TEM) will be taken from the AS of the weld (where sigma banding is predicted[27]), from any
banded areas that may appear, and from the base metal for comparison. Verification of the
sigma phase can be made through the combination of energy dispersive x-ray spectroscopy to
determine composition and electron diffraction to determine the structure of the particles.

7.3 IGC Susceptibility

The standard test
a) b) method of electrochemical
reactivation (EPR) for
detecting sensitization of 304
and 304L SS, ASTM G 108-
94[34], requires extensive
preparation of the samples
(polishing to 1 µm diamond
paste), and is easily influenced
by changes in temperature and
scan rate. However, Akashi
Figure 8. a) Schematic diagram of the double loop EPR test. Evaluation et.al. developed a double loop
is by the ratio of Ir : Ia [33]and b) example reactivation current ratios in the
base metal, HAZ, stir zone and AS of 304 SS (contains banded sigma
EPR test which requires less
phase in the AS).[29] sample preparation and is less
sensitive to temperature and
scan rate changes.[33, 35] This test uses the ratio of the maximum currents generated, anodic
(Ia) : reactivation (Ir) (Figure 8a). SS samples will be tested post FSW using the double loop EPR
test. Four regions will be tested for comparison, the base metal for background on the effect of
pre-irradiated sensitization, the HAZ zone, the stir zone, from the center of the weld and the
advancing side. This will then give an idea of the effect of FSW, if any, on sensitization of the
weld area, and possible extent/ effects of sigma formation (example Figure 8b). One limitation of
this test is its lack of response to highly sensitized materials. Thus, correlation of this test with a
 Rebecca Schaller
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ferric sulfate – 50% sulfuric acid test (ASTM A 262-B[36]) may be necessary if higher levels of
sensitization occur.[33] Initial testing and screening of samples will be by double loop EPR
tests, then ASTM A 262-B tests, which are more responsive to mid to severe levels of
sensitization, will be used if higher sensitization levels are present.

7.4 Weld Heat Modeling

Temperature measurements taken during welding will be used to validate a three-
dimensional numerical temperature model. P. Ulyssse originally applied this to aluminum alloy
and a similar model was used by Nandan et. al. for mild steel, but thus far none have been
applied to FSW of irradiated stainless steel.[37],[32] The model is based on the conductive
convective energy conservation equation:

c pu      (k )  Q (2)

Where  is density, cp is the specific heat, u is the velocity vector, k is the thermal conductivity,
 is the temperature and Q is the internal heat generation.[37],[38] The temperature distribution
is obtained by solving this equation with specific boundary conditions.* This model assumes that
90% of the plastic deformation is converted into heat. The reference frame of the model is
attached to the rotating pin of the tool, while the material passes through the defined finite
element mesh (Figure 9a). Loss of heat to the backside of the weld is not taken into account in
this model for computational simplification. However, the welding side is represented with a
transfer of heat to the ambient (or in UWFSW, to the water) through convection. Both rotational
speed of the pin, and travel speed are accounted. A considerable advantage is provided by
modeling, assuming its validation
a) b) through experimentation. It can provide
a temperature gradient at the pin (Figure
9b), where thermocouples would be
destroyed in experimentation.
Temperature analysis gained from these
models can provide a basis for phase
predictions within the weld
microstructure and insight into further
Figure 9. a) 3-d finite element mesh b) example plot of optimization of FSW.
temperature contours in K and velocity vectors.[32]

8. Summary
Friction Stir Welding is a viable option for welding of higher temperature materials.
However, irradiation assisted damage to materials in LWRs is of great concern to the resulting
microstructures of the FSWs. Study of optimization of welding irradiated materials is explored
here and considers directly the effects of sensitization, He embrittlement, and sigma formation.
The welding methods presented in this study are all developed to help alleviate these problems
and increase fracture toughness. Through the proposed microstructural characterization and
corrosion characterization, the quality of these welds can be studied. Also, with the use of
temperature modeling, predictions can be made for further optimization conditions not found
experimentally. These temperature models will help to predict both the heat generated in the
welds, and give an implication of the possible resulting microstructures that develop.
Experimental analysis combined with microstructural results will help to establish the quality of
the welds with respect to corrosion resistance and fracture toughness (IASCC susceptibility).
 Rebecca Schaller
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 Rebecca Schaller
Q u a l i f y i n g E x a m | 11

*
Thermal Boundary conditions [35]:
1. Backside of weld: uz = 0; Tx = ty = 0;  / z  0 .
Welding side: Tx = 0; Ty = 0; q  h(   ) .
a
2.
3. Incoming: ux = V; uy = uz = 0;    in .
Outgoing: Tx = 0; Ty = 0; Tz = 0; q  h(   ) .
a
4.
Vertical Sides: Tx = 0; Ty = 0; Tz = 0; q  h(   ) .
a
5.
6. Gap: Tx = 0; Ty = 0; Tz = 0;  / z  0 .
Rotating Tool: Vt = Ωr; 0  r  Rtool ; q  h(   ) .
a
7.
8. Tool shoulder: Tt  C (u t  Vt )
9. Pin: Vt = Ωr; 0  r  R pin
10. Pin bottom: uz = -vpin; ux = uy = 0