Using Metallography to

Understand Heat
Treatment Results
George F. Vander Voort
Consultant – Struers Inc.
Vander Voort Consulting L.L.C.
As-Rolled Microstructures
 As-Rolled W1 Tool Steel (1.31% Carbon)

4% Picral 2% Nital

Microstructure of as-rolled Fe – 1.31% C – 0.35% Mn – 0.25% Si high-carbon water

hardenable tool steel. Note the Widmanstätten intragranular cementite that precipitated
as pro-eutectoid cementite before the eutectoid reaction. Originals at 1000X.
 As-Rolled W1 Tool Steel (1.31% Carbon)

Alkaline sodium picrate, 90 °C (194 °F) – 60 s Beraha’s sulfamic acid etch

Microstructure of the as-rolled Fe – 1.31% C – 0.35% Mn – 0.25% Si specimen with the
intergranular carbide network clearly visible after etching with alkaline sodium picrate, 90
°C – 60 s (left) and with Beraha’s sulfamic acid etch (100 mL water, 3 g K2S2O5 and 2 g
NH2SO3H), (right). Both at 500X.
Annealed Microstructures
 Annealing – Continuous Cooling Transformations

Schematic examples of full annealing cycles that use a continuous slow cooling
rate. Through the transformation range.
 Annealing – Isothermal Transformations

Schematic examples of full annealing cycles that use isothermal holds through
the transformation range.
 Annealing 4140 Effect of Austenitizing Temperature

1380 °F, 749 °C 1450 °F, 788 °C 1550 °F, 843 °C

Ac1 = 1380 °F, 749 °C

Ac3 = 1460 °F, 793 °C

Illustration of the influence of the austenitizing temperature on the annealed

microstructure of 4140 alloy steel (slow cooled 20 °F/h to 1100 °F/593 °C), 4% picral.
 Annealing S5 Tool Steel – Effect of Starting Microstructure

20 µm 20 µm 20 µm

Starting Structure - Ferrite and 1300 °F, 704 °C – 16 h, AC Full Anneal

Coarse Pearlite Sub-Critical Anneal

Influence of starting microstructure on the spheroidize annealed microstructure of S5 tool

steel (4% picral). Note that both annealed structures exhibit carbide films around the free
ferrite grains in the starting structure. They will persist through hardening.
 Annealing S5 Tool Steel – Effect of Starting Microstructure

20 µm 20 µm 20 µm

Starting Structure - Ferrite and 1300 °F, 704 °C – 16 h, AC Full Anneal

Fine Pearlite Sub-Critical Anneal

Influence of starting microstructure on the spheroidize annealed microstructure of S5

tool steel (4% picral). The lower ferrite content and finer interlamellar spacing of the
pearlite yielded better carbide distributions with less carbide grain boundary films.
 Annealing S5 Tool Steel – Effect of Starting Microstructure

20 µm 20 µm 20 µm

Starting Structure - Lower Bainite 1300 °F, 704 °C – 16 h, AC Full Anneal

Sub-Critical Anneal

Influence of starting microstructure on the spheroidize annealed microstructure of S5

tool steel (4% picral). Note the improved carbide distribution with the lower bainite
starting microstructure. There is some linearity to the carbide distribution, but there are
no continuous films. The sub-critical anneal gave a coarser carbide distribution.
Annealing S5 Tool Steel – Effect of Starting Microstructure

20 µm 20 µm
20 µm

Starting Structure - Tempered 1300 °F, 704 °C – 16 h, AC Full Anneal

Martensite Sub-Critical Anneal

Influence of starting microstructure on the spheroidize annealed microstructure of S5

tool steel (4% picral). The tempered martensite starting structure yielded the best
carbide distribution using both annealing methods. Again, the sub-critical anneal gave
the coarsest carbide distribution and lowest annealed hardness.
Grain Boundary Carbides in Wrought, Annealed or
Quenched and Tempered Microstructures
Avoiding Grain Boundary Carbides in 52100 Bearing Steel

Electrolytic Alkaline Sodium Picrate 1000X 4% Picral

Left: 52100 coils were opened up and air was blown over the bars after hot
rolling, then mill annealed.
Right: 52100 coils were austenitized, polymer quenched and tempered, then mill
annealed. Note the absence of any cementite in the ferrite grain boundaries.
Grain Boundary Carbides in Q&T 420 MSS

Vilella’s Reagent Beraha’s Sulfamic Acid Etchant #4

Grain boundary carbide networks in quenched and tempered 420 martensitic

stainless steel. It was austenitized at 1900 °F (1038 °C), air quenched and
tempered at 350 °F (177 °C). These networks were present after hot working
and persisted through spheroidization annealing and hardening.
Grain Size Control in Wrought Microstructures
 Al “killing” before
solidification controls
austenite grain size by
forming AlN; but AlN will
go into solution above
the “grain coarsening”
temperature, followed by
rapid grain growth.

Steels that are not given

Al additions will
experience grain growth
over a range of
temperatures unless
residual carbides are
present to inhibit grain
growth.

Grain coarsening behavior of aluminum-killed alloy steels and non-Al-killed steels.

 Grain Growth of 1040 Carbon Steel During Normalizing

1600 °F (871 °C), AC 1800 °F (982 °C), AC 2000 °F (1093 °C), AC

Influence of the normalizing temperature upon the grain size and microstructure of 1040
carbon steel (2% nital), all at 100X magnification.
 Prior-Austenite Grain Size Control

50 µm 50 µm

Prior-austenite grain boundaries in 43B17 alloy steel (Fe – 0.17% C – 1.85% Ni – 0.75% Cr – 0.25% Mo –
0.003% B) revealed by etching with aqueous saturated picric acid plus 1% HCl and a wetting agent. The
specimen at the left was given a normal heat treatment (1550 °F or 843 °C – 30 min, oil quench, 446 °F or 230
°C temper) and has a fine grain size. The specimen on the right was “mock carburized” (1700 °F or 925 °C for
8 h, oil quench and tempered at 230 °C) and rapid grain growth has begun.
(B-treated steels are not suitable for carburizing; the nitrogen must be tied up permanently with Ti or Zr)
Isothermal vs Continuous Cooling Microstructures
Isothermal Formation of Bainite in 5160 Alloy Steel

Thin specimens were

austenitized at 1525 ºF
(830 ºC) and quenched
into a bath at 1000 ºF (538
ºC) and held for 30
seconds before being
quenched into water to
form upper bainite; and, a
second specimen was
quenched into a bath at
650 ºF (353 ºC) and held
for 5 minutes to form
lower bainite.

Time-Temperature-Transformation (TTT) diagram for 5160 alloy steel.

 Isothermally Formed Upper Bainite in 5160

2% Nital 1000X 4% Picral

Upper bainite (dark or outlined) and as-quenched martensite (gray or white – “M”) in 5160
alloy steel (Fe – 0.6% C - 0.85% Mn – 0.25% Si – 0.8% Cr) that was austenitized at 830 °C (1525
°F) for 30 min., isothermally held at 538 °C (1000 °F) for 30 sec to partially transform the
austenite, and then water quenched (untransformed austenite formed martensite).
 Isothermally Formed Lower Bainite in 5160

2% Nital 1000X 4% Picral

Lower bainite (dark) and as-quenched martensite (white/gray – “m”) in 5160 alloy steel (Fe –
0.6% C - 0.85% Mn – 0.25% Si – 0.8% Cr) that was austenitized at 830 °C (1525 °F) for 30 min.,
isothermally held at 343 °C (650 °F) for 5 minutes to partially transform the austenite, and
then water quenched (untransformed austenite formed martensite).
Isothermal Formation of Bainite in 4140 Alloy Steel

Thin specimens were

austenitized at 1550 ºF (843
ºC) and quenched into a bath
at 1050 ºF (566 ºC) and held
for 15 minutes before being
quenched into water to form
upper bainite; and, a second
specimen was quenched into
a bath at 775 ºF (413 ºC) and
held for 30 seconds to form
lower bainite.

Time-Temperature-Transformation (TTT) diagram for 4140 alloy steel.

 Isothermally Formed Upper Bainite in 4140

2% Nital 1000X 4% Picral

Microstructure of 4140 alloy steel (Fe – 0.4% C – 0.9% Mn – 0.2% Si – 1% Cr – 0.2% Mo)
austenitized at 843 °C (1550 °F), isothermally transformed at 566 °C (1050 °F) for 15 min., and
water quenched, to partially transform austenite to upper bainite (arrow in segregation streak
shows the initiation of bainitic ferrite surrounded by martensite; the untransformed austenite
was converted to martensite).
 Isothermally Formed Lower Bainite in 4140

2% Nital 1000X 4% Picral

4140 alloy steel (Fe – 0.4% C – 0.9% Mn – 0.2% Si – 1% Cr – 0.2% Mo) austenitized at 843 °C
(1550 °F), isothermally transformed at 413 °C (775 °F) for 30 sec., and water quenched, to
partially transform austenite to lower bainite (surrounded by martensite; the untransformed
austenite was converted to martensite).
Continuous Cooling Transformations of 9260 Alloy Steel

Microstructures will be
shown using cooling rates
from the austenitizing
temperature to below the
Ms temperature at rates
from 3000 ºF/minute to
2.5 ºF/minute.

Continuous Cooling Transformation (CCT) diagram for 9260 alloy steel.

 Continuously Transformed Microstructures of 9260 Alloy Steel

20 µm 20 µm 20 µm 20 µm
20 µm

3000 °F/min 800 °F/min 550 °F/min 250 °F/min 2.5 °F/min
833 HV 654 HV 551 HV 374 HV 282 HV

Influence of continuous cooling rate on the microstructure of 9260 alloy steel (4% picral). The
structures range from a very high amount of martensite and some bainite at the grain
boundaries to a structure of mostly pearlite with some ferrite in grain boundaries. All images at
500X.
Continuous Cooling Transformations of 8640 Alloy Steel

Microstructures will be
shown using cooling
rates from the
austenitizing temperature
to below the Ms
temperature at rates from
1000 ºF/minute to
2.5 ºF/minute.

Continuous Cooling Transformation (CCT) diagram for 8640 alloy steel.

 Continuously Transformed Microstructures of 8640 Alloy Steel

1000 °F/min 550 °F/min 100 °F/min 25 °F/min 2.5 °F/min

605 HV 473 HV 308 HV 278 HV 250 HV

Influence of continuous cooling rate on the microstructure of 8640 alloy steel (4% picral).
The structures range from a very high amount of martensite and some bainite at the grain
boundaries to a structure of mostly pearlite with some ferrite in grain boundaries. All
images at 500X.
Continuous Cooling Transformations of 3140 Alloy Steel

Microstructures will be
shown using cooling rates
from the austenitizing
temperature to below the
Ms temperature at rates
from 550 ºF/minute to
2.5 ºF/minute.

Continuous Cooling Transformation (CCT) diagram for 3140 alloy steel.

 Continuously Transformed Microstructures of 3140 Alloy Steel

20 µm 20 µm 20 µm 20 µm 20 µm

550 °F/min 250 °F/min 50 °F/min 10 °F/min 2.5 °F/min

634 HV 287 HV 316 HV 265 HV 235 HV

Influence of continuous cooling rate on the microstructure of 3140 alloy steel (4% picral).
The structures range from a very high amount of martensite and some bainite at the grain
boundaries to a structure of mostly bainite and then to pearlite with grain-boundary ferrite to
ferrite grains and pearlite colonies. All images at 500X.
Quenched and Tempered Martensitic Microstructures
 5160 Alloy Steel – Q&T
All Specimens: 1525 °F, 830 °C, Oil Quench
As-Quenched
Quenched & Tempered
Martensite
at 400 °F, 204 °C
63 HRC
Tempered Martensite
58 HRC

20 µm 20 µm

Quenched & Tempered

Quenched & Tempered
at 800 °F, 427 °C
at 1200 °F, 649 °C
Tempered Martensite
Tempered Martensite
47 HRC
28 HRC

2% Nital Etch 20 µm 20 µm
All at 500X
 4140 Alloy Steel – Q&T
All Specimens: 1600 °F, 871 °C, Oil Quench

As Quenched Quenched & Tempered

Martensite at 400 °F, 204 °C
55 HRC Tempered Martensite
53 HRC

20 µm 20 µm

Quenched & Tempered Quenched & Tempered

at 800 °F, 427 °C at 1200 °F, 649 °C
Tempered Martensite Tempered Martensite
45 HRC 26 HRC

2% Nital Etch
20 µm 20 µm
All at 500X
 8620 Alloy Steel – Q&T
All Specimens: 1600 °F, 871 °C, Oil Quench

As Quenched Quenched & Tempered

Martensite at 400 °F, 204 °C
45 HRC Tempered Martensite
44 HRC

20 µm 20 µm

Quenched & Tempered Quenched & Tempered

at 800 °F, 427 °C at 1200 °F, 649 °C
Tempered Martensite Tempered Martensite
38 HRC 26 HRC

2% Nital Etch 20 µm 20 µm
All at 500X
 Under-Austenitization vs Over-Austenitization

20 µm
20 µm

4140 alloy steel, 1425 °F, 774 °C, Water Quench A2 Tool Steel, 2000 °F, 1093 °C, Air Quench
Left: Ferrite-martensite microstructure of 4140 alloy steel austenitized within the two-phase α+γ
field, 2% nital.
Right: Coarse-grained martensitic microstructure of over-austenitized A2 tool steel (2% nital).
Both at 500X Magnification.
Carburized and Q&T Microstructures
 Carburized 8720 – 25.4% Retained Austenite

10 µm 10 µm

2% Nital 6% Nital + 1% Zephiran Chloride

X-ray diffraction revealed 25.4% retained austenite in this specimen. The x-ray beam senses
the surface to a depth of at least half a mm. The above images were taken at 1000X. Image
analysis performed on the specimen etched with 6% nital plus 1% zephiran chloride
(benzalkonium chloride, a wetting agent) yielded 13.3%.
 Carburized 8720 – 25.4% Retained Austenite

10 µm 10 µm

Meyer-Eichholz No. 2 Etch 10% Sodium Metabisulfite Tint Etch

X-ray diffraction revealed 25.4% retained austenite in this specimen. The x-ray beam senses
the surface to a depth of at least half a mm. The above images were taken at 1000X. Image
analysis performed on the specimen etched with the Meyer-Eichholz No. 2 reagent gave
6.2% retained austenite while etching with 10% Na2S2O5 gave 7.1% retained austenite.
 Carburized 8720 – 19.7% Retained Austenite

10 µm 10 µm

2% Nital 6% Nital + 1% Zephiran Chloride

X-ray diffraction revealed 19.7% retained austenite in this specimen. The x-ray beam
senses the surface to a depth of at least half a mm. The above images were taken at 1000X.
Image analysis performed on the specimen etched with 6% nital plus 1% zephiran chloride
(benzalkonium chloride, a wetting agent) yielded 8.5%.
 Carburized 8720 – 19.7% Retained Austenite

10 µm 10 µm

Meyer-Eichholz No. 2 Etch 10% Sodium Metabisulfite Tint Etch

X-ray diffraction revealed 19.7% retained austenite in this specimen. The x-ray beam
senses the surface to a depth of at least half a mm. The above images were taken at
1000X. Image analysis performed on the specimen etched with the Meyer-Eichholz No. 2
reagent gave 6.0% retained austenite while etching with 10% Na2S2O5 gave 5.7% retained
austenite.
 Carburized 8720 – 16.2% Retained Austenite

10 µm 10 µm

2% Nital 6% Nital + 1% Zephiran Chloride

X-ray diffraction revealed 16.2% retained austenite in this specimen. The x-ray beam
senses the surface to a depth of at least half a mm. The above images were taken at 1000X.
Image analysis performed on the specimen etched with 6% nital plus 1% zephiran chloride
(benzalkonium chloride, a wetting agent) yielded 1.2%.
 Carburized 8720 – 16.2% Retained Austenite

10 µm 10 µm

Meyer-Eichholz No. 2 Etch 10% Sodium Metabisulfite Tint Etch

X-ray diffraction revealed 16.2% retained austenite in this specimen. The x-ray beam
senses the surface to a depth of at least half a mm. The above images were taken at 1000X.
Image analysis performed on the specimen etched with the Meyer-Eichholz No. 2 reagent
gave 0.8% retained austenite while etching with 10% Na2S2O5 gave 1.1% retained austenite.
 Properly Carburized 8620 Alloy Steel

Mounting
Compound

Unaffected Core

Carburized gear teeth made with 8620 alloy steel (Fe – 0.2% C – 0.8% Mn – 0.25% Si – 0.55%
Ni – 0.5% Cr – 0.2% Mo) with a gradation of carbon and microstructure revealed by tint
etching with Beraha’s sulfamic acid reagent (100 mL water, 3 g potassium metabisulfite, 2 g
sulfamic acid and 0.7 g ammonium bifluoride) and viewed with polarized light plus sensitive
tint. Original at 50X.
 Properly Carburized 8620 Alloy Steel

Case Core

Case and core microstructures of the carburized 8620 alloy steel specimen in the previous slide
revealing high-carbon plate martensite and low-carbon lath martensite, respectively, after tint
etching and viewing with polarized light and sensitive tint. Originals at 500X.
Carburized 8620 – Lower Bainite Case/Lath Martensite Core
Case – to – Core Transition
Bright Field Illumination Polarized Light + Sensitive Tint Filter

Case Core Case Core

10% sodium metabisulfite was used to reveal the microstructural change from the
lower bainite case to the lath martensite core (100X). Lower bainite was desired in the
case for better resistance to low-cycle fatigue stresses.
Carburized 8620 – Lower Bainite Case/Lath Martensite Core
Lower Bainite Case

Bright Field Illumination Polarized Light + Sensitive Tint Filter

Microstructure of the case of carburized (0.95% C potential) 8620 alloy steel (500X). It was
carburized at 1750 °F (954 °C), then quenched into a 50/50 mix of sodium nitrite and
potassium nitrate at 480 °F (249 °C) and held 120 minutes. It was air cooled and tempered at
480 °F for 240 minutes to an aim case hardness of 52-60 HRC (etched with 10% sodium
metabisulfite). The lower bainite case performs better under low-cycle fatigue conditions.
Carburized 8620 – Lower Bainite Case/Lath Martensite Core
Lath Martensite Core

Bright Field Illumination Polarized Light + Sensitive Tint Filter

Lath martensitic core structure revealed using 10% sodium metabisulfite (500X).
Carburized 8620 – Lower Bainite Case/Lath Martensite Core
Lower Bainite Case Lath Martensite Core

2% nital used to reveal the lower bainite case and the lath martensite core (500X).
Heavy Grain Boundary Carbide Networks in Failed 8620 Gear

Alkaline sodium picrate (90 °C – 60s) reveals cementite networks.

Heavy Grain Boundary Carbide Networks in Failed 8620 Gear

Near-surface region of the improperly carburized 8620 specimen previously illustrated. The
specimen was etched with near-boiling alkaline sodium picrate to color the massive cementite
particles. Note that they form almost continuous networks around the prior-austenite grain
boundaries (present during carburizing), which is very bad for toughness. Original at 500X.
Heavy Grain Boundary Carbide Networks in Failed 8620 Gear

10 µm

Surface of an improperly carburized and Very coarse plate martensite; white regions
hardened 8620 mold, note the shrinkage gap (top are retained austenite and massive cementite
arrows). Decarburization during hardening has particles present, as indicated by the arrows.
caused ferrite (large up arrow) and pearlite 10% sodium metabisulfite, 1000X
(smaller up arrow) to form. 2% Nital.
 Poorly Carburized P5 Plastic Mold Steel – Service Failure
Case 100X (59.5 HRC) Case 1000X Core 400X (22 HRC)

This carburized P5 plastic mold die failed early in service due to the massive grain boundary
carbide films in the hardened case which drastically degraded the toughness. In the core, the
structure consisted of ferrite grains (yellow arrows) and lath martensite. Note that additional ferrite
precipitated on the ferrite grains in the core during quenching after carburizing. 2% Nital etch.
 Extensive Grain-
Boundary
Carbide Films in
the Carburized
50X 100X
Case of the
Failed P5 Plastic
Mold Steel Die

200X 500X

Color tint etched with 10% sodium metabisulfite, polarized light plus a sensitive tint filter.
 Etchant: 10%
Na2O2O5
500X

Etchant:
Klemm’s I
500X

Klemm’s I vividly revealed the ferrite in the P5 core present during austenitizing versus ferrite
that precipitated onto the pre-existing ferrite during quenching (due to inadequate
hardenability). Note the crystallographic orientation effect in the primary ferrite.
Nitrided, Carbonitrided and Borided Q&T
Microstructures
Nitrided H13 Mold With an Excellent Service Life

AISI H13 mold that performed well in service. Note the absence of a brittle compound
layer as in the next slide. Etched with 2% nital followed by 10% Na2S2O5, 100X (left) and
500X (right). Note the white grain boundary carbide films in the 500X view.
 Nitrided H13 Mold With a Very Short Service Life

AISI H13 mold that broke in early in service due to the presence of this brittle compound
layer (white arrows). Etched with 2% nital followed by 10% Na2S2O5, 100X (left) and 500X
(right). Note the white grain boundary carbide films in the 500X view. Compare these
images to the previous slide with a similar mold with excellent service life.
 Microstructure of Nitralloy 135 extrusion barrel etched with 2% nital followed by 10%
Na2S2O5 (left two at 200 and 500X) and with a 10:1 mix of 4% picral and 2% nital (right two
at 200 and 500X).
 Good Nitrided Nitralloy 135 Extrusion Barrel

Microstructure of Nitralloy 135 extrusion barrel etched with alkaline sodium picrate at 90 °C
for 60 seconds to color the grain boundary films (yellow arrows) brown proving that they
are cementite; both images at 500X.
 Failed Nitrided 41B50 Chuck Jaw for a Lathe
Microstructure of gas nitrided
41B50 alloy steel previously
quench and tempered to 325
HV (tempered martensite).
The surface was electroless
Ni plated before mounting as
the outer edge of the iron
nitride “white layer” is
considerably softer than the
inner layer (very hard and
brittle). The left view (original
at 50X) reveals the depth of
the nitrided case. The right
view (original at 200X) reveals
some intergranular cementite
films (yellow arrows). The red
arrows point to MnS colored
white by the tint etch (Tint
etched with Beraha’s CdS
Arrow at right – Maximum Affect reagent).
Depth of Nitrided Surface.
 Failed Nitrided 41B50
Chuck Jaw for a Lathe

Microstructure of the broken nitrided Lustre Die (41B50+S) chuck jaw with a brittle compound
layer (note crack in layer, black arrows). The grain boundary films (red arrows) are Fe3C due to
the inward diffusion of carbon during nitriding (10% Na2S2O5).
 Failed Nitrided 41B50 Chuck Jaw for a Lathe
Ni
Electroless Ni Plating

MnS

Etching the failed Lustre Die chuck jaw with alkaline sodium picrate at 90 °C for 90
seconds colored the cementite (violet arrows) in the third zone of the compound layer
(cementite has been reported to be found in the compound layer along with ε and γ’
phases). The yellow arrows point to the three zones in the compound layer. The green
arrows point to sulfide inclusions.
 Failed Nitrided 41B50 Chuck Jaw for a Lathe

Electroless Ni Plating

Failed Lustre Die nitrided specimen etched with a 10:1 solution of 4% picral to 2%
nital: left: 100X; right: 500X. Yellow arrows point to the three zones in the compound
layer as shown in the previous slide.
 Ion Nitrided H13 Tool Steel
Mounting Compound

Affected
Depth

Ion nitrided surface of type H13 tool steel (Fe – 0.4% C – 0.35% Mn – 1% Si – 5% Cr – 0.9% V
– 1.35% Mo) previously quenched and tempered. The black arrow points to a white, iron
nitride layer at the surface (tempered martensite; Vilella’s reagent). The yellow arrow points
to an embedded abrasive particle from shot blasting the surface before nitriding.
Carbonitrided 8720 Part with a Good Service Life

50 µm 20 µm

Microstructure of carbonitrided type 8720 alloy steel (Fe – 0.2% C – 0.8% Mn – 0.25%
Si – 0.55% Ni – 0.5% Cr – 0.25% Mo) after quenching and tempering. The surface was
plated with Cr for edge protection. There is considerable retained austenite (white
patches) between martensite plates (black) in the carbonitrided surface. Specimen
was etched with 2% nital.
 Borided As-Rolled 42CrMo4 Alloy Steel
Mount

P P B

50 µm 10 µm

Microstructure of a borided 42CrMo4 as-rolled alloy steel (Fe – 0.42% C – 0.75% Mn –

0.4% Si - 1.1% Cr – 0.2% Mo). Note the acicular nature of the iron-boride layer. The matrix
contains pearlite (P) and bainite (B). Etched with 2% nital.
Decarburized Surfaces of Steels
 Decarburized 1080 Bar Surface

Decarburized surface of an as-rolled, eutectoid carbon steel (Fe – 0.8% C – 0.21% Mn –

0.22% Si). The matrix should be nearly all pearlite, but there is ferrite at the surface to a
considerable depth (arrows). The specimen was etched with 4% picral. The original
magnifications were 200X (left) and 500X (right).
 Decarburized Q&T 52100 Steel Bearing Steel

Both at 100X
Magnification
bars are 100
µm

Etched with
4% Picral and
2% Nital

Decarburized surfaces of a failed 52100 bearing steel component that was austenitized at 1650
°F (899 °C), oil quenched, tempered at 930 °F (499 °C), and then, because of a low surface
hardness, was annealed at 1435 °F (780 °C), transverse orientation for the plane-of-polish.
 Decarburized 420 Stainless Steel Mold

Maximum
Affected
Depth

100 µm

Microstructure at the surface of a decarburized, hardened specimen of type 420

martensitic stainless steel (Fe – 0.35% C – 13% Cr) tint etched with Beraha’s sulfamic acid
reagent (No. 4) and viewed with polarized light plus sensitive tint. Note the “free ferrite”
(arrows) at the surface (complete loss of carbon) and the change in the appearance of the
martensite in the partially decarburized zone.
 Conclusions
• Metallography is a necessary tool to determine the quality of heat treatments or to
diagnose failures due to improper heat treatment.

• Proper specimen preparation is an absolute necessity.

• To examine surfaces and measure depths of affected layers or cracks, edge retention
must be good. This requires use of the best hot-mounting resins, such as DuroFast epoxy
hot-mounting resin.

• Nital is not the only etchant for steels and it is often not the best to use for a specific
steel grade and microstructure.

• Microindentation hardness testing is an important aid in understand heat treatment

results, particularly for surface hardened applications.

• Diagnosing failures due to improper heat treatment is aided by prior documented studies
of properly and improperly treated similar grades of steel – never stop experimenting and
learning!