Replication Microscopy Techniques

for NDE
A.R. Marder, Energy Research Center, Lehigh University
SURFACE REPLICATION is a well-
developed electron microscopy sample
preparation technique that can be used to
conduct in situ measurements of the micro-
structure of components. The in situ deter-
mination of microstructural deterioration
and damage of materials subjected to vari-
ous environments is an objective of any
nondestructive evaluation (NDE) of struc-
tural components. The need to assess the
condition of power plant and petrochemical
metallic components on a large scale recent-
ly led to the application of surface replica-
tion to the problem of determining remain-
ing life. The usual method of metallographic
investigation, which may involve cutting
large pieces from the component so that
laboratory preparation and examination can
be performed, usually renders the compo-
nent unfit for service or necessitates a cost-
ly repair. As a result, metallographic inves-
tigations are avoided, and important
microstructural information is not available
for evaluating the component for satisfacto-
ry performance. Therefore, an in situ or
field microscopy examination is needed to
aid in the proper determination of compo-
nent life.
The replica technique for the examination
of surfaces has been extensively used for
studying the structure of polished-and-etched
specimens and for electron fractographic ex-
amination (see the article "Transmission
Electron Microscopy" in Volume 12 of the
9th Edition of Metals Handbook for a discus-
sion of replication techniques in fractogra-
phy). Surface replication was the predomi-
nant technique in electron microscopy prior
to being supplemented by thin-foil transmis-
sion and scanning electron microscopy. Re-
cently, the replication microscopy technique
has become an important NDE method for
microstructural analysis, and an American
Society for Testing and Materials specifica-
tion has been written for its implementation
(Ref 1).
Specimen Preparation
Mechanical Polishing Methods. Compo-
nents in service usually have a well-devel-
oped corrosion or oxidation product or a
decarburized layer on the surface that must
be removed before replication. Coarse-
grinding equipment can be used as long as
the proper precautions are taken to prevent
the introduction of artifacts into the struc-
ture due to overheating or plastic deforma-
tion. Sandblasting, wire wheels, flap
wheels, and abrasive disks have all been
used. After the initial preparation steps are
completed, standard mechanical polishing
techniques can be used. Field equipment is
commercially available to help the metallog-
rapher reproduce the preparation steps nor-
mally followed in the laboratory. Depending
on the material, various silicon carbide
abrasive disks of different grit size, together
with polishing cloth disks with diamond
paste or alumina of varying grit size, can be
used to prepare for the etching step. Final-
ly, any appropriate etchant for the material
being examined can be applied to develop
the microstructure. For the proper identifi-
cation of such microstructural features as
creep cavities, a maximum double or triple
etch-polish-etch procedure should be used
(Ref 2). The etchants used for the various
materials investigated by the replication
technique are described in Volume 9 of the
9th Edition of Metals Handbook and in Ref
3.
Electrolytic Preparation Technique. Al-
though electrolytic polishing and etching
techniques have often been employed as the
final mechanical polish step in sample prep-
aration, inherent problems still exist in this
process. The electropolishing technique
uses an electrolytic reaction to remove ma-
terial to produce a scratch-free surface.
This is done by making the specimen the
anode in an electrolytic cell. The cathode is
connected to the anode through the electro-
lyte in the cell. Specimens can be either
polished or etched, depending on the ap-
plied voltage and current density, as seen in
the fundamental electropolishing curve in
Fig. 1. However, the pitting region must be
avoided so that artifacts are not introduced
into the microstructure. It is virtually im-
possible to prevent pitting without precise
control of the polishing variables, and pits
#
~ E t c h i n g l P o l i s h i n g
/ i ~ ~, ~ >1 ~
f
P i t t i n g
V o l t a g e
- , u " . 1 C u r r e n t d e n s i t y - v o l t a g e curve f o r e l e c t r o p o l -
i s h i n g
can often be mistakenly identified as creep
voids.
Several portable electropolishing units
are commercially available. The most im-
portant variables (time, bath temperature,
electrolyte composition, and the current
density-voltage relationship) have been in-
vestigated for a selected group of electro-
lytes (Ref 4). A direct comparison of elec-
tropolishing units and the precautions
necessary for handling certain electrolytes
are given in Ref 5.
It should be noted that there are areas in
both fossil and nuclear plants in which
neither acid etches nor electropolishing
methods and materials are allowed because
of the potential for intergranular stress-
corrosion cracking. Stainless steel piping in
nuclear plants can be replicated to deter-
mine defects by manual polishing without
etchants. Generator retaining rings have
been replicated by manual polishing to re-
solve NDE indications, because they are
extremely sensitive to stress-corrosion
cracking and no acids or caustics are al-
lowed to be used (Ref 6).
Replication Techniques
Replication techniques can be classified
as either surface replication or extraction
replication. Surface replicas provide an im-
age of the surface topography of a speci-

ASM Handbook, Volume 17: Nondestructive Evaluation and Quality Control
ASM Handbook Committee, p 52-56
Copyright 1989 ASM International
All rights reserved.
www.asminternational.org
T a b l e 1 C o m p a r i s o n o f r e p l i c a
t e c h n i q u e s
Type Advantages Disadvantages
Surface replicas
Acetate . . . . . . . Excellent resolution Coating required
Acrylic . . . . . . . . Direct viewing Adhesion
Rubber . . . . . . . . Easy removal Resolution
Extraction replicas
Direct stripped
plastic . . . . . . Easy preparation Particle retention
Positive
carbon . . . . . . Excellent particle Coating required
retention with
two-stage etching
Direct carbon.. Excellent resolution Not applicable to
in situ studies
men, while ext ract i on repl i cas lift part i cl es
f r om t he speci men. The advant ages and
di sadvant ages of some t ypi cal repl i cat i on
t echni ques are given in Tabl e 1.
5 u d a t e R e p l i c a s . Repl i cat i on of a sur-
face can i nvol ve ei t her di rect or i ndi rect
met hods. I n t he di rect , or single-stage,
met hod, a repl i ca is made of t he speci men
surface and subsequent l y exami ned in t he
mi cr oscope, while in t he i ndi rect met hod,
t he final repl i ca is t aken f r om an earlier
pr i mar y repl i ca of t he speci men surface.
Onl y t he di rect met hod will be consi der ed in
this article because it lends itself mor e fa-
vor abl y t o on-si t e preparat i on. The most
ext ensi vel y used di rect met hods i nvol ve
plastic, carbon, or oxi de repl i ca material.
All di rect met hods except plastic met hods
are dest ruct i ve and t herefore requi re furt her
preparat i on of t he speci men before maki ng
additional replicas.
Plastic replicas lend t hemsel ves t o in-plant
nondest ruct i ve exami nat i on because of their
relative simplicity and short preparat i on
time. Plastic replicas can be exami ned with
the light optical mi cr oscope, t he scanni ng
R e p l i c a t i o n M i c r o s c o p y T e c h n i q u e s f o r N D E / 5 3
el ect ron mi croscope, and the transmission
el ect ron mi croscope, dependi ng on the res-
olution required. As illustrated in Fig. 2, t he
plastic replica t echni que involves softening a
plastic film in a solvent, applying it t o t he
surface, and t hen allowing it t o harden as t he
solvent evaporat es. Aft er careful removal
from t he surface, the plastic film contains a
negative image, or replica, of t he mi crost ruc-
ture t hat can be directly exami ned in the light
mi croscope or, after some preparation, in
the el ect ron mi croscope. Doubl e-faced t ape
is used t o bond t he replica t o the glass slide
in order t o obtain large, fiat, undi st ort ed
replica surfaces.
Ther e are some significant advant ages of
t he replica t echni que over t he use of port a-
ble mi cr oscopes in t he field (Ref 5):
* A per manent r ecor d of t he speci men is
obt ai ned
Bet t er resol ut i on and hi gher magnifica-
t i on can be used
Cont ami nat i on of t he pol i shed surface is
mi ni mi zed
Ti me spent in an unpl easant or hazar dous
envi r onment is minimized
Scanni ng el ect ron mi cr oscopy can be uti-
lized
Several materials, including acet at e,
acryl i c resin, and rubber, can be used in t he
surface repl i ca t echni que (Ref 5). The
choi ce of material depends on t he geomet r y
of t he component and t he mi crost ruct ural
feat ures t o be exami ned.
I n t he acet at e met hod, an acet at e t ape is
wet t ed with acet one and applied t o t he
surface; ot her less volatile sol vent s, such as
met hyl acet at e, can be used when large
areas are replicated. For i mproved, resolu-
tion, t he back side of t he replica can be
pai nt ed with any fast -dryi ng bl ack paint or
ink pri or t o removal , or f or t he same effect,
evapor at ed coat i ngs of car bon, al umi num,
Softened acetate tape
/ ~ Tape applied t o
surface and d rie d
\
Polished-and- /
etched p a r t ~ [ ~
Tape rem oved
w ith negative
replica o f
surface
F i g . 2 Schematic of the plastic replica technique
or gol d can be applied at a s hadow angle of
45 t o t he f r ont side of t he repl i ca after
removal .
I n t he acryl i c cast i ng resi n met hod, dams
are requi red becaus e a powder is mi xed
with a liquid on t he surface t o be repl i cat ed.
Af t er hardeni ng, t he repl i ca can be exam-
ined di rect l y in an opt i cal mi cr oscope with-
out f ur t her processi ng. I f adhesi on is a
pr obl em, a composi t e repl i ca can be made
of an initial l ayer of Parl odi an l acquer be-
fore t he acryl i c l ayer is applied.
I n t he dent al i mpressi on r ubber met hod,
uncur ed liquid r ubber material (for exam-
ple, GE RTV60 silicon r ubber compound) is
pour ed ont o t he surface t o be repl i cat ed and
is cont ai ned by a dam. Af t er r emoval , t he
repl i ca can be exami ned di rect l y or can be
coat ed f or bet t er resol ut i on.
Plastic
/
' - - - ~ u ~ i , i - - F irst e t c h / " " "~" 'JJ'. ~./nc;usion ~ ~ irs t etch
\ \ . / / . e
(~ ~ ) ~ , / / / ~ ) " M etal
(a) (b)
Carbon
? ~ / J "n L , , ~ ~ J
Carbon
(c) (d)
''ul|~" 3 Positive carbon extraction replication steps, (a) Placement of plastic after the first etch. (b) After the second etch. (c) After the deposition of carbon. (d) The positive
replica offer the plastic is dissolved
5 4 / M e t h o d s o f N o n d e s t r u c t i v e E v a l u a t i o n
(a)
(c)
=.===-.. 4 P r o p a g a t i o n o f d i f f e r e n t c r o c k t y p e s . ( a )
c o r r o s i o n
E x t r a c t i o n R e p l i c a s . Several different ex-
traction replica techniques can be used to
characterize small particles that are embed-
ded in a matrix, such as small second-phase
particles in a steel (see the article "Analyt-
ical Transmission Electron Microscopy" in
Volume 10 of the 9th Edition of Metals
Handbook). More detailed descriptions of
the various extraction replica techniques
can be found in Ref 7 and 8.
After careful preparation of the surface
using normal polishing methods, the first
step in producing an extraction replica is to
etch the alloy heavily to leave the particles
of interest in relief. In the positive carbon
extraction replica, as shown in Fig. 3, a
piece of solvent-softened polymeric film
(cellulose acetate tape) is pressed onto the
surface exposed by this first etch (Ref 5).
Once the solvent has evaporated, one of
two steps can be taken. The tape can be
carefully pulled from the specimen to pro-
duce a negative of the surface, or the spec-
imen can undergo a second etch to free the
particles exposed by the first etch (Fig. 3).
In the second etch, the specimen can be
etched through the plastic; most plastics are
quite permeable to etching solutions, and
the specimen etches almost as rapidly as
without the plastic film (Ref 9). Carbon is
then evaporated in a vacuum onto the plas-
tic replica. The carbon and plastic contain-
ing the particles now make up the positive
replica. The cellulose acetate is then dis-
solved, and the positive carbon replica is
allowed to dry. It should be noted that for
the negative carbon extraction replica tech-
(b)
( d )
C r e e p . ( b ) Fatigue (c) S t r e s s c o r r o s i o n . ( d ) I n t e r g r a n u l a r
nique, vacuum deposition of carbon onto
the surface of the specimen is required, and
therefore this replica method is not applica-
ble to NDE.
Mi crost ruct ural A n a l y s i s
C r a c k d e t e r m i n a t i o n is important to help
establish the root cause of a potential failure
in a component. After a preliminary evalu-
ation of the crack to assess crack shape and
length by using magnetic flux or dye pene-
trant, the replica method is then used on
unetched specimens to assist in the crack
evaluation. Figure 4 schematically shows
the propagation of different types of cracks
in a steel structure (Ref 10). Each crack has
its own characteristics, and it is often pos-
sible to make a correct determination of
crack type. It is important to determine
whether the crack is the original defect or
has been caused by service conditions or
damage. Once the crack type is identified,
the proper corrective action, such as elim-
inating a corrosive environment or reducing
stress levels, can be attempted. Figure 5
shows the replication of surface cracks in a
boiler tube.
Creep Damage. Creep defects cause the
majority of failures in power plant compo-
nents operating under stress and thermal
load, and the replica method is especially
suitable for the detection of these defects.
Therefore, the replica method has become
an especially important tool in the deter-
mination of remaining life in such compo-
nents as boiler tubes, steam piping, and
@
j -
(a)
% ~,
2 0 _ _ . ~ m
( b )
Surface c r a c k i n a b o i l e r t u b e . C o m p a r i s o n
Fi g. 5 o f t h e ( a ) a c t u a l m i c r o s t r u c t u r e a n d ( b ) t h e
r e p l i c a o f t h e c r a c k
turbine components. The replica method
reveals defects due to creep at a much
earlier stage than other NDE techniques.
Creep defects begin as small holes or cav-
ities at grain boundaries or second phases.
With time and stress, these holes or cavi-
ties can link up and form cracks that
eventually lead to failure of the component
(Fig. 6). Creep cracks are usually very
localized, and they form in welds, bends,
or other highly stressed regions. Determin-
ing the remaining life of components nor-
mally depends on assessments of regular
inspections, as indicated in Table 2. Figure
7 shows a comparison of creep voids in a
surface replica and the corresponding bulk
microstructure.
P r e c i p i t a t e A n a l y s i s . The detection of
various deleterious precipitates in compo-
nents subjected to high temperature and
stress can lead to improved life assessment
R e p l i c a t i o n M i c r o s c o p y T e c h n i q u e s f o r N D E / 5 5
(a) (b) (c) (d)
F i g , 6 Schematic o f creep crock formation. Small cavities (a) link up over time (b) and form intergranulor crocks (c) and eventually macrocracks (d).
T a b l e 2 C r e e p d a m a g e c l a s s i f i c a t i o n
Class Nature Action
1 . . . . . . . . . . . . . . . . . . . . . . . . . No creep defects
2 . . . . . . . . . . . . . . . . . . . . . . . . . A few cavities
3 . . . . . . . . . . . . . . . . . . . . . . . . . Coalescent cavities
4 . . . . . . . . . . . . . . . . . . . . . . . . . Microscopic creep cracks
5 . . . . . . . . . . . . . . . . . . . . . . . . . Macroscopic creep cracks
Source: Ref 11
None
Reinspection after 20 000 h of service
Reinspection after 15 000 h of service
Reinspection after 10 000 h of service
Management must be informed immediately
(a)
(a) (b)
F i g . 8 Comparison of cT-phase formation as seen in (a) a replica and (b) the actual microstructure
(b)
F i g . 7 Comparison o f creep voids in (a) a replica
and (b) the actual microstructure
analysis of these components. The extrac-
tion replication technique is an excellent
nondestructive method of detecting these
precipitates.
Sigma phase is a deleterious FeCr com-
pound that can form in some stainless
steels, and its presence can severely limit
remaining life. Extraction replicas have
been used to determine the amount of (r
phase in the microstructure (Ref 12), and
the amount of ~ phase has been directly
related to the creep rate (Ref 13). Figure 8
shows an example of cr phase in an extrac-
tion replica.
The composition of carbides, and their
stability with time and temperature of expo-
sure, can indicate the remaining life of a
component. Extraction replicas have been
used to evaluate carbides, and it has been
suggested that changes in morphology and
chemistry can be used to assist the estima-
tion of effective exposure temperature for
use in determining the remaining life of
components (Ref 14). Figure 9 shows an
example of precipitates extracted from a
200 000-h exposed sample, together with
the accompanying chemical analysis.
A C K N O W L E D G M E N T
The author would like to acknowledge the
contributions of his colleagues A.O. Ben-
scoter, S.D. Holt, and T.S. Hahn in the
preparation of this article.
5 6 / M e t h o d s o f N o n d e s t r u c t i v e E v a l u a t i o n
(a)
F i g . 9 Extraction replica of the microstructure (a) and the
( b )
precipitate microchemical analysis (b) from an extraction replica
R E F E R E N C E S
1. "St andar d Practice for Production and
Evaluation of Field Metallographic
Repl i cas, " E 512-87, Annual Book of
ASTM Standards, Ameri can Society
for Testing and Materials
2. A.M. Bissel, B.J. Cane, and J. F. De-
Long, "Remanent Life Assessment of
Seam Welded Pi pewor k, " Paper pre-
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and Piping Conference, American Soci-
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3. G. F. Vander Voort, Metallography:
Principles and Practice, McGraw-Hill,
1984
4. T.S. Hahn and A.R. Marder, Effect of
Electropolishing Variables on the Cur-
rent Densi t y--Vol t age Relationship,
Metallography, Vol 21, 1988, p 365
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Metallographic Exami nat i on of Fer-
rous and Non-Ferrous Component s, "
Canadian Electrical Association, Nov
1985
6. J. F. DeLong, private communication
7. D. Kay, Ed. , Techniques f or Electron
Microscopy, Blackwell Scientific Publi-
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Nostrand Rheinhold, 1976
9. G. N. Maniar and A. Szirmae, in Man-
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10. P.B. Ludwigsen, Non-Destructive Ex-
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11. B. Neubauer and U. Wedel, NDT: Rep-
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ment of Power Plant Components, Pow-
er Eng., May 1984, p 44
12. F. Masuyama, K. Setoguchi, H.
Haneda, and F. Nanjo, Findings on
Creep-Fatigue Damage in Pressure
Parts of Long-Term Service-Exposed
Thermal Power Plants, in Residual Life
Assessment Nondest ruct i ve Examina-
tion and Nuclear Heat Exchanger Ma-
terials, PVP-Vol 98-1, Proceedings of
the Pressure Vessels and Piping Confer-
ence, American Society of Mechanical
Engineers, 1985, p 79
13. T. Fushimi, "Li f e Evaluation of Long
Term Used Boiler Tubes , " Paper pre-
sented at the Conference on Boiler
Tube Failures in Fossil Plants (Atlanta),
Electric Power Research Institute, Nov
1987
14. A. Afrouz, M.J. Collins, and R. Pilking-
ton, Microstructural Examination of
ICr-0.5Mo Steel During Creep, Met.
Technol., Vol 10, 1983, p 461