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Metallographic Techniques for Superalloys

Article  in  Microscopy and Microanalysis · August 2004

DOI: 10.1017/S1431927604883442

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 METALLOGRAPHIC TECHNIQUES FOR SUPERALLOYS

George F. Vander Voort1, Elena P. Manilova2, Gabriel M. Lucas1

1
Buehler Ltd., 41 Waukegan Road, Lake Bluff, IL 60044 USA
2
Polzunov Central Boiler and Turbine Institute, Politechnicheskays str., 24, 194021 St. Petersburg, Russia

Keywords: Metallography, Specimen Preparation, Etching, Microstructure

Abstract reduce the occurrence and degree of shrinkage gaps.

Superalloys are complex alloys of Fe-Ni, Ni, or Co-base
compositions. Their microstructure can be quite complex
due to the potential for a variety of phases that can be
formed by heat treatment or service exposure conditions.
The paper presents the use of new metallographic materials
to prepare these alloys with emphasis on modern, four- and
five-step practices. Different etchants are required to reveal
the structure of these alloys properly. Examples will be
presented showing the use of different etchants as a function
of alloy composition, heat treatment, and microstructural
phases.
Introduction
Preparation of superalloys for microstructural examination is
not exceptionally difficult. The procedures are similar to
those used to prepare stainless steels. Because they are face-
centered cubic “austenitic” alloys with exceptionally good
toughness, machinability is poorer than for steels and the
age hardened alloys, especially the cast alloys, can be more
difficult to section than most steels when they have a very
high ' content. FCC metals readily deform and work
harden, consequently aggressive sectioning methods (e.g.,
power-hacksawing or band sawing) will introduce
considerable damage which can be very difficult to remove
in the subsequent preparation steps. If these procedures
must be used, it is advisable to re-section the material with
the correct abrasive cutoff wheel (consumable type) with
abundant cooling. These newly prepared surfaces will
exhibit less damage and should be used as the starting
surface for metallographic preparation. Many preparation
problems can be traced to the generation of excessive
cutting damage. Always use an abrasive cut-off blade design
for metallographic work with superalloys. Otherwise, the
plane-of-polish will probably exhibit remnants of the
damage created during sectioning.
Preparation Methods
Mounting
Mounting of specimens may be performed, if desired,
depending upon the nature of the analysis. Mounting is
advisable for edge preservation whenever an exterior surface
is to be examined. Compression-mounting thermosetting
epoxy resins, such as Epomet thermosetting resin, provide
the best edge retention. Mounting presses that cool the
specimen back to ambient temperature under pressure
Shrinkage gaps degrade edge retention and lead to bleed-out
problems of solvents or etchants and stains that obscure the
edge inhibiting examination. Mounting may be merely a
convenience factor as the back of the mount is an ideal
surface for recording specimen details, or it may be useful to
facilitate use of automated preparation devices.
Grinding
Historically, grinding performed using a series of water-
cooled SiC papers of varying grit sizes (120, 240, 320, 400,
and 600 grit) generally at 240 - 300 rpm on a rotating wheel.
The specimen is held against the SiC paper by hand or
through the use of a fixture. Typically, grinding with each
paper is conducted for 60 - 120 seconds. If done manually,
the specimen is rotated 45 - 90 between papers so that the
grinding direction is not constant. Semiautomatic or
automatic grinding machines produce omni-directional
grinding patterns and yield superior flatness and edge
preservation. Unless specimens are porous or contain
cracks, a simple washing operation between steps is
adequate. Otherwise, ultrasonic cleaning with a suitable
solvent is required.
With today’s contemporary preparation methods, only one
grinding step is used and this may be performed using SiC
paper, or some other abrasive depending upon laboratory
through put or personal preference. To make this approach
work, sectioning must be performed with the best quality
metallographic cut-off wheels so that sectioning damage is
minimized. Then, the finest possible SiC grit size that
removes the sectioning damage in a reasonable time can be
used. Usually, 180- or 240-grit SiC paper can be used, or
products with an equivalent abrasive particle size. As the
size of the grinding abrasive increases, the depth of damage
created by the grinding step increases. Consequently, to
maximize the efficiency of the preparation method, and the
results, always use the finest possible abrasive size that will
remove the sectioning damage (which is minimized by the
use of the best possible abrasive wheel) and get all of the
specimens in the holder to the same common plane.
There are several alternatives to the use of SiC paper, and
these work well on superalloys. One can use a rigid grinding
disk (RGD) and a coarse size diamond abrasive, e.g., 45-
µm, added to the RGD. The RGD has a very high removal
rate and imparts exceptional flatness to the specimen.
However, if you are preparing solution annealed specimens,
or any non-age hardened specimen, the RGD chosen may be
too aggressive as residual deformation of the matrix may be
hard to control. The Apex Hercules S rigid grinding disk
has been specially formulated to avoid this problem.
Another grinding option is a Diamond Grinding Disk. These
have the diamond abrasive of various sizes, such as 70- and
45-µm, incorporated into the surface.
Polishing
In the traditional preparation method, grinding is followed
by two to four polishing steps, depending upon the quality
level needed. Polishing usually commences with either 6-
m or 3- m diamond abrasive, as a paste, slurry, or aerosol
with the appropriate liquid extender/lubricant on a cloth pad.
Historically, canvas, billiard, felt, nylon, or synthetic napless
or low-nap cloths were used for these abrasive sizes. Now,
rough polishing is conducted on napless cloths, such as
UltraPol™, UltraPad™, TexMet® 1000, or TriDent™
cloths. The choice is often a matter of personal preference or
a matter of cost. Wheel speeds are lower for polishing,
generally 120 - 150 rpm. In the traditional method, some
operators followed the first step with a second diamond
abrasive step, generally 3- or 1- m in size, or they used one
or two steps with aqueous aluminum oxide slurries. Cloths
and wheel speeds are similar. The time for each step is 60 -
120 seconds. Cleaning between polishing steps must be
performed carefully.
The most common fine polishing alumina abrasive sizes are
0.3- m (alpha alumina) and 0.05- m (gamma alumina).
Recently, acidic alumina slurries and basic colloidal silica
slurries have been employed for final polishing of
superalloys. These can be highly effective. Cleaning after
use of these abrasives requires careful scrubbing with cotton
soaked in a liquid detergent solution. Colloidal silica does
have some problems in its use. To clean the specimen
properly, and the cloth, stop adding abrasive with about 20 s
left in the cycle. With about 10 s left, direct the water jet
onto the cloth. When the machine stops, wash the specimens
and dry them with hot air. Despite such precautions,
specimens polished with colloidal silica can exhibit an
etching problem called “flashing.” For example, if an
etchant containing Cl- ions (such as glyceregia) is used, it
generally takes about a minute of swabbing to bring up the
structure. However, sometimes when swabbing a specimen
polished with colloidal silica, the surface darkens
immediately upon etching. Examination shows a craze-crack
pattern of deep scratches, Figure 1, while the structure is
poorly revealed. This scratch pattern cannot be removed by
repeating the final polishing step as the scratches are very
deep. This problem appears to be due to surface Passivation.
MasterPrep® alumina suspension is a good alternative to the
use of colloidal silica as it is totally free of this problem, as
well as staining. Other alumina polishing abrasives are made
by the calcinations process and they always contain
agglomerates. MasterPrep alumina is made by the sol-gel
process where the abrasive particles are precipitated from a
solution. Vibratory polishers are commonly used for final
polishing of superalloys. Cloths for final polishing, such as
MicroCloth®, often have a nap that is good for scratch
Figure 1. Example of “flashing” that can occur
when a specimen polished with colloidal silica is
etched with a reagent that contains chlorine ions
(glyceregia).
control. There are napless polishing cloths, such as the
synthetic polyurethane Chemomet® pad, that can be
effectively used for final polishing.
The contemporary practices utilize flat, napless cloths and
pads, except for the final step. But, even in the final step,
synthetic, napless polyurethane pads can be used. The
contemporary procedures rely upon use of automated
devices to improve specimen flatness and reproducibility of
the procedures. A five-step method is shown in Table 1.
For this method, use pressure-sensitive adhesive (psa)
backed SiC paper and cloths. A magnetic disk system, such
as the Apex system, can be used effectively. Charge the
choths with diamond in paste form and add MetaDi fluid
lubricant. During the cycle, add small amounts of MetaDi
Supreme diamond in suspension form to keep the cutting
rate high. If you have a grinder/polisher with a head speed
<100 rpm, you can use contra rotation (the head and platen
rotate in opposite directions) and the abrasive consumption
rate will be lower than if complementary rotation (head and
platen rotate in the same, counterclockwise, direction). Use
6 pounds of load per specimen (27 N) with step 1 at 240-300
rpm, steps 2 to 4 at 120-150 rpm and step 5 at 80-150 rpm.
The five-step method is conservative and will yield perfect
microstructures for Fe-Ni, Ni- and Co-base superalloys. If
the specimens are relatively easy to prepare, and most age-
hardened specimens are, step 4 can be eliminated. It is also
possible to substitute other materials for step 1. For
example, the ApexHercules S rigid grinding disk can be
used with an addition of 45-µm diamond slurry for 2-3
minutes at 150 rpm, 6 lbs. load and contra or complementary
rotation. Or, a 45-µm Diamond Grinding Disk can be used
with similar settings.
 Table 1. Contemporary Procedure for Ni-Based Superalloys
Surface Abrasive/Size Load Lb (N)/ Platen Speed Time
Specimen (rpm)/Direction (minutes)
Carbimet® waterproof 220-240 (P240-P280) grit SiC
discs (psa) water cooled 6 240-300 Until Plane
(27) Comp.
Ultra-Pol Silk Cloth 9-µm Metadi® Supreme Diamond
(psa) Suspension 6 100-150 5
(27) Comp.
3-µm Metadi® Supreme Diamond
Trident cloth (psa) Suspension 6 100-150 4
(27) Comp.
1-µm Metadi® Supreme Diamond
Trident cloth (psa) Suspension 6 100-150 3
(27) Comp.
Microcloth pad (psa) 0.05-µm Masterprep™ alumina slurry
6 80-150 2
(27) Contra

Table 2. Etchants for Superalloys

1. 15 ml HCl Glyceregia. Mix fresh; do not store. Good for about 20 minutes. Use by swabbing.
10 ml glycerol General purpose etch.
5 ml HNO3
2. 15 ml HCl Acetic glyceregia, stronger than glyceregia. Mix fresh; do not store. Good for about
10 ml Acetic acid 20 minutes. General purpose etch.
5 ml HNO3
1 - 2 drops glycerol
3. 15 ml HCl Mixed acids, for the most corrosion-resistance grades; e.g., Alloy 625. Mix fresh; do
10 ml Acetic acid not store. Good for 30 minutes. General purpose etch.
10 ml HNO3
4. 5 g CuCl2 Waterless Kalling’s reagent (number 2). This reagent can be made as a stock
100 ml HCl solution. Good grain boundary etch.
100 ml ethanol
5. 5 ml HF Electrolytic etch at 0.04 - 0.15 A/ m2, 6 - 12 V dc for Ni-based alloys. is in relief.
10 ml glycerol Stop etching when edges get brownish in color.
85 ml ethanol
6. 5 ml H2SO4 Add sulfuric to HCl, stir, allow to cool; add nitric. Discard when etch turns orange.
3 ml HNO3 Use under hood. Do not store.
92 ml HCl
7. 50 ml HCl Attacks in Ni-base alloys. Immerse for 10 - 15 seconds.
1 - 2 ml H2O2 (30%)
8. 10 g K3Fe (CN)6 Murakami’s reagent. Mix fresh; do not store. Carbide darkened at room
10 g KOH temperature; sigma darkened when used hot (75 C).
100 ml water
9. 50 ml lactic acid Lucas’s reagent for Fe-Ni, Ni- and Co-base superalloys. Use electrolytically at 1-2 V
150 ml HCl dc, for 10-20 s. Electrolyte can be made as a stock solution.
3 g oxalic acid
10. 100 ml water Mix and allow the solution to age for at least 1 h before use. Immerse specimen for a
100 ml HCl few seconds to reveal as-cast structure. Reagent can be made as a stock solution.
100 ml HNO3
3 g molybdic acid
Etching

Numerous etchants are used to reveal the structure of

superalloys. However, as for most metals, it is wise to
examine the polished surface carefully before etching.
Some minor second-phase particles can be easily observed
in the as-polished condition using bright field illumination.
Obviously, nonmetallic inclusions can be best observed in
the as-polished condition. Most wrought superalloys are
double vacuum-melted (VIM/VAR) and have extremely low
sulfur and oxygen contents and, thus, very low inclusion
contents. The sulfur content in many alloys is well below
0.001 wt. %, and no sulfides are observed. Cast superalloys
are generally made by vacuum induction melting (VIM) and
contain higher inclusion contents (and more nitrides and
carbides) than wrought alloys.

Several etchants are commonly used to reveal the general Figure 2b

structure of superalloys. Table 2 lists some of the most
commonly used etchants. Due to their excellent corrosion
resistance, most etchants work best by swabbing with cotton
soaked in the etchant. Immersion etching often results in a
more irregular etch response. Many of the etchants must be
mixed fresh and used within a short time span. Glyceregia
is the mildest of the first three etchants. If etching occurs
too slowly, use etchant 2 or 3.

Examples of Superalloy Microstructures

Cast Alloys

Metallographers are often requested to reveal the dendritic

structure of cast specimens and perform measurements of
the secondary dendrite arm spacing. Figure 2 shows the
microstructure of as-cast CNK7, a Russian cast alloy turbine
blade that was tested in creep for 20,100 hours at 700 ºC at a
load of 60 kg/mm2. The dendrites are shown after etching
with glycregia, waterless Kalling’s, and the Lucas Figure 2c
electrolytic reagent.
Figure 2. Dendritic solidification structure in
Russian alloy CNK7 creep-tested turbine blade
revealed using a) glyceregia, b) waterless
Kalling’s; and c) the Lucas electrolytic reagent (2
V dc, 10 s).

Figure 3 shows the dendrites in IN738 etched with a variety

of reagents. Note that these dendrites are much finer than
those in the CNK7 creep-tested turbine blade. Waterless
Kalling’s reagent (Fig. 3a) and reagent 3 (the “15-10-10”
reagent, Fig. 3b) revealed the dendrites with less contrast
than the Lucas electrolytic etch.

Figure 2 a
 Figure 3a Figure 4a

Figure 3b Figure 4b

Figure 4c
Figure 3c
Figure 4. Dendritic solidification structure in
Figure 3. Dendritic solidification structure of
MAR-M247 revealed using a) glyceregia, b)
IN738 revealed by a) waterless Kalling’s
Lucas reagent (2 V dc, 10 s); and c) the molybdic
reagent, b) the 15-10-10 reagent (No. 3, Table 1);
acid reagent.
and c) the Lucas reagent (2 V dc, 10s).
 Figure 6b
Figure 5. Dendritic solidification structure of
MAR-M509 etched with the Lucas reagent (2 V
dc, 10 s).

Figure 4 shows the as-cast dendritic structure in MAR-M247

after etching with glyceregia (Fig. 4a), the Lucas electrolytic
etch (Fig. 4b) and the molybdic acid etch. The molybdic
acid reagent produced the strongest contrast.

The dendritic structure of cast MAR-M509, a Co-based

superalloy, is shown in comparison in Figure 5 etched with
the Lucas electrolytic reagent.

Wrought Alloys

Wrought alloys are evaluated for grain size and the presence
of second-phase precipitates. To illustrate the effectiveness
of the preparation method, and the use of different etchants,
several examples will be shown below. Figure 6 shows the
microstructure of Alloy 718, the most commonly produced
superalloy. This specimen is a non-rotating grade with a fine
grain size and considerable delta phase and large MC-type
primary carbides.
Figure 6c
Figure 6. Microstructure of Alloy 718 (non-
rotating grade) with a fine grain size,
considerable delta and large primary MC carbides
revealed using a) glyceregia, b) the “15-10-10”
etch (No. 3); and c) the Lucas reagent (2 V dc, 20
s).

In comparison to Figure 6, Figure 7 shows the

microstructure of premium quality, rotating grade Alloy
718. It actually contained less primary MC carbides,
although Figures 7a and b illustrate examples of the
stringers present, and some delta is present but less than in
the previous example (non-rotating grade). Etching with
glyceregia only outlined the carbides after about one minute
of swabbing. The “15-10-10” reagent produced a grain
contrast etch. The Lucas reagent revealed the fine grain
structure and the delta phase properly.

Figure 6a
 In some cases metallographers examine the microstructure
of specimens after forging and the grain structure is not fully
recrystallized as demonstrated in Figure 8 that shows the
structure of as-forged Carpenter Custom Age 625 Plus. This
alloy is too corrosion resistant to use glyceregia. Figure 8 a
and b show the results of etching with the “15-10-10”
reagent, developed for this grade, and with the Lucas
reagent. Both revealed the structure well.

Figure 7a

Figure 8a

Figure 7b

Figure 8b

Figure 8. Partially recrystallized grain structure

of as-forged Custom Age 625 PLUS revealing a
“necklace” type duplex grain structure after
etching with a) the “15-10-10” reagent and b) the
Lucas reagent (2 V dc, 20 s).

The final example shows the microstructure of a wrought,

fully annealed Co-based alloy, Haynes 188. Figure 9 shows
Figure 7c
the specimen etched with a) the “15-10-10” reagent and b)
with the Lucas reagent (2 V dc, 20 s). Note that both
Figure 7. Microstructure of premium quality Alloy 718
reagents reveal some dislocation etch pitting.
revealed using a) glyceregia, b) the “15-10-10” reagent;
and c) Lucas reagent (2 V dc, 20 s).
 Figure 9a

Figure 9b

Figure 9. Microstructure of wrought, annealed

Haynes 188 etched with a) the “15-10-10”
reagent and with b) the Lucas reagent (2 V dc, 20
s).

Conclusions

A modern preparation cycle with five steps was presented in

this paper. This procedure works perfectly for all Fe-Ni, Ni-
and Co-based superalloys. For age-hardened alloys, step 4
can be eliminated to save time. Other products can be
substituted for SiC in the initial grinding step. Always
section specimens with an abrasive cut-off wheel designed
for the metallographic preparation of superalloys. Lesser
quality (“production” or shop wheels) will impart far more
damage that may be impossible to remove. After proper
sectioning, commence preparation with the finest possible
abrasive size. Modern napless woven or pressed cloths and
pads produce far better results, controlling flatness and
reducing artifacts. MasterPrep alumina suspension, made by
the sol-gel process, eliminates etching problems when
chlorine ion containing reagents are used. A new reagent,
the Lucas electrolytic reagent was illustrated. It is a versatile
reagent for superalloys.

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