ASM Handbook, Volume 9: Metallography and Microstructures Copyright © 2004 ASM International®

G.F. Vander Voort, editor, p899–917 All rights reserved.

DOI: 10.1361/asmhba0003779 Color images cited in this article appear at end of article. www.asminternational.org

Metallography and Microstructures of

Titanium and Its Alloys
Luther M. Gammon, Robert D. Briggs, John M. Packard, Kurt W. Batson, Rodney Boyer, and Charles W. Domby,
The Boeing Company

METALLOGRAPHY is a complex process
with many variables that involve compromises
between time, resources, and the end product or
purpose of the investigation. For example, a re-
search lab may benefit from the more time-con-
suming method of vibratory polishing, while a
production quality-control lab may not require
specimen preparation with a vibratory polisher.
A lab for teaching also may benefit from the
training experience of manual polishing, or pol-
ishing may be done with semiautomatic polish-
ing machines.
With a little forethought and planning, excel-
lent metallographic samples can be produced in
a short time for light microscopy of titanium and
its alloys. This article describes the fundamentals
of titanium metallographic sample preparation.
Representative micrographs are also presented
for each class of titanium alloys, which include
unalloyed titanium, alpha alloys, alpha-beta al-
loys, and beta titanium alloys. Metallography
and metallographic sample preparation of tita-
nium alloys are also described in more detail in
Ref 1 and 2.

Types of Titanium Alloys

Titanium is an allotropic element; that is, it

Fig. 1 Cross section through the abrasive saw-cut edge
of a Ti-6Al-4V sample. Note there is less than 5
lm depth of disturbed material requiring removal for
proper specimen preparation, seen as a thin layer at the
surface. This layer would be deeper in commercially pure
titanium and more difficult to discern.
exists in more than one crystallographic form.
Fig. 2 This micrograph shows the impact of mounting At room temperature, titanium has a hexagonal
defects on edge retention. Note the edge round-
ing near the air bubble and the sharp edge where the
mounting material filled the gap. This shows the impor-
tance of good-quality mounting techniques and materials.

Fig. 4 Mount with two specimens for manual polishing

Fig. 3 Sample holders for semiautomated polishing machines. (a) Fixed-sample holder with load applied from a central or polishing on a semiautomated polisher with a
column. (b) Nonfixed specimen mover plate with load applied over one mount non-fixed specimen mover plate
900 / Metallography and Microstructures of Nonferrous Alloys
close-packed (hcp) crystal structure, which is re-
ferred to as “alpha” phase. This structure trans-
forms to a body-centered cubic (bcc) crystal
structure, called “beta” phase, at 883 ⬚C (1621
⬚F).
Alloying elements generally can be classified
as alpha or beta stabilizers. Alpha stabilizers,
such as aluminum and oxygen, increase the tem-
perature at which the alpha phase is stable. Beta
stabilizers, such as vanadium and molybdenum,
result in stability of the beta phase at lower tem-
peratures. This transformation temperature from
an alpha-beta phase (or all-alpha phase) to all
beta is known as the beta transus temperature.
The beta transus is defined as the lowest equilib-
rium temperature at which the material is 100%
beta.
Below the beta transus temperature, titanium
will be a mixture of ␣ Ⳮ b if the material con-
tains some beta stabilizers, or it will be all alpha
if it contains no beta stabilizers. The beta transus
is important, because processing and heat treat-
ment are often carried out with reference to some
incremental temperature above or below the beta
transus. Alloying elements that favor the alpha
crystal structure and stabilize it by raising the
beta transus temperature include aluminum, gal-
lium, germanium, carbon, oxygen, and nitrogen.
Two groups of elements stabilize the beta
crystal structure by lowering the transformation
temperature. The beta isomorphous group con-
sists of elements that are miscible in the beta
phase, including molybdenum, vanadium, tan-
talum, and niobium. The other group forms eu-
tectoid systems with titanium, having eutectoid
temperatures as much as 333 ⬚C (600 ⬚F) below
the transformation temperature of unalloyed ti-
tanium. The eutectoid group includes manga-
nese, iron, chromium, cobalt, nickel, copper, and
silicon. Two other elements that often are alloyed
in titanium are tin and zirconium. These ele-
ments have extensive solid solubilities in alpha
and beta phases. Although they do not strongly
promote phase stability, they retard the rates of
transformation and are useful as strengthening
agents.
Fig. 5 Etched with Kroll’s reagent for 45 s. Abusively
polished example of a Ti-6Al-4V fastener result-
ing in a smeared and scratched surface. Excessive etching
cannot correct poor specimen preparation. Note the severe
distortion in microstructure and edge rounding.
Alloy Classes. Titanium alloys have generally pose of the investigation. There is a large differ-
been classified as alpha alloys, alpha-beta alloys, ence between methods used in a research envi-
and beta alloys. Alpha alloys have essentially an ronment, where time may not be as pressing as
all-alpha microstructure. Beta alloys are those al- in a production environment, or in a college in-
loys from which a small volume of material can structional lab where the facilities may not be as
be quenched into ice water from above its beta elaborate.
transus without martensitic decomposition of the Sectioning. Common methods for sectioning
beta phase. Alpha-beta alloys contain a mixture titanium metallographic samples include the
of alpha and beta phases at room temperature. band saw, abrasive cut-off wheel, and slow-
Within the alpha-beta class, an alloy that con- speed wafering wheels. Band sawing titanium
tains less than 2 to 3% beta, such as Ti-8Al-1Mo- should be done with slow blade speed using a
1V, may also be referred to as a “near-alpha” or
“super-alpha” alloy.
The principal alloying element in alpha alloys
is aluminum (oxygen is the principal alloying
element in commercially pure titanium), but cer-
tain alpha alloys and most commercially pure
(unalloyed) titanium contain small amounts of
beta-stabilizing elements. Similarly, beta alloys
contain small amounts of alpha-stabilizing ele-
ments as strengtheners in addition to the beta
stabilizers.
The beta alloys can be further broken down
into beta and “near-beta.” This distinction is nec-
essary, because the phase transformations that
occur, the reaction kinetics, and the processing
could be different if the alloy is a near-beta (lean)
alloy, such as Ti-10V-2Fe-3Al, or a rich beta al-
loy, such as Ti-13V-11Cr-3Al.
Further information on the metallurgy, selec-
tion, processing, and application of titanium al-
loys is contained in Ref 3 and in Properties and
Selection: Nonferrous Alloys and Special-Pur-
pose Materials, Volume 2 of the ASM Handbook
(see, for example, the articles “Wrought Tita-
nium and Titanium Alloys” and “Titanium and
Titanium Alloy Castings”).
Specimen Preparation
Specimen preparation comprises many de-
tailed steps. The first stages of sample prepara-
tion are equipment dependant, while the final
polish step is driven by the needs of the inves-
tigator. Sufficient attention must be paid to each
step or the quality of the finished mount may be
compromised.
The method chosen depends on two factors:
the facilities and equipment present and the pur-
Fig. 7 Ti-6Al-4V alloy with Widmanstätten alpha in a
beta matrix after furnace cooling from above the
transus. Beta anneal temperature was 1040 ⬚C (1900 ⬚F).
Samples were etched with the oxalic tinting reagent for 15
s after polishing by (a) four-step method for optimizing re-
moval of deformed material, (b) four-step method for opti-
mizing edge retention, or (c) three-step semiautomated
method for optimizing preparation time (note the lack of
detail in the dark regions). See text for description of pol-
ishing procedures. See also Fig. 58 in the article “Selected
Fig. 6 A 200 cm (8 in.) wax wheel with relief grooves Color Images” in this Volume for color version.
 Metallography and Microstructures of Titanium and Its Alloys / 901

toothed blade and high pressure applied to the
workpiece. If a high blade speed and low pres-
sure are applied to the workpiece, damage in the
form of cold work will be introduced into the
sample, possibly preventing the true microstruc-
ture from being observed. With all three cutting
methods, sufficient amounts of coolant should be
used to prevent the introduction of heat damage
into the sample. Abrasive cut-off wheels should
be a soft rubber-bonded abrasive type. The ero-
sion of the rubber-bonded wheel will continually
provide a fresh cutting surface and prevent tita-
nium debris from loading up on the blade. If a
dull band saw blade is used or if an abrasive
blade has loaded up with cutting debris, the sam-
ple will be damaged from overheating and cold
work. Figure 1 shows the edge of a cross section
cut with an abrasive cut-off wheel.
Mounting. The sample should also be de-
greased and dried before mounting to ensure ad-
equate adhesion of the mounting media. Careful
consideration is also necessary for making a
proper metallurgical mount.
The first consideration is choosing the most
appropriate mounting medium. Titanium is a
very abrasion-resistant material, and it is essen-
tial that the titanium be mounted correctly to pro-
duce a quality metallographic sample. The se-
lection of mounting material has a significant
impact on edge retention and the surface flatness
of the mount. Failure to use the proper mounting
media may cause rounding of the interface be-
tween the mount and sample, resulting in poor
edge retention. It can also cause rounding or fa-
ceting of the overall mount surface. (See the ar-
ticle “Mounting of Specimens” in this Volume
for more information on mounting and edge re-
tention.)
In selecting a mounting material, it is recom-
mended to use a mineral- or glass-filled hot-com-
pression thermosetting resin. While the costs of
the filled resins are higher than the traditional
bakelite or epoxy resins, the performance of
filled resins is superior, as the filler can allow
close matching of the abrasive wear resistance
of the specimen and the mount. The cost-to-ben-
efit ratio makes filled resins a good choice when
transparency is not needed. When transparency
is needed or voids are present in a part with com-
plex shape, it is necessary to use an alternative
cold-setting material such as a clear epoxy. This
can be vacuum impregnated into sample voids
and irregularities such as the gap in Fig. 2.
The second consideration is the sample con-
figuration, which refers to the position and num-
ber of samples in a mount. The method of pol-
ishing can determine the sample configuration,
as described in more detail in the article “Mount-
ing of Specimens” in this Volume. In general,
there are three types of polishing methods:
● Semiautomatic polishing machine with sam-
ples held in a “fixed” sample holder (Fig. 3a)
● Semiautomatic polishing machine with sam-
ples held in a “nonfixed” sample holder
(Fig. 3b)
● Manual or hand polishing
Polishing with a fixed-sample holder in a sem-
iautomated machine is achieved by a powerhead
that moves the sample holder around the polish-
ing platen. In this method, mounted samples are
fixed in place within a rigid sample holder, and
central force loading is applied to all specimens
in the holder through a centrally located column.
In this method, three or six mounted samples
must be symmetrically placed in the holder in
order to ensure good flatness of the specimens
after polishing. The mount surface thus remains
flat, as the samples are held in-plane by the sam-
ple holder. This method provides optimal edge
retention and flatness and is the recommended
sample preparation method for operators requir-
ing larger volumes of throughput. With this
method, each mount can contain only one spec-
imen.
In the semiautomated nonfixed (or individual
force) method, the specimens sit in a hole in a
holder (a thin plate), and a piston comes down
and presses each specimen against the working
surface. In this case, two or more specimens
should always be placed in each mount (Fig. 4).
By centering them in each side of the mount, the
specimens support the mount so it will not tend
to rock back and forth. The result is a flatter sam-
ple with better edge retention. This is still not as
good as the fixed method. A single specimen
should never be mounted in the center of a
mount. The result is usually a convex and/or fac-
eted mount surface with poor edge retention. The
mount will have the tendency to rock back and
forth about the small, hard specimen, rounding
the mount surface and degrading the quality of

Table 1 Etchants for examination of titanium and titanium alloys

Etchant Comments Etchant Comments
Macroetchants Microetchants (continued)
50 mL HCl, 50 mL H2O General-purpose etch for ␣ 10 mL HF, 10 mL HNO3, 30 Chemical polish and etch for
Ⳮ b alloys mL lactic acid most alloys
30 mL HNO3, 3 mL HF, 67 Used at room temperature to 2 mL HF, 98 mL H2O Reveals ␣ case for most
mL H2O (slow) to 10 mL 55 ⬚C (130 ⬚F) for 3–5 alloys
HNO3, 8 mL HF, 82 mL min. Reveals grain size 98 mL saturated oxalic acid Reveals ␣ case (interstitial
H2O (fast) and surface defects in H2O, 2 mL HF contamination) for most
15 mL HNO3, 10 mL HF, 75 Etch about 2 min. Reveals alloys
mL H2O flow lines and defects 6 g NaOH, 60 mL H2O, heat Good ␣-b contrast, general
Two-stage etch(a) consisting Reveals ␣ and b segregation to 80 ⬚C (180 ⬚F), add 10 microstructures for most
of: (1) 8 mL HF, 10 mL (aluminum segregation) mL H2O2 alloys
HNO3, 82 mL H2O and 2 mL HF, 98 mL H2O, then General-purpose etch for
(2) 18 g/L (2.4 oz/gal) of 1 mL HF, 2 mL HNO3, 97 near-␣ alloys(b)
NH4HF2 (ammonium mL H2O
bifluoride) in H2O 10 mL KOH (40%), 5 mL Stains ␣, transformed b
H2O2, 20 mL H2O
Microetchants
18.5 g benzalkonium General-purpose etch for Ti-
1–3 mL HF, 10 mL HNO3, Reveals hydrides in chloride, 33 mL ethanol, Al-Zr and Ti-Si alloys
30 mL lactic acid unalloyed titanium 40 mL glycerol, 25 mL
1 mL HF, 30 mL HNO3, 30 Reveals hydrides in HF
mL lactic acid unalloyed titanium 2 mL HF, 4 mL HNO3, 94 Reveals microstructure in
Kroll’s reagent: 1–3 mL HF, General-purpose etch for mL H2 aged Ti-13V-11Cr-3Al
2–6 mL HNO3, H2O to most alloys 50 mL 10% oxalic acid, 50 Etch 12–20 s. General-
1000 mL mL 0.5% HF with H2O purpose etch for b alloys
10 mL HF, 5 mL HNO3, 85 General-purpose etch for 10 s with Kroll’s, then 10–15 Brings out aged structure in
Fig. 8 Deformed grain structure from drilling in solution
mL H2O most alloys s with 50 mL 10% oxalic Ti-10V-2Fe-3Al
treated and aged Ti-6Al-4V. Solution treatment
1 mL HF, 2 mL HNO3, 50 Removes etchant stains for acid, 50 mL 0.5% HF with
was at 925 ⬚C (1700 ⬚F) and aged. Polishing was the four-
mL H2O2, 47 mL H2O most alloys H2O
step method for edge retention, and it was etched with the
oxalic tint etch to reveal the deformed grain structure from (a) Two-stage etch procedure: Degrease (if necessary) and clean, making sure the surface is water-break free. Immerse in solution (1) at 45–55 ⬚C
drilling. (a) Depth of the cold work as evidenced by the (110–135 ⬚F) for 2–3 min and rinse thoroughly in clean cold water. Immerse in agitated bath of solution (2) at room temperature for 1–2 min. Rinse
disturbed microstructure to a depth of 310 lm. (b) Normal thoroughly in clean cold water, rinse thoroughly in clean hot water at 90–100 ⬚C (190–210 ⬚F), blow dry with clean compressed air. Solutions must
be used fresh. (b) First etchant stains ␣ phase; second etchant removes stain.
microstructure for comparison
902 / Metallography and Microstructures of Nonferrous Alloys
the edge. This convex surface will have an ad-
verse effect on the appearance of the microstruc-
ture. A similar-sized mount with two small sam-
ples in the holders will reduce the rocking effect,
making it possible to prepare a flatter sample.
Manual or hand polishing is similar to the
semiautomatic nonfixed method. Two or more
specimens should always be mounted in each
sample. The only difference is that the mass of
titanium in the mount for hand preparation
should be kept to a minimum to facilitate grind-
ing and maintain a uniform applied pressure
across the mount.
Grinding. The purpose of grinding is to re-
move the damage caused by the sectioning pro-
cess. Sectioning methods, such as slow-speed
wafering, that do not introduce much damage
into the sample do not require extensive grinding
and decrease sample preparation time.
Semiautomated grinding with a specimen
mover plate or the fixed holder can be done with
semiautomated polishers using diamond-embed-
ded platens or platens with proprietary coatings
designed for applied diamond suspensions.
There is a wide assortment of diamond platens
on the market to be used with automated grind-
ing.
For a 20 to 30 cm (8 to 12 in.) diamond-
embedded platen, the following parameters
should be used. Keep in mind that there are many
possible ways to accomplish a grinding opera-
tion depending on the complexity of the part,
amount of material to be removed, and time
available. Various combinations of these steps
can be used:
● The speed should be ⬍150 rpm (note: tita-
nium machines work best at high pressure and
low speed).
● The applied pressure should be 40 to 70 N (9
to 15 lbf ) per 38 mm (1.5 in.) diam mount.
● Grinding step A uses 70 lm or 220 grit dia-
mond.
● Grinding step B uses 1200 grit diamond.
● Always use a sufficient amount of coolant to
prevent heat damage.
With proper sectioning most ordinary samples
can be ground with a single 220 grit finish fol-
lowed by a 9 lm diamond suspension on either
a grinding platen with a proprietary coating or a
woven non-nap silk cloth.
Table 2 Typical compositions of microetchants suitable in most applications of titanium
metallography
Name Typical composition
Kroll’s reagent 1.5 mL HF
4 mL HNO3
94 mL H2O
Oxalic reagent (tint etch) 20 mL HF
20 g oxalic
98 mL H2O
Ammonium bifluoride 1 g ammonium bifluoride
(ABF) (NH4FHF)
99 mL H2O
Lactic hydride reagent Mix fresh 5 mL lactic acid
and 5 mL stock solution (3
mL HF, 97 mL HNO3)
Grinding by hand usually involves the use of such as silk or a proprietary platen designed
silicon-carbide papers. The following parameters for diamond suspension application is used.
should be observed: ● A 3 lm diamond suspension on a polyester
cloth with an emulsified oil-based lubricant is
● The speed should be kept to no more than 150 used.
rpm. ● Speed should be 120 to 150 rpm.
● Always use new paper. The maximum paper ● Direction of specimen holder rotation should
lifetime is 15 s (or perhaps up to 60 s max in be complementary to the rotation of the
one-time manual grinding). Abrasives platen.
quickly lose their cutting ability and smear ● Applied force should be 40 to 80 N (9 to 18
the sample and introduce cold-work damage. lbf ) per 38 mm (1.5 in.) diam mount.
● Apply as much pressure as can be controlled
when holding the sample to the paper. High
pressure and slow speed will produce favor-
able results.
● The common grit progression sequence is 120
(or 240), 320, and 600 grit. If the sectioning
process produces a fine smooth face, it is pos-
sible to start the grinding process with 320 or
600 grit papers, but there must be sufficient
material removal to eliminate all cutting dam-
age.
● Always use sufficient amounts of coolant or
water to prevent heat damage.
Polishing can be broken down into two
phases, the intermediate polish and final polish.
The purpose of polishing is to gradually remove
the trace amounts of damage and the surface
scratches introduced during the grinding opera-
tions. Again, there are numerous methods doc-
umented for intermediate and final polishing that
may fit different operations. The list below dis-
cusses of a few of the procedures. An example
of abusive polishing is shown in Fig. 5 after etch-
ing. Excessive etching cannot correct poor spec-
imen preparation.
Intermediate polishing is the bridge step or
steps between grinding and ⬍1 lm final step or
steps. It can be done successfully by either the
semiautomated or hand method. The semiauto-
mated method is generally recommended be-
cause it is very effective with typical removal
rates of 5 lm/min and as much as 25 lm/min
with minimal cold work introduced into the sam-
ple. It can be utilized both as a fine grinding and
a polishing step at the same time. Several sem-
iautomated intermediate polishing parameters
have been found effective:
● A 9 lm diamond suspension with an alcohol-
based lubricant on a woven non-nap cloth
Notes Figures
... Fig. 5, 9–11, 13, 14, 16, 35,
37, 56
15 s for Ti-6Al-4V. Do not Fig. 9–11, 15, 28, 46, 50, 57,
remove etch products. 58, 62, 64 Fig. 9 Coarse lamellar alpha revealed by different
etches in Ti-6Al-4V structure after beta anneal at
1040 ⬚C (1900 ⬚F) and furnace cooling. Preparation was
Do not remove etch Fig. 9–11, 47–49, 61 four-step polishing with final polish of 16 h on vibratory
products. polisher and 10% alumina slurry. Slightly uncrossed polar-
ized light for all three etches: (a) ammonium bifluoride
Commercially pure titanium ... (ABF) tint etch, 60 s; (b) Kroll’s reagent, 15 s; (c) oxalic tint
hydrides etch, 60 s. See also Fig. 59 in the article “Selected Color
Images” in this Volume for color version.

There are two options for intermediate hand pol-
ishing; the beeswax platen and the traditional
nap cloth diamond method. The nap cloth and
diamond option is not recommended where edge
retention is critical. The sequence used for hand
polishing is typically:
1. A 6 lm diamond slurry on nap cloth is used.
2. A 3 lm diamond slurry on nap cloth is used.
3. Apply as much pressure as possible without
rocking the specimen.
A recommended intermediate hand-polishing
method using a beeswax wheel is an effective,
inexpensive method that routinely produces
quality samples. About 2.5 mm (0.10 in. of bees-
wax is cast on the platen into which relief
grooves (Fig. 6) are cut at a spacing of 10 to 14
grooves per inch. Polishing is done with a paste
made with 5 lm alumina and hydrogen peroxide.
While polishing with the paste, drops of 3% hy-
drogen peroxide (or higher percentage with pro-
tective gloves) may be applied to the wheel.
Higher percentages of hydrogen peroxide can be
more effective. Another way is to polish with the
alumina paste, followed by a Kroll’s etch, re-
peating this cycle until a clean microstructure
can be observed. A combination of these steps
can prove effective as well. This method has
proven very effective for labs without automated
polishers. The beeswax wheel would be an ex-
cellent choice for the small lab or classroom.
Final Polishing. There are three methods for
final polishing: hand polishing, semiautomated,
and vibratory polishing. For hand polishing a 50/
50 mix of 3% hydrogen peroxide and a 10% so-
lution of a 0.05 lm premixed alumina suspen-
sion is used. These suspensions are available
from several suppliers. A nap cloth or a closed-
cell chemical-resistant foam pad is recom-
mended. For increased edge retention a Dacron
or polyester cloth is preferred.
A semiautomatic method is used for most ti-
tanium alloys as well as commercially pure (CP)
titanium when not inspecting for hydrides. The
same 50/50 mix of 3% hydrogen peroxide and a
diluted 0.05 lm premixed alumina suspension is
used on a closed-cell chemical-resistant foam
Fig. 10 Ti-6Al-4V plate heated at 885 ⬚C (1625 ⬚F) for 15 min, air cooled. (a) Ammonium bifluoride (ABF) tint etch, 60 s; slightly uncrossed polarized light. (b) Kroll’s reagent, 15
s. (c) Oxalic tint etch, 15 s
Metallography and Microstructures of Titanium and Its Alloys / 903
pad (neoprene rubber cloth). The wheel speed
should be 120 to 150 rpm and the force should
be ⬍15 N (3.4 lbf ) per 38 mm (1.5 in.) diam
mount. Head rotation should be in the comple-
mentary direction. For even better edge reten-
tion, a Dacron or polyester cloth may be used
with the same parameters except the force should
be 25 to 40 N (5.6 to 9.0 lbf) per 38 mm (1.5
in.) diam mount. The foam pad usually produces
a clearer overall microstructure, but with slight
edge rounding. Polishing times will vary, with
much longer times required for CP titanium than
the more highly alloyed materials.
The vibratory polisher set up with a short-nap
woven synthetic cloth is the preferred method to
produce a finish with the least amount of defor-
mation to the microstructure. However, this pro-
cess can take a considerable amount of time. A
10% solution of premixed 0.05 lm alumina on
a short-nap synthetic cloth may be used. This
will optimize removal of deformation from pre-
vious steps, but will yield slight edge rounding
and require polishing for 8 to 16 h with a weight
of only about 0.3 kg (11 oz). More weight will
round the edges more.
The vibratory polisher set up with a non-nap
polyester cloth is the preferred method to pro-
duce a microstructure that provides optimal edge
retention and little or no deformation to the mi-
crostructure. The same suspension is used on a
Dacron or polyester non-nap cloth. A weight of
1.0 to 1.5 kg (2.2 to 3.3 lb) is attached to a 38
to 50 mm (1.5 to 2 in.) mount with double-back
tape. The polishing time is 1 h. This method
works well on hybrid materials containing tita-
nium as well as other materials. It optimizes edge
retention.
Example: Comparison of Polishing Meth-
ods. Micrographs of a beta-annealed Ti-6Al-4V
structure are shown in Fig. 7 for three different
polishing preparations, as described below. Each
procedure is designed for a different purpose.
Polishing to Optimize Removal of Deformed
Material (Fig. 7a). In this example, polishing
was accomplished with a four-step method for
optimizing removal of deformed material. This
method is best for overall polish quality:
1. 200 grit diamond-embedded platen
2. 9 lm proprietary grinding platen
3. 3 lm polyester cloth
4. 16 h on vibratory polisher with short-nap syn-
thetic cloth and 10% solution of premixed
0.05 lm alumina suspension
Polishing to Optimize Edge Retention (Fig.
7b). In this example, the same material and etch
is used, but polishing was accomplished by the
following four-step method for optimizing edge
retention:
1. 220 grit diamond-embedded platen
2. 9 lm proprietary grinding platen
3. 3 lm polyester cloth
4. 1 h on vibratory polisher with non-nap poly-
ester cloth and 10% solution of premixed 0.05
lm alumina suspension
Another example is Fig. 8 from Ti-6Al-4V ma-
terial solution treated at 925 ⬚C (1700 ⬚F) and
aged. It was polished with the four-step method
for edge retention. It was etched with the oxalic
tint etch to reveal the deformed grain structure
from drilling. Figure 8(a) shows the depth of the
cold work as evidenced by the disturbed micro-
structure to a depth of 310 lm. Figure 8(b)
shows the normal microstructure for compari-
son.
Polishing to Optimize Preparation Time (Fig.
7c). In this example, the same material and etch
is used. Polishing was accomplished with a
three-step, semiautomated method for optimiz-
ing preparation time:
1. 220 grit diamond-embedded platen
2. 9 lm proprietary grinding platen
3. Closed-cell chemical-resistant foam pad with
a 50/50 mix of 3% hydrogen peroxide and a
0.05 lm premixed alumina suspension
Total time to prepare sample is less than 20 min.
Note that the addition of an intermediate 3 lm
polyester cloth step will further improve this pro-
cess. Also note the lack of detail in the dark re-
gions in Fig. 7(c).
Etchants. There are numerous choices of
etchants for revealing titanium alloy microstruc-
904 / Metallography and Microstructures of Nonferrous Alloys

ture. Table 1 lists various etchants, and a more
extensive listing is also contained in Ref 1. How-
ever, this article focuses on three types of etch-
ants that can easily handle nearly all the needs
in any laboratory. The three etchants are Kroll’s
reagent and two tint etches: an oxalic-acid tint
etch and an ammonium bifluoride (ABF) tint
etch (Table 2).
The etching time will vary depending on the
alloy and heat treat condition of the sample. It is
a good practice to document successful etching
practices in the laboratory. When using the tint
etchants, it is critical not to swab the specimen
after etching. Just wash with warm tap water.
Any swabbing or contact will disturb the surface. fine detail without overetching. However, it is
The etchant products highlight the grain orien- difficult to show etched microstructure in tita-
tation. The use of tint etchants on specimens nium alloy fasteners due to the cold work from
where cold work (plastic and elastic deforma- rolling the threads. Figures 12 and 13 show the
tion) is left from the sample preparation is not crest area of the thread. Note the lighter structure
recommended. Kroll’s reagent is more forgiving at the crest where the cold work is greatest.
in that case. Kroll’s reagent, the most common etchant or
Comparison of contrast developed by the reagent used on titanium alloys (Table 2), is used
three etchants is shown for three types of struc- for bringing out the general microstructure in al-
tures or conditions: pha-beta alloys. It is a relatively low-contrast
etchant. Figure 16 shows examples of etched mi-
● Coarse lamellar structure after slow furnace
crostructures from the same Ti-6Al-4V overaged
cool of T-6Al-4V from beta anneal at 1035
plate with varying etch severity with (Kroll’s)
⬚C (1900 ⬚F) revealed by Kroll’s reagent and
reagent. Etchant time is a compromise between
tint etches (Fig. 9)
detail and contrast. The shorter times reveal
● Worked structure in Ti-6Al-4V plate air
more detail, while longer etching times result in
cooled after heat treatment at 885 ⬚C (1625
more contrast. As etching time increases, all de-
⬚F) revealed by Kroll’s reagent and tint etches
tail is lost in the contrast (see Fig. 16d). It is
(Fig. 10)
better to underetch than overetch. Figure 16(a)
● Bimodal structure representative of an alpha/
is underetched; however, it has all the detail nec-
beta forging revealed by Kroll’s reagent and
essary to analyze the specimen correctly. Figure
tint etches (Fig. 11). The light phase in Fig.
16(b) is a good compromise at 15 s.
11(b)—primary alpha in a matrix of trans-
Oxalic acid is a tint etch that stains the micro-
formed beta, a lamellar alpha/beta structure
structure and provides more contrast in the mi-
as clearly illustrated in the inset of Fig. 11(c)
Figures 12 to 15 are all of a Ti-6Al-4V solu-
tion treated and aged fastener with rolled threads.
Examples are shown etched with both oxalic
acid and Kroll’s reagent. Both etchants show the

Fig. 13 Etched with Kroll’s reagent for 15 s. Ti-6Al-4V

fastener solution treated and aged. 1 h vibra-
tory polisher, non-nap polyester cloth and alumina. Note
Fig. 12 Oxalic tint etch for 15 s. Ti-6Al-4V fastener so- the crest lap, which is typical for a rolled thread.
lution treated and aged. 1 h vibratory polisher,
non-nap polyester cloth and alumina. Note: the mounted
parts were vacuum impregnated with hydrated rhodamine-
dyed epoxy. Note the crest lap, which is typical for a rolled
thread.

Fig. 11 Ti-6Al-4V die forging, mill-annealed. (a) Am-

monium bifluoride (ABF) tint etch, 60 seconds;
slightly uncrossed polarized light. (b) Kroll’s reagent, 15 s;
slightly uncrossed polarized light. (c) Oxalic tint etch, 15
s; slightly uncrossed polarized light. See also Fig. 60 in the
article “Selected Color Images” in this Volume for color
version.
Fig. 14 Etched with Kroll’s reagent for 15 s. Ti-6Al-4V
fastener solution treated and aged. 1 h vibra-
tory polisher, non-nap polyester cloth and alumina.
Fig. 15 Oxalic tint etch for 15 s. Ti-6Al-4V fastener so-
lution treated and aged. 1 h vibratory polisher,
non-nap polyester cloth and alumina. Note: This mount
was vacuum impregnated with hydrated, rhodamine-dyed
epoxy.

crostructure in alpha-beta alloys. Etching with
oxalic acid requires a better quality polish. It is
good for revealing grain orientation, heat effects,
and alpha-rich regions formed by exposure to
alpha stabilizers such as oxygen or nitrogen.
Note: do not remove the etching products or
swab during the procedure.
Ammonium bifluoride (ABF) is another tint
etch. It is similar to oxalic acid and also provides
more contrast in the microstructure of alpha-beta
alloys. Both reagents will reveal grain orienta-
Fig. 16 Micrographs from solution treated and overaged Ti-6Al-4V plate after etching with Kroll’s reagent for (a) 5 s,
(b) 15 s, (c) 30 s, and (d) 60 s. All specimens polished for 1 h with vibratory polisher, non-nap polyester cloth
and alumina. In the severe etch (d), note that fine detail is etched away and the relief is becoming excessive.
Fig. 18 Same as Fig. 17. There is a higher volume frac-
tion of more elongated alpha in the area of high
aluminum content. 50⳯. Courtesy of C. Scholl
Metallography and Microstructures of Titanium and Its Alloys / 905
tion. It is most often used for investigating alpha
case or alpha-enriched areas in the microstruc-
ture. Note: do not remove the etching products
or swab during the procedure.
Macroexamination
Macrostructural examination of titanium al-
loys provides useful information about material
processing, both melting and metalworking. It is
Fig. 19 Ti-6Al-4V alpha-beta processed billet illustrat-
ing macroscopic appearance of a high intersti-
tial defect. See also Fig. 20. Actual size
used for detection of melting defects or anoma-
lies, qualitative assessment of grain refinement
and uniformity, as well as determination of grain
flow in forged products. Macroetching of tita-
nium alloys is discussed in the article “Ma-
croetching” in this Volume.
Four principal defects are to be found in ma-
crosections of ingot, forged billet, or other sem-
ifinished product forms. These include high-alu-
minum defects (HADs or type II defects), high
interstitial defects (HIDs, also referred to as type
I defects or low-density interstitial defects), beta
flecks and high-density inclusions (HDI), High-
aluminum defects are areas containing an abnor-
mally high amount of aluminum. These are soft
areas in the material (Fig. 17, 18) and are also
referred to as “alpha segregation.” Defects re-
ferred to as “beta segregation” are sometimes as-
sociated with alpha segregation. These are areas
in which aluminum is depleted. The high inter-
stitial defects (Fig. 19, 20) are normally high in
oxygen and/or nitrogen, which stabilize the al-
pha phase. These defects are hard and brittle;
they are normally associated with porosity, as
shown in Fig. 21.
Fig. 17 Ti-6Al-4V alpha-beta processed billet illustrat-
ing the macroscopic appearance of a high-alu-
minum defect. See also Fig. 18. 1.25⳯. Courtesy of C.
Scholl
Fig. 20 Same as Fig. 19. The high oxygen content re-
sults in a region of coarser and more brittle ox-
ygen-stabilized alpha than observed in the bulk material.
100⳯
906 / Metallography and Microstructures of Nonferrous Alloys

Fig. 22 Ti-6Al-6V-2Sn alpha-beta alloy forging, solution treated, quenched, and aged. Hand forging at 925 ⬚C (1700
⬚F), solution treated for 2 h at 870 ⬚C (1600 ⬚F), water quenched, aged 4 h at 595 ⬚C (1100 ⬚F), and air cooled.
(a) “Primary” alpha grains (light) in a matrix of transformed beta containing acicular alpha. Kroll’s reagent (ASTM 192).
150⳯. (b) Same structure is the same as in (a), except that alloy segregation has resulted in a dark “beta fleck” (center of
Fig. 21 Ti-8Al-1Mo-1V, as forged. Ingot void (black),
micrograph) that shows no light “primary” alpha. See also Fig. 23 and 24. Etchant: Kroll’s reagent (ASTM 192). 75⳯
surrounded by a layer of oxygen-stabilized al-
pha (light). The remaining structure consists of elongated
alpha grains in a dark matrix of transformed beta. Etchant:
Kroll’s reagent (ASTM 192). 25⳯ mary alpha and transformed beta. The beta fleck transus lower than that of the bulk material. Beta
is a result of the local composition with a higher flecks occur if the temperature is above the tran-
beta-stabilizer content that results in a local beta sus in the “flecked” region. This condition is ap-
Beta flecks are regions enriched in a beta-sta-
bilizing element due to segregation during ingot
solidification. Their occurrence in alpha-beta al-
loys is uncommon. Flecking becomes more of a
problem with beta alloys, which have much
higher amounts of beta-stabilizing additions.
The problem is most prevalent in iron- and chro-
mium-bearing alloys. This enrichment of a lo-
calized region with beta stabilizers lowers the
beta transus, locally changing the microstructure
and thereby enabling their detection.
This microstructural modification can take
two forms. In alpha-beta alloys, such as Ti-6Al-
6V-2Sn, vanadium enrichment lowers the beta
transus, but is not sufficient to stabilize the beta
to room temperature. When working or heat Ti-6Al-6V-2Sn ␣ Ⳮ b forged billet illustrating macroscopic appearance of beta flecks that appear as dark spots.
treating the material high in the ␣ Ⳮ b phase Fig. 24
See also Fig. 22 and 23. Etchant: 8 mL HF, 10 mL HNO3, 82 mL H2O, then 18 g/L (2.4 oz/gal) of NH4HF2 in
field, the microstructure observed (after cooling H2O. Less than 1⳯. Courtesy of C. Scholl
back to room temperature) will consist of pri-

Fig. 23 Ti-6Al-6V-2Sn forging, solution treated for 11⁄4
h at 870 ⬚C (1600 ⬚F), water quenched, and
aged 4 h at 575 ⬚C (1070 ⬚F). Structure: same as in Fig.
22(b), but higher magnification shows a small amount of
light, acicular alpha in the dark “beta fleck.” See also Fig.
24. Etchant: 2 mL HF, 8 mL HNO3, 90 mL H2O. 200⳯
Fig. 25 Ti-10V-2Fe-3Al pancake forging. (a) Beta forged about 50% Ⳮ alpha-beta finish forged about 5%, with heat
treatment at 750 ⬚C (1385 ⬚F), 1 h, water quench, Ⳮ 540 ⬚C (1000 ⬚F), 8 h. (a) Lamellar alpha with a small
amount of equiaxed alpha in an aged beta matrix. Etched 10 s with Kroll’s reagent, then 50 mL of 10% oxalic acid, 50
mL of 0.5% HF. 400⳯. Courtesy of R. Boyer. (b) Same as (a), but amount of ␣ Ⳮ b finish forging is 2%. Micrograph
illustrates darkened aged beta surrounding a lighter etched beta fleck. See also Fig. 26. Same etch as (a). 50⳯. Courtesy
of T. Long
 Metallography and Microstructures of Titanium and Its Alloys / 907

Fig. 26 Same as Fig. 25(b), but at higher magnification

to demonstrate the reduced amount of alpha in
the beta fleck. The alpha observed (light) is primary alpha; Fig. 27 Ti-6Al-2Sn-4Zr-2Mo alpha-beta forged billet macroslice illustrating “tree rings,” which represent minor com-
the alpha that forms upon aging is too fine to resolve. Same positional fluctuations. The slices are from two ingot locations. Etchant unknown. 0.63⳯. Courtesy of W.
etch as Fig. 25(a). 200⳯. Courtesy of T. Long Reinsch

parent in Fig. 22 and 23. A beta fleck could go

undetected if the final processing and heat treat- Microexamination in nearly all cases by using just the polarizer
ment are conducted at a temperature low enough (plane-polarized light) or using the analyzer for
that the beta transus suppression is not sufficient slightly uncrossed polarized light. This also acts
to cause a microstructural perturbation. The ef- Bright-field illumination reveals microstruc- as a neutral density filter for capturing the digital
fects of beta flecks on properties in such alloys ture of properly prepared specimens in most image. High-quality, strain-free objectives are
as Ti-6Al-4V and Ti-6Al-6V-2Sn are still in cases, but image enhancement can be achieved desirable for any polarized light microscopy,
question, but the effect is not a major one.
Beta flecks are more of a problem with near-
beta alloys; they are observed macroscopically
as shiny spots or flecks. Their appearance is
similar in ␣ Ⳮ b alloys (Fig. 24). The beta-sta-
bilizer enrichment in the flecked regions of beta
alloys, however, is sufficient to stabilize the beta
down to room temperature. To guarantee mate-
rial that will be fleck-free, producers must solu-
tion treat samples at a certain temperature below
the beta transus, assuring the user that the ma-
terial will not form beta flecks if heat treated to
a temperature up to or below the test tempera-
ture. The material will then form alpha, but beta
fleck regions will be above or much nearer the
transus. Therefore, they will be void of alpha or
contain a significantly lower volume fraction of
alpha upon cooling to room temperature, as
shown in Fig. 25 and 26. These regions in beta
alloys will be harder, will have higher strength
and lower ductility, and will have lower low-cy-
cle fatigue strength than the bulk material.
Tree rings (Fig. 27) are another macrostruc-
tural anomaly observed in titanium alloy macro-
sections. This phenomenon represents very mi-
nor composition variations that occur during
melting. The appearance of tree rings is normally
only a cosmetic nuance, not a cause for concern.
Grain flow of forgings is useful for evaluating
the forging process. For high-quality forgings, in
general, the grain flow should conform to the
general shape of the part. There should be no
forging laps, seams, or areas of grain flow that
appear as though they could produce forging laps Fig. 28 Variation in appearance with changes in illumination of a Ti-6Al-4V specimen with oxalic tint etch (15 s).
Material was beta annealed at 1050 ⬚C (1925 ⬚F) and furnace cooled. (a) Illuminated and examined with
in subsequent operations. In addition, the part slightly uncrossed (45–129) polarized light. (b) Illuminated and examined with slightly uncrossed (45–139) polarized light.
should be uniformly recrystallized and suffi- (c) Plane-polarized light illumination. (d) Bright-field illumination. See also Fig. 61 in the article “Selected Color Images”
ciently worked in all areas. in this Volume for color version.
908 / Metallography and Microstructures of Nonferrous Alloys

Alpha Structures
Generally, two types of alpha are present: pri-
mary alpha and secondary alpha or transformed
beta (Fig. 29, 30). The primary alpha is that pres-
ent during prior hot working, remnants of which
persist through heat treatment. The secondary al-
pha is produced by transformation from beta.
This may occur upon cooling from above the
beta transus (Fig. 29d) or high within the alpha-
beta phase field (Fig. 29b and c) by aging or by
aging of the beta (Fig. 30d). The aged alpha is
usually too fine to resolve using light (optical)
microscopy. The alpha in these areas has differ-
ent appearances and may be acicular or lamellar,
platelike, serrated, or Widmanstätten.
Equiaxed alpha grains, such as are shown in
Fig. 31 and 32 are usually developed by anneal-
ing cold-worked alloys above the recrystalliza-
tion temperature. Elongated alpha grains (Fig.
33, 34) result from unidirectional working of the
metal and are commonly found in longitudinal
sections of rolled or extruded alloys.
The microstructure of titanium alloys is
strongly influenced by the processing history and
heat treatment. The effect of cooling rate on Ti-
5Al-2.5Sn annealed above the beta transus can
be seen in Fig. 35. This is also illustrated for Ti-
6Al-4V in Fig. 36. As the cooling rate increases,
the lamellar alpha (or martensite, depending on
the alloy and cooling rate) becomes finer. Coarse
and finer lamellar structures in alloy Ti-6Al-4V
are also shown, respectively, in Fig. 9 and 28
after furnace cooling from different temperatures
above the beta transus. The extent of lamellar
Fig. 29 Ti-6Al-2Sn-4Zr-6Mo, forged at 870 ⬚C (1600 ⬚F). (a) Solution treated 2 h at 870 ⬚C (1600 ⬚F), water quenched, alpha in the Ti-10V-2Fe-3Al lean beta alloy is
and aged 8 h at 595 ⬚C (1100 ⬚F), and air cooled. Elongated “primary” alpha grains (light) in aged transformed
beta matrix containing acicular alpha. (b) Solution treated at 915 ⬚C (1675 ⬚F) instead of at 870 ⬚C (1600 ⬚F), which
shown in Fig. 37. The structure is completely
reduced the amount of “primary” alpha grains in the ␣ Ⳮ b matrix. (c) Solution treated at 930 ⬚C (1710 ⬚F), which reduced lamellar alpha (Fig. 37a) when heat treatment is
the amount of alpha grains and coarsened the acicular alpha in the matrix. (d) Solution treated at 955 ⬚C (1750 ⬚F), which below the beta transus. When heat treated just
is above the beta transus. The resulting structure is coarse, acicular alpha (light) and aged transformed beta (dark). All below the beta transus, a beta structure develops
etched with Kroll’s reagent (ASTM 192). 500⳯
with some residual alpha (Fig. 37b). When
heated above the transus and cooled, the struc-
while non-strain-free objectives or objectives comparative micrographs from the examination ture of Ti-10V-2Fe-3Al is completely beta.
with a long working distance will compromise of a Ti-6Al-4V specimen with different illumi- The effect of forging temperature is illustrated
the polarized light image. Figure 28 provides nation modes. for Ti-8Al-1Mo-1V in Fig. 38. As the forging

Fig. 30 Ti-15V-3Cr-3Al-3Sn cold-rolled strip that has been annealed at 790 ⬚C (1450 ⬚F) for 10 min and aged at various times to illustrate the progression of aging and what is
termed “decorative aging,” a technique used to determine the extent of recrystallization. (a) Not aged. (b) Aged 2 h at 540 ⬚C (1000 ⬚F). (c) Aged 4 h. (d) Aged 8 h. Grains
in center are completely aged (uniform alpha precipitation throughout the grains). An 8 h age results in a fully aged structure. All etched with Kroll’s reagent. All 200⳯. Courtesy of P.
Bania

Fig. 31 High-purity (iodide-process) unalloyed tita-
nium sheet, cold rolled, and annealed 1 h at
700 ⬚C (1290 ⬚F). Equiaxed, recrystallized grains of alpha.
Etchant: Kroll’s reagent (ASTM 192). 250⳯
Fig. 32 Ti-6Al-4V plate, recrystallize annealed at 925
⬚C (1700 ⬚F) 1 h, cooled to 760 ⬚C (1400 ⬚F) at
50 to 55 ⬚C/h (90 to 100 ⬚F/h), then air cooled. Equiaxed
alpha with intergranular beta. The alpha-alpha boundaries
are not defined. Etchant: 50 mL oxalic acid in H2O, 50 mL
1% HF in H2O. 500⳯. Courtesy of J.C. Chesnutt
temperature increases, the amount of trans-
formed beta increases until the forging tempera-
ture is above the beta transus, at which point the
structure is 100% transformed beta. The effect
of the amount of forging deformation is illus-
trated for Ti-6Al-2Sn-4Zr-2Mo and Ti-5Al-6Sn-
2Zr-1Mo-2.5Si, respectively in Fig. 39 and 40.
Sufficient working of the cast Widmanstätten
structure at a temperature below the beta transus
causes recrystallization of the lamellar structure
to a more equiaxed structure. Sufficient working
Metallography and Microstructures of Titanium and Its Alloys / 909
Fig. 33 Commercial-purity (99.0%) unalloyed titanium sheet. (a) As-rolled to 1.0 mm (0.040 in.) thick at 760 ⬚C (1400
⬚F). Grains of alpha, which have been elongated by cold working. (b) Same as in (a), but annealed 2 h at 700
⬚C (1290 ⬚F) and air cooled. Recrystallized alpha grains, particles of TiH (black), and particles of beta (also black) stabilized
by impurities. (c) Same as in (a), but annealed 1 h at 900 ⬚C (1650 ⬚F)—just below the beta transus—and air cooled.
Recrystallized grains of “primary” alpha and transformed beta containing acicular alpha. (d) Same as in (a), but annealed
2 h at 1000 ⬚C (1830 ⬚F) and air cooled. Colonies of serrated alpha plates; particles of TiH and retained beta (both black)
between the plates of alpha. All etched with Kroll’s reagent (ASTM 192). 250⳯
and proper heat treatment can produce a com- Alpha Case. Unless heat treatments are per-
pletely equiaxed crystal structure (Fig. 32). The formed in an inert atmosphere, oxygen and ni-
microstructural behavior trends will be similar trogen will be absorbed at the surface, stabilize
for all-alpha and ␣ Ⳮ b alloys. the alpha, and form a hard, brittle layer referred
Acicular or lamellar alpha is the most common
transformation product formed from beta during
cooling. It is a result of nucleation and growth on
crystallographic planes of the prior beta matrix.
Precipitation normally occurs on multiple vari-
ants or orientations of this family of habit planes,
as illustrated in Fig. 29(d) and 41. A packet or
cluster of acicular alpha grains aligned in the
same orientation is referred to as a “colony.”
When correlating this type of microstructure with
properties such as fatigue or fracture toughness,
colony size is often regarded as an important mi-
crostructural feature. The multiple orientations of
alpha have a basketweave appearance character-
istic of alpha Widmanstätten structure. Lamellar
alpha forming from small beta grains also may
have a singular orientation (Fig. 42).
Under some conditions, the long grains of al-
pha produced along preferred planes in the beta
matrix take on a wide, platelike appearance, as
shown in Fig. 35(a). Under other conditions, Fig. 34 Ti-6Al-4V, as-forged at 955 ⬚C (1750 ⬚F), below
grains of irregular size and with jagged bound- the beta transus. Elongated alpha (light),
caused by low reduction (20%) of a billet that had coarse,
aries, called “serrated alpha,” are produced platelike alpha, in a matrix of transformed beta containing
(Fig. 43). acicular alpha. Etchant: Kroll’s reagent (ASTM 192). 250⳯
910 / Metallography and Microstructures of Nonferrous Alloys

Fig. 35 Ti-5Al-2.5Sn, hot worked below the alpha transus, annealed 30 min at 1175 ⬚C (2150 ⬚F), which is above the beta transus. (a) Furnace cooled to 790 ⬚C (1450 ⬚F) in 6 h,
and furnace cooled to room temperature in 2 h. Coarse, platelike alpha. Etchant: Kroll’s reagent (ASTM 192). 100⳯. (b) Air cooled from the annealing temperature instead
of furnace cooled. The faster cooling rate produced acicular alpha that is finer than the platelike alpha in (a). Prior beta grains are outlined by the alpha that was first to transform.
Etchant: Kroll’s reagent (ASTM 192). 100⳯. (c) Water quenched from the annealing temperature instead of furnace cooled and shown at a higher magnification. The rapid cooling
produced fine acicular alpha. A prior beta grain boundary can be seen near the center of the micrograph. Etchant: Kroll’s reagent (ASTM 192). 250⳯

Fig. 36 Ti-6Al-4V bar, held for 1 h at 1065 ⬚C (1950 ⬚F), above the beta transus. (a) Furnace cooled. Platelike alpha
(light) and intergranular beta (dark). (b) Air cooled. The structure consists of acicular alpha (transformed beta);
prior beta grain boundaries. Etchant for both (a) and (b): 10 mL HF, 5 mL HNO3, 85 mL H2O. 250⳯

Fig. 37 Effect of heat treatment temperature below, near, and above the transus temperature on etched appearance of lean beta alloy Ti-10V-2Fe-3Al. All specimens were polished
with four-step procedure ending up with 16 h on vibratory polisher (10% alumina slurry), etched with Kroll’s reagent for duration noted, and examined under slightly
uncrossed polarized light (a) lamellar alpha after air cool (AC) from temperature about 70 ⬚C (130 ⬚F) below beta transus (730 ⬚C, or 1350 ⬚F, for 2 h). (b) Heat treated just below the
beta transus (788 ⬚C, or 1450 ⬚F, for 2 h, AC), where almost all of the alpha has gone back into solution. One grain in this view contains residual alpha. (c) All-beta structure from beta
heat treatment. Duration of etching with Kroll’s reagent: (a) 15 s, (b) and (c) 60 s
 Metallography and Microstructures of Titanium and Its Alloys / 911

to as an “alpha case” (Fig. 44, 45). This case is phase, at compositions greater than about 6 wt% Martensite
normally removed by chemical milling or ma- Al. This ordered phase is submicron in size and
chining. A part should not be put into service can be observed only by electron microscopy Martensite is a nonequilibrium supersaturated
unless this alpha case has been removed. (Fig. 51). alpha-type structure produced by diffusionless
Figures 46 to 50 show alpha case layers
caused by interstitial oxygen migration through
the surface. This illustrates the increase in alpha
case thickness as the thermal exposure is in-
creased with longer times or higher tempera-
tures. The oxygen migration causes an increase
in hardness beyond the visible depth of the alpha
case layer.
Ti3Al (Alpha-2) Ordered Phase. The alpha
phase can decompose to ␣ Ⳮ Ti3Al, an ordered

Fig. 39 Ti-6Al-2Sn-4Zr-2Mo forged ingot. (a) Forged and held 1 h at 1010 ⬚C (1850 ⬚F), air cooled, heated to 970 ⬚C
(1775 ⬚F), and immediately air cooled. Acicular alpha (transformed beta); prior beta grain boundaries. (b)
Same as (a), but reduced 15% by upset forging while at 970 ⬚C (1775 ⬚F). The structure consists of slightly deformed
acicular alpha (transformed beta), boundaries of elongated prior beta grains. Both etched with Kroll’s reagent (ASTM 192).
100⳯

Fig. 40 Ti-5Al-6Sn-2Zr-1Mo-2.5Si forging. (a) Reduced 75% by upset forging starting at 980 ⬚C (1800 ⬚F), annealed 1
h at 980 ⬚C (1800 ⬚F), air cooled, and stabilized 2 h at 595 ⬚C (1100 ⬚F). Fine alpha grains (light); intergranular
beta. (b) Same as (a), except upset forged starting at 1150 ⬚C (2100 ⬚F), which is above the beta transus temperature.
Distorted acicular alpha (light constituent); intergranular beta; and boundaries of elongated prior beta grains. Both etched
with HF, HNO3, HCl, glycerol (ASTM 193). 100⳯

Fig. 38 Ti-8Al-1Mo-1V forging. (a) Forged with a start-

ing temperature of 900 ⬚C (1650 ⬚F), which is
below the normal temperature range for forging this alloy.
Structure: equiaxed alpha grains (light) in a matrix of trans-
formed beta (dark). (b) Forged with starting temperature of
1005 ⬚C (1840 ⬚F), which is within the normal range, and
air cooled. Equiaxed grains of “primary” alpha (light) in a
matrix of transformed beta (dark) containing fine acicular
alpha. (c) Starting temperature for forging was 1095 ⬚C
(2000 ⬚F), which is above the beta transus temperature, and Fig. 41 Ti-6Al-5Zr-4Mo-1Cu-O.2Si casting. (a) As-cast. Microstructure: transformed beta containing acicular alpha
the finished forging was rapidly air cooled. The structure (light platelets). A thin film of alpha phase (light) is evident at the prior beta grain boundaries. (b) Same as (a),
consists of transformed beta containing coarse and fine but solution treated 1 h in argon at 845 ⬚C (1550 ⬚F), air cooled, and aged 24 h at 500 ⬚C (930 ⬚F). Acicular alpha (light)
acicular alpha (light). All etched with Kroll’s reagent (ASTM and aged beta; alpha platelets at prior beta grain boundaries. Both etched with 10 mL HF, 30 mL HNO3, 50 mL H2O
192). 250⳯ (ASTM 187). 500⳯
912 / Metallography and Microstructures of Nonferrous Alloys

(martensitic) transformation of the beta. There
are two types of martensite: ␣⬘, which has a hex-
agonal crystal structure, and ␣⬙, which has an
orthorhombic crystal structure. Martensite can
be produced in titanium alloys by quenching
(athermal martensite) or by applying external
stress (stress-induced martensite). The ␣⬙ can be
formed athermally or by a stress-assisted trans-
formation (see Fig. 52, 53). However, ␣⬘ can be
formed only by quenching. Examples of ␣⬘
structures are exhibited in Fig. 54 and 55. Aging
of the martensite results in its decomposition to
␣ Ⳮ b.
Beta Structures
In alpha-beta and beta alloys, some equilib-
rium beta is present at room temperature. A non-
equilibrium, or metastable, beta phase can be
produced in alpha-beta alloys that contain
enough beta-stabilizing elements to retain the
beta phase at room temperature on rapid cooling
from high in the ␣ Ⳮ b phase field. The com-
position of the alloy must be such that the tem-
perature for the start of martensite formation is
depressed to below room temperature. One hun-
dred percent beta can be retained by air cooling
beta alloys. The decomposition of this retained
beta (or martensite, if it forms) is the basis for
heat treating titanium alloys to higher strengths.
Aged Structures
The alpha that forms upon aging of retained
beta is often too fine to be resolved by optical
microscopy, particularly with beta and near-beta
alloys. Aging of ␣⬘ martensite results in the for-
mation of equilibrium ␣ Ⳮ b, but most aged
martensite structures cannot be distinguished
from unaged martensite by optical microscopy.
Unresolved alpha precipitation is shown in
Fig. 56 for alloy Ti-10V-2Fe-3Al with Kroll’s
etch. Figures 57 and 58 are light micrographs of
cold-rolled and aged Ti-15V-3Cr-3Al-3Sn foil.
The white regions indicate there was less or no
heat treatment response. Precipitation of alpha
during aging of beta results in some darkening
of the aged beta structure. The progression of
aging response in alloy Ti-15V-3Cr-3Al-3Sn is
shown in Fig. 30.
Other precipitation products include:
● Eutectoid products
● x phase (Fig. 59), which is a transition phase
(potentially resulting in severe embrittlement)
● Phase splitting
Phase splitting, or phase separation only, occurs
in the solute-rich beta alloys; b r br Ⳮ b1 where

Fig. 42 Ti-6Al-4V forging. (a) Solution treated 1 h at 955 ⬚C (1750 ⬚F), air cooled, and annealed 2 h at 705 ⬚C (1300
⬚F). Equiaxed alpha grains (light) in transformed beta matrix (dark) containing coarse, acicular alpha. (b) Same Fig. 43 Unalloyed titanium sheet. Same as Fig. 33, but
as in (a), except water quenched from the solution treatment (before the anneal) instead of air cooled. Structure is similar annealed 2 h at 1000 ⬚C (1830 ⬚F) and air
to that in (a), but the faster cooling resulted in finer acicular alpha in the transformed beta. Both etched with Kroll’s reagent cooled. Colonies of serrated alpha plates; particles of TiH
(ASTM 192). 500⳯ and retained beta (both black) between the plates of alpha.
Etchant: Kroll’s reagent (ASTM 192). 250⳯

Fig. 44 Ti-7Al-2Mo-1V plate, heated to 1010 ⬚C (1850
⬚F), which is above the beta transus. Surface
layer of white, oxygen-stabilized alpha (alpha case); the
remainder of the structure is acicular alpha (transformed
beta). Etchant: 2 mL HF, 8 mL HNO3, 90 mL H2O. 450⳯
Fig. 45 Ti-6Al-4V plate diffusion-bonded joint (bonded
at 925 ⬚C, or 1700 ⬚F) illustrating bond-line
contamination. The white horizontal band is an area of O2
and/or N2 enrichment. An alpha case is also observable on
the exterior surface. Etchant: 50 mL H2O, 50 mL 10% ox-
alic acid, 1 mL HF. 58⳯. Courtesy of J.C. Chesnutt
Fig. 46 Alpha case in Ti-6Al-4V after exposure to 760
⬚C (1400 ⬚F) for 90 min. Preparation: oxalic tint
etch for 60 s, and four-step edge-retention process ending
with 1 h on vibratory polisher with a non-nap polyester
cloth and alumina. See also Fig. 62 in the article “Selected
Color Images” in this Volume for color version.

Fig. 47 Alpha case in Ti-6Al-4V after exposure to 885
⬚C (1625 ⬚F) for 90 min. Preparation: ammo-
nium bifluoride tint etch for 60 s, and four-step edge-reten-
tion process ending with 1 h on vibratory polisher with a
non-nap polyester cloth and alumina. See also Fig. 63 in
the article “Selected Color Images” in this Volume for color
version.
br is solute-rich beta and b1 is solute lean beta.
The solute lean beta is designated b⬘ (Fig. 60).
This is not an important decomposition product
from a practical standpoint, because it does not
occur in commercial alloys with heat treatments
that are used. The x phase and phase splitting
can only be observed using electron microscopy.
Other Structures
Hydrides. Figure 61 shows hydrides in com-
mercially pure (CP) titanium sheet located at the
weld heat-affected zone (HAZ). The black nee-
dles in this micrograph are a result of hydrogen
migrating to high residual stress areas and form-
ing a titanium hydride. In most cases, because of
their brittle nature, hydrides will result in micro-
cracks. Material with this extent of hydrides will
be very brittle. Commercially pure titanium is
more difficult to polish than more highly alloyed
titanium alloys because it is softer and retains
more cold work. The same polishing method
used for titanium alloys will also work for CP
titanium, but longer final polishing times may be
needed. Do not use hydrogen peroxide or etch-
polish to remove residual cold work induced by
previous polishing steps. Etching will mask the
hydrides. It is best just to add more time to the
last two steps. If hand polishing with a 5 lm
alumina and beeswax wheel, it can take 20 min.
Revealing hydrides in CP titanium with an
ABF etch (Fig. 61) requires a perfectly polished
surface. The lactic hydride reagent (Table 2) may
be more easily applied to reveal the presence of
hydrides with etching times ranging from 11⁄2 to
3 min. A 3 min etch can provide good contrast
to reveal hydrides with a light microscope. An
etch of 11⁄2 min may provide subtle contrast un-
der a light microscope, but examination in a
scanning electron microscope can easily reveal
microcracks associated with hydride cracking.
Heat-Affected Zones. Heat damage from
machining, sample excision, or preparation is of-
ten confused with alpha case. The difference can
Metallography and Microstructures of Titanium and Its Alloys / 913
Fig. 48 Alpha case in Ti-SP 700 (Ti-4.5Al-3V-2Mo-2Fe)
after exposure to 900 ⬚C (1650 ⬚F) for 90 min.
Preparation: ammonium bifluoride tint etch for 60 s, and
four-step edge-retention process ending with 1 h on vibra-
tory polisher with a non-nap polyester cloth and alumina.
See also Fig. 64 in the article “Selected Color Images” in
this Volume for color version.
be determined by making 10 g Knoop indents
since the heat-damaged layer will be softer than
the base material but would be harder in an alpha
case area. Unlike heat damage from straight ther-
mal exposure (which results in a harder surface),
heat damage from mechanical sources during
preparation results in a softer surface. In the ex-
ample of Fig. 62, the layer is softer from heat
damage, yielding a larger indent. Another ex-
Fig. 50 Alpha case in Ti-10V-2Fe-3Al after exposure to
790 ⬚C (1450 ⬚F) for 2 h. Preparation: Oxalic
tint etch for 60 s, and four-step edge-retention process end-
ing with 1 h on vibratory polisher with a non-nap polyester
cloth and alumina
Fig. 49 Alpha case in Ti-SP 700 after exposure to 760
⬚C (1400 ⬚F) for 90 min. Preparation: ammo-
nium bifluoride tint etch for 60 s, and four-step edge-reten-
tion process ending with 1 h on vibratory polisher with a
non-nap polyester cloth and alumina
ample is shown in Fig. 63 of a heat-affected zone
from a molten fine, which had a 50% knockdown
factor on fatigue life.
Figures 64 and 65 show heat damage from a
lab-induced lightening strike. Note the compro-
mise in etching time in Fig. 64, where the heat-
affected zone is underetched, while the base ma-
terial is overetched. Figure 65 shows the effects
of intraply arcing and heat-affected zone from a
lab-induced lightning strike.
Other Techniques
Several metallographic techniques have been
developed for specific purposes, including re-
crystallization studies and microstructure/frac-
ture topography correlations. Decoration aging
Fig. 51 Ti-8Al (with 1800 ppm O2) sheet aged to pre-
cipitate the ordered alpha-2 (Ti3Al) phase. The
dark-field transmission electron micrograph illustrates ␣2
precipitates (light) in an alpha matrix. 105,600⳯. Courtesy
of J.C. Williams
914 / Metallography and Microstructures of Nonferrous Alloys

Fig. 52 Ti-8.5Mo-0.5Si water quenched from 1000 ⬚C (1830 ⬚F). Thin-foil transmission electron micrograph illustrating
heavily twinned athermal ␣⬙ martensite. 5000⳯. Courtesy of J.C. Williams

was developed to study the extent of recrystal-
lization in beta alloys. After recrystallization an-
nealing, the material is given a partial age at a
time and temperature appropriate for the alloy of
interest. The incompletely recrystallized grains
retain some dislocation substructure (stored en-
ergy) that accelerates the aging process, resulting
in a more rapidly aged grain. These grains then
etch darker than the recrystallized ones, making
it easy to identify the extent of recrystallization.
This effect is illustrated in Fig. 30.
Another technique utilizes deep macroetching
and thermal etching. The deformed specimen is
polished, then subjected to overetching to pro-
duce deep grooves at the deformed grain bound-
aries. Next, the specimen is subjected to the re-
crystallization cycle of interest in a hard vacuum
(10ⳮ6 torr), followed by oil quenching. The ma-
terial recrystallizes and thermal etching occurs,
which differentiates between different grains, be-
cause surface atoms evaporate or sublimate at
different rates on different crystallographic
planes. Different grains will have different crys-
tallographic planes at the exposed surface.
The original grain boundaries are observable
as ghost boundaries, due to the deep macroetch-
ing used previously. Therefore, the recrystallized
and original microstructures can be observed si-
multaneously. This permits studying not only the
recrystallized structure, but also the recrystalli-
zation nucleation sites. The ghost boundaries can
be removed by repolishing and chemically etch-
ing. This technique is illustrated in Fig. 66. Fig-
ure 66(a) demonstrates the as-deformed structure
that has been heavily etched. The specimen was
recrystallized at 925 ⬚C (1700 ⬚F) for 1 h in a
vacuum of 10ⳮ6 torr. Recrystallization in
vacuum caused thermal etching of the recrystal-
lized grains (Fig. 66b shows recrystallized struc-
ture). The prior unrecrystallized structure can
still be observed as ghost boundaries remaining
from the initial overetching.
Subgrain boundaries can be revealed using a
relatively simple technique. The specimen is
electropolished and viewed in the scanning elec-
tron microscope in the backscattered electron
mode. The contrast and delineation of subgrains
are due to differences in crystallographic orien-
tation. Electropolishing occurs at different rates
on different crystallographic planes, similar to
the thermal etching phenomenon.
Fig. 53 Ti-10V-2Fe-3Al, beta solution treated, water
quenched, and strained 5% at room tempera-
ture. This Nomarski interference micrograph illustrates de-
formation-induced ␣⬙ martensite in a beta matrix. No etch.
500⳯. Courtesy of J.E. Costa
Several techniques have been developed to
observe fracture topography and microstructure
simultaneously in the scanning electron micro-
scope using its large depth of field. A very sim-
ple method involves selective polishing and
etching of the fracture face. The fracture face and
machined surfaces are first masked with a suit-
able maskant, such as a stop-off lacquer, which
can be applied with a small paint brush. Selected
areas of the fracture face are left unmasked. The

Fig. 54 Ti-6Al-2Sn-4Zr-2Mo forgings, finish forged

starting at 970 ⬚C (1775 ⬚F), air cooled, ma-
chined to 13 mm (0.5 in.) diam test bars, reheated to 995
⬚C (1825 ⬚F), the beta transus, held for 1 h, and air cooled.
The microstructure is entirely ␣⬘. Etched with Kroll’s re-
agent (ASTM 192). 100⳯
Fig. 55 ␣⬘ martensite in Ti-6Al-4V. (a) Light micrograph of bar, held for 1 h at 955 ⬚C (1750 ⬚F), which is below the
beta transus, and water quenched. Equiaxed “primary” alpha grains (light) in a matrix of ␣⬘ (martensite). Etched
with 10 mL HF, 5 mL HNO3, 85 mL H2O. 250⳯. (b) Thin foil transmission electron micrograph of the same microstructure
as in (a), but at higher magnification. The large light grains are primary alpha; the darker region is acicular ␣⬘ martensite
in a beta matrix. 5880⳯. Courtesy of J.C. Williams
 Metallography and Microstructures of Titanium and Its Alloys / 915

Fig. 56 Fine, unresolved alpha precipitation in light micrograph of aged Ti-10V-2Fe-3Al alloy. The white phase is
primary alpha in an aged beta matrix, dark background. Slightly uncrossed polarized light, and a four-step
polishing ending up with 16 h on vibratory polisher 10% alumina slurry. Etched with Kroll’s reagent for 15 s (a) and 7 s
(b)
specimen is then electropolished, which will af-
fect only the unmasked areas, and etched. Study-
ing the interface between the polished and etched
Fig. 58 Structure from cold-rolled and aged foil of beta
alloy Ti-15V-3Cr-3Al-3Sn. Oxalic tint etch for
15 s, 1 h vibratory polisher, non-nap polyester cloth and
alumina. The white regions indicate there was no or a
lesser heat treat response (alpha precipitation).
Fig. 57 Structure from cold-rolled and aged foil of beta
alloy Ti-15V-3Cr-3Al-3Sn. Oxalic tint etch for
3 s, 1 h vibratory polisher, non-nap polyester cloth and
alumina
and the masked areas permits a correlation of
microstructural features and fractographic de-
tails, as shown in Fig. 67. This technique is use-
ful for correlating general microstructural de-
tails, but it may be difficult to pinpoint a specific
area to study. iron inclusion, as determined in Fig. 68(b) by
Precision sectioning techniques have also precision sectioning. The cleavage zone at point
been developed. The area of interest on the frac- C in Fig. 68(a) is due to the TiFe2 zone seen at
ture face, such as crack origin, is first located. point C in Fig. 68(b). Below the TiFe2, the struc-
The specimen is then cut on a plane perpendic- ture consists of transformed Widmanstätten al-
ular to the fracture face close to the area of in- pha. The section (Fig. 68b) was taken at line AB
terest. The distance from the cut face to the area in Fig. 68(a).
of interest is measured. Next, the specimen is
placed in a metallurgical mount, then ground and
polished the measured distance for metallurgical REFERENCES
analysis of the precise area of interest and cor-
1. G.F. Vander Voort, Metallography: Principles
relation of microstructure to fractographic fea-
and Practice, McGraw-Hill, 1984, reprinted
tures. An example of this technique is shown in
by ASM International, 1999
Fig. 68. The microstructure and fracture face can
2. Struers Metallographic Application Guide:
be observed simultaneously using the scanning
Titanium Alloys, Struers
electron microscope by carefully dissolving the
3. M.J. Donachie, Jr., Titanium: A Technical
mount material. This fatigue specimen had an
Guide, 2nd ed., ASM International, 2000
internal origin at point A, which initiated at an

Fig. 59 A titanium-iron binary alloy, beta solution
treated, water quenched, and aged to form x.
The x is the light precipitate in this thin-foil transmission
electron micrograph. In alloys where the x has a high lat-
tice misfit, the x is cuboidal to minimize elastic strain in
the matrix. 320,000⳯. Courtesy of J.C. Williams
Fig. 60 Ti-40Nb (at.%), beta solution heat treated at
900 ⬚C (1650 ⬚F), water quenched, then aged
at 400 ⬚C (750 ⬚F) for 24 h. The dark precipitate is b⬘ (solute
lean beta phase) in a solute-enriched beta matrix. Thin-foil
transmission electron micrograph. 31,000⳯. Courtesy of
J.C. Williams
Fig. 61 Ammonium bifluoride tint etch for 10 s. Com-
mercially pure titanium sheet. Four-step polish-
ing ending up with 16 h on vibratory polisher, 10% alumina
slurry
916 / Metallography and Microstructures of Nonferrous Alloys

Fig. 64 Oxalic tint etch for 15 s. Ti-15V-3Cr-3Al-3Sn

foil heat-affected zone. This is from a lab-in-
duced lightning strike. Note the compromise in etching
time. The heat-affected zone is underetched and the base
material is overetched. 1 h vibratory polisher, non-nap
polyester cloth and alumina

Fig. 62 Ti-6Al-4V heat damage. Oxalic tint etch for 15 s. Four-step edge retention process ending up with 1 h on a
vibratory polisher and alumina

Fig. 65 Hybrid Ti-6Al-4V carbon-reinforced polymer

composite with arcing and heat damage from
a lab-induced lightning strike. Note the heat-affected zone.
The vertical line shows the original surface of the titanium
fastener and the extent of intraply arcing. Because of its
complex shape, the specimen was vacuum impregnated
with hydrated rhodamine-dyed two-part epoxy after sec-
tioning on a wafering saw. This sample was prepared with
a five-step edge retention process; 220 grit, 9 lm, 3 lm
Fig. 63 Ti-6Al-4V plate fatigue specimen with molten fine and heat-affected zone 1 h vibratory polisher with non- silk, 3 lm non-nap polyester and ending up with 1 h on a
nap polyester cloth and alumina vibratory polisher with a non-nap polyester cloth and 10%
alumina solution.
 Metallography and Microstructures of Titanium and Its Alloys / 917

Fig. 67 Scanning electron micrograph (SEM) image

Fig. 66 Ti-10V-2Fe-3Al deformed at 1150 ⬚C (2100 ⬚F).
(a) Etched with 60 mL H2O, 40 mL HNO3, 10
mL HF for 30 min. (b) Etched with 60 mL H2O, 40 mL
HNO3, 10 mL HF for 30 min Ⳮ thermally etched at 925
⬚C (1700 ⬚F) for 1 h in vacuum (10ⳮ6 torr). Magnification
not given. Courtesy of D. Eylon
from Ti-6Al-4V beta-annealed fatigued plate
specimen. (a) SEM at the polished and etched/unetched
fracture topography interface showing microstructure/frac-
ture topography correlation. Secondary cracks are a result
of intense slip bands. (b) SEM that illustrates “furrows” or
“troughs” that are defined by the lamellar alpha plates.
These furrows link up as the crack progresses. Kroll’s re-
agent. 2000⳯. Courtesy of R. Boyer
Fig. 68 Ti-6Al-4V powder metallurgy compact, hot
isostatically pressed at 925 ⬚C (1700 ⬚F), 103
MPa (15 ksi), for 2 h. (a) Scanning electron micrograph. No
etch. 80⳯. (b) Optical micrograph. Etchant: Kroll’s reagent.
16⳯. Courtesy of D. Eylon

Fig. 58 Ti-6Al-4V alloy with Widmanstätten alpha in a
beta matrix after furnace cooling from above
the transus. Beta-anneal temperature was 1040 ⬚C (1900
⬚F). Samples were etched with the oxalic tinting reagent for
15 s after polishing by (a) the four-step method for optimiz-
ing removal of deformed material, (b) the four-step method
for optimizing edge retention, or (c) the three-step semi-
automated method for optimizing preparation time (note
the lack of detail in the dark regions). See text for descrip-
tion of polishing procedures. Color version of Fig. 7 in the
article “Metallography and Microstructures of Titanium and
Its Alloys”
Color Micrographs of Titanium Alloys / 543
Fig. 59 Coarse lamellar alpha revealed by different
etches in Ti-6Al-4V structure after beta anneal
at 1040 ⬚C (1900 ⬚F) and furnace cooling. Preparation was
four-step polishing, with final polish of 16 h on vibratory
polisher and 10% alumina slurry. Slightly uncrossed polar-
ized light illumination for all three etches. (a) Ammonium
bifluoride tint etch, 60 s. (b) Kroll’s reagent, 15 s. (c) Oxalic
tint etch, 60 s. Color version of Fig. 9 in the article “Met-
allography and Microstructures of Titanium and Its Alloys”
Fig. 60 Ti-6Al-4V die forging, mill-annealed. (a) Am-
monium bifluoride tint etch, 60 s. Slightly un-
crossed polarized light illumination. (b) Kroll’s reagent, 15
s. Slightly uncrossed polarized light illumination. (c) Oxalic
tint etch, 15 s. Slightly uncrossed polarized light illumina-
tion. Color version of Fig. 11 in the article “Metallography
and Microstructures of Titanium and Its Alloys”
544 / Color Micrographs of Titanium Alloys

Fig. 61 Variation in appearance with changes in illumination of a Ti-6Al-4V specimen with oxalic tint etch (15 s).
Material was beta annealed at 1050 ⬚C (1925 ⬚F) and furnace cooled. (a) Illuminated and examined with
slightly uncrossed (45–129) polarized light. (b) Illuminated and examined with slightly uncrossed (45–139) polarized light.
(c) Plane-polarized light illumination. (d) Bright-field illumination. Color version of Fig. 28 in the article “Metallography
and Microstructures of Titanium and Its Alloys”

Fig. 62 Alpha case in Ti-6Al-4V after exposure to 760
⬚C (1400 ⬚F) for 90 min. Preparation: oxalic tint
etch for 60 s, and four-step edge-retention process, ending
with 1 h on vibratory polisher with a non-nap polyester
cloth and alumina. Color version of Fig. 46 in the article
“Metallography and Microstructures of Titanium and Its Al-
loys”
Fig. 63 Alpha case in Ti-6Al-4V after exposure to 885
⬚C (1625 ⬚F) for 90 min. Preparation: ammo-
nium bifluoride tint etch for 60 s and four-step edge-reten-
tion process, ending with 1 h on vibratory polisher with a
non-nap polyester cloth and alumina. Color version of Fig.
47 in the article “Metallography and Microstructures of Ti-
tanium and Its Alloys”
Fig. 64 Alpha case in Ti-SP 700 (Ti-4.5Al-3V-2Mo-2Fe)
after exposure to 900 ⬚C (1650 ⬚F) for 90 min.
Preparation: ammonium bifluoride tint etch for 60 s and
four-step edge-retention process, ending with 1 h on vibra-
tory polisher with a nonnap polyester cloth and alumina.
Color version of Fig. 48 in the article “Metallography and
Microstructures of Titanium and Its Alloys”