APPENDIX D

Etching Techniques for Ni-base Alloys

and Welds

The microstructure of Ni-base welds can be revealed using a variety of etching

techniques. Weld metal, the partially melted zone around the weld, and sometimes the HAZ, are not homogeneous, so they tend to etch differently than
base metals. A Ni-base weldment may involve two different alloys, or even
joints of a Ni-base alloy to a ferrous material. Various etchants and etching
techniques have been found to provide results of interest to the investigator.
The etching techniques described here can be divided into chemical methods
or electrolytic methods. In general, chemical methods are simpler to apply and
require less equipment, so they tend to be favored by the non-specialist.
Electrolytic methods tend to be favored by those who specialize in the examination of corrosion-resistant alloys.
The following tables (D4.1D4.3) include etching techniques that the
authors have found useful in examining the microstructure of Ni-base alloy
welds. This is not meant to be an exhaustive list, but merely what the authors
commonly use for the materials listed. More extensive listings of etchants and
etching methods can be found in the ASM Metals Handbook (1), the CRC
Handbook of Metal Etchants (2), and Metallography of Superalloys (3).

Welding Metallurgy and Weldability of Nickel-Base Alloys, by John N. DuPont, John C. Lippold,
and Samuel D. Kiser
Copyright 2009 John Wiley & Sons, Inc.

419

420

APPENDIX D

TABLE D4.1

ETCHING TECHNIQUES FOR Ni-BASE ALLOYS AND WELDS

Macro Etchants.

Etchant

Composition/Use

Notes

Lepitos

a) 15 g (NH4)2S2O8
(ammonium persulfate)and
75 ml water, b) 250 g FeCl3
and 100 ml HCl, c) 30 mL
HNO3. Mix a and b, then
add c, immerse for 30
120 sec at room
temperature
Equal parts HCL, HNO3, and
acetic acids.
Use fresh. Swab at room
temperature.

Macroetch for general structure of

base metals and welds. Good for
determining weld penetration
and measuring grain size. Not
effective at revealing
solidification structure.

Mixed acids

A general attack etch that reveals

both macro and microstructure.
This etchant must be used within
a few minutes of mixing and then
discarded when it turns orange in
color.
Reveals general structure.

HCL and
peroxide

Equal parts HCL and H2O2.

Immerse or swab at room
temperature.

TABLE D4.2

Micro Etchants (Swab or Immerse).

Etchant

Composition/Use

Notes

Mixed acids

Equal parts HCL, HNO3,

and acetic acids.
Use fresh. Swab at room
temperature.

Glyceregia

15 ml glycerol, 10 ml HCl,
and 5 ml HNO3.
Use fresh. Immerse or
swab at room
temperature.

Nitric-Acetic

10 ml HNO3 and 90 ml
acetic acid.
Immerse or swab at room
temperature.

A general attack etch will reveal

segregation patterns,
precipitates, and grain
boundaries. This etchant must
be used within a few minutes
of mixing and then discarded
when it turns orange in color.
Can also use 15/25/5 and 20/10/5
ratios. A general purpose etch
similar to Mixed Acids, but
not so aggressive. It outlines
ferrite and austenite, attacks
martensite and sigma phase,
and reveals carbides and grain
boundaries. Good for NiCrFe
and NiFeCr alloys. It should
also be used fresh, and
discarded when it becomes
orange in color.
Use for Ni and NiCu alloys.

APPENDIX D ETCHING TECHNIQUES FOR Ni-BASE ALLOYS AND WELDS

421

TABLE D4.2 Continued

Etchant

Composition/Use

Nitric-Hydrofluoric

HCL/Bromine

Nital

TABLE D4.3
Etchant

Notes

20 ml HNO3 and 3 ml
hydrofluoric acid (HF).
Immerse or swab at room
temperature.
Immerse in concentrated
HCL for 3 seconds,
then rinse in alcohol.
Immerse in mixture of
1 part bromine and 99
parts methanol for
1020 seconds.
5 ml HNO3 and 95 ml
methanol.
Swab or immerse at room
temperature.

General microstructure etchant.

Can also use 30/3 and 50/3
ratios.
Use for NiCrMo and NiFeCrMo
alloys to reveal grain
boundaries. Caution: do not
breathe bromine fumes.

Etches carbon and low alloy

steels. Use for dissimilar welds
with these steels. See Table
D4.3may also be used as an
electrolytic etchant

Micro Etchants (Electrolytic).

Composition/Use

Notes

10% Chromic

10 g CrO3 (chromic
acid) and 90 mL
water. Use at room
temperature. Etch at
36 volts for 560
seconds.

Phosphoric

80 mL H3PO4 and
10 mL water.
Use at room
temperature. Etch at
3 volts for 510
seconds.
5 ml HF, 10 ml glycerol,
85 ml ethanol.
Use at room
temperature. Etch at
612 volts.
5 ml HNO3 and 95 ml
methanol.

A good general etchant for revealing

the microstructure of base metals
and welds. Reveals segregation
behavior and grain boundaries in
weld metals.
May be used for dissimilar welds with
carbon steels if the carbon steel is
previously immersion etched with
nital.
50/50 and 20/80 ratios may also be used.
Reveals grain boundaries in NiFeCo
and NiCrFe alloys.
Tends to pit the sample if overetched.

Hydrofluoric
and Glycerol

Nital

Reveals gamma prime precipitation in

Ni-base superalloys.

Reveals grain boundaries in NiCr,

NiFeCr, and NiCrFe alloys.

422

APPENDIX D

ETCHING TECHNIQUES FOR Ni-BASE ALLOYS AND WELDS

REFERENCES
1. Metals Handbook Ninth Edition, Volume 9, pp. 305309. ASM International,
Materials Park, OH. 1985
2. CRC Handbook of Metal Etchants, Walker, P. and Tarn, W. H., editors. CRC Press,
Boca Raton, FL. Pages 11881199. 1991.
3. Metallography of Superalloys, G.F. Vander Voort, Buehler Ltd., October 2003.