Understanding Heat Treatment

Results Using Metallography

As-Hot Rolled Microstructures
 4% Picral 2% Nital

Microstructure of hot-rolled Fe – 0.94% C – 0.51% Mn – 0.32% Si – 1.34% Cr alloy

steel revealing a fully pearlitic matrix. Picral revealed a network of cementite in the
prior-austenite grain boundaries (arrows). This is not visible using nital. Originals at
1000X.
 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.
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. Original at 500X magnification. Note also some intragranular
Widmanstätten cementite.
 Beraha’s Sulfamic Acid Reagent Klemm’s I Reagent

Color etching of the as-rolled hypereutectoid Fe-1.31% C – 0.35% Mn – 0.25% Si

specimen clearly revealed the intergranular cementite films. Beraha’s sulfamic acid
etch (100 mL water, 3 g K2S2O5 and 2 g NH2SO3H) (left) and Klemm’s I reagent
(right) were used. Original magnifications were 500X. Taken with polarized light
and sensitive tint.
 20 µm
20 µm

O1 A2

20 µm

S4

Examples of the variation in microstructure possible in as-hot rolled tool steels (2% nital).
Annealing
Schematic examples of full annealing cycles that use a continuous
slow cooling rate. Through the transformation range.
Schematic examples of full annealing cycles that use isothermal holds through
the transformation range.
 4% Picral 2% Nital

Microstructure of annealed (871 °C, 1600 °F – 1 hour, slow cool) SAE 4140 alloy steel
(Fe – 0.4% C – 0.85% Mn – 0.95% Cr – 0.2% Mo) revealing proeutectoid ferrite and
coarse lamellar pearlite. Note that nital, because it is sensitive to crystal orientation,
does not reveal the cementite lamellae well in all packets (arrows point to examples).
Originals at 1000X.
 Annealing
4140

20 µm 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), 4% picral.
 Annealing
W1 Tool
Steel

20 µm
20 µm

Hot Rolled and Slow Cooled 1600 °F, 871 °C, Oil Quench

20 µm
20 µm

As Above + Spheroidize Anneal As Above + Spheroidize Anneal

Influence of starting microstructure on spheroidize annealed

microstructure of W1 (1.05% C) tool steel (4% picral).
 S5 Tool
Steel

20 µm 20 µm

Ferrite plus Coarse Pearlite 1300 °F, 704 °C – 16 h, AC

20 µm

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

20 µm
20 µm

Ferrite and Fine Pearlite 1300 °F, 704 °C – 16 h, AC

20 µm

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

20 µm 20 µm

Lower Bainite 1300 °F, 704 °C – 16 h, AC

20 µm

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

20 µm 20 µm

Tempered Martensite 1300 °F, 704 °C – 16 h, AC

20 µm

Full Anneal
Influence of starting microstructure on the spheroidize annealed microstructure
of S5 tool steel (4% picral).
Normalizing
 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).
Grain coarsening behavior of alloy steels.
Isothermal Transformations
Time-Temperature-Transformation (TTT) diagram for 5160 alloy steel.
 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).
 2% Nital 10% Sodium Metabisulfite

Upper bainite and as-quenched martensite 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). Etched with 2% nital (left) and
aqueous 10% Na2S2O5 (right) which colored the martensite light brown and the upper
bainite blue.
 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).
Time-Temperature-Transformation (TTT) diagram for 4140 Alloy Steel.
 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.
 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).
 20 µm

Microstructure of austempered ductile iron tint etched with Beraha’s CdS reagent
containing large graphite nodules (arrow), bainite (blue and brown) and retained
austenite (white) when viewed with polarized light plus sensitive tint.
Continuous Cooling Transformations
Continuous Cooling Transformation (CCT) diagram for 9260 alloy steel.
 20 µm
20 µm 20 µm

3000 °F/min; 833 HV 800 °F/min; 654 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).
Continuous Cooling Transformation (CCT) diagram for 8640 alloy steel.
Examples of dilatometer curves used to
create CCT diagrams (in this case, for
8640 alloy steel).
1000 °F/min; 605 HV 550 °F/min; 473 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).
Continuous Cooling Transformation (CCT) diagram for 3140 alloy steel.
 20 µm
20 µm 20 µm

550 °F/min; 634 HV 250 °F/min; 387 HV 50 °F/min; 316 HV

20 µm
20 µm

10 °F/min; 265 HV 2.5 °F/min; 235 HV

Influence of continuous cooling rate on the microstructure of 3140 alloy steel (4% picral).
 20 µm
20 µm

1200 °F/min; 319 HV 850 °F/min; 243 HV

20 µm
20 µm

250 °F/min; 219 HV 2.5 °F/min; 149 HV

Influence of continuous cooling rate on the microstructure of 4620 alloy steel (4% picral).
Quenched and Tempered
Microstructures
 5160
Alloy
Steel

20 µm 20 µm

1525 °F, 830 °C, Oil Quench – 63 HRC 1525 °F, OQ, 400 °F, 204 °C – 58 HRC

20 µm 20 µm

1525 °F, OQ, 800 °F, 427 °C – 47 HRC 1525 °F, OQ, 1200 °F, 649 °C – 28 HRC

Martensitic and tempered martensitic microstructure of 5160 alloy steel (2% nital).
 4140
Alloy
Steel

20µm
µm
2020µm
µm 20

1600 °F, 871 °C, Oil Quench – 55 HRC 1600 °F, OQ, 400 °F, 204 °C – 53 HRC

20 µm 20 µm

1600 °F, OQ, 800 °F, 427 °C – 45 HRC 1600 °F, OQ, 1200 °F, 649 °C – 26 HRC

Martensitic and tempered martensitic microstructure of 4140 alloy steel (2% nital).
 8620
Alloy
Steel

20 µm 20 µm

1600 °F, 871 °C, Water Quench – 45 HRC 1600 °F, WQ, 400 °F, 204 °C – 44 HRC

20 µm
20 µm

1600 °F, WQ, 800 °F, 427 °C – 38 HRC 1600 °F, WQ, 1200 °F, 649 °C – 26 HRC

Martensitic and tempered martensitic microstructure of 8620 alloy steel (2% nital).
 20 µm 20 µm

1144 alloy steel 1524 alloy steel

20 µm

1541 alloy steel

Tempered martensite in low alloy steels (1700 °F, 927 °C, water quenched,
tempered 300 °F, 149 °C, 4% picral etch.
 20 µm 20 µm

41B17 alloy steel 8625 alloy steel

Martensitic microstructure of low-carbon alloy steels (1725 °F, 940 °C,

water quenched), 2% nital.
 20 µm 20 µm

S1 – Q+T, 58/59 HRC O1 – Q+T, 58 HRC

20 µm

M2 HSS – Q+T, 64/65 HRC

Tempered martensitic tool steel microstructures (2% nital).