Effects of Metallographic

Preparation Procedures on
Creep Damage Assessment
T. L. da Silveira and I. Le May*
Faculdade de Engenharia Souza Marques and COPPE/UFRJ, Rio de Janeiro, RJ, Brazil;
fMetallurgical Consulting Services Ltd., P.O. Box 5006, Saskatoon, Canada S7K 4E3; and
COPPE/UFRJ, Rio de Janeiro, RJ, Brazil

Specimens taken from a ruptured Cr-Mo steel steam tube and a cast austenitic reformer
tube exposed at high temperature for extended time have been examined for creep dam-
age, using mechanical polishing procedures. It is demonstrated that the presence of dam-
age may be observed readily or missed depending on the surface preparation procedure
followed. The nature of the observed damage is discussed together with the ways in
which the surface preparation procedures affect its disclosure. The implications of me-
tallographic preparation procedures on the assessment of creep damage and remaining
life estimation are reviewed, and a procedure to ensure reliable identification of such
damage is recommended.

INTRODUCTION steels according to Neubauer and Wedel

In the assessment of the extent of damage
by creep deformation in high temperature
plant such as power station steam gener-
ators and petrochemical equipment, me-
tallography is playing an increasingly im-
portant role. This may be from in situ me-
tallographic examination of critical regions
such as headers, bends, tees, areas show-
ing wall thickness changes, and welded
joints, or from laboratory examination of
specimens cut from these. The damage is
commonly assessed on the basis of the ex-
tent to which grain boundary voids or cav-
ities are observed and on the degree to
which these have linked up to form micro-
cracks or macrocracks. The remaining safe
life of the component is then estimated
from the characteristic features of the dam-
age. Figure I shows schematically the basis
of damage parameter assessment from the
observation of replicas taken from Cr-Mo
[1].
It is important that the metallographic
methods used identify clearly the presence
of voids, cavities, or microcracks when
these are to form the basis on which con-
tinued operation of a plant is decided.
For some time the authors have been en-
gaged in an extensive study of damage as-
sessment methods and of remaining life
prediction in high temperature steam
p o w e r generators and petrochemical
plant, and some aspects of this work have
been reported elsewhere [2, 3]. During this
period extensive use has been made of
metallography, and it has been found that
the apparent extent of damage is influ-
enced greatly by the mechanical polishing
procedures used. This article presents the
salient observations illustrating this prob-
lem, and attempts to identify the form of
the creep damage centers that are devel-
oped and the reasons for their disclosure

75
(~Elsevier Science Publishing Co., Inc,, 1992 MATERIALS CHARACTERIZATION 28:75-85 (1992)
655 Avenue of the Americas, N e w York, NY 10010 1044-5803/92:S3.50
76 T. L. da Silveira and I. Le May

0 frOclure
damage corresponding /
parameter action In plant /
#
A , observe D/
B • o b l e r v o , fix ~ ~-'~"T~I
I n s p e c t i o n Intervals ~ • I , ~,|.. I

.: o • " ,.p:,.

,reap ..n,..

exposure lima
FIG. 1. Schematic showing basis of damage parameter assessment and remaining life estimation from obser-
vation of replicas according to Neubauer and Wedel [1].

or nondisclosure. The significance of the led to failure. The specimen is s h o w n after

observations in terms of remaining life as- successive wet grinding on 120, 240, 400,
sessment p r o c e d u r e s is reviewed, and a a n d 600 grit silicon carbide papers, fol-
metallographic p r o c e d u r e to identify creep lowed by h a n d polishing with 1 t~m alu-
d a m a g e in a reliable m a n n e r is suggested.

EXPERIMENTAL

Samples of material from a n u m b e r of com-

p o n e n t s have b e e n examined, and two
specific cases will be described here. The
first was a 90 ° b e n d in a steam tube of 1Cr,
½Mo steel that had failed by longitudinal
cracking after 70,000 h o u r s of service u n d e r
an internal pressure of 16.5 MPa and at a
t e m p e r a t u r e that had b e e n higher than the
design value of 490°C for a considerable
period: the tube outside diameter was 168
m m a n d the wall thickness 14.2 mm. A
b e n d such as this is a relatively c o m m o n
place in which local creep d a m a g e (and
possible rupture) m a y occur. The second
example was of a weld in a reformer tube
of ASTM A297 grade HK-40 cast austenitic 4 0 0 prn
steel (23-37 Cr, 19-22 Ni, 0.35-0.45 C) that
had been in service for approximately
70,000 h o u r s at about 950°C. FIG. 2. Section adjacent to longitudinal crack (at right)
in Cr-Mo steel after finishing polishing on 1 i~m
Figure 2 shows a transverse cross-sec- alumina. Note the small surface crack, and absence
tion of the Cr-Mo tube at the external sur- of extensive creep voids. The arrowhead points to the
face adjacent to the longitudinal crack that outside surface of the tube.
Creep Damage Assessment
mina with distilled water lubrication. No
evidence was apparent of aligned creep
voids on boundaries after all scratches had
been removed. Figure 3 shows the same
section after etching in 2% Nital: the grain
boundaries are now well defined, as may
be seen at higher magnification, but no
cavities or voids are evident on them.
However, if the polishing time is ex-
tended, the as-polished surface can show
the presence of what appear to be aligned
grain boundary voids and microcracks.
4ooum~
Fro. 3. (a) Same section as shown in Fig. 2 but after
etching in 2% Nital. The higher magnification (b)
shows the apparent continuity of grain boundaries.
Arrowheads indicate a common reference feature (an
artifact)
77
~4oo'pm
100prn
b~
FIG. 4. Same section as in Figs. 2 and 3 after extende,
polishing, showing apparent grain boundary void
and microcracks. Arrowheads indicate common ret
erence points in lower magnification (a) and highe
magnification (b) views.
Figure 4 shows the same specimen as see~
in Figs. 2 and 3, after continued hand pol
ishing on 1 ~m alumina, the extent of th
polishing being until widespread apparer
voids were disclosed. The microstructur
after etching in 2% Nital is shown in Fi~
5, in which the "cavities" may be seen t
lie along grain boundaries oriented no1
mally to the hoop stress in the tube.
In an internally pressurized Cr-Mo tub
such as is discussed here, it is establishe
that creep damage is much more extensiv
near the outer surface, decreasing to sho~
78 T. L. da Silveira and I. Le May

FIG. 5. Same view as in Fig. 4 after etching in 2% Nital. The arrowheads indicate a common feature in lower
magnification (a) and higher magnification (b) views.

little, if any, void formation near to the in-
side diameter [1]. In the tube reported on
here, no microcracking or apparent void
formation was observed from the center of
the tube wall to the inner surface after me-
tallographic examination. This was the
case independent of the polishing proce-
dure used.
A series of polishing and etching steps
on a specimen adjacent and parallel to
those shown in Figs 2-5 was made. The
procedure used was hand polishing with
6 p,m diamond followed by final hand pol-
ishing with I ptm diamond; these polishing
steps followed wet hand grinding in the
same sequence as previously to 600 grit.
Figure 6(a) shows a region at the external
surface after one polishing sequence: the

FIG. 6. Specimen of Cr-Mo tube adjacent to the specimens illustrated in Figs. 2-5, showing low magni-
fication views: (a) polished; (b) after etching in 2% Nital and repolishing; (c) after an additional etching and
polishing sequence; (d) after further etching and a fourth polishing sequence; (e) after further etching,
grinding, and repolishing. (f-j) show the same sequence but at higher magnification and after etching in each
case.
Creep DamageAssessment 79

longitudinal crack was heat treated by

holding it at 900°C for 20 minutes, followed
by air cooling. Figure 7 shows the surface
after polishing in a m a n n e r similar to that
used to prepare the specimen s h o w n in
Fig. 2, while Fig. 8 shows its appearance
after etching in 2% Nital. In these photo-
micrographs there is an absence of aligned
voids, as in Figs. 2 and 3, while the mi-
crostructure is altered greatly from having
been austenitized and air cooled. Figures
9 and 10 s h o w c o r r e s p o n d i n g views after
e x t e n d e d polishing and e x t e n d e d polish-

400 pm

FIG. 7. Carefully polished section of Cr-Mo steel

tcrack at left~ after thermal treatment. Note minimal
indications o! voids. ]?hearrowhead points to the out-
side surface of the tube.

surface cracks are s h o w n up sharply and

clearly' and there is very limited evidence
of cavity or void formation. Figure 6(b) il-
lustrates the same area after etching in 2%
Nital and repolishing on both grades of
diamond: the cracks appear to be signifi-
cantly wider, although the evidence of
aligned voids is still very limited. Figure
6(c and d) s h o w the same area after addi-
tional etching and polishing sequences,
and extensive aligned grain b o u n d a r y cav-
ities and microcracks are disclosed. Finally,
Fig. 6(e) illustrates the same area after re-
grinding on 600 grit p a p e r and polishing
with 6 ~ m and 1 ~ m diamond; the ap-
pearance is similar to that s h o w n in Fig.
6(a). In the sequence of p h o t o m i c r o g r a p h s
given in Fig. 6(f-j), the same area is s h o w n
at higher magnification after similar pol-
ishing cycles, but following the etching
step in each case.
To d e t e r m i n e better the nature of the FIG. 8. Section of heat treated material shown in Fig.
local regions w h e r e a p p a r e n t voids were 7 after etching in 2% Nital. (a) shows an overall low
disclosed u p o n e x t e n d e d polishing, an-- magnification view, while (b) shows the recrystallized
other :section of material adjacent to the structure and an absence of pores or microcracks.
 80 T. L. da Silveira and I. Le May

ing followed by etching, respectively, and

FIG. 9. Heat treated section as in Fig. 7, but after ex-
tended polishing.
well-defined apparent voids and micro-
cracks are seen, lying normal to the direc-
tion of the hoop stress. The voids and mi-
crocracks do not, however, lie along grain
boundaries. Thus, it appears that the same
regions of damage produce apparent voids
u p o n extended polishing as were disclosed
in the n o n - h e a t - t r e a t e d condition. Be-
cause of the recrystallization of the matrix,
the grain boundaries are no longer coin-
cidental with the damage centers from
which the polish-etch procedure leads to
the development of these cavities. Also,
the damage centers are not affected by the
thermal treatment.
The section cut from the weld metal of
the reformer tube of HK-40 austenitic steel
is s h o w n in Fig. 11(a) following grinding
a n d mechanical polishing conducted as de-
scribed for the Cr-Mo steel s h o w n in Fig.
2, and subsequent etching in Aqua Regia
saturated with CuCl2. The section is ad-
jacent to the inner surface of the tube,
transverse to the tube length. This inner

FIG. 10. As in Fig. 9, but etched in 2% Nital. (a) shows an overall view, while (b) shows that the apparent
microcracks and voids do not correspond to the grain boundaries of the recrystallized structure.
Creep Damage Assessment 81

FrG. 11. Reformertube wall adjacent to inner surface (right). (a) After lightlypolishing, with minimal voids
disclosed; (b) after extended polishing, indicatingaligned voids. Etched in Aqua Regia saturated with CuCI2.
The arrowheads indicate the same feature. The arrows indicate the inner surface of the tube.

region is where creep damage takes place
preferentially in reformer tubes, the den-
sity of voids that may be observed decreas-
ing to virtually zero at the outside surface
[4]. Voids are not clearly defined, although
there are some indications of their pres-
ence. Figure 11(b) shows the same area
after regrinding on 600 grit paper to re-
move all signs of etching, and repolishing
for an extended period on 1 ~m alumina,
until aligned voids became clearly appar-
ent. Again, the specimen was etched in
Aqua Regia saturated with CuC12.
DISCUSSION
centrated near the inner surface [5, 6]. The
observations show that the apparent pres-
ence or absence of voids and microcracks
in these two distinctly different alloys de-
pends greatly on the process of surface
preparation.
Several aspects emerging from the re-
sults require discussion: these are the way
in which the mechanical polishing process
may influence the appearance of voids; the
physical meaning of the apparent voids
and microcracks revealed by metallo-
graphic examination; and the appropriate
metallographic procedures to be used in
determining the extent of creep damage.

Figure 5 shows what is accepted as being MECHANICAL POLISHING AND

typical of advanced creep damage accu-
mulation in unfired superheated steam
transfer Cr-Mo steel piping in a transverse
section close to the external surface [1]. In
a similar manner, Fig. 11(b) shows the ex-
pected appearance of creep damage in a
high alloy austenitic reformer tube, con-
VOID DISCLOSURE
The observations have shown that appar-
ent voids are disclosed in creep-damaged
material upon either extended mechanica]
polishing following grinding, or repeated
mechanical polish-etch cycles.
82
In principle there are three possibilities
to explain these observations. First, the
voids may have been obscured by a
smeared surface layer produced by grind-
ing or polishing, which is a well-known
phenomenon [7]. However, in the present
case, as Fig. 3 shows, grain boundaries are
defined clearly without any evidence of
smearing, or of the presence of microcracks
or voids. Figures 4 and 5 show well-de-
veloped microcracks and apparent voids at
the same region, these figures showing the
surface after e x t e n d e d mechanical
polishing.
The second possibility relates to the fill-
ing of cavities by debris produced during
polishing. To check on this, specimens
were examined in the scanning electron
microscope with energy dispersive x-ray
analysis. No evidence of any localized pick
up of polishing material was observed. In
addition, the cleaning procedure used after
polishing was identical for specimens in
which apparent voids were noted and in
which none was detected.
The third possibility is that the apparent
voids present after extended polishing do
not exit as cavities within the bulk material.
They are seen upon extended polishing or
after a series of polish-etch cycles, sug-
gesting that material may have been pulled
out around small damage centers or pre-
cipitates, or alternatively that surface relief
has developed locally by means of polish-
ing or pitting attack, or both. The apparent
cavities and microcracks develop at those
grain boundaries in which vacancy accu-
mulation would occur during diffusion
controlled creep at low stresses. These
boundaries are normal to the principal ten-
sile stress.
It should be noted that extended polish-
ing and polish-etch cycles have been uti-
lized to disclose apparent voids not seen
on initial polishing using both alumina and
diamond polishing compounds. Similar re-
sults have been obtained during prelimi-
nary investigations made with automatic
polishing equipment, and it is hoped that
these will be described at a later date.
T. L. da Silveira and I. Le May
THE PHYSICAL MEANING OF THE VOIDS
AND MICROCRACKS
During diffusion controlled creep at low
stress conditions, as is appropriate for both
alloys reported on here, the controlling
mechanism involves a flow of vacancies to
grain boundaries normal to the principal
stress axis and the deformation of the ad-
jacent matrix to preserve coherence be-
tween grains [8]. The development of grain
boundary voids and subsequent micro-
cracks in metals during diffusion creep has
been widely reported. However, contro-
versy exists about the extent to which void
formation occurs in many commercial al-
loys during high temperature service, and
some authors have maintained the neces-
sity of conducting polish-etch sequences
that are considered to exaggerate the dam-
age and enlarge the voids to ensure their
detection [9].
While there are specific alloys and con-
ditions in which significant and readily ob-
served voids may be formed, the obser-
vations reported here suggest that, in the
commercial alloys of interest, the voids and
microcracks are largely artifacts produced
during polishing and etching, but have
physical significance in that they indicate
regions where damage has accumulated
during the process of creep.
The polishing of specimens of the Cr-Mo
steel after the matrix had been recrystal-
lized by thermal treatment demonstrates
that the creep damage at points along the
original grain boundaries is not removed
by this means. Its presence may still be dis-
closed in its original positions, and not
along the recrystallized grain boundaries,
as shown in Fig. 10. If the damage was an
accumulation of vacancies or dislocations,
the thermal treatment would have elimi-
nated it. That it is not eliminated suggests
the presence of surfaces, such as decohe-
sion between grains or at grain boundary
precipitates. The actual size of any regions
of decohesion or of grain boundary precip-
itates must be very small, as they are not
seen during examination by normal light
Creep Damage Assessment
microscopy. However, the size of the mi-
crocracks indicated during extended pol-
ishing, as may be seen in Figs. 5 and 10,
for example, suggests that there is exten-
sive damage along the original grain
boundaries. The linking of the many fine
and aligned regions of decohesion to pro-
duce apparent microcracks upon pro-
longed polishing or repeated polish-etch
cycles may relate to the pulling out of ma-
terial or precipitates, or to preferential re-
lief developing along the regions of de-
cohesion, as already discussed.
It is important to note that, upon ex-
tended polishing or upon repeated polish-
etch cycles, no pores or microcracks were
disclosed on those grain boundaries on
which creep damage accumulation would
not be expected, and no such artifacts were
developed in regions of the material away
from the creep damaged areas.
The foregoing discussion is to some ex-
tent speculative in terms of the exact na-
ture of the damage. However, it suggests
the need for a better understanding of the
physical mechanisms of the creep damage
process.
APPROPRIATE PROCEDURES TO
IDENTIFY CREEP DAMAGE
In the assessment of the extent of creep
damage and the prediction of safe remain-
ing life in high temperature plant, it is es-
sential that the metallographic methods
utilized to disclose the possible presence
of damage are reliable. The observations
reported indicate that, in regions where
considerable creep damage has taken
place, voids or microcracks may not be dis-
cerned by normal methods of light mi-
croscopy when mechanical polishing is uti-
lized, even though this is of a good quality,
allowing microstructural surface details to
be shown clearly.
An important point is that a mechani-
cally polished surface of a creep-damaged
component in which no grain boundary
voids are apparent can be made to display
83
them upon extended polishing; it may be
returned to an apparently void-free con-
dition by regrinding on 600 grit and me-
chanically polishing. Additional polishing
for an extended time can then show up the
apparent voids in the same positions as
previously. Thus apparent voids can be se-
quentially displayed and eliminated in the
same specimen.
In conducting extended mechanical pol-
ishing of a steel of the Cr-Mo type, it is
believed that damaged material is being
pulled out at interfaces, most probably at
grain boundary carbides. Etching may pro-
mote localized attack. As a consequence,
the creep damage is emphasized and the
aligned carbides and locally fine decohe-
sion appear to be linked in the manner of
microcracks. In the case of the cast austen-
itic steel, fine grain boundary microvoids
may also be present after extensive creep
damage, and extended polishing probably
serves to exaggerate them by the rounding
of their edges.
Creep cracking is thought to develop by
a linking of the voids or local points of de-
cohesion and, once a crack has developed,
its apparent width increases as a result of
extended polishing, or through a series of
polish-etch steps. This is seen in Fig. 6.
The important point for damage assess-
ment procedures is that creep damage can
be reliably observed in terms of aligned ap-
parent voids and microcracks. Their actual
size and number are secondary factors that
may be subject to large variations and may
bear little relation to the actual size of ()pen
volumes in the bulk material. Thus, dam-
age assessment procedures that depend on
quantitative assessment of voids and mi-
crocracks may be in serious error. Stereo-
logical analyses to determine size distri-
butions, as recently developed [10], are de-
pendent on accurate disclosure of void
sizes.
As indicated already, some authors sug-
gest that clear definition of voids requires
a series of mechanical polish-etch steps [9],
while others utilize electropolishing f11].
Both procedures are reported to emphasize
84
and exaggerate the size of voids and mi-
crocracks disclosed. The present studies
indicate that either extended mechanical
polishing or a polish-etch sequence may be
utilized to identify creep damage unequiv-
ocally, although the apparent voids dis-
closed may well be larger than any micro-
voids originally present. The extent to
which continued polishing should be done
is, however, difficult to quantify, and thus
the polish-etch sequence is considered a
more reliable procedure, although it is be-
lieved that its efficacy depends primarily
on the mechanical polishing steps and,
hence, polishing time.
As a consequence, the authors suggest
that, to identify creep damage reliably
through the disclosure of aligned apparent
voids and microcracks produced from
damage centers by means of mechanical
polishing, a series of thee mechanical pol-
ish-etch steps should be followed as a
minimum.
CONCLUSIONS
Mechanical polishing of creep-damaged
specimens of high temperature alloys may
show indications of the presence or ab-
sence of voids and microcracks depending
on the polishing procedure used. Pro-
longed polishing or repeated polish-etch
cycles show up indications of creep dam-
age clearly.
The nature of creep damage along grain
boundaries is considered to be very local,
without large voids being developed, and
these features, apparent after extended
polishing or a series of polish-etch cycles,
are considered to be largely artifacts. In the
case of Cr-Mo steel, they are believed to be
due to the pull out of matrix or precipitates
at damage centers along grain boundaries.
In cast austenitic steels they may be seen
because of the exaggeration caused by the
rounding of their edges, as well as from
the effects of precipitates.
Estimation of the extent of creep damage
and of remaining life should not be based
upon quantitative measurements of the
T. L. da Silveira and I. Le May
number and apparent surface area or vol-
ume of voids and microcracks disclosed by
metallography, but should be based on an
appreciation of the distribution of the dam-
age centers disclosed.
To define unequivocally the presence or
absence of creep damage using mechanical
polishing, it is suggested that a minimum
of three polish-etch cycles be utilized.
Finally, it should be pointed out that the
detailed mechanisms whereby creep dam-
age is accumulated at boundaries normal
to the principal tensile stress are not clear
for the alloys in question. More detailed
studies using scanning electron micros-
copy and energy dispersive x-ray analysis
are underway.
This work was carried out with the aid of a grant
from the International Development Research
Centre, Ottawa, Canada. Acknowledgement is
also given for support from Conselho Nacional
de Desenvolvimento Cientifico e Technol6gico,
Brazil, and from the Natural Sciences and En-
gineering Research Council, Canada. Thanks
are expressed to Roberto Dimas and Alexandre
Goncalves Celestino for their assistance in the
work, and to the reviewer for his helpful and
constructive comments.
References
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creeping components by means of replicas, In
ASME International Conference on Advances in Life
Prediction Methods (D. A. Woodford and J. R.
Whitehead, eds.), ASME, New York (1983), pp.
307-313.
2. I. Le May and T. L. da Silveira, Creep damage
assessment in petrochemical plant, Proc. Internat.
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3. T. L. da Silveira and I. Le May, Metallographic
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techniques of in-place analysis, in Microstructural
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Originally submitted August 1988; revised manuscript ac-
cepted August 1991.