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George F.

Vander Voort
Buehler Ltd.
Lake Bluff, Illinois USA
Contemporary Procedure for Ni-Based Superalloys
Surface Abrasive/Size Load Platen Time
Lb (N) Speed (min.)
CarbiMet 180-240 (P180-P280)
6 240-300 Until
waterproof grit SiC
(27) Comp. Plane
discs (psa) water cooled
Ultra-Pol Silk 9-m MetaDi
6 100-150 5
Cloth (psa) Supreme Diamond
(27) Comp.
Suspension
3-m MetaDi
TriDent cloth 6 100-150 5
Supreme Diamond
(psa) (27) Comp.
Suspension
1-m MetaDi
TriDent cloth 6 100-150 3
Supreme Diamond
(psa) (27) Comp.
Suspension
MicroCloth 0.05-m
6 80-150 3
pad (psa) MasterPrep
(27) Contra
alumina slurry
Common Etchants
15 mL HCl Glyceregia. Mix fresh; do not store. Good for
10 mL glycerol about 20 minutes. Use by swabbing. General
5 mL HNO3 purpose etch.
15 mL HCl Acetic glyceregia, stronger than glyceregia. Mix
10 mL Acetic acid fresh; do not store. Good for about 20 minutes.
5 mL HNO3 General purpose etch.
1 - 2 drops glycerol
15 mL HCl Mixed acids, for the most corrosion-resistance
10 mL Acetic acid grades; e.g., Alloy 625. Mix fresh; do not store.
10 mL HNO3 Good for 30 minutes. General purpose etch.
5 g CuCl2 Waterless Kallings reagent (number 2). This
100 mL HCl reagent can be made as a stock solution. Good
100 mL ethanol grain boundary etch.
Lucas Reagent

50 mL lactic acid Lucass reagent for Fe-Ni, Ni- and Co-base


150 mL HCl superalloys. Use electrolytically at 1-2 V dc, for
3 g oxalic acid 10-20 s. Electrolyte can be made as a stock
solution.

Molybdic Acid Reagent


100 mL water Molybdic acid reagent to reveal the dendritic
100 mL HCl structure of cast Ni-base superalloys. Mix and
100 mL HNO3 alloy to stand >1 h before use. Immerse
3 g molybdic acid specimen for several seconds. Can be stored.
Example of flashing, an etching problem that can occur when a reagent
containing chlorine ions is used to etch a specimen final polished with colloidal
silica. The surface etches very fast producing deep scratches. Electrolytic etchants
do not flash. This specimen was alloy 718 etched with glycregia.
Directionally solidified cast Ni-base eutectic alloy (Courtesy of W.
Yankauskas, TRW.
Macrostructure of a VIM (vacuum induction melted) ingot of Fe-52% Ni alloy. A slice was
cut transverse to the ingot axis and hot acid etched (50% HCl at 70 C) revealing the
solidification pattern. There is a very thin surface zone of small grains. Below the surface,
there is a zone of columnar grains and the central portion is equiaxed but coarse, with the
size increasing going towards the center. The scale is in inches.
Dendrites in as-cast Monel (Ni 30% Cu) revealed using Berahas
reagent (50 mL water 50 mL HCl 2 g ammonium bifluoride 1 g
potassium metabisulfite). Originals at 50X (left) and 100X (right).
Magnification bars are 200 and 100 m long, respectively.
Waterless Kallings 15 HCl - 10 Acetic Acid -
10 HNO3

Lucas Reagent
2 V dc, 10s

Dendritic structure of cast IN-738 alloy (Ni 0.17C 16Cr 8.5Co 2.6W
1.75 Mo 0.9Nb 1.75Ta 3.4Al 0.01B 0.1Zr).
Glyceregia Lucas Reagent
2 V dc, 10 s

Molybdic Acid Reagent

Dendritic structure of cast MAR-M247 alloy.


Glyceregia Waterless Kallings

Lucas Reagent
2 V dc, 10s

Dendritic solidification structure in cast Russian alloy CNK7 (Ni 0.08C


15Cr 9Co 7W 0.4Mo 3.5Ti 4.2Al 0.01B 0.02Ce).
Microstructure of cast Russian Ni-base alloy CNK7 turbine blade etched with
15 mL HCl-10 mL acetic acid-10 mL HNO3..
200 m

Dendritic microstructure of Alloy 718 (Ni 0.04C 18.5Fe 19Cr 3Mo


0.9Ti 5.1Nb+Ta 0.5Al) in the as-cast condition after tint etching with
Berahas reagent. The white particles are Laves phase.
Microstructure of Ren 41 (Ni 0.09C 11Co 19Cr 10Mo
3.1Ti 1.5Al 0.01B) after electroslag remelting (ESR) and
etching with 15 mL HCl-10 mL acetic acid-10 mL nitric acid. The
magnification bar is 20 m long.
Microstructure at a freckle found on a Ren 41 macroetch disc.
Bright Field Polarized Light + Sensitive Tint

The microstructure of hot worked, annealed and cold drawn Monel 400 (Ni 32% Cu - <0.3% C -
<2% Mn - <0.5% Si) revealed using Berahas selenic acid etch for copper (longitudinal axis is
horizontal). Monel alloys are very difficult to color etch, especially wrought alloys (as-cast alloys are
easier). Bright field revealed a weak image as the interference film produce is thin (inclusions,
arrows, can be seen). When this occurs, polarized light will often enhance the image quality
dramatically (the sensitive tint filter enhances coloration), as shown. Note the deformed, twinned
FCC alpha grain structure. The magnification bars are 50 m long.
Martensitic structure (335 HV) of Greek Ascoloy (Fe
0.17C 13Cr 2Ni 3W) revealed using Vilellas
reagent.
Martensitic (345 HV) grain structure of Moly Ascoloy (Fe 0.11C
0.7Mn 11.75Cr 2.5Ni 1.75Mo 0.32V 0.03N) etched with Vilellas
reagent.
Glyceregia Berahas Tint Etch

Coarse grains
near surface

Grain structure of A286 (Fe 0.05C 26Ni 15Cr 1.25Mo 0.3V 2.15Ti 0.2Al
0.003B) solution annealed at 1650 F/899 C.
1825 F/996 C 1875 F 1024 C

1900 F 1038 C

Effect of solution annealing temperature on recrystallization in austenitic alloy 330 (Fe


0.05C 36Ni 19Cr) revealed by etching with 10% oxalic acid at 6 V dc for 10 s).
1925 F 1052 C 1950 F 1066 C

Effect of solution annealing temperature on recrystallization in austenitic alloy 330


(etched with 10% oxalic acid at 6 V dc for 10 s).
Bright Field Dark Field

Nomarski DIC

As-rolled alloy 330 solution annealed at 1975 F/1079 C (10% Oxalic acid, 6 V dc, 10 s).
15 HCl - 10 Acetic
Glyceregia
Acid - 10 HNO3

Lucas Reagent
2 V dc, 10 s
Grain structure of solution annealed and aged non-rotating quality alloy 718
with a fine grain size, considerable delta and large primary MC carbides.
Glyceregia 15 HCl - 10 Acetic Acid -
10 HNO3

Lucas Reagent
2 V dc, 10 s

Grain structure of premium quality alloy 718 in the forged and aged condition.
Note that glyceregia did not reveal the grain structure, only primary MC carbides.
Austenitic grain structure of fine grained alloy 718 in the solution annealed
and aged condition etched with glyceregia revealing delta phase pinning the
boundaries. The magnification bar is 10 m long.
954 C/1750 F 1066 C/1950 F

Microstructure of alloy 718 solution annealed at 954 and 1066 C and


etched with glyceregia. Note differences in magnification. The low solution
annealing temperature does not dissolve the delta phase, as happens with
the high solution annealing temperature. Delta is used to control the grain
size for best cryogenic properties. MC type carbides are observed in both
specimens.
954 C/1750 F SA + DA 1066 C/1950 F SA + DA

Microstructure of alloy 718 solution annealed at 954 and 1066 C and double
aged; etched with glyceregia. Note differences in magnification. The low solution
annealing temperature does not dissolve the delta phase, as happens with the high
solution annealing temperature. Delta is used to control the grain size for best
cryogenic properties. MC type carbides are observed in both specimens. The
strengthening phase is much too fine to be seen with light microscopy. Note that
the structure looks the same before or after aging (although the hardnesses are
different).
Delta phase in Alloy 718 solution annealed at 954 C (1750 F) and aged 100 h
at 1600 F/871 C (etched with glyceregia)
100X 200X

500X

As-forged microstructure of Carpenters Thermo-Span alloy, controlled


expansion Fe-based superalloy (Fe 0.02C 5.5Cr 24.5Ni 29Co 0.85Ti
4.8Nb 0.45Al) etched with glyceregia.
Microstructure at the center of a 12-inch diameter (300-mm) bar of
as-forged Alloy 600 (Ni 15.5Cr 8Fe 0.1 max. C) etched with
glyceregia (magnification bar is 50-m long). There are carbides in
the grain boundaries.
Austenitic grain structure of Alloy 617 (Ni 0.01C 22Cr 12.5Co 9Mo
1.2Al), solution annealed and aged, etched with 15 mL HCl-10 mL acetic
acid-10 mL HNO3, magnification bar is 100 m long.
Glyceregia 15 mL HCl-10 mL acetic acid-10 mL HNO3

Austenitic grain structure of alloy X-750 (Ni 0.04C 7Fe 15.5Cr 2.5Ti
0.95Nb+Ta 0.7Al) in the solution annealed and aged condition revealed
using glyceregia (left) and 15 mL HCl-10 mL acetic acid-10 mL nitric acid
(right). The magnification bars are 100 and 50 m, left and right,
respectively.
Microstructure of as-forged Waspaloy (Ni 0.07C 13.5Co 19.5Cr
4.3Mo 3Ti 1.4Al 0.07Zr 0.006B) etched with 15 mL HCl-10 mL
acetic acid-10 mL HNO3, magnification bar is 50 m long.
1010 C (1850 F) 1038 C (1900 F)

All magnification
Influence of bars are 100 m long
solution
annealing
temperature on
grain growth in
1066 C (1950 F)
Waspaloy
Microstructure of wrought, solution annealed and double aged (about 42 HRC)
Waspaloy, a nickel-based superalloy tint etched with Berahas BIV reagent
revealing twinned austenitic grains. Viewed in bright field. The magnification
bar is 100 m long.
Glyceregia 15-10-10

Lucas reagent, 1.2 V


dc, 40 s

Microstructure of forged, rotating-grade Waspaloy in the solution annealed


and aged condition.
Glyceregia 15-10-10

Lucas Reagent, 2 V
dc, 20 s
Microstructure of forged, rotating grade Waspaloy in the solution annealed and
aged condition. A necklace-type bimodal grain size distribution was observed.
Microstructure of an as-forged bar of an experimental composition similar to
alloy 625 revealing a necklace type bimodal grain size distribution due to
partial recrystallization. The specimen was etched with acetic glyceregia. The
magnification bar is 100 m long.
As-Polished Acetic Glyceregia

Microstructure of alloy 625 (Ni 0.05C 21.5Cr 9Mo 3.7Nb+Ta) after


solution annealing at 1850 F/1010 C revealing carbides (left, as polished)
and the grain structure (right, revealed using acetic glyceregia). The
hardness was 191 HV.
15 HCl - 10 Acetic Acid - 10 HNO3 Lucas Reagent, 2 V dc, 10 s

Partially recrystallized grain structure of as-forged Carpenter Custom Age


625 PLUS alloy (Ni 0.01C 20.5Cr 8.25Mo 3.5Nb 1.3Ti) revealing a
necklace type duplex grain structure.
1680 F/916 C 1845 F/1007 C

Microstructure of hot rolled Custom Age 625 PLUS alloy with finish rolling
temperatures of 1680 F/916 C (left, partially recrystallized) and at 1845
F/1007 C (right, fully recrystallized) revealed using 15 mL HCl 10 mL
acetic acid 10 mL HNO3.
Finish Roll at 1680 F/916 C + SA and DA Finish Roll at 1845 F/1007 C + SA and DA

Grain structure of the Custom Age 625 PLUS alloy specimens finish rolled at
1680 (left) and 1845 F (right) after solution annealing and double aging
revealed using 15 mL HCl 10 mL acetic acid 10 mL HNO3.
Austenitic grain structure of Carpenters Custom Age 625 Plus alloy in
the solution annealed and aged condition after etching with acetic
glyceregia. The magnification bar is 100 m long.
Bright Field Dark Field

Microstructure of as-hipped (hot isostatically pressed) powder-


metallurgy (P/M) Ren 95 alloy (Ni 0.15C 8Co 14Cr 3.5Mo 3.5W
2.5Ti 3.5Al 3.5Nb) revealing grain boundary carbides and coarse
gamma prime in an austenitic matrix after etching with glyceregia.
Microstructure of as-hipped (hot isostatically pressed) P/M Ren 95 alloy
revealing grain boundary carbides and coarse gamma prime in an austenitic
matrix after etching with glyceregia. Prior-particle shapes are clearly visible
at low magnification.
Lucas Reagent, 2 V dc, 10 s Molybdic Acid Reagent

Microstructure of Russian P/M turbine blade alloy EP741NP (Ni 0.04C 9Cr
15.8Co 3.9Mo 5.5W 1.8Ti 2.6Nb 0.25Hf) revealing the coarse grain
structure in grain contrast (other etchants simply darkened the matrix
uniformly). The specimen was Hiped and heat treated (2210 F 8 h, furnace
cool to 2120 F, air cool; age at 1600 F for 32 h, air cool).
15 mL HCl 10 mL acetic acid Molybdic Acid Reagent
10 mL HNO3

Microstructure of Russian P/M turbine blade alloy EP741NP revealing


coarse gamma prime and carbides at prior-particle boundaries.
Grain structure and carbides in Hastelloy B (Ni 0.02C 28Mo 5Fe -
0.3V) revealed using 15 mL HCl 10 mL acetic acid 10 mL HNO3.
Kallings No. 2 Berahas BIV

Lucas Reagent, 2 V dc,


10 s
Microstructure of Russian ZMI-3U Ni-base alloy (Ni 0.08C 13.25Cr
5.5Co 5W 1.2Mo 4.9Ti 2.9Al 0.075Nb 0.015B 0.01Zr) turbine
blade after 39000 h service.
Grain structure of Haynes Alloy G30 (Ni 0.01C 30Cr 15Fe 5.5Mo 2.5W)
revealed using (left) 15 mL HCl 10 mL acetic acid 10 mL HNO3 and (right)
with the Lucas reagent at 2 V dc for 20 s.
Grain structure of Haynes alloy HR-160 (Ni 0.05C - 29Co 28Cr 2.75Si
2Fe 0.5Mn) revealed using 15 mL HCl 10 mL acetic acid 10 mL
HNO3 (209 HV).
Fusion weld in Haynes HR-160 Alloy
37Ni-29Co-28Cr-2.75Si-2Fe-0.5Mn-0.05C

200m

200m

Base Metal

Top (left) and bottom (right, above)


sides of a butt weld between two sheet 100m

specimens of HR-160 alloy etched with


15 HCl-10 HNO3-10 Acetic acid. The Weld
arrows point to the fusion line. Metal
FCC grain structure of solution annealed and aged (398HV) U-520 (Ni
0.04C 19Cr 12.5Co 6.7Mo 3.1Ti 2Al 1W 0.007B) etched with
15 mL HCl 10 mL acetic acid 10 mL HNO3.
Grain structure of U-700 (Ni - <0.15C 18.5Co 15Cr 5.2Mo 3.5Ti
4.25Al 0.05B) strip etched with 15 mL HCl 10 mL acetic acid 10 mL
HNO3 showing a range of grain sizes.
Coarse gamma prime in as-forged U-720 (Ni 0.015C 16Cr 14.7Co
3Mo 1.25W 5Ti 2.5Al 0.015B) revealed by etching with 15 mL HCl
10 mL acetic acid 10 mL HNO3.
Contemporary Procedure for Co and Alloys
Surface Abrasive/Size Load Platen Time
Lb (N) Speed (min.)
CarbiMet 180-240 (P180-P280)
6 240-300 Until
waterproof grit SiC
(27) Comp. Plane
discs (psa) water cooled
Ultra-Pol Silk 9-m MetaDi
6 100-150 8
Cloth (psa) Supreme Diamond
(27) Comp.
Suspension
3-m MetaDi
TriDent cloth 6 100-150 6
Supreme Diamond
(psa) (27) Comp.
Suspension
1-m MetaDi
TriDent cloth 6 100-150 4
Supreme Diamond
(psa) (27) Comp.
Suspension
MicroCloth 0.05-m
6 80-150 3
pad (psa) MasterPrep
(27) Contra
alumina slurry
15 HCl 10 Acetic Lucas Reagent, 2 V
Acid 10 HNO3 dc, 10 s

Berahas Reagent

Dendritic structure of cast MAR-M509 Co-based alloy revealed using three


different reagents.
Microstructure of wrought 99.99% pure cobalt, etched with lactic acid,
nitric acid and water (80:10:10). Magnification bar is 100 m long.
100 m 100 m

Elgiloy (Co-20% Cr-15% Fe-15% Ni-7% Mo-2% Mn 0.05% B-0.15% C) that


was hot rolled and solution annealed producing partial recrystallization. Etched
with 15 mL HCl 10 mL acetic acid 10 HNO3, left: bright field, right:
Nomarski DIC.
Microstructure of Elgiloy, a Co-based alloy used for watch springs (Co 20%
Cr 15% Fe 15% Ni 2% Mn 7% Mo 0.05% B 0.15% C) after hot
rolling and solution annealing (1040 C 2 hours, water quenched). The
specimen is partially recrystallized. The specimen was tint etched with Berahas
IV plus 1 g FeCl3 per 100 mL. The specimen was viewed with polarized light
plus sensitive tint. The magnification bar is 100 m long.
100 m 100 m

Elgiloy (Co-20% Cr-15% Fe-15% Ni-7% Mo-2% Mn 0.05% B-0.15% C) that


was hot rolled and solution annealed producing partial recrystallization. Etched
with 15 mL HCl 10 mL acetic acid 10 HNO3, left: bright field, right:
Nomarski DIC.
Microstructure of Elgiloy, a Co-based alloy used for watch springs after hot
rolling and solution annealing (1090 C 2 hours, water quenched). The
specimen is fully annealed. The specimen was tint etched with Berahas IV plus
1 g FeCl3 per 100 mL. The specimen was viewed with polarized light plus
sensitive tint. The magnification bar is 100 m long.
100 m 100 m

Elgiloy (Co-20% Cr-15% Fe-15% Ni-7% Mo-2% Mn 0.05% B-0.15% C) that


was hot rolled and solution annealed producing full recrystallization. Etched
with 15 mL HCl 10 mL acetic acid 10 HNO3, left: bright field, right:
Nomarski DIC.
Microstructure of Elgiloy, a Co-based alloy used for watch springs after hot rolling
and solution annealing (1150 C 2 hours, water quenched). Note the annealing
twins. The specimen was tint etched with Berahas IV plus 1 g FeCl3 per 100 mL.
The specimen was viewed with polarized light plus sensitive tint. The magnification
bar is 100 m long.
Elgiloy (Co-20% Cr-15% Fe-15% Ni-7% Mo-2% Mn 0.05% B-0.15% C) that
was hot rolled and solution annealed producing full recrystallization. Etched with
15 mL HCl 10 mL acetic acid 10 HNO3, left: bright field, right: Nomarski DIC.
15HCl 10 Acetic Acid 10 HNO3 Lucas Reagent, 2 V dc, 20 s

Grain structure of Haynes 188 (Co 0.1C 1.5Fe 22Ni


20Cr 14W 0.08La) after etching with 15 mL HCl 10 mL
acetic acid and 10 mL HNO3(left) and the Lucas reagent at 2
V dc for 20s (right). Note that the etchants produced
dislocation etch pits.
Cold Reduced 35% Cold Reduced 35% + Solution Anneal

Microstructure of L605 (Co 0.1C 10Ni 20Cr 15W 1.5Mn


0.5Si) after a 35% cold reduction (left) and then after solution
annealing at 1149 C (2100 F) and revealed using 15 mL HCl-10 mL
acetic acid-10 mL nitric acid. The magnification bars are both 50 m
long. L605 is also known as Haynes alloy 25.
MP35N

Microstructure of MP35N; left bright field; right Nomarski DIC (etched


with 15 mL HCl 10 mL acetic acid 10 mL HNO3)