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Revealing
Prior-Austenite Grain
Boundaries in
Heat-Treated Steels
h
here
are a number of wellestablished
(see ASTM E 112,
e
ffor example) procedures that
aare used to decorate the PGBs
during a heat-treatment cycle, e.g., the
McQuaid-Ehn carburizing test (Fig. 1)
and the oxidation test. In some mediumcarbon steels, at a specic cooling rate,
proeutectoid ferrite will precipitate at the
PGBs, while in high-carbon steels (generally hypereutectoid tool steels), proeutectoid cementite will precipitate on the
PGBs upon slow cooling from elevated
temperatures. These conditions are often
seen in as-cast or as-rolled steels, as shown
Fig. 4. Intergranular SCC cracks in 4340 alloy steel revealed by etching with saturated aqueous picric acid, plus HCl and Nacconol 90G wetting agent (80C 60 sec.), magnication bars
are 20 m long).
a)
b)
Fig. 5. Etching with 2% nital (a) reveals packets of lath martensite; etching with aqueous
saturated picric acid solution with HCl and a wetting agent at 20C (b) faintly revealed
the prior-austenite grain boundaries in SAE 723, Grade 3, Class 3 pressure vessel steel (Fe
- 0.33%C - 0.25%Mn - 0.13%Si - 3.55%Ni - 1.66%Cr - 0.48%Mo - 0.12%V). Using aqueous
saturated picric acid plus HCl and a wetting agent at 90C, however, revealed the prior-austenite grain boundaries: (c) bright-eld illumination and (d) dark-eld illumination.
including the saturated aqueous picricacid solution. Without the wetting agent
added, saturated aqueous picric acid was
an excellent general-purpose etchant
for steels, but PGBs were not revealed.
When this wetting agent was added, general-structure etching was suppressed and
PGBs were revealed. None of the other
wetting agents tried were as effective. A
number of studies on the use of wetting
agents in etchants have been reviewed.[10]
The original tridecyl version of this wetting agent has branched molecular chains,
which are difcult to manufacture and
have poor biodegradability. More recent
versions have linear chains and are biodegradable. Kilpatrick[14] evaluated the dodecyl version of this wetting agent, which
is more easily made, readily biodegradable
and works as well. Consequently, this wetting agent is the most commonly used today for revealing PGBs.
FEATURE | Materials
Characterization & Testing
a)
b)
Fig. 6. Prior-austenite grain boundaries are not revealed in martensitic A-350 (LF3) alloy
steel (Fe - 0.07%C - 0.74%Mn - 3.66%Ni - 0.2%Cr - 0.07%Mo (1350F temper) using nital (a)
but are revealed using aqueous saturated picric acid plus HCl and a wetting agent at 90C 2 minutes (b, as etched).
or the beaker will ip over). This was followed by light repolishing to remove some
of the etch detail within the grains. Other
etchants for revealing PGBs have been
developed; reference [4] lists 28 reagents
published prior to 1984 for this purpose.
Experimental Procedure
Before specimens can be etched, they must
be properly prepared to a very high quality level. The rst and most critical step is
sectioning, which must be conducted to
induce minimal damage. Use abrasive cutoff machines (avoid torch cutting, shearing, band saws or power hack saws as they
induce far too much damage) with a blade/
wheel designed for metallography and for
steels of the hardness level being prepared.
Generally, mounting is performed but
may not be necessary if the structure at the
edges of the sample is not important (as in
a)
b)
Fig. 8. Prior-austenite grain boundaries revealed in 8620 alloy steel using aqueous saturated picric acid plus HCl and a wetting agent at 80-90C, 60 seconds; specimen as-quenched
(a) and after tempering at 400F (b). Prior-austenite grain boundaries revealed in 8620
alloy steel using aqueous saturated picric acid plus HCl and a wetting agent at 80-90C, 60
seconds; after an 800F (c) and a 1200F (d) temper.
a)
b)
c)
d)
Fig. 9. Prior-austenite grain boundaries revealed in fully martensitic 4140 alloy steel using
aqueous saturated picric acid plus HCl and a wetting agent at 80-90C; specimen in the
as-quenched condition (a) and after a 400F (b) temper. Prior-austenite grain boundaries
revealed in fully martensitic 4140 alloy steel using aqueous saturated picric acid plus HCl
and a wetting agent at 80-90C; after an 800F (c) and a 1200F (d) temper.
FEATURE | Materials
Characterization & Testing
a)
b)
Figure 10: Prior-austenite grain boundaries in 4340 alloy steel isothermally transformed to
lower bainite using aqueous saturated picric acid plus HCl and a wetting agent after tempering at 300F (a) and 500F (b). These specimens were back polished after etching.