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 some-
times 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 exami-
nation of corrosion-resistant alloys.
The following tables (D4.1–D4.3) 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 ETCHING TECHNIQUES FOR Ni-BASE ALLOYS AND WELDS

TABLE D4.1 Macro Etchants.

Etchant Composition/Use Notes
Lepito’s a) 15 g (NH4)2S2O8 Macroetch for general structure of
(ammonium persulfate)and base metals and welds. Good for
75 ml water, b) 250 g FeCl3 determining weld penetration
and 100 ml HCl, c) 30 mL and measuring grain size. Not
HNO3. Mix a and b, then effective at revealing
add c, immerse for 30– solidification structure.
120 sec at room
temperature
Mixed acids Equal parts HCL, HNO3, and A general attack etch that reveals
acetic acids. both macro and microstructure.
Use fresh. Swab at room This etchant must be used within
temperature. a few minutes of mixing and then
discarded when it turns orange in
color.
HCL and Equal parts HCL and H2O2. Reveals general structure.
peroxide Immerse or swab at room
temperature.

TABLE D4.2 Micro Etchants (Swab or Immerse).

Etchant Composition/Use Notes
Mixed acids Equal parts HCL, HNO3, A general attack etch will reveal
and acetic acids. segregation patterns,
Use fresh. Swab at room precipitates, and grain
temperature. boundaries. This etchant must
be used within a few minutes
of mixing and then discarded
when it turns orange in color.
Glyceregia 15 ml glycerol, 10 ml HCl, Can also use 15/25/5 and 20/10/5
and 5 ml HNO3. ratios. A general purpose etch
Use fresh. Immerse or similar to Mixed Acids, but
swab at room not so aggressive. It outlines
temperature. 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.
Nitric-Acetic 10 ml HNO3 and 90 ml Use for Ni and NiCu alloys.
acetic acid.
Immerse or swab at room
temperature.
 APPENDIX D ETCHING TECHNIQUES FOR Ni-BASE ALLOYS AND WELDS 421

TABLE D4.2 Continued

Etchant Composition/Use Notes
Nitric-Hydrofluoric 20 ml HNO3 and 3 ml General microstructure etchant.
hydrofluoric acid (HF). Can also use 30/3 and 50/3
Immerse or swab at room ratios.
temperature.
HCL/Bromine Immerse in concentrated Use for NiCrMo and NiFeCrMo
HCL for 3 seconds, alloys to reveal grain
then rinse in alcohol. boundaries. Caution: do not
Immerse in mixture of breathe bromine fumes.
1 part bromine and 99
parts methanol for
10–20 seconds.
Nital 5 ml HNO3 and 95 ml Etches carbon and low alloy
methanol. steels. Use for dissimilar welds
Swab or immerse at room with these steels. See Table
temperature. D4.3—may also be used as an
electrolytic etchant

TABLE D4.3 Micro Etchants (Electrolytic).

Etchant Composition/Use Notes
10% Chromic 10 g CrO3 (chromic A good general etchant for revealing
acid) and 90 mL the microstructure of base metals
water. Use at room and welds. Reveals segregation
temperature. Etch at behavior and grain boundaries in
3–6 volts for 5–60 weld metals.
seconds. May be used for dissimilar welds with
carbon steels if the carbon steel is
previously immersion etched with
nital.
Phosphoric 80 mL H3PO4 and 50/50 and 20/80 ratios may also be used.
10 mL water. Reveals grain boundaries in NiFeCo
Use at room and NiCrFe alloys.
temperature. Etch at Tends to pit the sample if overetched.
3 volts for 5–10
seconds.
Hydrofluoric 5 ml HF, 10 ml glycerol, Reveals gamma prime precipitation in
and Glycerol 85 ml ethanol. Ni-base superalloys.
Use at room
temperature. Etch at
6–12 volts.
Nital 5 ml HNO3 and 95 ml Reveals grain boundaries in NiCr,
methanol. NiFeCr, and NiCrFe alloys.
422 APPENDIX D ETCHING TECHNIQUES FOR Ni-BASE ALLOYS AND WELDS

REFERENCES

1. Metals Handbook Ninth Edition, Volume 9, pp. 305–309. 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 1188–1199. 1991.
3. Metallography of Superalloys, G.F. Vander Voort, Buehler Ltd., October 2003.