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George F. Vander Voort
Director, Research & Technology
Buehler Ltd
Lake Bluff, Illinois USA
Macrostructure of a VIM (vacuum induction melted) ingot of Fe-52% Ni alloy. A slice was
cut transverse to the ingot axis and hot acid etched (50% HCl at 70 °C) revealing the
solidification pattern. There is a very thin surface zone of small grains. Below the surface,
there is a zone of columnar grains and the central portion is equiaxed but coarse. The scale
is in inches.
Transverse Concast Discs, 430 SS
Macrostructure of 5-inch square (127 mm) continuously cast billets of type 430 stainless
steel (Fe - 0.03% C – 0.34% Mn – 0.48% Si – 17.78% Cr – 0.26% Ni – 0.05% Mo –
0.07% Cu) taken at three random locations along the strand. The discs were cut
transverse to the growth direction and were hot acid etched. Note the thin region of fine
grains at the surface, the large columnar zone and the central equiaxed zone (of varying
coarseness). Note that there are some fine cracks present.
Transverse Concast Discs, 316 SS
Macrostructure of 9-inch (229 mm) square continuously cast discs of type 316 austenitic
stainless steel (Fe < 0.08% C – 17% Cr – 12% Ni – 2.5% Mo) after hot acid etching. Discs
cut transverse to the growth direction (strand axis). There is a very thin surface layer of
equiaxed grains and the columnar grains go to the center. There is no central equiaxed
grain zone.
Longitudinal Concast Discs, 303 SS
Macrostructure of 6-inch square (152 mm) continuously cast type 303 austenitic stainless
steel (Fe - <0.15% C - >0.15% S – 18% Cr – 9% Ni – <0.6% Mo) taken at random along the
strand length parallel to the strand length. Note that there is a shallow surface zone of fine
equiaxed grains and the columnar zone goes all the way to the center, where there is a
shrinkage cavity (left disc, red arrow). A stirring line (light etching line due to disturbing
the columnar growth with magnetic stirring) can be seen in each (see arrows). The disc on
the right was cut just off the centerline, so the central shrinkage cavity was missed.
Macrostructure of directionally solidified Ni-base eutectic alloy (etched with 1 mL H2O2
and 99 mL HCl, courtesy of W. Yankausas, TRW, Inc.)
Scanning electron microscope view of dendrites on the surface of a type 304 austenitic
stainless steel electron-beam melt button (Robinson backscattered electron detector,
original at 230X magnification).
Dendritic structure of permanent mold cast A356 aluminum revealed using Weck’s
reagent (viewed with polarized light and sensitive tint, 50X)
As-continuously cast (concast) 3004 aluminum (Al – 1.25% Mn – 1.05% Mg) tint etched
with Weck’s reagent and viewed with crossed polarized light plus sensitive tint.
Magnification bar is 50 µm long. Reveals segregation (“coring”) within the dendrites and
intermetallics between the dendrites.
As-cast 206 aluminum (Al – 4.4% Cu – 0.3% Mg – 0.3% Mn) tint etched with Weck’s
reagent and viewed with crossed polarized light plus sensitive tint. Magnification bar is
50 µm long.
As-cast 319 aluminum (Al – 6.0% Si – 3.5% Cu) tint etched with Weck’s reagent
and viewed with crossed polarized light. Magnification bar is 100 µm long.
Dendritic microstructure of phosphorous-deoxidized copper (Cu – 0.02% P) in
the as-cast condition revealed by Klemm’s I reagent (original at 50X in bright
field illumination). Magnification bar is 200 µm long.
As-cast hypoeutectic Cu – 4.5% P tint etched with potassium dichromate reagent which
colors the copper-rich proeutectic dendrites and the alpha-copper portion of the eutectic.
Note that the color variations indicate compositional differences in the growing dendrites.
Between the Cu dendrites is the eutectic of copper (colored) and copper phosphide, Cu3P
(white). Original at 200X.
As-cast eutectic Cu – 8.4% P tint etched with potassium dichromate reagent which
colored the alpha-copper portion of the eutectic of alpha copper and copper
phosphide, Cu3P (white). Original at 200X.
As-cast hypereutectic Cu – 10.5% P tint etched with Klemm’s II reagent which colors
the -copper phase in the eutectic of Cu and copper phosphide. The large white
particles are proeutectic copper phosphide, Cu3P and the white, unetched part of the
eutectic is copper phosphide. Original at 500X.
200 µm 100 µm
Bright Field Nomarski DIC, Bar is 100 µm
Microstructure of sand-cast Cu – 4% Sn etched with Beraha’s PbS tint etch revealing the
dendritic cast structure. 63 HV.
100 µm
Microstructure of sand cast Cu – 37% Zn revealing some beta phase between the
alpha dendrites using Nomarski DIC and an as-polished specimen.
As Cast, 99 HV 800 °C – 1 h, FC to RT, 88 HV
Microstructure of sand cast Cu – 42% Zn revealed using Beraha’s PbS tint etchant. Note
the change in beta-phase morphology with the heat treatment.
Dendrites in as-cast Monel (Ni – 30% Cu) revealed using Beraha’s reagent (50
mL water – 50 mL HCl – 2 g ammonium bifluoride – 1 g potassium
metabisulfite). Originals at 50X (left) and 100X (right). Magnification bars are
200 and 100 µm long, respectively.
Waterless Kalling’s 15 HCl - 10 Acetic Acid
- 10 HNO3
Lucas’ Reagent
2 V dc, 10s
Dendritic structure of cast IN-738 alloy (Ni – 0.17C – 16Cr – 8.5Co – 2.6W – 1.75
Mo – 0.9Nb – 1.75Ta – 3.4Al – 0.01B – 0.1Zr).
Dendritic cast structure of IN 738 etched with 60% HCl and viewed in bright field.
Left: 50x; right: 100x.
Glyceregia Waterless Kallings
Lucas’ Reagent
2 V dc, 10s
Dendritic solidification structure in cast Russian alloy CNK7 (Ni – 0.08C –
15Cr – 9Co – 7W – 0.4Mo – 3.5Ti – 4.2Al – 0.01B – 0.02Ce).
Dendritic cast structure of CNK-7 Ni-base superalloy etched with 60% HCl and
viewed with polarized light plus sensitive tint, 50x.
Dendritic microstructure of Alloy 718 in the as-cast condition after tint
etching with Beraha’s reagent. The white particles are Laves phase. The
magnification bar is 200 µm long.
Glyceregia Lucas’ Reagent
2 V dc, 10 s
Molybdic Acid Reagent
Dendritic structure of cast MAR-M247 alloy.
Acicular ferrite (arrows) in an as-cast low-carbon steel (Fe – 0.09% C – 0.39% Mn –
0.04% Si – 0.068% Al) revealed by Klemm’s I reagent (viewed with crossed
polarized light plus sensitive tint). Original at 100X magnification.
Dendritic as-cast microstructure of Fe – 0.2% C – 0.6% Mn – 0.1% Si carbon steel etched
with 2% nital and viewed with bright field illumination. Left: 50x; right: 100x.
As-cast Hadfield Mn steel, solution annealed at 1900 F (1038 C), and aged at 1065
F (575 C) which precipitated carbides at the austenite grain boundaries; etched
with 10% sodium metabisulfite, 200X.
Microstructure of as-cast and annealed HP9-4-20 alloy steel (Fe – 0.19C –
0.3Mn – 8.83Ni – 4.46Co – 0.76Cr – 1.01Mo – 0.09V etched with 2% nital (left)
and with Beraha’s sulfamic acid reagent number 4 (right). Note the grain
boundary running horizontally (arrow, right).
Interior
Acicular microstructure of as-cast Fe – 2.95% C – 0.61% Mn – 29.3% Cr etched
with Beraha’s sulfamic acid (3-2-1) reagent and viewed with bright field, 200x.
Dendritic structure of as-cast M-50 bearing steel (Fe – 0.8% C – 4% Cr – 1% V
– 4.5% Mo) after VAR (vacuum arc remelting) revealed by modified Beraha’s
reagent (300 mL water – 1 mL HCl – 2.5 g ammonium bifluoride – 0.5 g
potassium metabisulfite). Original at 20X (magnification bar is 500 µm long).
Well-formed flakes of graphite in gray cast iron. As-polished; original at 200X.
Eutectic cells in gray cast iron revealed by etching with Klemm’s I reagent and
enhanced by using polarized light with sensitive tint. Original at 50X magnification.
Microstructure of pearlitic gray cast iron tint etched with Beraha’s CdS reagent.
Original at 500X.
Shrinkage cavities in white cast iron. Note the dendritic appearance as there was not
enough liquid metal to fill in the interdendritic region. Original magnifications are
200X (left) and 500X (right). Etched with 2% nital.
Microstructure of white cast iron revealed using 2% nital and consisting of
lamellar pearlite and cementite (white). Original at 1000X.
C
G
Microstructure of Ni-Hard cast iron (Fe – 3.3% C – 0.9% Mn – 0.9% Si – 1.8% Cr – 4.4% Ni – 0.4%
Mo) revealing massive cementite (C), Ledeburite (arrows) and patches of plate martensite and retained
austenite. Etched with aqueous 10% Na2S2O5. Original at 500X. Ledeburite is the eutectic of cementite
and austenite where, with cooling, the austenite usually transforms to ferrite and cementite in the form
of pearlite (not in this case due to the high alloy content). Some graphite (G) is also present.
Ledeburite in a white cast iron (Fe – 4.0% C – 0.3% Si – 0.16% Mn – 0.91% Cr) etched
with Beraha’s sulfamic acid reagent (100 mL water, 3 g K2S2O5 and 2 g NH2SO3H) .
Original at 500X magnification. Taken in polarized light with sensitive tint.
Two clusters of spheroidal graphite nodules in austempered ductile iron.
Viewed with crossed polarized light plus sensitive tint. Original at 500X.
Microstructure of pearlitic ductile iron revealed using Beraha’s CdS tint etch. Note
the ferrite rings (“bull’s eyes”) around the nodules or nodule clusters. Viewed with
polarized light plus sensitive tint. Original at 500X.
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Heat treated ductile cast iron tint etched with Beraha’s CdS film reagent and viewed with polarized
light plus sensitive tint. Note the oddly-shaped graphite nodule (bottom, center) and the white (not
colored) cementite particles. The martensite is colored blue and brown and there are small patches of
(white) retained austenite between martensite “needles”. Original at 1000X.
Microstructure of austempered ductile iron tint etched with Beraha’s CdS reagent
containing large graphite nodules (arrow), bainite (blue and brown), also called
“ausferrite” and retained austenite (white) when viewed with polarized light plus
sensitive tint. Original at 500X.
Temper nodules of graphite in malleable cast iron after a ferritizing anneal. The
ferrite matrix was colored using Beraha’s sulfamic acid reagent (original at 500X in
crossed polarized light plus sensitive tint). Magnification bar is 20 µm long.
As-cast Nihard cast iron (Fe – 2.98% C – 0.64% Mn – 0.85% Si – 4.4% Ni – 2.34% Cr) containing
cementite (white), retained austenite (light brown), manganese sulfides (gray particles) and plate
martensite “needles” (light blue and medium blue) after tint etching with Beraha’s CdS reagent and
viewing with polarized light plus sensitive tint. Original at 1000X.
Alloyed white cast iron (Fe – 2.2% C – 0.9% Mn – 0.5% Si – 12.7% Cr – 0.4% Mo
– 0.1% V) with a martensitic matrix and a network of eutectic alloy carbides
(white). Etched with Vilella’s reagent. Original at 200X.
SEM views of sponge iron powder before compaction.
Polished sponge iron particles etched with 2% nital to reveal the
ferrite grain boundaries.
As-polished specimens showing the distribution and size of the voids.
Ferrite grain structure observed after etching with 2% nital. Some of the
black-looking voids are un-reacted graphite.
As-polished (left) and etched (right, 2% nital) examples of the
microstructure after sintering 5 minutes.
As-polished (left) and etched (right, 2% nital) examples of the
microstructure after sintering 10 minutes.
As-polished (left) and etched (right, 2% nital) examples of the microstructure after
sintering 20 minutes
As-polished (left) and etched (right, 2% nital) examples of the microstructure
after sintering 30 minutes
SEM views of Co-Cr-Mo powder before compaction.
10 µm
10 µm
Dendritic solidification structure of polished CCM PLUS powder particles
etched with a 10:1 mix of HCl and H2O2 (3 % conc.).
As-hip’ped (hot isostatically pressed) CCM Plus Co-Cr-Mo alloy, etched
with a 10:1 mixture of HCl – H2O2 (3% conc.)
10 µm
2.5-inch Diam, As-Forged Bar 1.5-inch Diam., As-Rolled Bar
CCM Plus Co-Cr-Mo alloy bar, etched with a 10:1 mixture of
HCl – H2O2 (3% conc.)
Bright Field Dark Field
Microstructure of as-hipped (hot isostatically pressed) powder-
metallurgy (P/M) René 95 alloy (Ni – 0.15C – 8Co – 14Cr – 3.5Mo – 3.5W –
2.5Ti – 3.5Al – 3.5Nb) revealing grain boundary carbides and coarse
gamma prime in an austenitic matrix after etching with glyceregia.
Microstructure of as-hipped (hot isostatically pressed) P/M René 95 alloy
revealing grain boundary carbides and coarse gamma prime in an austenitic
matrix after etching with glyceregia. Prior-particle shapes are clearly visible
at low magnification.
Hot working occurs at a temperature that is relatively close to the
melting point of the metal or alloy. This temperature is normally
well above the recrystallization temperature. A homogenization
cycle may be used, particularly with highly alloyed compositions,
prior to hot working to permit alloy diffusion and enhance
chemical homogeneity. Too high a temperature must be avoided
so that “burning” or grain-boundary liquation (incipient melting)
does not occur.
The temperature during the last hot working pass is also
important as it controls the grain size in the as-rolled
microstructure and may influence problems such as “banding”
in steels. If the finishing temperature is low, recrystallization will
not occur and the grain structure will be coarse and elongated
and will contain residual deformation (dislocations). “Warm”
working occurs below the recrystallization temperature
Hot Working with 1600 F
Finishing Temperature:
Fe – 0.046% C Steel
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Hot Working with 1400
Finishing Temperature
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Fe – 0.046% C Steel
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Hot Working with 1200
Finishing Temperature
Fe – 0.046% C Steel
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Hot Working with 1000
Finishing Temperature
Fe – 0.046% C Steel
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Hot Working with 1600
Finishing Temperature
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Fe – 0.11% C Steel
Transverse
Longitudinal
Microstructure of hot rolled Fe – 0.11% C – 0.50% Mn - <0.01% Si – 0.066% Al
carbon steel with a finishing temperature of 1600 °F (871 °C). Note the equiaxed
ferrite grains and pearlite patches (top – longitudinal plane, bottom – transverse
plane). No deformation is present in the ferrite phase. Etched with 2% nital;
originals at 500X (magnification bars are 20 µm long).
Hot Working with 1400
Finishing Temperature
F
Fe – 0.11% C Steel
Microstructure of hot rolled Fe – 0.11% C – 0.50% Mn - <0.01% Si – 0.066% Al
carbon steel with a finishing temperature of 1400 °F (760 °C). Note the nearly
equiaxed ferrite grains and elongated pearlite patches. Some deformation is
visible in the ferrite, particularly in the transverse specimen. Etched with 2% nital;
originals at 500X (magnification bars are 20 µm long).
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Hot Working with 1200
Finishing Temperature
Fe – 0.11% C Steel
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Hot Working with 1000
Finishing Temperature
Fe – 0.11% C Steel
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Hot Working with 1600
Finishing Temperature
F
Fe – 0.22% C Steel
Transverse
Longitudinal
Microstructure of hot rolled Fe – 0. 22% C – 0.99% Mn - 0.02% Si – 0.059% Al
carbon steel with a finishing temperature of 1600 °F (871 °C). Note the equiaxed
ferrite grains and pearlite patches. No deformation is visible in the ferrite phase.
Etched with 2% nital; originals at 500X (magnification bars are 20 µm long).
Hot Working with 1400
Finishing Temperature
F
Fe – 0.22% C Steel
Transverse
Longitudinal
Microstructure of hot rolled Fe – 0. 22% C – 0.99% Mn - 0.02% Si – 0.059% Al
carbon steel with a finishing temperature of 1400 °F (760 °C). Note the equiaxed
ferrite grains and banded (layered) pearlite. No deformation is visible in the
ferrite phase. Etched with 2% nital; originals at 500X (magnification bars are 20
µm long).
Hot Working with 1200
F Finishing
Temperature
Fe – 0.22% C Steel
Transverse
Longitudinal
Microstructure of hot rolled Fe – 0. 22% C – 0.99% Mn - 0.02% Si – 0.059% Al
carbon steel with a finishing temperature of 1200 °F (649 °C). Note the elongated
ferrite grains and banded (layered) pearlite patches. Little deformation is visible
in the ferrite phase. Etched with 2% nital; originals at 500X (magnification bars
are 20 µm long).
Hot Working with 1000
Finishing Temperature
F
Fe – 0.22% C Steel
Transverse
Longitudinal
Microstructure of hot rolled Fe – 0. 22% C – 0.99% Mn - 0.02% Si – 0.059% Al
carbon steel with a finishing temperature of 1000 °F (538 °C). Note the elongated
ferrite grains and banded (layered) pearlite patches. Substantial deformation is
visible in the ferrite phase. Etched with 2% nital; originals at 500X (magnification
bars are 20 µm long).
Microstructure of hot forged, quenched and tempered HP9-4-20 alloy steel (Fe –
0.19C – 0.3Mn – 8.83Ni – 4.46Co – 0.76Cr – 1.01Mo – 0.09V etched with 2% nital
(left) and with Beraha’s sulfamic acid reagent number 4 (right). (Compare these
images with previously shown as-cast images)
Cold Working
Cold working occurs at temperatures below the
recrystallization temperature. Typically, it is performed
at room temperature. For low-melting point metals
and alloys, deformation at room temperature can be
above the recrystallization temperature. There are a
variety of cold working methods, such as rolling,
swaging, extrusion and drawing. Cold worked
structures normally exhibit deformed grain structures
with considerable slip (bcc and fcc metals) or
mechanical twinning (hcp metals).
Annealing
Annealing is a process where the metal is heated to
a temperature sufficient to fully recrystallize a cold
worked microstructure. In steels, annealing may be
performed on a hardened steel to return it to a soft
condition suitable for machining. Tool steels are
usually given a special annealing process to
spheroidize the carbide, which minimizes its
hardness. Certain Fe-based alloys may be given
special annealing practices to improve electrical or
magnetic behavior.
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Microstructure of low-carbon (0.003%) sheet steel with 20% (top) and 30%
(bottom) reduction in thickness. Note the slight elongation of the grains after
reduction. Longitudinal planes are shown after etching with 2% nital. A few
inclusions and carbides are also present. Slip lines are noticeable after 30%
deformation. Original micrographs at 500X magnification. Magnification bars are
20 µm long.
Microstructure of low-carbon (0.003%) sheet steel with 40% (top) and 50%
(bottom) reduction in thickness. Note the increased elongation of the grains after
reduction. Longitudinal planes are shown after etching with 2% nital. A few
inclusions and carbides are also present. Slip lines are noticeable after
deformation. Original micrographs at 500X magnification. Magnification bars are
20 µm long.
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Sheared end of 6061-F (Al – 1% Mg – 0.6% Si – 0.2% Cr – 0.27% Cu) extruded rod
electrolytically etched with Barker’s reagent (30 V dc, 2 min.) and viewed with polarized
light plus sensitive tint revealing the heavily elongated grains from extruding and the
compression of the sheared end. Magnification bar is 100 µm long.
Cu – 5% Sn – 0.15% P, Cold Drawn
Microstructure of wrought phosphor bronze, Cu – 5% Sn – 0.15% P, cold drawn
revealing heavily cold-worked, elongated FCC grains (note slip lines). Tint etched
with Klemm’s II. Original at 200X, polarized light and sensitive tint.
Cu – 10% Zn, Hot Extruded, CW, Anneal 600 °C
Klemm’s I, XP+ST
Potassium Dichromate
Microstructure of wrought, cold worked and annealed (600 °C, 1112 °F) Cu
– 10% Zn. The structure, which is fully recrystallized, consists of FCC alpha
grains and annealing twins. Tint etching reveals the grain structure much
better than the potassium dichromate etch. Originals at 100X. 54 HV.
Cu – 10% Zn, Hot Extruded, CW, Anneal 750 °C
200 µm
NH4OH and H2O2, Original at 50X Beraha’s PbS
Microstructure of wrought, cold worked and annealed (750 °C, 1382 °F) Cu
– 10% Zn. The structure consists of FCC alpha grains (with a duplex size
distribution) and annealing twins. (Compare with 600 °C anneal)
Cu – 20% Zn, Hot Extruded and Cold Worked
Cold worked wrought alpha brass, Cu – 20% Zn. Note heavy slip lines in
the alpha grains. Original at 100X. Swab etched with equal parts of NH4OH
and H2O2 (3% conc.).
Cu – 20% Zn, Hot Extruded, CW and Annealed
100 µm 100 µm
500 °C Anneal 600 °C Anneal
Microstructure of Cu – 20% Zn, hot extruded, cold worked and annealed at 500
vs. 600 °C, revealing a variation in grain size. The specimens were tint etched with
Beraha’s PbS reagent.
Cu–30% Zn, Hot Extruded, Cold Reduced 30%
Wrought cartridge brass, Cu-30% Zn, cold reduced 30%, revealing cold worked
FCC grains (note slip lines) and annealing twins. Tint etched with Klemm’s I
reagent (original at 100X, crossed polarized light plus sensitive tint).
Cu–30% Zn, Hot Extruded, Cold Reduced 50%
Wrought cartridge brass, Cu-30% Zn, cold reduced 50%, revealing heavily
cold worked FCC grains (note slip lines) and annealing twins. Tint etched
with Klemm’s I reagent (original at 100X, crossed polarized light plus
sensitive tint).
Cu–30% Zn, Hot Ext., Cold Red. 50%, Annealed
260 °C - 30 minutes
Microstructure of wrought cartridge
371 °C - 30 minutes
brass, Cu-30% Zn, cold reduced 50%, and
annealed: 260 °C (500 °F) for 30 min. did not visibly alter the cold worked FCC
grains (note slip lines) and annealing twins; 371 °C (700 °F) for 30 min. produced
partial recrystallization. Tint etched with Klemm’s I reagent (Originals at 100X,
crossed polarized light plus sensitive tint).
Cu–30% Zn, HE, CR 50%, Annealed 427 °C
8 minutes
4 minutes
Microstructure of wrought cartridge brass, Cu – 30% Zn, cold reduced 50%,
annealed at 427 °C (800 °F): 4 minutes did not visibly affect the cold worked
grain structure (note heavy slip lines); 8 minutes has produced the start of
recrystallization. Tint etched with Klemm’s I (Originals at 100X, crossed
polarized light (off crossed) plus sensitive tint).
Cu–30% Zn, HE, CR 50%, Annealed 427 °C
30 minutes
15 minutes
Microstructure of wrought cartridge brass, Cu – 30% Zn, cold reduced 50%,
annealed at 427 °C (800 °F): 15 minutes has partially recrystallized the FCC grain
structure with some remaining coarse cold worked grains; 30 minutes has
increased the degree of recrystallization. Tint etched with Klemm’s I (originals at
100X, crossed polarized light (off crossed)).
Cu–30% Zn, HE, CR 50%, Annealed 482 °C
100 µm
15 minutes, Off XP, Original 100X 40% CR, 60 min., XP+ST
Microstructure of wrought cartridge brass, Cu – 30% Zn, cold reduced
50%, annealed at 482 °C (900 °F): – 15 min. has fully recrystallized the
FCC grain structure, but it is duplex distribution; 60 min. has increased
the grain size. Tint etched with Klemm’s III.
Cu–30% Zn, HE, CR 50%, 704 °C – 30 min.
Klemm’s III, Original at 50X Beraha’s PbS, Original at 50X
Microstructure of wrought cartridge brass, Cu – 30% Zn, cold reduced 50% and
annealed at 704 °C (1300 °F) – 30 min. producing a fully recrystallized, and
grown, equiaxed FCC grain structure with annealing twins. Polarized light and
sensitive tint.
Cu – 22% Zn – 2% Al, CD, Annealed 600 & 750 °C
600 °C, Bar is 200 µm, 74 HV 750 °C, Bar is 200 µm, 61 HV
Microstructure of wrought aluminum brass, Cu – 22% Zn – 2% Al, cold
drawn and annealed producing equiaxed alpha grains containing annealing
twins. Tint etched with Beraha’s PbS.
Cu – 22% Zn – 2% Al, CD, Annealed at 850 °C
200 µm
Microstructure of wrought aluminum brass, Cu – 22% Zn – 2% Al, annealed at
850°C (1562 °F) producing equiaxed alpha grains containing annealing twins. 57
HV; ASTM 00.
Cu – 3% Si – 1% Mn, “Half Hard”
Annealed and cold drawn (“half-hard”) Everdur, Cu – 3% Si – 1% Mn, tint
etched with Klemm’s I. Note that certain grains, with the same color and crystal
orientation, have been lightly deformed compared to the rest. Original at 100X.
Viewed with polarized light and sensitive tint.
Cu – 40% Zn, “Muntz Metal”
100 µm 100 µm
504 °C – 1 h, Water Quench 649 °C – 1 h, Water Quench
Microstructure of Muntz Metal, Cu – 40% Zn ( - brass) heated to various
temperatures in the + phase field and quenched showing an increase in beta
phase (colored) and a decrease in preferred orientation. Tint etched with
Klemm’s I reagent (bright field).
Cu – 40% Zn, “Muntz Metal”
100 µm
100 µm
Bright Field Nomarski DIC
Microstructure of Muntz Metal, Cu – 40% Zn, heated to 716 °C (1320
°F), held 1 h and water quenched producing still more beta phase
(colored), of larger size, and with less preferred orientation. Nomarski
DIC of this specimen tint etched with Klemm’s I reagent reveals the
grain and twin structure in the un-etched alpha phase (not colored).
Cu – 40% Zn, “Muntz Metal”
Microstructure of Muntz metal, Cu – 40% Zn, heated to 843 °C (1550 °F)
into the beta field, held 1 hour, and air cooled. Note the three prior-beta
grains transformed to alpha and ordered beta (same color within each beta
grain) revealed by Klemm’s I reagent (bright field).
100 µm 100 µm
Elgiloy (Co-20% Cr-15% Fe-15% Ni-7% Mo-2% Mn –0.05% B-0.15% C) that
was hot rolled and solution annealed producing partial recrystallization. Etched
with 15 mL HCl – 10 mL acetic acid – 10 HNO3, left: bright field, right:
Nomarski DIC.
Microstructure of Elgiloy, a Co-based alloy used for watch springs (Co – 20%
Cr – 15% Fe – 15% Ni – 2% Mn – 7% Mo – 0.05% B – 0.15% C) after hot
rolling and solution annealing (1040 °C – 2 hours, water quenched). The
specimen is partially recrystallized. The specimen was tint etched with Beraha’s
IV plus 1 g FeCl3 per 100 mL. The specimen was viewed with polarized light
plus sensitive tint. The magnification bar is 100 µm long.
100 µm 100 µm
Elgiloy (Co-20% Cr-15% Fe-15% Ni-7% Mo-2% Mn –0.05% B-0.15% C) that
was hot rolled and solution annealed producing partial recrystallization. Etched
with 15 mL HCl – 10 mL acetic acid – 10 HNO3, left: bright field, right:
Nomarski DIC.
Microstructure of Elgiloy, a Co-based alloy used for watch springs after hot
rolling and solution annealing (1090 °C – 2 hours, water quenched). The
specimen is fully annealed. The specimen was tint etched with Beraha’s IV plus
1 g FeCl3 per 100 mL. The specimen was viewed with polarized light plus
sensitive tint. The magnification bar is 100 µm long.
100 µm 100 µm
Elgiloy (Co-20% Cr-15% Fe-15% Ni-7% Mo-2% Mn –0.05% B-0.15% C) that
was hot rolled and solution annealed producing full recrystallization. Etched
with 15 mL HCl – 10 mL acetic acid – 10 HNO3, left: bright field, right:
Nomarski DIC.
Microstructure of Elgiloy, a Co-based alloy used for watch springs after hot rolling
and solution annealing (1150 °C – 2 hours, water quenched). Note the annealing
twins. The specimen was tint etched with Beraha’s IV plus 1 g FeCl3 per 100 mL.
The specimen was viewed with polarized light plus sensitive tint. The magnification
bar is 100 µm long.
Elgiloy (Co-20% Cr-15% Fe-15% Ni-7% Mo-2% Mn –0.05% B-0.15% C) that
was hot rolled and solution annealed producing full recrystallization. Etched with
15 mL HCl – 10 mL acetic acid – 10 HNO3, left: bright field, right: Nomarski DIC.
Cold Reduced 35% Cold Reduced 35% + Solution Anneal
Microstructure of L605 (Co – 0.1C – 10Ni – 20Cr – 15W – 1.5Mn –
0.5Si) after a 35% cold reduction (left) and then after solution
annealing at 1149 °C (2100 °F) and revealed using 15 mL HCl-10 mL
acetic acid-10 mL nitric acid. The magnification bars are both 50 µm
long. L605 is also known as Haynes alloy 25.
Microstructure_Evolution.pptx

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Microstructure_Evolution.pptx

  • 1. George F. Vander Voort Director, Research & Technology Buehler Ltd Lake Bluff, Illinois USA
  • 2.
  • 3.
  • 4. Macrostructure of a VIM (vacuum induction melted) ingot of Fe-52% Ni alloy. A slice was cut transverse to the ingot axis and hot acid etched (50% HCl at 70 °C) revealing the solidification pattern. There is a very thin surface zone of small grains. Below the surface, there is a zone of columnar grains and the central portion is equiaxed but coarse. The scale is in inches.
  • 5. Transverse Concast Discs, 430 SS Macrostructure of 5-inch square (127 mm) continuously cast billets of type 430 stainless steel (Fe - 0.03% C – 0.34% Mn – 0.48% Si – 17.78% Cr – 0.26% Ni – 0.05% Mo – 0.07% Cu) taken at three random locations along the strand. The discs were cut transverse to the growth direction and were hot acid etched. Note the thin region of fine grains at the surface, the large columnar zone and the central equiaxed zone (of varying coarseness). Note that there are some fine cracks present.
  • 6. Transverse Concast Discs, 316 SS Macrostructure of 9-inch (229 mm) square continuously cast discs of type 316 austenitic stainless steel (Fe < 0.08% C – 17% Cr – 12% Ni – 2.5% Mo) after hot acid etching. Discs cut transverse to the growth direction (strand axis). There is a very thin surface layer of equiaxed grains and the columnar grains go to the center. There is no central equiaxed grain zone.
  • 7. Longitudinal Concast Discs, 303 SS Macrostructure of 6-inch square (152 mm) continuously cast type 303 austenitic stainless steel (Fe - <0.15% C - >0.15% S – 18% Cr – 9% Ni – <0.6% Mo) taken at random along the strand length parallel to the strand length. Note that there is a shallow surface zone of fine equiaxed grains and the columnar zone goes all the way to the center, where there is a shrinkage cavity (left disc, red arrow). A stirring line (light etching line due to disturbing the columnar growth with magnetic stirring) can be seen in each (see arrows). The disc on the right was cut just off the centerline, so the central shrinkage cavity was missed.
  • 8. Macrostructure of directionally solidified Ni-base eutectic alloy (etched with 1 mL H2O2 and 99 mL HCl, courtesy of W. Yankausas, TRW, Inc.)
  • 9. Scanning electron microscope view of dendrites on the surface of a type 304 austenitic stainless steel electron-beam melt button (Robinson backscattered electron detector, original at 230X magnification).
  • 10.
  • 11. Dendritic structure of permanent mold cast A356 aluminum revealed using Weck’s reagent (viewed with polarized light and sensitive tint, 50X)
  • 12. As-continuously cast (concast) 3004 aluminum (Al – 1.25% Mn – 1.05% Mg) tint etched with Weck’s reagent and viewed with crossed polarized light plus sensitive tint. Magnification bar is 50 µm long. Reveals segregation (“coring”) within the dendrites and intermetallics between the dendrites.
  • 13. As-cast 206 aluminum (Al – 4.4% Cu – 0.3% Mg – 0.3% Mn) tint etched with Weck’s reagent and viewed with crossed polarized light plus sensitive tint. Magnification bar is 50 µm long.
  • 14. As-cast 319 aluminum (Al – 6.0% Si – 3.5% Cu) tint etched with Weck’s reagent and viewed with crossed polarized light. Magnification bar is 100 µm long.
  • 15. Dendritic microstructure of phosphorous-deoxidized copper (Cu – 0.02% P) in the as-cast condition revealed by Klemm’s I reagent (original at 50X in bright field illumination). Magnification bar is 200 µm long.
  • 16. As-cast hypoeutectic Cu – 4.5% P tint etched with potassium dichromate reagent which colors the copper-rich proeutectic dendrites and the alpha-copper portion of the eutectic. Note that the color variations indicate compositional differences in the growing dendrites. Between the Cu dendrites is the eutectic of copper (colored) and copper phosphide, Cu3P (white). Original at 200X.
  • 17. As-cast eutectic Cu – 8.4% P tint etched with potassium dichromate reagent which colored the alpha-copper portion of the eutectic of alpha copper and copper phosphide, Cu3P (white). Original at 200X.
  • 18. As-cast hypereutectic Cu – 10.5% P tint etched with Klemm’s II reagent which colors the -copper phase in the eutectic of Cu and copper phosphide. The large white particles are proeutectic copper phosphide, Cu3P and the white, unetched part of the eutectic is copper phosphide. Original at 500X.
  • 19. 200 µm 100 µm Bright Field Nomarski DIC, Bar is 100 µm Microstructure of sand-cast Cu – 4% Sn etched with Beraha’s PbS tint etch revealing the dendritic cast structure. 63 HV.
  • 20. 100 µm Microstructure of sand cast Cu – 37% Zn revealing some beta phase between the alpha dendrites using Nomarski DIC and an as-polished specimen.
  • 21. As Cast, 99 HV 800 °C – 1 h, FC to RT, 88 HV Microstructure of sand cast Cu – 42% Zn revealed using Beraha’s PbS tint etchant. Note the change in beta-phase morphology with the heat treatment.
  • 22. Dendrites in as-cast Monel (Ni – 30% Cu) revealed using Beraha’s reagent (50 mL water – 50 mL HCl – 2 g ammonium bifluoride – 1 g potassium metabisulfite). Originals at 50X (left) and 100X (right). Magnification bars are 200 and 100 µm long, respectively.
  • 23. Waterless Kalling’s 15 HCl - 10 Acetic Acid - 10 HNO3 Lucas’ Reagent 2 V dc, 10s Dendritic structure of cast IN-738 alloy (Ni – 0.17C – 16Cr – 8.5Co – 2.6W – 1.75 Mo – 0.9Nb – 1.75Ta – 3.4Al – 0.01B – 0.1Zr).
  • 24. Dendritic cast structure of IN 738 etched with 60% HCl and viewed in bright field. Left: 50x; right: 100x.
  • 25. Glyceregia Waterless Kallings Lucas’ Reagent 2 V dc, 10s Dendritic solidification structure in cast Russian alloy CNK7 (Ni – 0.08C – 15Cr – 9Co – 7W – 0.4Mo – 3.5Ti – 4.2Al – 0.01B – 0.02Ce).
  • 26. Dendritic cast structure of CNK-7 Ni-base superalloy etched with 60% HCl and viewed with polarized light plus sensitive tint, 50x.
  • 27. Dendritic microstructure of Alloy 718 in the as-cast condition after tint etching with Beraha’s reagent. The white particles are Laves phase. The magnification bar is 200 µm long.
  • 28. Glyceregia Lucas’ Reagent 2 V dc, 10 s Molybdic Acid Reagent Dendritic structure of cast MAR-M247 alloy.
  • 29. Acicular ferrite (arrows) in an as-cast low-carbon steel (Fe – 0.09% C – 0.39% Mn – 0.04% Si – 0.068% Al) revealed by Klemm’s I reagent (viewed with crossed polarized light plus sensitive tint). Original at 100X magnification.
  • 30. Dendritic as-cast microstructure of Fe – 0.2% C – 0.6% Mn – 0.1% Si carbon steel etched with 2% nital and viewed with bright field illumination. Left: 50x; right: 100x.
  • 31. As-cast Hadfield Mn steel, solution annealed at 1900 F (1038 C), and aged at 1065 F (575 C) which precipitated carbides at the austenite grain boundaries; etched with 10% sodium metabisulfite, 200X.
  • 32. Microstructure of as-cast and annealed HP9-4-20 alloy steel (Fe – 0.19C – 0.3Mn – 8.83Ni – 4.46Co – 0.76Cr – 1.01Mo – 0.09V etched with 2% nital (left) and with Beraha’s sulfamic acid reagent number 4 (right). Note the grain boundary running horizontally (arrow, right).
  • 33. Interior Acicular microstructure of as-cast Fe – 2.95% C – 0.61% Mn – 29.3% Cr etched with Beraha’s sulfamic acid (3-2-1) reagent and viewed with bright field, 200x.
  • 34. Dendritic structure of as-cast M-50 bearing steel (Fe – 0.8% C – 4% Cr – 1% V – 4.5% Mo) after VAR (vacuum arc remelting) revealed by modified Beraha’s reagent (300 mL water – 1 mL HCl – 2.5 g ammonium bifluoride – 0.5 g potassium metabisulfite). Original at 20X (magnification bar is 500 µm long).
  • 35. Well-formed flakes of graphite in gray cast iron. As-polished; original at 200X.
  • 36. Eutectic cells in gray cast iron revealed by etching with Klemm’s I reagent and enhanced by using polarized light with sensitive tint. Original at 50X magnification.
  • 37. Microstructure of pearlitic gray cast iron tint etched with Beraha’s CdS reagent. Original at 500X.
  • 38. Shrinkage cavities in white cast iron. Note the dendritic appearance as there was not enough liquid metal to fill in the interdendritic region. Original magnifications are 200X (left) and 500X (right). Etched with 2% nital.
  • 39. Microstructure of white cast iron revealed using 2% nital and consisting of lamellar pearlite and cementite (white). Original at 1000X.
  • 40. C G Microstructure of Ni-Hard cast iron (Fe – 3.3% C – 0.9% Mn – 0.9% Si – 1.8% Cr – 4.4% Ni – 0.4% Mo) revealing massive cementite (C), Ledeburite (arrows) and patches of plate martensite and retained austenite. Etched with aqueous 10% Na2S2O5. Original at 500X. Ledeburite is the eutectic of cementite and austenite where, with cooling, the austenite usually transforms to ferrite and cementite in the form of pearlite (not in this case due to the high alloy content). Some graphite (G) is also present.
  • 41. Ledeburite in a white cast iron (Fe – 4.0% C – 0.3% Si – 0.16% Mn – 0.91% Cr) etched with Beraha’s sulfamic acid reagent (100 mL water, 3 g K2S2O5 and 2 g NH2SO3H) . Original at 500X magnification. Taken in polarized light with sensitive tint.
  • 42. Two clusters of spheroidal graphite nodules in austempered ductile iron. Viewed with crossed polarized light plus sensitive tint. Original at 500X.
  • 43. Microstructure of pearlitic ductile iron revealed using Beraha’s CdS tint etch. Note the ferrite rings (“bull’s eyes”) around the nodules or nodule clusters. Viewed with polarized light plus sensitive tint. Original at 500X.
  • 45. Heat treated ductile cast iron tint etched with Beraha’s CdS film reagent and viewed with polarized light plus sensitive tint. Note the oddly-shaped graphite nodule (bottom, center) and the white (not colored) cementite particles. The martensite is colored blue and brown and there are small patches of (white) retained austenite between martensite “needles”. Original at 1000X.
  • 46. Microstructure of austempered ductile iron tint etched with Beraha’s CdS reagent containing large graphite nodules (arrow), bainite (blue and brown), also called “ausferrite” and retained austenite (white) when viewed with polarized light plus sensitive tint. Original at 500X.
  • 47. Temper nodules of graphite in malleable cast iron after a ferritizing anneal. The ferrite matrix was colored using Beraha’s sulfamic acid reagent (original at 500X in crossed polarized light plus sensitive tint). Magnification bar is 20 µm long.
  • 48. As-cast Nihard cast iron (Fe – 2.98% C – 0.64% Mn – 0.85% Si – 4.4% Ni – 2.34% Cr) containing cementite (white), retained austenite (light brown), manganese sulfides (gray particles) and plate martensite “needles” (light blue and medium blue) after tint etching with Beraha’s CdS reagent and viewing with polarized light plus sensitive tint. Original at 1000X.
  • 49. Alloyed white cast iron (Fe – 2.2% C – 0.9% Mn – 0.5% Si – 12.7% Cr – 0.4% Mo – 0.1% V) with a martensitic matrix and a network of eutectic alloy carbides (white). Etched with Vilella’s reagent. Original at 200X.
  • 50.
  • 51. SEM views of sponge iron powder before compaction.
  • 52. Polished sponge iron particles etched with 2% nital to reveal the ferrite grain boundaries.
  • 53. As-polished specimens showing the distribution and size of the voids.
  • 54. Ferrite grain structure observed after etching with 2% nital. Some of the black-looking voids are un-reacted graphite.
  • 55. As-polished (left) and etched (right, 2% nital) examples of the microstructure after sintering 5 minutes.
  • 56. As-polished (left) and etched (right, 2% nital) examples of the microstructure after sintering 10 minutes.
  • 57. As-polished (left) and etched (right, 2% nital) examples of the microstructure after sintering 20 minutes
  • 58. As-polished (left) and etched (right, 2% nital) examples of the microstructure after sintering 30 minutes
  • 59. SEM views of Co-Cr-Mo powder before compaction.
  • 60. 10 µm 10 µm Dendritic solidification structure of polished CCM PLUS powder particles etched with a 10:1 mix of HCl and H2O2 (3 % conc.).
  • 61. As-hip’ped (hot isostatically pressed) CCM Plus Co-Cr-Mo alloy, etched with a 10:1 mixture of HCl – H2O2 (3% conc.)
  • 62. 10 µm 2.5-inch Diam, As-Forged Bar 1.5-inch Diam., As-Rolled Bar CCM Plus Co-Cr-Mo alloy bar, etched with a 10:1 mixture of HCl – H2O2 (3% conc.)
  • 63. Bright Field Dark Field Microstructure of as-hipped (hot isostatically pressed) powder- metallurgy (P/M) René 95 alloy (Ni – 0.15C – 8Co – 14Cr – 3.5Mo – 3.5W – 2.5Ti – 3.5Al – 3.5Nb) revealing grain boundary carbides and coarse gamma prime in an austenitic matrix after etching with glyceregia.
  • 64. Microstructure of as-hipped (hot isostatically pressed) P/M René 95 alloy revealing grain boundary carbides and coarse gamma prime in an austenitic matrix after etching with glyceregia. Prior-particle shapes are clearly visible at low magnification.
  • 65.
  • 66. Hot working occurs at a temperature that is relatively close to the melting point of the metal or alloy. This temperature is normally well above the recrystallization temperature. A homogenization cycle may be used, particularly with highly alloyed compositions, prior to hot working to permit alloy diffusion and enhance chemical homogeneity. Too high a temperature must be avoided so that “burning” or grain-boundary liquation (incipient melting) does not occur. The temperature during the last hot working pass is also important as it controls the grain size in the as-rolled microstructure and may influence problems such as “banding” in steels. If the finishing temperature is low, recrystallization will not occur and the grain structure will be coarse and elongated and will contain residual deformation (dislocations). “Warm” working occurs below the recrystallization temperature
  • 67. Hot Working with 1600 F Finishing Temperature: Fe – 0.046% C Steel /'
  • 68. Hot Working with 1400 Finishing Temperature F Fe – 0.046% C Steel . r;~ -~'} ) .. .
  • 69. Hot Working with 1200 Finishing Temperature Fe – 0.046% C Steel F _ . ., /' ,_ .-
  • 70. Hot Working with 1000 Finishing Temperature Fe – 0.046% C Steel F ---..:.~ - ~.-- ~ . tI1--_ ~- ~ . - .
  • 71. Hot Working with 1600 Finishing Temperature F Fe – 0.11% C Steel Transverse Longitudinal Microstructure of hot rolled Fe – 0.11% C – 0.50% Mn - <0.01% Si – 0.066% Al carbon steel with a finishing temperature of 1600 °F (871 °C). Note the equiaxed ferrite grains and pearlite patches (top – longitudinal plane, bottom – transverse plane). No deformation is present in the ferrite phase. Etched with 2% nital; originals at 500X (magnification bars are 20 µm long).
  • 72. Hot Working with 1400 Finishing Temperature F Fe – 0.11% C Steel Microstructure of hot rolled Fe – 0.11% C – 0.50% Mn - <0.01% Si – 0.066% Al carbon steel with a finishing temperature of 1400 °F (760 °C). Note the nearly equiaxed ferrite grains and elongated pearlite patches. Some deformation is visible in the ferrite, particularly in the transverse specimen. Etched with 2% nital; originals at 500X (magnification bars are 20 µm long).
  • 73. . '._ .::- '_"':::~~;...~ - .- :>- _ ~/ <:> --"- E. .~ Hot Working with 1200 Finishing Temperature Fe – 0.11% C Steel F ,- ~ 'ii~bOII!5:"';"'',
  • 74. Hot Working with 1000 Finishing Temperature Fe – 0.11% C Steel F .-...,.,.---- ./
  • 75. Hot Working with 1600 Finishing Temperature F Fe – 0.22% C Steel Transverse Longitudinal Microstructure of hot rolled Fe – 0. 22% C – 0.99% Mn - 0.02% Si – 0.059% Al carbon steel with a finishing temperature of 1600 °F (871 °C). Note the equiaxed ferrite grains and pearlite patches. No deformation is visible in the ferrite phase. Etched with 2% nital; originals at 500X (magnification bars are 20 µm long).
  • 76. Hot Working with 1400 Finishing Temperature F Fe – 0.22% C Steel Transverse Longitudinal Microstructure of hot rolled Fe – 0. 22% C – 0.99% Mn - 0.02% Si – 0.059% Al carbon steel with a finishing temperature of 1400 °F (760 °C). Note the equiaxed ferrite grains and banded (layered) pearlite. No deformation is visible in the ferrite phase. Etched with 2% nital; originals at 500X (magnification bars are 20 µm long).
  • 77. Hot Working with 1200 F Finishing Temperature Fe – 0.22% C Steel Transverse Longitudinal Microstructure of hot rolled Fe – 0. 22% C – 0.99% Mn - 0.02% Si – 0.059% Al carbon steel with a finishing temperature of 1200 °F (649 °C). Note the elongated ferrite grains and banded (layered) pearlite patches. Little deformation is visible in the ferrite phase. Etched with 2% nital; originals at 500X (magnification bars are 20 µm long).
  • 78. Hot Working with 1000 Finishing Temperature F Fe – 0.22% C Steel Transverse Longitudinal Microstructure of hot rolled Fe – 0. 22% C – 0.99% Mn - 0.02% Si – 0.059% Al carbon steel with a finishing temperature of 1000 °F (538 °C). Note the elongated ferrite grains and banded (layered) pearlite patches. Substantial deformation is visible in the ferrite phase. Etched with 2% nital; originals at 500X (magnification bars are 20 µm long).
  • 79. Microstructure of hot forged, quenched and tempered HP9-4-20 alloy steel (Fe – 0.19C – 0.3Mn – 8.83Ni – 4.46Co – 0.76Cr – 1.01Mo – 0.09V etched with 2% nital (left) and with Beraha’s sulfamic acid reagent number 4 (right). (Compare these images with previously shown as-cast images)
  • 80.
  • 81.
  • 82. Cold Working Cold working occurs at temperatures below the recrystallization temperature. Typically, it is performed at room temperature. For low-melting point metals and alloys, deformation at room temperature can be above the recrystallization temperature. There are a variety of cold working methods, such as rolling, swaging, extrusion and drawing. Cold worked structures normally exhibit deformed grain structures with considerable slip (bcc and fcc metals) or mechanical twinning (hcp metals).
  • 83. Annealing Annealing is a process where the metal is heated to a temperature sufficient to fully recrystallize a cold worked microstructure. In steels, annealing may be performed on a hardened steel to return it to a soft condition suitable for machining. Tool steels are usually given a special annealing process to spheroidize the carbide, which minimizes its hardness. Certain Fe-based alloys may be given special annealing practices to improve electrical or magnetic behavior.
  • 85. Microstructure of low-carbon (0.003%) sheet steel with 20% (top) and 30% (bottom) reduction in thickness. Note the slight elongation of the grains after reduction. Longitudinal planes are shown after etching with 2% nital. A few inclusions and carbides are also present. Slip lines are noticeable after 30% deformation. Original micrographs at 500X magnification. Magnification bars are 20 µm long.
  • 86. Microstructure of low-carbon (0.003%) sheet steel with 40% (top) and 50% (bottom) reduction in thickness. Note the increased elongation of the grains after reduction. Longitudinal planes are shown after etching with 2% nital. A few inclusions and carbides are also present. Slip lines are noticeable after deformation. Original micrographs at 500X magnification. Magnification bars are 20 µm long.
  • 87. - _ ..---- . ~ - . ":""" -- - - -,..--:- -- - F_ ..... -- ..._ -_ -- -- -..._-
  • 89. Sheared end of 6061-F (Al – 1% Mg – 0.6% Si – 0.2% Cr – 0.27% Cu) extruded rod electrolytically etched with Barker’s reagent (30 V dc, 2 min.) and viewed with polarized light plus sensitive tint revealing the heavily elongated grains from extruding and the compression of the sheared end. Magnification bar is 100 µm long.
  • 90. Cu – 5% Sn – 0.15% P, Cold Drawn Microstructure of wrought phosphor bronze, Cu – 5% Sn – 0.15% P, cold drawn revealing heavily cold-worked, elongated FCC grains (note slip lines). Tint etched with Klemm’s II. Original at 200X, polarized light and sensitive tint.
  • 91. Cu – 10% Zn, Hot Extruded, CW, Anneal 600 °C Klemm’s I, XP+ST Potassium Dichromate Microstructure of wrought, cold worked and annealed (600 °C, 1112 °F) Cu – 10% Zn. The structure, which is fully recrystallized, consists of FCC alpha grains and annealing twins. Tint etching reveals the grain structure much better than the potassium dichromate etch. Originals at 100X. 54 HV.
  • 92. Cu – 10% Zn, Hot Extruded, CW, Anneal 750 °C 200 µm NH4OH and H2O2, Original at 50X Beraha’s PbS Microstructure of wrought, cold worked and annealed (750 °C, 1382 °F) Cu – 10% Zn. The structure consists of FCC alpha grains (with a duplex size distribution) and annealing twins. (Compare with 600 °C anneal)
  • 93. Cu – 20% Zn, Hot Extruded and Cold Worked Cold worked wrought alpha brass, Cu – 20% Zn. Note heavy slip lines in the alpha grains. Original at 100X. Swab etched with equal parts of NH4OH and H2O2 (3% conc.).
  • 94. Cu – 20% Zn, Hot Extruded, CW and Annealed 100 µm 100 µm 500 °C Anneal 600 °C Anneal Microstructure of Cu – 20% Zn, hot extruded, cold worked and annealed at 500 vs. 600 °C, revealing a variation in grain size. The specimens were tint etched with Beraha’s PbS reagent.
  • 95. Cu–30% Zn, Hot Extruded, Cold Reduced 30% Wrought cartridge brass, Cu-30% Zn, cold reduced 30%, revealing cold worked FCC grains (note slip lines) and annealing twins. Tint etched with Klemm’s I reagent (original at 100X, crossed polarized light plus sensitive tint).
  • 96. Cu–30% Zn, Hot Extruded, Cold Reduced 50% Wrought cartridge brass, Cu-30% Zn, cold reduced 50%, revealing heavily cold worked FCC grains (note slip lines) and annealing twins. Tint etched with Klemm’s I reagent (original at 100X, crossed polarized light plus sensitive tint).
  • 97. Cu–30% Zn, Hot Ext., Cold Red. 50%, Annealed 260 °C - 30 minutes Microstructure of wrought cartridge 371 °C - 30 minutes brass, Cu-30% Zn, cold reduced 50%, and annealed: 260 °C (500 °F) for 30 min. did not visibly alter the cold worked FCC grains (note slip lines) and annealing twins; 371 °C (700 °F) for 30 min. produced partial recrystallization. Tint etched with Klemm’s I reagent (Originals at 100X, crossed polarized light plus sensitive tint).
  • 98. Cu–30% Zn, HE, CR 50%, Annealed 427 °C 8 minutes 4 minutes Microstructure of wrought cartridge brass, Cu – 30% Zn, cold reduced 50%, annealed at 427 °C (800 °F): 4 minutes did not visibly affect the cold worked grain structure (note heavy slip lines); 8 minutes has produced the start of recrystallization. Tint etched with Klemm’s I (Originals at 100X, crossed polarized light (off crossed) plus sensitive tint).
  • 99. Cu–30% Zn, HE, CR 50%, Annealed 427 °C 30 minutes 15 minutes Microstructure of wrought cartridge brass, Cu – 30% Zn, cold reduced 50%, annealed at 427 °C (800 °F): 15 minutes has partially recrystallized the FCC grain structure with some remaining coarse cold worked grains; 30 minutes has increased the degree of recrystallization. Tint etched with Klemm’s I (originals at 100X, crossed polarized light (off crossed)).
  • 100. Cu–30% Zn, HE, CR 50%, Annealed 482 °C 100 µm 15 minutes, Off XP, Original 100X 40% CR, 60 min., XP+ST Microstructure of wrought cartridge brass, Cu – 30% Zn, cold reduced 50%, annealed at 482 °C (900 °F): – 15 min. has fully recrystallized the FCC grain structure, but it is duplex distribution; 60 min. has increased the grain size. Tint etched with Klemm’s III.
  • 101. Cu–30% Zn, HE, CR 50%, 704 °C – 30 min. Klemm’s III, Original at 50X Beraha’s PbS, Original at 50X Microstructure of wrought cartridge brass, Cu – 30% Zn, cold reduced 50% and annealed at 704 °C (1300 °F) – 30 min. producing a fully recrystallized, and grown, equiaxed FCC grain structure with annealing twins. Polarized light and sensitive tint.
  • 102. Cu – 22% Zn – 2% Al, CD, Annealed 600 & 750 °C 600 °C, Bar is 200 µm, 74 HV 750 °C, Bar is 200 µm, 61 HV Microstructure of wrought aluminum brass, Cu – 22% Zn – 2% Al, cold drawn and annealed producing equiaxed alpha grains containing annealing twins. Tint etched with Beraha’s PbS.
  • 103. Cu – 22% Zn – 2% Al, CD, Annealed at 850 °C 200 µm Microstructure of wrought aluminum brass, Cu – 22% Zn – 2% Al, annealed at 850°C (1562 °F) producing equiaxed alpha grains containing annealing twins. 57 HV; ASTM 00.
  • 104. Cu – 3% Si – 1% Mn, “Half Hard” Annealed and cold drawn (“half-hard”) Everdur, Cu – 3% Si – 1% Mn, tint etched with Klemm’s I. Note that certain grains, with the same color and crystal orientation, have been lightly deformed compared to the rest. Original at 100X. Viewed with polarized light and sensitive tint.
  • 105. Cu – 40% Zn, “Muntz Metal” 100 µm 100 µm 504 °C – 1 h, Water Quench 649 °C – 1 h, Water Quench Microstructure of Muntz Metal, Cu – 40% Zn ( - brass) heated to various temperatures in the + phase field and quenched showing an increase in beta phase (colored) and a decrease in preferred orientation. Tint etched with Klemm’s I reagent (bright field).
  • 106. Cu – 40% Zn, “Muntz Metal” 100 µm 100 µm Bright Field Nomarski DIC Microstructure of Muntz Metal, Cu – 40% Zn, heated to 716 °C (1320 °F), held 1 h and water quenched producing still more beta phase (colored), of larger size, and with less preferred orientation. Nomarski DIC of this specimen tint etched with Klemm’s I reagent reveals the grain and twin structure in the un-etched alpha phase (not colored).
  • 107. Cu – 40% Zn, “Muntz Metal” Microstructure of Muntz metal, Cu – 40% Zn, heated to 843 °C (1550 °F) into the beta field, held 1 hour, and air cooled. Note the three prior-beta grains transformed to alpha and ordered beta (same color within each beta grain) revealed by Klemm’s I reagent (bright field).
  • 108. 100 µm 100 µm Elgiloy (Co-20% Cr-15% Fe-15% Ni-7% Mo-2% Mn –0.05% B-0.15% C) that was hot rolled and solution annealed producing partial recrystallization. Etched with 15 mL HCl – 10 mL acetic acid – 10 HNO3, left: bright field, right: Nomarski DIC.
  • 109. Microstructure of Elgiloy, a Co-based alloy used for watch springs (Co – 20% Cr – 15% Fe – 15% Ni – 2% Mn – 7% Mo – 0.05% B – 0.15% C) after hot rolling and solution annealing (1040 °C – 2 hours, water quenched). The specimen is partially recrystallized. The specimen was tint etched with Beraha’s IV plus 1 g FeCl3 per 100 mL. The specimen was viewed with polarized light plus sensitive tint. The magnification bar is 100 µm long.
  • 110. 100 µm 100 µm Elgiloy (Co-20% Cr-15% Fe-15% Ni-7% Mo-2% Mn –0.05% B-0.15% C) that was hot rolled and solution annealed producing partial recrystallization. Etched with 15 mL HCl – 10 mL acetic acid – 10 HNO3, left: bright field, right: Nomarski DIC.
  • 111. Microstructure of Elgiloy, a Co-based alloy used for watch springs after hot rolling and solution annealing (1090 °C – 2 hours, water quenched). The specimen is fully annealed. The specimen was tint etched with Beraha’s IV plus 1 g FeCl3 per 100 mL. The specimen was viewed with polarized light plus sensitive tint. The magnification bar is 100 µm long.
  • 112. 100 µm 100 µm Elgiloy (Co-20% Cr-15% Fe-15% Ni-7% Mo-2% Mn –0.05% B-0.15% C) that was hot rolled and solution annealed producing full recrystallization. Etched with 15 mL HCl – 10 mL acetic acid – 10 HNO3, left: bright field, right: Nomarski DIC.
  • 113. Microstructure of Elgiloy, a Co-based alloy used for watch springs after hot rolling and solution annealing (1150 °C – 2 hours, water quenched). Note the annealing twins. The specimen was tint etched with Beraha’s IV plus 1 g FeCl3 per 100 mL. The specimen was viewed with polarized light plus sensitive tint. The magnification bar is 100 µm long.
  • 114. Elgiloy (Co-20% Cr-15% Fe-15% Ni-7% Mo-2% Mn –0.05% B-0.15% C) that was hot rolled and solution annealed producing full recrystallization. Etched with 15 mL HCl – 10 mL acetic acid – 10 HNO3, left: bright field, right: Nomarski DIC.
  • 115. Cold Reduced 35% Cold Reduced 35% + Solution Anneal Microstructure of L605 (Co – 0.1C – 10Ni – 20Cr – 15W – 1.5Mn – 0.5Si) after a 35% cold reduction (left) and then after solution annealing at 1149 °C (2100 °F) and revealed using 15 mL HCl-10 mL acetic acid-10 mL nitric acid. The magnification bars are both 50 µm long. L605 is also known as Haynes alloy 25.