Nuclear Technology

ISSN: 0029-5450 (Print) 1943-7471 (Online) Journal homepage: http://www.tandfonline.com/loi/unct20

Materials Requirements for Pressurized Water

Reactor Steam Generator Tubing

Ph. Berge & J. R. Donati

To cite this article: Ph. Berge & J. R. Donati (1981) Materials Requirements for Pressurized Water
Reactor Steam Generator Tubing, Nuclear Technology, 55:1, 88-104, DOI: 10.13182/NT81-A32833

To link to this article: http://dx.doi.org/10.13182/NT81-A32833

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 MATERIALS REQUIREMENTS FOR
PRESSURIZED WATER REACTOR
STEAM GENERATOR TUBING
Ph. BERGE and J. R. DONATI Electricite de France
Direction des Etudes et Recherches
2 Rue Louis-Murat, 75384 Paris, France
Received November 10, 1980
Accepted for Publication March 12,1981
Downloaded by [University of Florida] at 18:36 23 October 2017
Considerable research and development work on
the behavior of steam generator tubing materials has
been performed during the last ten years. These
studies relate mainly to such austenitic alloys as
18-10 stainless steels, Alloys 800, 600, or 690, some-
times with different heat treatments or surface finish.
From these studies, tentative conclusions on the best
selection to be made for this application are drawn,
the different candidate materials being compared
with respect to
1. mechanical and thermal characteristics that
can act on design and manufacturing processes
of steam generators
2. susceptibility to corrosion product release in
the primary coolant, which is responsible for
a good part of the irradiation dose received
by the operation and maintenance personnel
3. corrosion resistance and, in particular, stress
corrosion susceptibility in different solutions
that are or can be met in operating conditions.
I. INTRODUCTION
For the last ten years, considerable research and
development work has been performed on pressurized
water reactor (PWR) steam generator tubing mate-
rials. They relate mainly to such austenitic alloys as
18-10 stainless steels, Alloys 800, 600, or 690,
sometimes with different heat treatments or surface
finish. It is well recognized that all the problems that
have affected the PWR steam generators cannot be
solved only by good material selection. Nevertheless,
the alloys that have been, or could be, selected by
the different vendors show marked differences in
the required mechanical and thermal properties and
in their resistance to corrosion in normal or faulted
operating conditions. Our purpose, in this paper,
is to compare these properties and show how they
meet the requirements of this application.
II. MATERIALS FOR TUBES-DEFINITION
AND PROPERTIES
II.A. Material Choice-Heat Treatments
Based on their mechanical and thermal properties
and on their corrosion resistance, the best materials
for steam generator tubes appear to be only austenitic
stainless steels and alloys. The initial choice was
18-10 stainless steels (AISI Types 304, 316, and 347).
Thus, the steam generators of the French CHOOZ
power station are equipped with tube bundles made
of Type 316 stainless steel, which have operated
satisfactorily during 70 000 h of service. Nonetheless,
these stainless steels are known to be very susceptible
to stress corrosion cracking in a number of environ-
ments and notably in the presence of chlorides and
oxygen. Different operational problems have stimu-
lated research to develop austenitic materials more
resistant to this type of corrosion.
Consequently, Alloy 600 has been introduced,
and since 1967 has equipped a large number of steam
generators, notably those produced by Westinghouse
Electric Corporation (WEC), Combustion-Engineering,
and Babcock & Wilcox. An alloy with intermediate
nickel content, Alloy 800, has equally been con-
sidered for this application and is used in the Federal
Republic of Germany for the power units built by
Kraftwerk Union.
Laboratory tests and the results of service ex-
perience show nonetheless that Alloys 600 and 800
can be, under certain extreme conditions of mechan-
ical stress or contamination of the secondary water,
 susceptible to stress corrosion cracking. To overcome
this problem, studies have developed in two directions
simultaneously.
II.A.l. Improvement of Performance of
Existing A lloys
Improvement of the performance of existing
alloys notably seeks to reduce as far as possible the
residual fabrication stresses, which form a major
part of the total stress in service. 1 The different
solutions envisaged have been described and com-
pared in detail elsewhere. 2 As far as Alloy 600 is
concerned, cooperative studies carried out by Elec-
tricite de France (EdF), Framatome, and WEC
have led to the adoption of a 10- to 15-h heat treat-
ment around 700°C (715 ± 15°C) on straight tubes
in the factory, completed with a shorter duration
treatment at the same temperature on the bends of
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<250-mm radius.
This treatment has several effects, which are
dealt with in more detail below.
1. It greatly reduces the residual stresses due to
straightening and belt polishing of the tubes, as
well as those particularly high stresses found in small
radius bends (see Sec. III.C).
2. It removes the cold work introduced at the
surface of the tubes by the same straightening and
polishing operations and by sandblasting the internal
skin, which results in a reduction in the stress level
in large radius bends (see Sec. III.C) and probably
a reduction in the rate of corrosion product release
in the primary coolant (Sec. III.A.l).
3. It makes the alloy less sensitive to intergranular
corrosion by selecting a sufficient time at tempera-
ture to rehomogenize the chromium content in the
vicinity of the precipitated carbides. In addition,
the quantity of chromium carbides likely to precipi-
tate during subsequent aging at the service tempera-
ture is considerably reduced (see Sec. III.B.5).
4. It improves the intrinsic resistance to stress
corrosion in caustic solutions, and probably also in
pure water, with the hypothesis that these two
phenomena are essentially of the same type (see,
for example, Sees. III.A.2 and III.B.3).
II.A.2. Consideration of Other Alloys
Because of the importance of tests needed to
qualify a new material for service use, solutions of
this type have taken longer to develop than the heat
treatment referred to above. The studies have been
carried out principally on the two following mate-
rials:
1. Alloy 690, with an austenitic structure, which
is likely, as a result of its chromium content
higher than Alloy 600, to perform more
satisfactorily with respect to several corrosion
phenomena 3
2. 45% ferrite duplex stainless steel, considered
because of the better resistance to stress
corrosion of this type of microstructure. 4
It should be emphasized that, while Alloy 690
does not present any major difference with respect
to Alloy 600 for industrial tube fabrication, extrusion
and heat treatment of the duplex stainless steel are
both very delicate operations.
II.B. Properties of the Different Materials
II.B.l. Chemical Composition
The specified chemical composition for each
different alloy is laid out in Table I, and for Alloy
600, the particular specification used for French
power stations is shown. One should note the reduc-
tion in the maximum carbon content and the desire
to maintain the chromium content in the upper
part of the allowable range (to improve the resistance
to intergranular corrosion) and the cobalt content
as low as possible (to limit the presence of ^ C o in
the primary circuit).
II.B.l. Mechanical Properties
Table II compares the tensile properties at am-
bient temperature and at 343°C for the different
materials under discussion. Note that Alloys 600 and
690 have the best characteristics among the austenitic
materials.
Generally, the results for finished tubes satisfy
the minima specified without difficulty. In the case
of Alloy 600, for which we have a large number of
test results, it has been shown nonetheless that it is
desirable to avoid the carbon contents that are
sufficiently low to allow a total dissolution of chro-
mium carbides during the final annealing treatment
(carbon < 0.010% for 980°C, for example). In such a
case, one would risk, due to grain growth and to the
absence of intragranular carbides, obtaining weak
values for the yield stress. Heat treatment of ~ 1 0 h
at 700°C can equally produce a slight decrease in the
yield stress. However, the maximum value of this
drop ( ~ 5 0 MPa) applies to the tubes with the highest
degree of cold work due to straightening and which
have, therefore, a yield stress well above the specified
minimum.
Alloy 690 is often delivered with a final annealing
temperature on the order of 1040°C. This high value
does not appear to be essential from the point of view
of stress corrosion resistance, and it would appear
preferable to use the same temperature as for Alloy
600 (^980°C) to benefit from the improvement that
can thereby be achieved in mechanical properties.
 TABLE I

Chemical Composition of Materials Used for Steam Generator Tubes (wt%)

Carbon Sulfur Phosphorus Silicon Manganese Nickel Chromium

Alloy 600
Balance
ASTMB163 <0.15 <0.015 - - - <0.5 <1.0 14 to 17
(>72)

14.00 to 17.00
Specification for EdF plants 0.010 to 0.050 <0.015 <0.025 <0.50 <1.00 >72.00
15.50 3

Alloy 690
ASME code case 1484-3 <0.05 <0.015 - - - <0.50 <0.50 >58 27 to 31

Alloy 800
ASTM B163 <0.10 <0.015 - - - <1.0 <1.5 30 to 35 19 to 23

Type 316 stainless steel

ASTM A376 <0.08 <0.03 <0.03 <0.75 <2.00 11 to 14 16 to 18
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Duplex stainless steel

Typical Creusot-Loire
composition <0.06 _ <1 6 to 8 20 to 22

Molybdenum Titanium Aluminum Iron Copper Cobalt

Alloy 600
ASTM B163 - - - 6 to 10 <0.5 <0.10

<0.10
Specification for EdF plants <0.50 <0.50 6.00 to 10.00 <0.50
0.05 b

Alloy 690
ASME code case 1484-3 - - - - 7 to 11 <0.50 <0.10

Alloy 800
ASTM B163 0.15 to 0.6 0.15 to 0.6 Balance <0.75 <0.10

Type 316 stainless steel

ASTM A376 2 to 3 - - - - Balance - - - - <0.10

Duplex stainless steel

Typical Creusot-Loire
composition 2 to 3 —
Balance .— . . .

a
Desirable minimum value.
b
Desirable maximum value.

The tensile properties of the duplex stainless
steel are extremely high but this steel may show
a tendency to a ' - t y p e embrittlement that affects the
ferrite at service temperature, a phenomenon that
is accentuated when the stress-relieving treatment
of the weld of the channel head to the tube plate
is carried out by putting the bottom part of the
steam generator in a furnace. If the effects on the
impact strength are of little importance in the case
of a thin tube, it has been observed that the
embrittled state shows noticeably greater suscep-
tibility to stress corrosion cracking in caustic solu-
tions.
High-cycle fatigue tests (20 Hz), in alternating
tension (0 - o m a x ) on tubes thinned over the central
part, have been carried out in air and in pure water
under pressure at 320°C (Ref. 5). Figure 1 shows that
the fatigue limit at 10 7 cycles is 225 MPa ( a m a x = 450
MPa). The comparison of the different alloys studied
shows that Alloy 600 heat treated at 700°C or Alloy
690 behave much like Alloy 600 mill annealed, and
that the effect of pressurized water environment is
 TABLE II
Tensile Properties of Steam Generator Tubes

Room Temperature
343°C
Yield Strength Ultimate Strength Elongation Yield Strength
(MPa) (MPa) (%) (MPa)

Alloys 600 and 690 a 275 to 450 >550 >30 243 b

Alloy 600
mill annealed or heat treated at 700°C c 275 to 450 >550 >30 >215
a
Alloy 800 275 to 450 >550 >30 213 b
d
Duplex stainless steel 500 750 40 370
e
Type 316 stainless steel >200 >510 >35
a
ASME Code Case 1484-3.
indicative average value.
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Specification for EdF plants.

d
Typical values for tubes.
e
ASTM A 376.

negligible in this type of test. The resistance to
fatigue may be of interest since fatigue ruptures have
been reported 6 in once-through boilers.
II. B. 3. Physical Characteristics
Table III shows the values of thermal conduc-
tivity and coefficient of expansion for the different
alloys considered compared with those of ferritic
and austenitic stainless steels. This comparison under-
lines the interest of the duplex stainless steel and of
FATIGUE TESTS
Fig. 1. High-cycle fatigue tests on Alloys 600 and 690 tubes.
MA = mill annealed, HT = heat treated.
Alloys 600 and 690 with respect to the two param-
eters considered, compared to austenitic alloys with
a lower nickel content. In particular, their thermal
expansion coefficient, closer to that of ferritic steel,
assures a better leaktightness when assembling the
tubes by expansion in the tube plate. This parameter
should be allowed for particularly when the stress
relieving at 620°C of the channel head welds is
carried out in a furnace and affects the tube ends.
According to our tests, it would even seem in this
case that the slight difference existing between
expansion coefficients for Alloys 600 and 690
should be sufficient to manifest itself in a difference
in leaktightness of the expanded ends after heat
treatment, to the disadvantage of Alloy 690.
This phenomenon would have only small practical
significance (existence of a weld ensuring leaktight-
ness, little influence on the pull-out force) if there
wasn't the concern that, because of the penetration
of the secondary water between tube and tube plate,
there is an increased risk of corrosion in this very
sensitive zone (stress corrosion cracking, pitting,
intergranular corrosion, denting).
This situation can lead one to choose particular
methods of construction when using Alloy 690,
similar to those used when the tubes are of Alloy
800 or in austenitic stainless steel (local heat treat-
ment of the channel head welds for example).
The thermal expansion coefficient enters else-
where in the calculation of stresses in the bends
(differential expansion between hot and cold legs),
the stresses induced by this effect being higher for
18-10 stainless steels and Alloy 800 than for Alloy
600.
As far as Alloys 600 and 690 are concerned, it
 TABLE III

Physical Properties of Steam Generator Materials*

Thermal Expansion Coefficient Thermal Conductivity

[(mm/mm per °C) X 10 6 ] (W-m/m 2 per °C)

20 to 300°C 20 t o 600°C 300°C

Ferritic steels 12 14 55 to 35
Alloy 600 14.0,14.2 15.3 18.3,19.2, a 20.9
Alloy 690 14.6,15.3 16.2 17.9 , a 18.8
Alloy 800 15.0,16.2 17.0 15.5,16.7
Duplex stainless steel 13.8 to 14.6 b c

18-8 stainless steels 17.5 18.5 17.0,18.3

*As given by INCO or Creusot-Loire.

a
Tests performed by Commissariat a l'Energie Atomique (CEA).
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b
Depending on ferrite content between 45 and 35%.
°Similar to ALLOY 600, according to Creusot-Loire.

has been shown that heat treatment of tubes at can lead to an enhanced release rate over several
700°C has absolutely no effect on the thermal con- thousand hours, compared to an as-annealed tube of
ductivity. the same chemical composition. As far as the chro-
mium content of the alloy is concerned, it would
appear to be an important factor because of the small
III. CORROSION RESISTANCE
solubility of chromium oxides in the low oxygen
containing primary medium. This is confirmed by
The most important material requirement is an
the results shown in Fig. 2 and reported by Sedriks
excellent resistance to corrosion under all conditions
et al., 3 ' 10 which show an excellent behavior of Alloy
found in operation, both normal and faulted. In
690 and also of Alloy 800, compared to Alloy 600.
fact, a large amount of the radiation doses absorbed
by the personnel during operation and maintenance
comes from long life isotopes carried by corrosion
products in primary circuits. Consequently, it is
absolutely necessary to obtain the smallest release
of corrosion products from the large surface areas
of the steam generators. In addition, the greatest
number of problems affecting the tubes comes from
corrosion, which can take many complex forms
according to the chemical conditions to which the
tubes are subjected.

III.A. Corrosion by the Primary Coolant

III.A.l. Release of Corrosion Products to the Circuits
A number of laboratory studies have been made
on the release rate of different austenitic materials
in pure water or primary coolant (boric acid, lithium
hydroxide, hydrogen). 7 There is considerable scatter-
ing in the results obtained, which can be explained
by the small amount of oxide released by laboratory-
size coupons and the complex role played by temper-
ature, pH, and hydrogen. Nonetheless, two factors Chromium (%)
seem to markedly influence the release rate: the Fig. 2. Effect of chromium content on material lost to
surface condition of the tubes 8 ' 9 and the chromium stream in 316 deaerated water flowing at a velocity
content of the alloy. Sandblasting the inside surface of 5.5 m/s (see Ref. 3).
 III.A.2. Stress Corrosion Cracking in the
Primary Medium
After various operational periods, the steam
generator tubes in Alloy 600 of several PWRs have
shown evidence of cracking starting from the primary
side. 11 These defects are found at the ends of the
roll expanded zones 12 (in such cases, they propagate
perpendicular to the highest residual stresses resulting
from the mechanical expansion), or in the vicinity of
the tube support plates when denting has occurred, 1 3
or also in the upper part of the tubes bent to the
smallest radius (first row). 12 These defects are attrib-
uted to i n t e r g r a n u l a r stress corrosion cracking
despite a chemical composition of the coolant gen-
erally considered unlikely to provoke this type of
corrosion in austenitic steels and alloys. But since
1959, Coriou et al. 14 had drawn attention to the
risk of stress corrosion cracking of Alloy 600 under
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high stress in pure, high-temperature, oxygen free
water. These results have given rise to long controver-
sies between research workers for nearly 30 years.
It is now accepted that this type of corrosion can
affect Alloy 600 (Refs. 15 and 16). The time to
rupture varies greatly from one heat to another
and appears to be very sensitive to the test tempera-
ture between 290 and 355°C (Ref. 17). The cracking
mechanism in such a medium and the scattering of
the results have never been clearly explained. We have
introduced the hypothesis that the same phenomenon
could be studied in dilute sodium hydroxide solutions
(0.4% by weight), bearing in mind the numerous
similarities between the phenomena produced in
both media. 18 Corrosion in dilute sodium hydroxide
solutions is presented in Sec. III.B.3.
The phenomenon has never been observed on
Alloys 800 or 690 nor on stainless steels. Coriou
et al. 14 indicated that it only affects austenitic alloys
with high nickel content. Heat treatment at 700°C
gives Alloy 600 a more resistant structure to this
type of corrosion 1 6 ' 1 7 ' 1 9 and greatly reduces the
level of residual fabrication stresses in the tubes.
Thus, it reduces the risk of this type of corrosion
appearing in plants using such thermally treated
tubes.
The risk of "pure water" cracking of Alloy 600
after a certain time, which can indeed be long if
the stresses are reduced, is certainly a weak point
for this alloy compared to the other alternate
materials.
III.B. Corrosion from the Secondary Side
The greatest number of observed incidents of
corrosion starts from the secondary side. 15 ' 20 The
presence of impurities in the feedwater, frequently
due to the accidental in-leakage of cooling water
through the condenser and the concentration of these
impurities or other additions on the tubes as a result
of boiling 21 has led to many different types of corro-
sion. Material resistance to each type of corrosion
must be considered separately, as their mechanisms
are different.
III.B.1. Corrosion by Phosphate Solutions
The phenomenon of acidic sodium phosphate
concentration leading to a general attack of the tubes
by the formation of iron, chromium, and nickel
phosphates, either nonprotective or soluble, has
been studied at length. 20 ' 22 The different materials
compared appear to behave very similarly in these
concentrated phosphate solutions. In many cases,
treatment of secondary water with phosphates has
been abandoned.
III.B.2. Pitting Corrosion
Model boiler tests have shown that when feed-
water is contaminated with seawater, pits can appear
on all the austenitic materials that have been tested.
In contrast, pitting has rarely been observed on steam
generator tubes of nuclear power stations and, as
far as we know, has never given rise to leaks from
primary to secondary medium. Therefore, it does not
appear that resistance to pitting corrosion in service
conditions is an important criterion of selection for
these austenitic alloys. In addition, comparative
tests between Alloys 600, 600 thermally treated,
690, 800, and austenitic stainless steels carried out
at EdF have shown that resistance to pitting is similar
in high-temperature chloride solutions. Low-tempera-
ture corrosion tests have shown the favorable effect
of molybdenum for 18-10 stainless steel and the
unfavorable effect of thermal treatments giving struc-
tures heavily sensitized to intergranular corrosion
(1 h at 700°C for Alloy 600, for example). By extend-
ing the duration of the treatment at 700°C to 10 to
16 h, this unfavorable effect is suppressed. It was also
noted in these tests that the surface preparation of
the tube markedly affects the susceptibility to pitting
corrosion: A high roughness has a very unfavorable
effect as was noted earlier for stainless steels in
ferric chloride. 23
III.B.3. Stress Corrosion Cracking
III.B. 3.a In the Presence of Chlorides. The favorable
role of nickel with respect to stress corrosion of
austenitic alloys in chloride environment is well
known. The main reason for adopting Alloy 600
for steam generator tubing in seawater-cooled plants
was its resistance to this type of corrosion. The
18-10 type stainless steels are known to be very
sensitive to chloride stress corrosion cracking. Duplex
stainless steels are much more resistant. 4 Nonetheless,
model boiler tests 24 (with a heat flux of 10 to 17
W/cm 2 ) have shown that a duplex stainless steel tube
 can crack after 1500 h in case of seawater in-leakage
in the area of the tube in contact with magnetite
deposits (Fig. 3). After 10 000 h in the same con-
ditions, an Alloy 800 tube shows an 800-jum-deep
transgranular crack (Fig. 4). After 25 000 h in these
conditions, neither Alloy 600 nor Alloy 690 has
shown leaks or cracks detectable by an eddy current
internal probe, which confirms their good resistance
to chloride stress corrosion cracking.
Note that Alloy 600 is not, however, completely
immune to chloride stress corrosion cracking. Previous
works mention cracking in hot chlorinated solutions
when the alloy is sensitized and submitted to high
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. 200 jum
I

Fig. 3. Model boiler tests with seawater contamination: Fig. 4. Model boiler test with seawater contamination: stress
stress corrosion cracking of a duplex stainless steel corrosion cracking of an Alloy 800 tube after
tube after 1500 h under magnetite deposits. 10 000 h.
 stresses. 25 In the same way, in our tests, C-Ring and
U-Bend-type specimens of Alloy 600 show deep
cracks (200 jum) localized only in the stressed area,
after 800 h of test in solutions containing boric acid
(50 g/fi of boron) and chlorides (2 g/C CI") at 100°C
(Fig. 5). Comparison with solutions of the same pH
but without boric acid seems to indicate an accelerat-
ing effect of boron. High-temperature tests in similar
solution are now being carried out.

III.B.3.b. Caustic Stress Corrosion Cracking. The

presence of sodium hydroxide has been considered
as responsible for stress corrosion cracking of Alloy
600 tubes in many steam generators. This sodium 50 ix m
hydroxide can come from the decomposition of
sodium carbonate in case of river water in-leakage Fig. 5. Stress corrosion cracking of Alloy 600 at 100°C in a
through the condenser. It can also be due to decom- solution containing boric acid (50 g/C boron) and
position of sodium phosphates by precipitation of a chloride (2 g/C CI"). U-bend specimen after 800 h.
Downloaded by [University of Florida] at 18:36 23 October 2017

phosphate less rich in sodium or by reaction of these

phosphates with iron oxides. When condensate polish-
ing is used, release of sodium hydroxide from the
resins can also occur. Boiling may cause sodium
hydroxide to concentrate in contact with the tubes in
confined areas where the flow rate is reduced. Ther-
modynamically, one can get sodium hydroxide con-
centrations of ~50% at the hot leg of the tubes. 2 1
Consequently, one must study the behavior of
materials in caustic solutions of a wide range of
concentrations.
We summarize here the results obtained at EdF
with fatigue pre-cracked specimens, type WOL or
DCB, which make it possible to evaluate the crack
propagation rate da/dt as a function of the stress
intensity factor Kj. The stress corrosion cracks pro-
pagated in these specimens are measured by scanning
electron microscopy examination after post-test
fracture of the specimens. The materials studied
are shown in Table IV.
The results obtained (Fig. 6) lead to the following
conclusions:

350°C WOL-TYPE SPECIMENS

10 10

- A l l o y 6 0 0 M A - N a O H 100 g/C

A l l o y 6 0 0 M A - N a O H 4 g/C

A l l o y 6 9 0 M A - N a O H 1 0 0 g/C
-C -C
E A l l o y 6 0 0 H T - N a O H 1 0 0 g/C 1 1
<0 I IB I*.
"oro A l l o y 6 0 0 H T - N a O H 4 g/C
tjI-D

A l l o y 6 9 0 H T - N a O H 100 g/C

0.1 0.1

A l l o y 6 9 0 M A - N a O H 4 g/C

0 10 20 30 40 50 60 0 10 20 30 40 50 60

K , (MPa \ / m ) K, (MPa \ / m )

Fig. 6. Stress corrosion tests in deaerated sodium hydroxide at 350°C on fracture mechanics-type specimens: comparison of
Alloys 600 and 690 behavior. Effect of heat treatment at 700°C for 16 h.
 TABLE IV
Characteristics of Alloys 600 and 690 Products Used for Caustic Stress Corrosion Tests on Fracture Mechanics-Type Specimens

Chemical Composition
(wt%)

Material Product Carbon Sulfur Phosphorus Silicon Manganese Nickel Chromium Iron

Plate
Alloy 600 0.072 0.006 0.011 0.27 0.34 73.5 16.0 8.6
20 mm thick

Alloy 690 Bar 0.015 0.002 0.012 0.09

0 100 mm 0.15 61.5 27.1 10.6

Tensile Properties

Room Temperature 343°C

Yield Ultimate Yield Ultimate

Strength Strength Elongation Strength Strength Elongation Grain Size
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Material Heat Treatment 3 (MPa) (MPa) (%) (MPa) (MPa) (%) (ASTM)

MA 950 to 980°C 360 760 36 290 680 35 8 to 9

MA + HT 1 6 h a t 700°C 350 740 37 300 690 35 id.
Alloy 600
SA 1150°C WQ 2 to 6
225 630 56 190 610 64
(heterogeneous)
SA + HT 1 6 h a t 700°C 307 713 36 263 660 39 id.

MA 1035°C 240 630 55 180 530 54 5 to 7

Alloy 690
MA + HT 16 h a t 700°C 242 624 54 id.
a
MA = mill annealed; HT = heat treated; SA = solution annealed, and WQ = water quenched.

1 . T h e curves da/dt = f(K[) show the existence
of a threshold value Kjscc below which no crack
propagation can be observed in these tests. Beyond
this threshold, the crack growth rate increases very
rapidly and reaches a high value, almost independent
of K{. The value of Kjscc and of the plateau crack
growth rate can be used to differentiate the behavior
of the alloys and the aggressiveness of the solution.
2. In 100 g/£ sodium hydroxide, Alloy 600 mill
annealed is the less resistant of all the alloys studied
(apart from 18-10 stainless steel for which the crack
propagation is extremely fast). For values of Kf
above 9 MPa V m , the propagation rate is higher than
6 /zm/h. The behavior of Inconel 690 is much better.
The corresponding Kjscc value is somewhat higher
and the plateau crack growth rate much lower.
Results on Alloy 800 are widely scattered.
3. In 4 g/G sodium hydroxide, Alloy 600 is still
very sensitive to cracking. The crack propagation
rate is only slightly lower than in the 100 g/C solu-
tion, but the value of K[scc is somewhat higher.
(One should note that the crack propagation rate in
pure water, evaluated in a different test by Bulischek
and Van Rooyen, 1 7 is shown to be very similar to
that obtained here in 4 g/£ sodium hydroxide solu-
tion, but the corresponding value of Kjscc un-
known.) At the same concentration, Alloy 690
has shown no significant cracking even for very high
values of Kj.
4. Heat treatment at 700°C improves the behavior
of mill-annealed Alloy 600. (The same result is
obtained when this treatment is applied after solution
annealing at 1150°C.) The improvement provided
by the heat treatment is equally noticeable in 4 g/fi
solution. The behavior of Alloy 690 in 100 g/£
sodium hydroxide is also much improved by heat
treatment at 700°C.
5. Tests on fracture mechanics-type specimens
can only be carried out on products of sufficient
thickness. In this study, we have used 20-mm-thick
plates or 100-mm-diam bars. Application of this to
steam generator tubes leads one to look at two
points:
a. Is the microstructure of the products studied
representative of tube microstructures?
 b. How can the results be applied to the small ALLOY 600, 350°C
cracks observed on steam generator tubes?

Alloy 600 tubes can exhibit a wide variety of

microstructures as a function of their chemical
composition (carbon content) and manufacturing
process (temperature of the annealing treatment). 2 6
These microstructures differ in the distribution of
chromium carbides (principally M 7 C 3 in the mill-
annealed condition) and in the grain size. The struc-
ture of the plate studied [grain size American Society
for Testing and Materials (ASTM) 8-9 and distribu-
tion of chromium carbides outside the grain boun-
daries] is characteristic of a relatively high carbon
content and a low annealing temperature. Such a
microstructure can be seen on m a n y tubes. In these
conditions, heat treatment for 16 h at 700°C causes
only a few carbides to precipitate at grain boundaries.
But we also mentioned above that very similar
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corrosion results were obtained when the heat treat-

m e n t of 16 h at 700°C was given to specimens
previously solution-annealed at 1150°C f o r 30 min,
which put a large n u m b e r of carbides into solution.
In this case the 700°C t r e a t m e n t produces an intense Initial crack depth a0 (mm)
precipitation of carbides at the grain boundaries
and inside the grains. Fig. 7. Time for propagation by caustic stress corrosion
cracking of an "infinite length" (>20-mm) longitu-
No specific formula gives the stress intensity
dinal crack in a 0 22.2- X 1.27-mm Alloy 600 tube
factor KJ for through-wall or partially penetrating from initial depth aQ to critical depth ac (tube burst-
cracks in tubes. A reasonable hypothesis, when the ing in case of secondary side depressurization).
thickness of a t u b e is small compared to its diameter,
is that cracks form between plane surfaces 1.27 m m
apart under a normal stress a. The crack shape is
assumed to be that of a half ellipse. Under such additional safety margin. The advantage of the heat
conditions, the stress intensity factor is given approxi- treatment can also be seen f o r a weak contamination
mately by the expression (NaOH = 4 g/C), rapid crack propagation occurring
for cracks of 60% thickness f o r heat-treated material
05 instead of 50% f o r mill-annealed material. As far as
(to)
5 '
Kj= 1.12 M c t ^ — (Ref. 27) , mill-annealed Alloy 690 is concerned, the correspond-
ing crack d e p t h is ~ 5 0 % f o r a caustic contamination
where M and Q are correcting factors.
reaching 100 g/£ and it becomes equal to that of
F r o m these results, it is possible t o q u a n t i f y the
the critical crack d e p t h f o r a 4 g/£ contamination.
advantage obtained by heat treating the tubes at
These fracture mechanic tests do not enable one
700°C from the point of view of crack propagation
to study the period corresponding to initiation and
rate under stress corrosion condition (Fig. 7). Thus,
slow crack growth. Crack initiation f o r u n n o t c h e d
when a strong sodium hydroxide contamination
specimens of various shapes has been studied by
(100 g/C) is present locally in contact with the
several authors. 1 8 ' 2 8 " 3 5 The curves (Fig. 8) summarize
tubes, a pre-existing longitudinal crack with depth
the results we obtained f o r various sodium h y d r o x i d e
> 1 7 % of the thickness a is likely to propagate very
concentrations at 350°C in autoclaves. The specimens
rapidly until reaching the critical depth of 66%
(C-rings) are machined f r o m industrial tubes of
thickness, which will allow bursting if the secondary
various origins. They are stressed at a theoretical
medium is depressurized. For a tube heat treated
value equal to the yield stress. A previous s t u d y 1 8
at 700°C, taking into account the microstructural
has shown that the real value of the stress could
and the stress relieving effects of the treatment,
be slightly different f r o m the yield stress as a result
crack depths smaller than ~ 4 0 % of thickness cannot
of stress relaxation. The actual stress is ~ 8 0 % of the
give rise to rapid propagation, which provides an
yield stress and even less for Type 316 stainless steel.
Taking into account some scatter in the results,
a
We suppose the length of the crack to be >20 mm. The we have plotted the minimum time (evaluated f r o m
values apply to tubes with 0 = 22.2 mm and thickness = 1.27 a large number of tests) t o obtain a 500-Mm deep
mm. crack, i.e., 40% of the thickness of a 1.27-mm tube.
 D E A E R A T E D CAUSTIC SODA a low strain rate in the spectrometer under high
SOLUTION—350°C vacuum (3 X 10"10 Torr). The results obtained, 3 7 in
C-RINGS STRESSED T O o ^ y s agreement with those of Airey, 38 confirm that the
A C C O R D I N G T O ASTM STP 425 only noticeable impurity observed at the grain
boundaries is phosphorus. The concentration of
4000 phosphorus appears to increase after treatment at
uOS 700°C, which does not readily explain the observed
improvement in the stress corrosion cracking resis-
E tance. It has been noted that this treatment increases
a. the tendency to hydrogen embrittlement as revealed
o 3000
o by bursting tests on disks under hydrogen pressure. 39
IT)
So, in this case, the mechanisms of caustic stress
O)
c corrosion cracking and of hydrogen embrittlement
"o appear to be different.
3
TJ 2000
C Studies have also been carried out to show the
possible role of carbon precipitation at grain bound-
a) aries on the resistance to stress corrosion. To compare
6 the deformation mode at 350°C of Alloy 600 mill
V'
1000
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E annealed and heat treated at 700°C, examination by

3 electron microscopy has been performed at EdF
£ on specimens previously submitted to 1200-h creep
40 100
NaOH concentration (g/ft)
Fig. 8. Resistance to stress corrosion cracking of Alloy 600
mill annealed or heat treated at 700°C, Alloy 690,
Alloy 800, and Type 316 stainless steel as a function
of sodium hydroxide concentration at 350°C.
It has been noted that the relative behavior of the
alloys varies as a function of the sodium hydroxide
concentration. (It has also been previously men-
tioned 1 8 that it varies with the applied stress.) The
results confirm the sensitivity of Alloy 600 to stress
corrosion in dilute sodium hydroxide solutions.
They also show the marked improvement due to heat
treatment at 700°C.
III.B.4. Hypothesis on the Mechanism Responsible
for Improvement of the Caustic Stress
Corrosion Resistance of Inconel 600
with Heat Treatment at 700"C
Several studies have been undertaken to explain
the intrinsic improvement of the behavior of Alloys
600 and 690 with heat treatment at 700°C. Use of
an Auger spectrometer has enabled us to study the
impurity segregation at the grain boundaries of Alloy
600. An intergranular surface can be obtained after
embrittlement of the specimen by cathodic hydrogen
charging at 200°C in a mixture of neutral and acidic
sulfates of sodium and potassium having the eutectic
composition, and saturated with water continuously
introduced into the bath (a technique developed by
Elkholy et al. 36 ). The specimen is then fractured at
tests under a stress approaching the yield stress and
on specimens submitted to a tensile strain of 2 or
10% at 350°C. These studies show that in these
materials at this temperature and for a maximum
strain of 2%, the deformation is generally planar
and results in the buildup of dislocations on the grain
boundaries. Fine intergranular precipitates as found
in heat-treated specimens can modify the strain
distribution at the grain boundary region as shown
by Lee and Vermilyea, 40 and reduce the ability of
this region to undergo shear. These authors con-
sidered this fact as a possible cause of corrosion at
the grain boundaries of sensitized Alloy 600. How-
ever, assuming that the strain rate is a critical factor
in the stress corrosion mechanism, one may suppose
that fine precipitates of chromium carbides can also
modify this strain rate in such a way as t o improve
the stress corrosion behavior of Alloys 600 and 690
in pure water and caustic solutions. The greater
corrosion susceptibility of these materials in the
sensitized condition in the tests mentioned by Lee
and Vermilyea could be explained by a different
behavior of the chromium depleted zones.
III.B.5. Corrosion by Sulfur-Containing Products
Alloy 600 tube damage has often been caused
by sulfur-containing products, identified by electron
microprobe examination. Certain cases involve
pits found on the outside of the tubes before
assembly and caused by prolonged storage under
humid conditions (Fig. 9). Another example was
discovered on one of the steam generators of the
Tihange power station in 1974 before starting up,
when a number of tubes were found leaking in
zones showing extensive intergranular embrittlement.
This embrittlement was associated with sulfur at the

V.
f-'-y
--'f v (according to German specification DIN 50 018)
Downloaded by [University of Florida] at 18:36 23 October 2017
Fig. 9 . Typical pit found on Alloy 600 tubes after prolonged
storage at room temperature under humid conditions.
X-ray microanalysis of the products found inside the
pit, showing the presence of sulfur and chlorides.
grain boundaries. Sulfur-containing pits were also
found on the outside of the tubes, in the crevice
between tube and tube plate, in the same steam
generator. Another case, somewhat similar, was
reported during a shutdown period of the Palisades
power station: Intergranular cracks were found and
also associated with the presence of sulfur-containing
products. In each of these different cases, the origin
of the sulfur was not positively identified: it could
have come from tube contamination by oils, by
sulfur dioxide from the atmosphere, by release
products from ion exchange resins or antifriction
or de-oxygenizing agents.
It is known that stainless steels and high nickel
alloys can be embrittled by sulfur. In addition, in
a laboratory, it is possible to reproduce different
corrosion attacks very similar to those due to sulfur-
containing products. Pits have been easily obtained
on Alloy 600 in dilute solutions of sulfurous acid
at 40°C (concentration of 0.6 wt% of S 0 2 ) . In the
case of "sensitized" tubes, these sulfurous acid solu-
tions produce an intergranular corrosion and some-
times also a deep i n t e r g r a n u l a r cracking under
mechanical tension. Similarly, we have shown that
a test in humid atmosphere containing S 0 2 at 40°C
can produce pitting in a very short time on Alloy
600, while Alloys 800 and 690 show a better resis-
tance.
Tubes in austenitic alloys when sensitized can
also suffer intergranular stress corrosion in poly-
thionic acids H 2 S x 0 6 (Fig. 10) without any pene-
tration being observed in the absence of mechanical
stresses. This stress corrosion phenomenon is closely
related to the chromium content of the alloy. T o
prove it, we used high purity alloys (carbon = 0.003%)
with 76 to 85% nickel, 8% iron, and variable chro-
mium contents melted in plasma furnaces by the
"Centre de Chimie Metallurgique de Vitry." A U-bend
specimen of the 7% chromium heat, in the solution-
annealed condition, gave transgranular cracking in
polythionic acids (Fig. 10) whereas no corrosion
occurred in heats with chromium contents >10%.
Solutions of polythionic acid can be prepared
by hydrogen sulfide bubbling in 6% sulfurous acid
solution at 0°C (according to ASTM G 35). Chro-
matographic analysis of these solutions has been
undertaken 4 1 and showed that tetrathionic acid could
reach a concentration of 0.3 M/9.. The classic prepara-
tion, long, unstable, and of poor reproducibility, can
thus be advantageously replaced by the dissolution
of commercial sodium tetrathionate. It is possible
to obtain stable solutions in which stress corrosion
cracking occurs after durations similar to those
obtained with classic solutions (Fig. 11) by dissolving
0.1 M (30.62 g) of 99% crystalline sodium tetra-
thionate (Na 2 S 4 0 6 , 2 H 2 0 ) in 1 £ of distilled water
at room temperature. The test can be carried out
at 40°C, which increases the sensitivity and does
not change the stability. This reagent was used in
our laboratory to evaluate residual fabrication stresses
of tubes, bends, and expanded zones of Alloy 600.
It appears, in conclusion, that to avoid all risks
of this type, one should use materials which, in the
as-fabricated condition or after a long service expo-
sure, are not sensitized to intergranular corrosion
(i.e., with no noticeable differences in chromium
content at the vicinity of the alloy grain boundaries).
Such a sensitization could occur if chromium carbides

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(a)
(b)
Fig. 10. Stress corrosion cracks in polythionic acids devel-
oped on (a) a low-chrome, high-purity nickel alloy
(85% N i - 7 % C r - 8 % Fe), solution annealed (trans-
granular cracking), and (b) a commercial Alloy 600
tube, sensitized 1 h at 700°C (intergranular cracking
along chromium depleted zones).
A L L O Y 600 SENSITIZED (1 h 700°C)
(D In polythionic acids
In Na 2 S 4 0 6 0.1 M
Q-
01
u
CO
Time (h)
Fig. 11. Comparison of stress/time diagrams for stress corro-
sion cracking of sensitized Alloy 600 in polythionic
acids and in sodium tetrathionate at room tempera-
ture.
precipitate either during cooling of the tubes after
annealing, or when stress relieving the welds of the
channel heads, or after a long service exposure if
the materials have a high carbon content in solution.
To overcome this risk, several solutions are
possible.
1. Greatly lower the carbon content of the alloy,
which results in a reduction of tensile properties
(see Sec. II.B.2). This loss can be compensated for
by cold working (as done in some cases with Alloy
800).
2. Raise the chromium content, as in Alloy 690,
which has a very good resistance to intergranular
corrosion, especially for the low carbon contents
presently obtained.
3. Perform a thermal treatment to precipitate
the chromium carbides before the final annealing
treatment, which will be then carried out at low
temperature.
4. Carry out the heat treatment at 700°C (under-
taken principally to reduce the residual fabrication
stresses and to obtain an optimal microstructure
to resist caustic stress corrosion cracking) for a dura-
tion long enough to rehomogenize chromium-depleted
zones. The final result of this heat treatment at
700°C cannot be achieved by the other solutions
described above, which need to be supplemented
by other operations, such as shot-peening of the
outside surface of the tubes, as done in Germany
for Alloy 800.
 II.C. Improvement of the Stress Corrosion Resistance by 300
Reducing the Residual Fabrication Stresses

Improvement of the stress corrosion resistance of 200

tubes has been achieved by reducing as far as possible
the residual stresses due to fabrication and assembly.
\
Heat treatment at 700°C of straight tubes and bends
nj
CL
100
/ \\
*
of <250-mm radius in Alloy 600 reduces the hoop /
stresses due to straightening and polishing (which
are normally at least 150 MPa) and the longitudinal
stresses due to bending (which for small radius bends 60 M) 180 300
can exceed 300 MPa) to < 5 0 MPa. • — 1 — •
This heat treatment was preferred to other stress -100 — t —
relieving methods using "mechanical" means (stress Angular abscissa (deg)
relieving by stretching or by internal pressure) for the (a) Hoop stress
improvement already mentioned concerning the
microstructure, and also because the mechanical
stress relieving methods, though appearing simple, 300 -t-
Downloaded by [University of Florida] at 18:36 23 October 2017

can have numerous difficulties.

V-<3>
Indeed, these methods, if applied without caution,
may themselves introduce residual stresses as high 200
as those that are meant to be relieved. 42 We have <0
CL
shown that this effect is caused by the existence on
the tube surface of a layer that has been heavily 100 - A 4 X
cold worked by straightening and belt polishing
and hence has higher mechanical properties than
the metal bulk. Whenever a tensile strain or an 0
internal pressure is applied, which slightly yields 120 (J) 240 360

plastically the underlying metal, this surface layer

remains elastic and ends up with a residual tension
when the load is removed (Fig. 12).
The same effect is also produced when making
a large radius bend from a tube cold worked by
straightening and polishing. The stresses on the bend
surface, over a depth of ~ 5 0 to 100 jum, can reach
values much above those normally expected (Fig. 13).
Heat treatment at 700°C carried out on straight tubes
before bending, in producing a recovery of the cold-
worked layer, avoids this effect and after bending
gives a much lower stress level at the surface of large
radius bends, which could be very difficult to stress
relieve in a furnace. For tubes that have been sand-
blasted internally, it is likely that the same effect
occurs.
For small radius bends, one must bear in mind
that, even stress relieved, they can be subjected to
service stresses much higher that those in straight
tubes due to ovalization or other geometric irregu-
larities. To minimize the consequences of this factor,
these irregularities must be reduced as much as
possible (with the additional advantage of making
internal control by eddy current probes easier).
Reduction of tube stresses in the expanded area
is accomplished in EdF power stations by mechanical
stress relieving of the transition zone between the
deformed part and the nondeformed part of the
tube. 4 3 This operation, which takes place after
expanding, consists of subjecting the transition zone
-100
A
Angular abscissa (deg)
(b) Longitudinal stress
Alloy 6 0 0 straight tubes
Residual stresses on the o.d. (x rays)
© As-received (straightened, polished)
(?) 0.4% plastic tensile strain
(3) 0.8% plastic tensile strain
Fig. 12. Effect of a stretching operation on the residual
stresses of an Alloy 600 tube superficially cold
worked by straightening and belt polishing.
to a controlled diametrical deformation using a tool
with rotating rollers. The high longitudinal stresses
in this zone are then reduced to < 1 0 0 MPa. Com-
pared with other processes leading directly to ex-
panded zones with low tensile stresses (internal
pressure or explosive bonding for example), the
method gives a much better leaktightness of the tube
to tube plate joint, which appears preferable, bearing
in mind the risks of corrosion in this area.
The different techniques used to stress relieve
Alloy 600 tubes are equally applicable to Alloy 690,
which has relaxation kinetics at 700°C very similar
to Alloy 600. For Alloy 690 one can even reduce the
heat treatment at 700°C to a few hours, which is
 300
200
a.
g nate choice to heat-treated Alloy 600. The lower
o
Intrados
Intrados
-V Fla nk Flank
-200
1V/
Downloaded by [University of Florida] at 18:36 23 October 2017
V
-300
-400
Angular abscissa (deg)
Longitudinal stress
Alloy 6 0 0 large radius bend (1500 mm)
Residual stresses on the o.d. (x rays)
© Straightened, polished, bended
(f) = (T) - 1 1 0 |im (electropolishing)
(3) Straightened, polished,
HT 10 h at 700°C, bended
Fig. 13. Effect of a superficial cold work of the straight
tube on the residual stresses after bending.
enough to get the stress level desired. As mentioned
above, due to the high chromium content of this
alloy, exposure at 700°C does not induce sensitivity
to intergranular corrosion and it is not necessary,
as with Alloy 600, to adjust the heat treatment
duration to rehomogenize the chromium content at
the vicinity of the carbides.
As far as the duplex stainless steel is concerned,
stress relieving by heat treatment is not possible
because of the risk of embrittlement already men-
tioned.
IV. CONCLUSION
The different characteristics of Fe-Cr-Ni austenitic
alloys have been compared to show how they meet
the PWR steam generator tubing requirements. It
has been shown that the 700°C treatment of Alloy
600 straight tubes and small radius bends, as applied
by WEC and Framatome, significantly improves the
resistance to stress corrosion cracking; it decreases
the stress level and gives the alloy a microstructure
that is more resistant to caustic stress corrosion crack-
ing and is not sensitized to intergranular corrosion.
Is there a better material than Alloy 600 heat
treated at 700°C that is considered as our reference
material at this time? Table V shows the benefits
and drawbacks of the two best alternate materials
that could be considered for a near-term application:
Alloys 800 and 690.
It appears to us that Alloy 690 is the best alter-
corrosion product release in the primary coolant and
the absence of risks of stress corrosion cracking in
"pure water" may be attractive enough to consider
its application in the future.
i
ACKNOWLEDGMENT
Some of the EdF data reproduced in this article have
been obtained in a research program that is part of the CEA-
EdF-Framatome-Westinghouse agreement. We thank the other
partners for permitting publication.
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 TABLE V
Comparison of Candidate Materials for Steam Generator Tubes to Alloy 600
Thermally Treated at 700°C Considered as the Reference Solution
Benefits
Versus Alloy 600 Heat Treated at 700°C
Better resistance to stress corrosion cracking in pure
water or low concentration caustic solutions
Alloy 800 Lower corrosion product release in the primary
coolant
Better resistance to stress corrosion cracking in pure
water or low concentration caustic solutions
Much lower corrosion product release in the primary
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Susceptibility to chloride stress corrosion cracking
Mechanical properties lower at service temperature
Thermal conductivity lower
Thermal expansion coefficient higher than for
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