Professional Documents
Culture Documents
O1 A2
20 µm
S4
Examples of the variation in microstructure 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
Hot Rolled
and Slow
Cooled
20 µm 1600 °F, 20 µm
OQ
HR+SC +
Spheroidize
Anneal
Norm+
20 µm Spheroidize 20 µm
Anneal
Influence of starting microstructure on spheroidize annealed
microstructure of W1 (1.05% C) tool steel (4% picral).
Annealing S5 Tool Steel
20 µm 20 µm
20 µm
Full Anneal
Influence of starting microstructure on the spheroidize annealed
microstructure of S5 tool steel (4% picral).
Annealing S5 Tool Steel
20 µm
20 µm
20 µm
Full Anneal
Influence of starting microstructure on the spheroidize annealed microstructure of S5 tool
steel (4% picral).
Annealing S5 Tool Steel
20 µm 20 µm
20 µm
Full Anneal
Influence of starting microstructure on the spheroidize annealed microstructure of S5
tool steel (4% picral).
Annealing S5 Tool Steel
20 µm 20 µm
20 µm
Full Anneal
Influence of starting microstructure on the spheroidize annealed microstructure of S5
tool steel (4% picral).
Normalizing
Grain Growth of 1040 Carbon Steel
100 µm 100 µm
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.
800 °F/min; 654 HV
20 µm 20 µm 20 µm
20 µm
250 °F/min; 374 HV 20 µm 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).
550 °F/min; 473 HV
Influence of continuous cooling rate on the microstructure of 8640 alloy steel (4% picral).
Continuous Cooling Transformation (CCT) diagram for 3140 alloy steel.
250 °F/min; 287 HV
20 µm 20 µm 20 µm
Influence of continuous cooling rate on the microstructure of 3140 alloy steel (4% picral).
850 °F/min; 243 HV
20 µm
20 µm
1200 °F/min; 319 HV
Influence of continuous cooling rate on the microstructure of 4620 alloy steel (4% picral).
Quenched and Tempered
Microstructures
5160 Alloy Steel
All: 1525 °F, 830 °C, Oil Quench
As Quenched
63 HRC
As Quenched
55 HRC
20 µm 20 µm
As Quenched
45 HRC
Martensitic and tempered martensitic microstructure of 8620 alloy steel (2% nital).
20 µm 20
µm
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 20 µm
µm
M2 HSS – Q+T,
20 µm
64/65 HRC
Tempered martensitic tool steel microstructures (2% nital).
Control of Austenitizing Temperature
20 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 (843 °C –
30 min, oil quench, 230 °C temper) and has a fine grain size. The specimen on the right was
“mock carburized” (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.
Solution Annealing
100 µm
Microstructure of Custom Flo 302-HQ austenitic stainless steel (Fe - <0.08% C – 18% Cr – 9%
Ni – 3.5% Cu) in the hot rolled and solution annealed condition after tint etching with
Beraha’s BI reagent. The structure is equiaxed, twinned FCC austenite. The faint vertical
lines are from alloy segregation (longitudinal direction is vertical). Viewed with polarized
light plus sensitive tint.
20 µm 20 µm
Hot Rolled and Slow Cooled 1900 °F, 1038 °C, Water Quench
1070 CS, 900 °F, 482 °C 1072 CS, 900 °F, 482 °C 1072 CS, 950 F, 510 C
1 µm
0.67 µm 1 µm
1080 CS, 900 °F, 482 °C 1070 CS, 900 °F, 482 °C – Cold Drawn
Light micrographs (4% picral) and TEM replicas of patented carbon steel wire.
Surface Treatments
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.
Carburizing
Mount
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.
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 P5 Plastic Mold Steel
100 µm
25 µm
Core
Etchant:
Klemm’s I
Transition
Zone
Klemm’s I vividly reveals the ferrite in the core present during austenitizing versus ferrite that
precipitated onto the pre-existing ferrite during quenching (due to inadequate hardenability).
Carburized 8620 – Lower Bainite
Case/Lath Martensite Core
Case – to – Core Transition
Bright Field Polarized Light + Sensitive Tint
Case and core structure revealed using Beraha’s Sulfamic Acid reagent; 100
mL water, 3 g potassium metabisulfite and 1 g sulfamic acid
Carburized 8620 – Lower Bainite
Case/Lath Martensite Core
Affected
Depth
Microstructure of gas nitrided 41B50 alloy steel (Fe – 0.5% C – 0.85% Mn – 0.25% Si – 0.95% Cr – 0.2% Mo – 0.003% B)
previously quench and tempered to 325 HV (tempered martensite). The surface was electroless nickel 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.
Microstructure of the broken nitrided Lustre Die (41B50+S) chuck jaw with a brittle
compound layer (note crack in layer (green arrow). The grain boundary films (red
arrows) are Fe3C due to the inward diffusion of carbon during nitriding (10% Na2S2O5).
Ni
Electroless Ni Plating
Mn
S
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.
Electroless Ni Plating
Failed Lustre Die nitrided specimen etched with a 10:1 solution of 4% picral
to 2% nital: left: 100X; right: 500X.
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.
AISI H13 mold that performed well in service. 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.
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).
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.
Ion Nitriding
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. The matrix is tempered martensite. Etch with Vilella’s reagent.
Carbonitriding
20 µm
50 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 quench 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.
Boriding
Mount
P
P B
50 µm 10 µm
10 µm
100 µm
Microstructure of wrought 7-Mo duplex stainless steel (Fe - <0.1% C – 27.5% Cr – 4.5% Ni –
1.5% Mo) solution annealed and then aged 48 h at 816 °C to form sigma. Electrolytic etching
with aqueous 20% NaOH (3 V dc, 10 s) revealed the ferrite as tan, the sigma orange, while
the austenite was not colored. The arrows point to austenite that formed during the
conversion of ferrite to sigma.
Retained Austenite
Carburized 8720 Alloy Steel
(Fe – 0.2% C – 0.8% Mn – 0.5% Cr – 0.55% Ni – 0.25% Mo)
10 µm
10 µm
10 µm 10 µm
10 µm
10 µm