Int. J. Pres. Ves.

& Piping59 (1994) 41-49

(~ 1994ElsevierScienceLimited
Printed in Northern Ireland. All rights reserved
0308-0161/94/$07.00
ELSEVIER

The performance of Alloy 625 in long-term

intermediate temperature applications
Charles Thomas
Industrial Research Ltd, PO Box 31-310, Lower Hutt, New Zealand

&

Peter Tail
Methanex New Zealand Limited, New Plymouth, New Zealand

Alloy 625 is frequently used in applications requiring a combination of high

strength and corrosion resistance. Examples of material exposed in service in a
petrochemical plant for 50 000 h at 500°C were found to have suffered severe
hardening and loss of ductility. The mechanical properties of the material and
the reasons for the change in properties are described along with remedial heat
treatments that were developed for on-site application to the entire vessels.

INTRODUCTION corrosion resistance while the addition of

Alloy 625
Alloy 625 (UNS N06625) has found widespread
applications in the aerospace and petrochemical
industries due to its excellent combination of
strength, at both ambient and elevated tempera-
tures, corrosion resistance and ease of fabrica-
tion. These properties have seen it used in the
aerospace industry for applications such as gas
turbine engine exhaust systems, spray bars,
thrust reverser systems, turbine shroud rings,
fuel/hydraulic line tubing and bellows amongst
many others. In the petrochemical industry, it
has been used in a wide variety of plant
applications including bubble caps, process
tubing, reaction vessels, distillation columns,
heat exchangers and valves. It has also found
widespread use in marine service for its
resistance to sea-water corrosion and in the
nuclear industry. Designed originally as a
solution strengthened alloy, j those elements used
to impart strength to Alloy 625 also proved
highly successful at providing excellent resistance
to corrosion. Chromium and molybdenum are
the main contributors to both strength and
41
niobium was found to significantly improve creep
strength.
Elements such as aluminium and titanium
which are known to produce an age hardening
response in nickel base alloys through the
precipitation of coherent Ni3(AI, Ti) y' phase
were kept to low levels with the intention of
producing a material with good thermal stability.
However, niobium has been subsequently
found to cause age hardening after significant
periods at approximately 650°C by the precipita-
tion of Ni3Nb or ),".1 4 Indeed, this behaviour led
to the development of Alloy 718 in which the age
hardening response was deliberately encouraged
and exploited by alloying with controlled levels
of titanium and aluminium. Nevertheless, the
concept of a strong, tough and corrosion resistant
material persisted and Alloy 625 has found
widespread application.
Intermediate temperature application--the
problem
As a result of experience in a petrochemical plant
in which less corrosion-resistant materials had
proved unsatisfactory, 5 Alloy 625 was specified
42 Charles Thomas, Peter Tait
for feed stock superheaters which operated at
between 480 and 560°C with the higher end of
this range being reached only occasionally.
Temperatures were typically limited to 500°C and
at the time that Alloy 625 was specified, no
reference to hardening at this temperature was
found and the general consensus from a variety
of material suppliers and laboratories was that
Alloy 625 would perform satisfactorily at these
temperatures.
At a routine plant outage, a small amount of
maintenance welding was undertaken and it was
found that the material weldability was poor and
cracking occurred. Subsequent on-site inspection
found that the material was significantly harder
than expected.
Samples of material which had been in service
for approximately 5 0 0 0 0 h have been made
available and a programme of work was
undertaken to characterise this material and
compare it with material supplied as new.
MATERIALS
The used Alloy 625 has been part of the shell of a
feed stock superheater. It had been supplied with
original plant and had been in service for
approximately 5 0 0 0 0 h (6 years). The heat
treatment prior to delivery was 1 h at 1000°C
followed by a quench. The new material tested
for comparison was supplied as being 'annealed
at 1050°C, rapid cooled'. The chemical composi-
tions are listed in Table 1.
Table 1. Material chemical composition
Cr Mo Nb Fe C Si AI Ti
Used 20. 8.4 3-78 4.2 <0-10 0.20 <0.05 0.08
New 23 9-0 3-24 4.1 <0-10 0.22 <0.05 0-25
MECHANICAL PROPERTIES
The basic mechanical properties of the materials
are listed in Table 2.
Charpy impact testing was conducted at both
room and plant operating temperatures of 500°C.
The elevated temperature testing was done by
soaking the specimens in a small fluidised-bed
furnace held at approximately 520°C. The
specimens were held in a stainless-steel test piece
Table 2. Mechanical properties of materials
New" Used
20°C 500°C 20°(2 500°C
UTS (MPa) 937 844 1 384 1 257
0.2% Proof (MPa) 461 375 1 083 995
% Elongation 46 40 6-7 21
%ROA 60 37 7 31
Charpy impact (J/cm 2) 178 197 19 30
Hardness H V (30) 230 444
" T h e test results for the new material were very similar to the
mechanical properties quoted on the test certificate for the used
material supplied at the time the vessel was manufactured.
holder used to accurately locate the specimen in
the testing machine and to which was strapped a
calibrated 'K-type' thermocouple. The specimens
were removed from the furnace and as rapidly as
possible placed in the testing machine. The actual
time between removal from the furnace and
impact was determined by reference to cooling
curves that had previously been produced using a
standard test piece to which a 'K-type'
thermocouple had been spot welded close to the
V-notch.
It can be seen by reference to Table 2 that the
Charpy impact properties of the used material
were poor. Consequently, it was decided to
measure the fracture toughness of the material.
Fracture toughness testing was conducted on
samples of the used material. Crack tip opening
displacement (CTOD) measurements were de-
termined using the technique described in BS
5762. 6 Using specimens of 1 3 m m nominal
thickness, the critical C T O D (maximum load)
Mn was determined at room temperature to be
0.022 mm.
0.13 C T O D testing is undertaken in order to
0.06
provide data to support engineering assessments
of pressure vessels and other similar equipment
under circumstances where linear elastic fracture
mechanics becomes invalid, i.e. when the
material in question exhibits some degree of
plasticity. In order to obtain a valid value of
fracture toughness in most metallic materials, a
certain minimum thickness of test piece must be
used. Below this minimum thickness, linear
elastic fracture mechanics (LEFM) do not apply
and valid measurements of fracture toughness,
K~c cannot be obtained. The standard for plain
strain fracture toughness 7 testing requires that
the test piece thickness and crack length should
 Alloy 625 in long-term temperature applications
both be greater than
x (K'c) 2
2.5 --~y/
where try is the 0.2% proof stress. C T O D testing
was chosen in the expectation that the used
material would exhibit some ductility. The value
of fracture toughness K at the m a x i m u m load was
calculated according to the procedures of either
BS5447 or BS5762 and found to be
2459 N / m m -3~2. The nominal thickness of the test
piece and the crack length were both 13 m m and
therefore the value of 2459 N / m m -3/2 just
qualified as being a valid value of K,c for
material of yield strength of 1083 MPa (see Table
2). The above equation would require that the
test piece should be at least 12-9mm thick. In
other words, the plasticity exhibited by the used
material in a test piece of this size was sufficiently
low that valid KI¢ values could be obtained.
Further evidence of the low ductility of the
used material was provided during pre-cracking
of one of the test pieces prior to C T O D testing.
Fatiguing was conducted in accordance with the
British Standards 6,7 at a fatigue stress intensity
(Kf) of 8 0 0 N / m m -3/2. Complete failure of a
particular test piece occurred during the fatiguing
operation when the crack had grown to a length
of 14.13mm (test piece thickness 12-85mm,
width 25.70mm). U n d e r the higher strain rate
conditions associated with the fatiguing opera-
tion, the fracture toughness was considerably
lower than when testing was conducted at usual
loading rates. Other than the fact that the crack
had been allowed to propagate slightly further
than was desirable, the conditions under which
the fatiguing operation was conducted were
comfortably within the requirements laid out in
the standards.
The C T O D results were used to indicate the
size of defect in the superheater that could lead
to catastrophic failure, using the techniques
described in British Standards Institution docu-
ment PD6493. 8 The procedure indicated that
surface breaking defects of the order of 2 m m
long by l m m deep were critical at room
temperature.
Following the discovery of the very low
ductility in the used material and therefore of
similar material that remained in service, an
attempt was made to recover some toughness by
a heat treatment that could be performed on the
vessel in situ during a maintenance shut-down.
43
Table 3. Charpy impact properties of used material after
heat treatment (room temperature)
Heat treatment Impact energy Hardness
(J/cm 2) HV(30)
600°C, 12 h 36 373
650°C, 12 h 61 307
700°C, 12 h 57 302
650°C, 3h 54 317
650°C, 6h 56 303
Such a heat treatment would have to be similar
to an in-situ post-weld heat treatment, for
example, and was therefore limited by both
temperature and duration. Samples of the used
material were heat treated at 600, 650 and 700°C
for 3,6 and 12h duration and the toughness
assessed by Charpy impact testing and hardness.
The results are presented in Table 3. C T O D
testing was undertaken on used material that had
been heat treated for 12 h at 700°C in a similar
manner to that for the used as-received material
and in this case the critical C T O D (maximum
load) was found to be 0-155mm at room
temperature. In contrast with the very small flaw
size considered critical in the used material (e.g.
2 mm long by 1 m m deep), the level of toughness
after heat treatment indicated that infinitely long
cracks up to 2.5 m m deep could be tolerated.
Again, this was estimated using the procedures
laid down in British Standards Institution
published document PD6493. 8
MICROSCOPY
Optical microscopy
The optical microstructures of the new, used and
used + heat treated (600°C, 12 h) are shown in
Figs 1, 2 and 3, respectively. The microstructure
of the new material was as expected, having a
mainly equiaxed grain structure and the anneal-
ing twins commonly observed in austenitic
materials. A range of small discrete particles,
presumably carbides of the (Mo, Nb)C o r Cr23C6
types were present both on the grain boundaries
and within the grains. Occasional larger particles
having the characteristic pink colouration of
Ti(C, N) were also present.
The microstructure of the used material was
essentially the same except that in the particular
etch used (15 parts HCI, 10 parts H N O 3 , 10 parts
44 Charles Thomas, Peter Tait

" .,7" ,¢. ...... . ..

..

• "°, 2(~,tl

Fig. 1. Microstructure of new material. Fig. 4. Surface detail of polished and etched sample of used
as-received material as seen in the scanning electron
microscope.

restricted to limited areas usually towards the

centre of larger grains. The microstructure shown
in Fig. 3 was heavily overetched in an attempt to
recreate this effect. While similar to the new
material, the u s e d + h e a t treated material ap-
peared to have a more extensive grain boundary
precipitation.

Scanning electron microscopy

The used material that had exhibited darkening

Fig. 2. Microstructure of used as-received material.
acetic acid: all acids concentrated laboratory
reagentsg), the matrix was heavily darkened (Fig.
2).
The darkening of the matrix observed in the
used material was not seen in the used + heat
treated material except in the material heat
treated at the lowest temperature of 600°C; in
this particular sample, the darkening effect was
of the matrix was examined in the scanning
electron microscope having been polished and
etched as for optical examination• Figure 4
illustrates what appears to be an extensive
precipitation of particles of approximately 50-
100 nm in size.
The u s e d + h e a t treated material had not
exhibited matrix darkening except for a limited
amount in those specimens aged at 600°C. A
scanning electron microscope (SEM) image of
such a specimen is shown in Fig. 5. In this case,

Fig. 5. Scanning electron microscope image of used material

Fig. 3. Microstructure of used + heat treated (600°C, 12 h) heat treated at the comparatively low temperature of 600°C;
material. polished and etched surface•
 Alloy 625 in long-term temperature applications 45

Fig. 6. Scanning electron microscope image of used material

heat treated at 700°C, 12 h; polished and etched surface.
(a)

the particles appear larger and much less

numerous than in the used material.
The other used + heat treated samples did not
exhibit matrix darkening and a typical SEM
image of the polished and etched material is
shown in Fig. 6 which illustrates an example of
grain boundary precipitation.
The fracture surfaces of Charpy impact test
pieces were examined in the scanning electron
microscope. The new material exhibited ductile
dimples on the fracture surface as would be
expected of a tough material. However, despite
the low ductility, the used material also exhibited
the surface dimples caused by microvoid
coalescence and typical of a ductile material.
There was no evidence of brittle or intergranular
fracture. Similarly, the used + heat treated
material had failed in the Charpy impact test
pieces in a ductile manner.
Transmission electron microscopy
Thin foils were prepared from new, used and
used + heat treated materials. Figure 7 shows
bright and dark field images of the used material
and it can be seen that there is extensive
precipitation.
A diffraction pattern (zone axis [001]),) taken
from this material is shown in Fig. 8(a). The
pattern is typical of a ), phase material but
several superlattice reflections are also evident
between the bright spots associated with the y
matrix. Some of the superlattice spots (those that
are streaked and the (110) spot) are due to
platelets of )," phase [10]. Following the
convention used by Paulonis et al. [10], the ),"
precipitate reflections are indexed relative to the
(b)
Fig. 7. (a) Bright, and (b) dark field images of used
as-received material. The dark field image is a composite of
three images each sourced from the same area of the foil but
using different superlattice diffraction spots (see below).
matrix; the "J'' index arises because the y " unit
cell dimension in the " c " direction is very close
to twice that of the fcc ), unit cell and also twice
the " a " and " b " unit cell dimensions of the y "
precipitates [11].
There were also a set of spots on this
diffraction pattern that were not accounted for.
Dark field images using these reflections were not
particularly helpful in identifying their source
except to say that they arose from distinct areas
in the matrix (Fig. 7), that were not readily
identifiable as separate precipitate particles or
phases and were not related to the y"
precipitates. The spots labelled ~240 and ~420 arise
from different areas than those labelled ~gO 22 and
4~0, suggesting that these additional spots are
associated with a c o m m e n s u r a t e superstructure in
the matrix, the origin of which is unknown.
46 Charles Thomas, Peter Tait

• • •

• • •

• • •
Fig. 9. Bright field image of the used + heat treated (700°C,
12 h) material.

• • +,
made generation of a dark field image difficult. In
addition, the unidentified reflections that had
(a)
been present in the diffraction patterns of used
material were not seen in the heat-treated
material.
Figure 9 also illustrates needle like precipitates
020 22O that were not found in either the new or the
as-received used material. It is believed that
O
these are small 6 phase platelets, 6 being the
orthorhombic form of Ni3Nb. 12,13
O In the thin foils of new and used material,
other precipitates were not found to any
O o
0,o °O significant extent. Energy dispersive X-ray
analysis (EDX) analysis of those particles that
were found tended to indicate that they were rich
in particularly molybdenum and niobium. This
O would suggest that they were carbides of the M6C
000 20O type. 14
In the u s e d + h e a t treated materials, grain
boundary precipitates had been seen when
examined in the scanning electron microscope.
(b)
Fig. 8. (a) Diffraction pattern obtained from used as
received material [00]y zone axis. (b) Diagrammatic
representation of indexed pattern. Spots (340), (½10) and
(110) were used to create the composite dark field image in
Fig. 7(b).

The structure of the u s e d + h e a t treated

material (700°C, 12 h) is shown in Fig. 9. The
precipitate density can be seen to be much lower
in the heat-treated material compared to the
as-received used material (Fig. 7). The diffraction
patterns obtained from the heat treated material
were similar to those of the as-received used
material except that the superlattice streaks Fig. 10. Typical grain boundary precipitate seen in the
attributed to the 7" precipitates were weaker; this used + heat treated (700°C, 12 h) material.
 Alloy 625 in long-term temperature applications
Similarly, grain boundary precipitates were
observed in thin foils. However, grain boundary
precipitation was certainly not continuous in this
material and many grain boundaries in the thin
foils appeared free of precipitates. Examples of a
precipitate is shown in Fig. 10. E D X analysis of
these precipitates was inconclusive due to their
small size. However, in addition to the M6C
carbides seen in the new and used materials,
particles with a modest enrichment in molybde-
num and niobium relative to the general material
analysis were observed and it was suspected that
these were blocky grain boundary 6 were other components in the vessel constructed
precipitates. 15
DISCUSSION
After approximately 50000h of service at
approximately 500°C, Alloy625 underwent sig-
nificant age hardening. The increase in strength
was dramatic, the 0.2% proof stress more than
doubling from 461 MPa to 1083 MPa (Table 1).
This degree of strengthening appears to be
significantly in excess of other reported results
for laboratory aged Alloy 625. 3"14"16 Indeed, only
materials that have been deliberately alloyed to
encourage an age hardening response by the
addition of titanium 4 or aluminium in Alloy 718
(Ref. 17), for example, exhibited comparable
tensile properties and hardnesses. The high
strength of the used material was also evident
when testing was conducted at the operating
temperature of 500°C.
More importantly however, the increase in
strength was accompanied by a massive reduction
in toughness and the consequences in terms of
the integrity of the pressure vessels in question
and indeed any similar plant, were of great
concern. Ductility of the used material as
indicated by elongation and reduction of area
measurements, was significantly higher at the
plant operating temperature. This trend was not
strongly reinforced by the Charpy impact tests
suggesting that elevated temperature toughness
was strain rate dependant. The improvement in
ductility at operating temperature compared to
room temperature was insufficient to allay fears
concerning the integrity of pressure containing
plant in which Alloy 625 has been exposed to
intermediate temperatures.
Preliminary assessments of fitness for purpose
47
by use of crack tip opening displacement tests
indicated that the vessels had negligible defect
tolerance and it was concluded without recourse
to more detailed analyses, that salvation for these
vessels lay in improving the material properties
rather than attempting to demonstrate their
integrity.
Trial laboratory heat treatments were chosen
in order that similar heat treatments could be
conducted on-site during a plant maintenance
shut down and were therefore constrained by
temperature and duration. For example, there
of carbon steel and, in addition, there was a
concern that at temperatures much above 700°C,
deformation of the vessel under its own weight
would occur. Fortunately, heat treatment at
comparatively modest temperatures of 650-
700°C and for reasonable times of 6-12 h proved
beneficial in regenerating some toughness. While
the increase in Charpy impact energy was not
massive (from 20 to 60J/cm2), it was most
welcome in increasing confidence as to the safety
of the vessels. The increase in CTOD value was
more dramatic from 0-02 mm to 0.15 mm and the
improvement in defect tolerance as indicated by
the procedures of PD6493 (Ref. 8) was highly
significant.
Examination of the material microstructure
showed that the hardening mechanism was
caused by precipitation of 7". In the optical
examination, the precipitation was too fine to be
resolved but the presence of a precipitate was
readily revealed by the heavy darkening of the
matrix. Similarly, scanning electron microscopy
examination revealed a myriad of uniform and
extremely fine precipitates. It was however, the
transmission electron microscopy that revealed
structures and diffraction patterns that confirmed
the presence of 7".2'""~ However, at this time the
reason for the additional diffraction spots seen on
the thin foils from the used material has not been
identified.
Age hardening of Alloy625 is a recognised
phenomenon ~,3 but not references to the
operation of Alloy 625 at 500°C have been found.
Typically, ageing experiments down to 600°C
have been conducted and at least two time-
temperature-transformation diagrams have been
constructed for Alloy 625 (reproduced in Ref. 3).
These differ largely in the predicted rate of
precipitation of the M23C6 and M6C type carbides
but neither of them would indicate through
48 Charles Thomas, Peter Tait
extrapolation that y" should be expected at 500°C
after 50 000 h.
Examples of Alloy 718 have been aged for up
to 50 000 h at temperatures as low as 538°C (Ref.
17) but the objective of that work was to assess
the possibility of softening by overageing of a
material that had previously been age hardened
deliberately. The work showed that aging for up
to 50 000 h caused a slight increase in strength of
age hardened Alloy718. Controlled aging of
Alloy 625 has shown 3 that 0.2% proof strengths
of up to 800 MPa and hardness of approximately
350HV can be achieved but these are con-
siderably lower than observed in the material
aged for 5 0 0 0 0 h at 500°C. Information pre-
viously available in the literature has indicated
that titanium and aluminium leading to the
precipitation of y' are necessary in order to
generate such high strengths.
The remedial heat treatments that were found
to improve toughness were believed to have
worked due to an over-ageing effect. Following
heat treatment, transmission electron microscope
examination of thin foils showed that the density
of 7" precipitates fell dramatically and the
intensity of the superlattice streaks on the
diffraction patterns due to y" was significantly
reduced. The extra reflections that had been seen
on diffraction patterns and were not identified
disappeared after heat treatment and it is
therefore possible that whatever caused these
reflections also contributed to the particularly
low toughness of the used material.
The heat treatments that were trialled and
found to improve toughness were quite short, the
longest being 12 h duration. Previous work has
reported on the overageing of alloys hardened by
precipitation of 7" but generally, reduction in
hardness would be slower. For example, 2 a
material aged at 650°C achieved a peak hardness
of 400 HV after about 500 h and the hardness fell
to only 350 HV after a total aging time of about
1000h. 2 However, a t i m e - t e m p e r a t u r e para-
meter such as Larson-Miller ( P = T(K+
log t)/1000; where T is absolute temperature, t
time (h), K is a constant and P the Larson-Miller
parameter) which is frequently used to describe
stress rupture times for example suggests 12 h at
650°C is approximately equivalent to 150 000 h at
500°C (for K = 20). While the presence of the
orthorhombic 6 form of Ni3Nb was not confirmed
by diffraction pattern or other analytical tech-
niques, it was believed that this formed after heat
treatment. Other damaging precipitates were not
observed to any great extent.
Once an age hardening material has been
over-aged, it is not possible to regenerate the
maximum hardness without recourse to a
solution heat treatment. In Alloy 625, this could
not occur at the low heat treatment temperatures
employed and it is therefore tempting to believe
that the problem will not re-occur since it is
highly unlikely that 7" can or will re-precipitate
at the operating temperature. However, while it
is undoubtedly true that the improvement in
properties after heat treatment was most
welcome relative to the very low toughness
observed in the used as-received material, the
toughness remained low compared to new
material. It is possible that this was due to the
formation of the orthorhombic 6 phase. Previous
work 3 has found that reduction in Charpy impact
energies from around 180 to J/cm 2 as seen here
occurred as a result of intermediate temperature
ageing and the ductility loss was attributed
primarily to the formation of the orthorhombic 6
phase.
At the ageing temperatures and short times
used in the heat treatments in this work, it is also
possible that the formation of 6 Ni3Nb may not
be complete and therefore, the reduction of
toughness due to this mechanism should not be
totally discounted.
The superheaters in question were sub-
sequently heat treated on-site by the use of
heating pads and the complete vessels were
raised to 700°C. They were subsequently
returned to service and have continued to
operate without problem.
ACKNOWLEDGEMENTS
The authors thank Margaret Borshevsky and
Peter Gilberd for their assistance with the
electron microscopy, Neil Briggs and Terry Sage
who undertook much of the mechanical testing
and Methanex New Zealand Limited and
Industrial Research Limited for permission to
publish this paper.
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