Using Metallography to Understand Heat

Treatment Results
George F. Vander Voort
Consultant – Struers Inc.
www.georgevandervoort.com
 As-Hot Rolled Microstructures

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.
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 As-Hot Rolled Microstructures

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.
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 Annealing – Continuous Cooling

Schematic examples of full annealing cycles

that use a continuous slow cooling rate.
Through the transformation range.
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 Annealing – Isothermal

Schematic examples of full annealing cycles that use

isothermal holds through the transformation range.

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 Annealing
4140

Effect of
Austenitizing
20 µm Temperature 20 µm

1380 °F, 749 °C 1550 °F, 843 °C

Ac1 = 1380 °F, 749 °C

Ac3 = 1460 °F, 793 °C
20 µm

1450 °F, 788 °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.

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 Annealing S5 Tool Steel

20 µm 20 µm

Starting Structure 1300 °F, 704 °C – 16 h, AC

Ferrite plus Coarse Sub-Critical Anneal
Pearlite

20 µm
Full Anneal
Influence of starting microstructure on the spheroidize annealed
microstructure of S5 tool steel (4% picral).
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 Annealing S5 Tool Steel

20 µm
20 µm

Starting Structure 1300 °F, 704 °C – 16 h, AC

Ferrite and Fine Sub-Critical Anneal
Pearlite

20 µm
Full Anneal
Influence of starting microstructure on the spheroidize annealed
microstructure of S5 tool steel (4% picral).
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 Annealing S5 Tool Steel

20 µm 20 µm

Starting Structure 1300 °F, 704 °C – 16 h, AC,

Lower Bainite Sub-Critical Anneal

20 µm
Full Anneal
Influence of starting microstructure on the spheroidize annealed
microstructure of S5 tool steel (4% picral).
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 Annealing S5 Tool Steel

20 µm 20 µm

Starting Structure 1300 °F, 704 °C – 16 h, AC

Tempered Martensite Sub-Critical Anneal

20 µm
Full Anneal
Influence of starting microstructure on the spheroidize annealed
microstructure of S5 tool steel (4% picral).
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 Grain Boundary Carbides

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). Left: Vilella’s reagent; Right:
Beraha’s Sulfamic Acid etch number 4.
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 Avoiding Grain Boundary Carbides

10 m 10 m

Electrolytic Alkaline Sodium Picrate 1000X 4% Picral

Microstructure of 52100 bearing steel. Left: Coils were opened up and air
was blown over the bars after hot rolling, then mill annealed. Right: Coils
were austenitized, polymer quenched and tempered, then mill annealed.
Note the absence of any cementite in the ferrite grain boundaries.
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 Grain Size Control

Al “killing”
before
solidification
controls
austenite grain
size by forming
AlN; but AlN
will go into
solution above
the “grain
coarsening”
temperature.

Grain coarsening behavior of aluminum-killed alloy steels.

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 Grain Growth of 1040 Carbon Steel

100 µm 100 µm

1600 °F, 871 °C, AC 1800 °F, 982 °C, AC

20 µm
2000 °F, 1093 °C, AC
Influence of the normalizing temperature upon the grain size and
microstructure of 1040 carbon steel (2% nital).
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 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)
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 Isothermal Formation of Bainite

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

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 Upper Bainite in 5160
2% Nital 4% Picral

Upper bainite (dark or outlined) and as-quenched martensite (gray or white) 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 forms martensite).
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 Lower Bainite in 5160
2% Nital 4% Picral

Lower bainite (dark) and as-quenched martensite (white/gray) 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 forms
martensite).
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 Isothermal Formation of Bainite

Time-Temperature-Transformation (TTT) diagram for 4140 Alloy Steel.

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 Upper Bainite in 4140
2% Nital 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). 4% picral etch does not reveal
the bainitic ferrite surrounded by martensite as well as nital.
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 Lower Bainite in 4140
2% Nital 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).
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 Continuous Cooling Transformations

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

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 800 °F/min; 654 HV

20 µm 20 µm
20 µm

3000 °F/min; 833 HV 550 °F/min; 551 HV

20 µm 20 µm
250 °F/min; 374 HV 2.5 °F/min; 282 HV
Influence of continuous cooling rate on the microstructure of 9260 alloy
steel (4% picral)
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 Continuous Cooling Transformations

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

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 550 °F/min; 473 HV

1000 °F/min; 605 HV 100 °F/min; 308 HV

25 °F/min; 278 HV 2.5 °F/min; 250 HV

Influence of continuous cooling rate on the microstructure of 8640 alloy
steel (4% picral).
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 Continuous Cooling Transformations

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

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 250 °F/min; 287 HV

20 µm 20 µm
20 µm
550 °F/min; 634 HV 50 °F/min; 316 HV

10 °F/min; 265 HV 20 µm 20 µm 2.5 °F/min; 235 HV

Influence of continuous cooling rate on the microstructure of 3140 alloy

steel (4% picral).
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 5160 Alloy Steel – Q&T
All: 1525 °F, 830 °C, Oil Quench

As Quenched
63 HRC

400 °F, 204 °C

20 µm 20 µm
58 HRC

800 °F, 427 °C

47 HRC

1200 °F, 649 °C

20 µm 20 µm
28 HRC
Martensitic and tempered martensitic microstructures of 5160 alloy steel
(2% nital).
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 4140 Alloy Steel – Q&T
All: 1600 °F, 871 °C, Oil Quench

As Quenched
55 HRC
20 µm 20 µm

400 °F, 204 °C

20 µm
20 µm 53 HRC

800 °F, 427 °C

45 HRC

1200 °F, 649 °C 20 µm

20 µm
26 HRC
Martensitic and tempered martensitic microstructure of 4140 alloy steel (2% nital).
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 8620 Alloy Steel – Q&T
All: 1600 °F, 871 °C, Water Quench

As Quenched
45 HRC

400 °F, 204 °C

20 µm 20 µm
44 HRC

800 °F, 427 °C

38 HRC

1200 °F, 649 °C

20 µm
20 µm 26 HRC

Martensitic and tempered martensitic microstructure of 8620 alloy steel (2% nital).
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 Carburized 8720 – 25.4% Retained Austenite

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 (magnification bar is 10 µm long). Image analysis performed on
the specimen etched with 6% nital plus 1% zephiran chloride (benzalkonium
chloride, a wetting agent) yielded 13.3%.
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 Carburized 8720 – 25.4% Retained Austenite

Meyer-Eichholz No. 2 10% Sodium Metabisulfite

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 (magnification bar is 10 µm long). 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.
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 Carburized 8720 – 19.7% Retained Austenite

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 (magnification bar is 10 µm long). Image analysis performed on
the specimen etched with 6% nital plus 1% zephiran chloride (benzalkonium
chloride, a wetting agent) yielded 8.5%.
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 Carburized 8720 – 19.7% Retained Austenite

Meyer-Eichholz No. 2 10% Sodium Metabisulfite

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 (magnification bar is 10 µm long). 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.
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 Carburized 8720 – 16.2% Retained Austenite

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 (magnification bar is 10 µm long). Image analysis performed on
the specimen etched with 6% nital plus 1% zephiran chloride (benzalkonium
chloride, a wetting agent) yielded 1.2%.
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 Carburized 8720 – 16.2% Retained Austenite

Meyer-Eichholz No. 2 10% Sodium Metabisulfite

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 (magnification bar is 10 µm long). 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.
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 Under-Austenitization

20 µm

4140 alloy steel, 1425 °F, 774 °C, Water Quench

Ferrite-martensite microstructure of 4140 alloy steel

austenitized within the two-phase + field, 2% nital

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 Over-Austenitization

20 µm

A2 Tool Steel, 2000 °F, 1093 °C, Air Quench

Coarse-grained martensitic microstructure of over-austenitized A2
tool steel (2% nital).
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 Induction Hardening

Transition

20 µm 20 µm

Surface Core

20 µm

Microstructure of 1045 carbon steel after induction hardening showing the case,
transition zone and core areas. The surface is fully martensitic with no visible
evidence of retained austenite. The core structure is pearlite with proeutectoid
ferrite in the grain boundaries. The transition zone contains martensite, bainite
and pearlite. The specimen was etched with 2% nital.
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 Properly Carburized 8620
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.
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 Properly Carburized 8620
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.
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 Poorly Carburized 8620 Steel

10 µm

Surface of an improperly carburized and hardened 8620 mold, note the

shrinkage gap (top arrows). Just below the surface, there are massive carbides
in the grain boundaries (see next slide). Decarburization during hardening has
caused ferrite (large up arrow) and pearlite (smaller up arrow) to form.
Specimen etched with 2% nital.

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 Poorly Carburized 8620 Steel

Improperly carburized surface of 8620 alloy steel (Fe – 0.2% C – 0.8% Mn – 0.55%
Ni – 0.5% Cr – 0.2% Mo) etched with aqueous 10% sodium metabisulfite. Note the
very coarse plate martensite (blue and brown “needles”). The white regions are
retained austenite but there are also white, massive cementite particles present,
as indicated by the arrows. Original at 1000X.
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 Heavy Grain Boundary Carbide
Networks in Failed 8620 Gear

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

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 Poorly Carburized 8620 Steel

Near-surface region of the improperly carburized 8620 specimen previously

illustrated. The specimen was re-polished and etched with 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.
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 Poorly Carburized P5 Plastic Mold Steel
Grain Boundary Carbide Films

100 µm

25 µm

Core – 22 HRC (Nomarski DIC)

Note: Old and New Ferrite (arrows)
10 µm
Case – 59.5 HRC 2% Nital
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Excessive grain boundary carbide networks in the failed P5 tool steel die (10%
sodium metabisulfite, polarized light plus sensitive tint).
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 Etchant: 10%
Na2O2O5

Etchant:
Klemm’s I

Klemm’s I vividly reveals the ferrite in the P5 core present during austenitizing
versus ferrite that precipitated onto the pre-existing ferrite during quenching
(due to inadequate hardenability).
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 Carburized 8620 – Lower Bainite
Case/Lath Martensite Core
Case – to – Core Transition
Bright Field Polarized Light + Sensitive Tint

Case Core Case Core

10% sodium metabisulfite used to reveal the microstructural
change from the lower bainitic case to the lath martensitic core.
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 Carburized 8620 – Lower Bainite
Case/Lath Martensite Core
Bainitic Case

Bright Field Polarized Light + Sensitive Tint

Microstructure of the case of carburized (0.95% C potential) 8620 alloy steel. 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.
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 Carburized 8620 – Lower Bainite
Case/Lath Martensite Core
Lath Martensite Core

Bright Field Polarized Light + Sensitive Tint

Lath martensitic core structure, with some ferritic areas,

revealed using 10% sodium metabisulfite.

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 Carburized 8620 – Lower Bainite
Case/Lath Martensite Core

Case – Lower Bainite Core – Lath Martensite

Case and core structure revealed using 2% nital.

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 Microstructure of salt-bath nitrided resulfurized 1214 carbon steel. The black
arrows point to the “compound layer” while the red arrows point to iron nitrides,
probably gamma prime, Fe4N. The specimen was etched with 2% nital.
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 Microstructure of salt bath nitrided 1214 resulfurized carbon steel (transverse
plane) exhibiting a compound layer (yellow arrows) and iron nitrides in the ferrite
matrix (red arrows). Left: 500X, right: 1250 X (oil immersion objective); etched with
10:1 solution of 4% picral and 2% nital. The small particles are MnS in a matrix of
ferrite and pearlite.
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 Gas Nitriding
Ni Plating
Ni
Compound
layer

Maximum
Affected
Depth

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). Tint etched with Beraha’s CdS reagent.
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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).
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 Failed Nitrided 41B50 Chuck Jaw

Ni
Electroless Ni Plating

MnS

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  and ’ phases). The yellow arrows point to the three zones
in the compound layer. The green arrows point to sulfide inclusions.
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 Failed Nitrided 41B50 Chuck Jaw

Electroless Ni Plating

Failed Lustre Die nitrided specimen etched with a 10:1 solution of 4% picral to 2%
nital: left: 100X; right: 500X.
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 Failed Nitrided H13 Mold

AISI H13 mold that broke 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.
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 Good Nitrided H13 Mold

AISI H13 mold that performed well in service in the same application.
Note the absence of a brittle compound layer as in the previous 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.

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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).
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 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.

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 Ion Nitrided H13 Tool Steel
Mount

Affected
Depth

10 µm

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 arrow points to a
white, iron nitride layer at the surface (tempered martensite; Vilella’s reagent).
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 Carbonitrided 8720

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.
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 Borided 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.

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 Decarburized 1080 Bar

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).
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 Decarburized 52100 Steel

Both at 100X
Magnification
bars are 100
m

Etched with 4%
Picral and 2%
Nital

Decarburized surfaces of 52100 bearing steel that was austenitized at 1650 F

(899 C), oil quenched, tempered at 930 F (499 C), and then annealed at
1435 F (780 C), transverse orientation for the plane-of-polish.

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 Decarburized 420 Stainless

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.
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 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!

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