Effect of Hot-Isostatic-Pressing Parameters

on the Microstructure and Properties of Powder

Ti-6Al-4V Hot-Isostatically-Pressed Samples
K. ZHANG, J. MEI, N. WAIN, and X. WU

Ti-6Al-4V powders have been hot-isostatically-pressed (‘‘HIPped’’) using a range of

hot-isostatic-pressing (‘‘HIPping’’) conditions, and the effects on microstructure and mechanical
properties have been assessed. The properties were measured on test samples machined from
HIPped powder billets and on samples that contained the as-HIPped surface. The fatigue limit
of samples that contained the as-HIPped surface was improved by using a new HIPping pro-
cedure. The machined samples that had been HIPped at 1203 K (930
C) exhibited a better
balance of properties than those HIPped at 1153 K (880
C) or 1293 K (1020
C). The fine
microstructure, formed from the martensitic structure of the atomized powder, coarsens with
the increase of temperature or time during HIPping. These changes have been correlated with
the corresponding changes in properties and with the fracture surfaces. The significance of these
observations, especially the fatigue properties of samples that contain the as-HIPped surface, is
discussed in terms of the properties of net-shape HIPped components.

DOI: 10.1007/s11661-009-0149-y
 The Minerals, Metals & Materials Society and ASM International 2010

I. INTRODUCTION The surface finish is known to be the major factor that

NET-SHAPE hot-isostatic-pressing (‘‘HIPping’’) is
becoming an accepted technology for the manufacture
of a range of engineering components.[1–4] The potential
economic advantages of net-shape HIPping of powder
to produce complex-shaped and fully dense components
from titanium and nickel-based alloys[5–7] and other
expensive metal powders have been investigated. In this
process, a containing capsule, together with internal
tooling, is filled with powder; the geometry of the
capsule and tooling is defined via computer modeling of
the shrinkage of the powder compact during the
densification process occurring during HIPping. The
capsule is pumped to backing pump pressure and sealed
vacuum tight, prior to HIPping under defined condi-
tions. The tooling and capsule (commonly of mild steel)
are then removed by machining or pickling.[7] Net-shape
HIPping can be used with titanium-based materials to
obtain cost reduction by reducing the amount of difficult
titanium machining and the large amount of material
loss.[8] It is essential that the factors that influence the
properties of such components are understood and that
the HIPping process parameters are optimized accord-
ing to specific application requirements.
K. ZHANG, formerly Research Fellow, with the IRC in Materials,
The University of Birmingham, is Metallurgist, with Intertek Derby,
ELT14 Rolls Royce, Elton Road, Derby, Derbyshire, DE24 8BJ,
United Kingdom. J. MEI and N. WAIN, Research Fellows, and
X. WU, Professor, are with the IRC in Materials, The University of
Birmingham, Edgbaston B15 2TT, United Kingdom. Contact e-mail:
x.wu.1@bham.ac.uk
Manuscript submitted August 20, 2009.
Article published online February 25, 2010
influences the fatigue properties of a component, and
net-shape hot-isostatically-pressed (‘‘HIPped’’) products
are designed to retain much of the as-HIPped surface.
Thus, the influence of the ‘‘as-HIPped surface’’ on the
fatigue properties of a component produced using net-
shape HIPping is an important aspect of the work
reported here. The term as-HIPped surface is used to
describe the final surface of the component after
HIPping after the tooling has been removed. This
surface is in direct contact with the mild steel tooling
during HIPping, and the as-HIPped surface is generated
after HIPping by acid etching to remove the tooling.
The overall aim of the work reported in this article is
to study the effect of HIPping variables (HIPping
temperature and HIPping procedure) on microstructure,
surface finish, and mechanical properties (tensile,
fatigue, and fracture toughness) of HIPped Ti-6Al-4V
powder; the main interest is the properties of samples
that contain the ‘‘as-HIPped’’ surface. There is a wealth
of data on properties of conventionally processed
samples (e.g., References 9 through 13) with which
these data can be compared. In earlier work, it was
shown, using conventional HIPping, that the surface
roughness downgraded the fatigue properties of
as-HIPped samples.[14] Thus, during conventional
HIPping, when the temperature and pressure are ramped
up in phase, the steel yields so that a rough surface on the
scale of the powder particles is generated. This rough-
ness is caused by the penetration of the powder particles
into the mild steel tooling, which occurs because the
steel has a lower yield stress at low temperatures than
does Ti-6Al-4V. As part of the current study, a new
HIPping procedure is used, which eliminates this surface
roughness and thus improves the fatigue properties.

METALLURGICAL AND MATERIALS TRANSACTIONS A VOLUME 41A, APRIL 2010—1033

 II. EXPERIMENTAL METHODS
AND MATERIALS
The Ti-6Al-4V powder in the size range of 50 to
400 lm used in this work was produced by StarMet
(Concord, MA), using the plasma rotating electrode
process (PREP). The as-received powder was generally
HIPped at 100 MPa for 4 hours at a preselected tem-
perature using a fixed heating rate of 5 K/min (5
C/min).
Chemical analyses of HIPped samples were carried out
by Incotest (Hereford, UK), and the analysis of the
samples for which the data are reported in this article is
shown in Table I. Measurements of the beta transus
showed that it was about 1293 K (1020
C), as expected
for Ti-6Al-4V of this composition; the calculated transus
is 1285 K (1012
C) (S. Fox, stephen.fox@timet.com,
private communication). In one HIPped sample, the
O content was found to be 2300 ppm rather than between
1700 and 2000 ppm, as found in all other samples.
The HIP cans, which were made from A1018 mild
steel with a surface finish of 1.6 lm, were typically
45 mm in diameter and 140-mm long, which allowed
tensile and fatigue samples to be machined from the
same HIPped sample. The conventional HIP procedure
is to ramp temperature and pressure in phase, taking
about 3 hours to reach the selected HIP temperature,
after which it is held, usually for 4 hours, before cooling
at about 5 K/min (5
C/min). Some samples were
HIPped using a different HIP procedure (U.K. Patent
Application 0807703) in order to improve the surface
finish of the as-HIPped samples. In this procedure, the
capsule with powder is heated to the HIPping temper-
ature, again taking about 3 hours, before the pressure is
increased. The basis of this patent is illustrated by the
compression tests illustrated in Figure 1. These tests
were carried out at the temperatures indicated on
samples of powder Ti64, which had been previously
HIPped at those temperatures. In addition, samples of
fully HIPped Ti64 and of the mild steel used as canning
material were tested at these temperatures. The data
show that the tooling is stronger than the partially
HIPped Ti-6Al-4V HIPped and tested below about
973 K (700
C). At these low temperatures, HIPping
results in samples that are only about 70 pct of full
density, as indicated on the curve for the Ti64 powder.
Between about 973 K (700
C) and 1123 K (850
C), as
consolidation progresses to between 80 and 90 pct full
density, the partially HIPped Ti64 is stronger. At higher
temperatures, the steel is stronger and in fact, at 1203 K
(930
C), the standard HIP temperature, it is about
twice as strong as the Ti64 even though the Ti64 HIPped
at this temperature is now >99.5 pct density. At this
temperature, the 0.2 pct proof stresses of the two
samples of Ti64 are identical, as would be expected
since prior to testing these samples had both been
Table I. Chemical Composition (Weight Percent) of Ti-6Al-4V Powder HIPped at 1203 K (930 °C)
Alloy O C H N
HIPped Ti-6Al-4V 0.20 0.034 0.0039
1034—VOLUME 41A, APRIL 2010
HIPped at 1203 K (930
C). Thus, using the new
procedure, the powder particles are flattened by, rather
than penetrating, the tooling, as occurs when the
temperature and pressure are increased in phase.[14]
With this technique, it takes about 2 hours to reach the
selected pressure, during which time the samples are at
the HIPping temperature. The samples are then held for
a further 3 hours at the HIPping temperature, under the
HIPping pressure, and subsequently cooled down. The
powder is thus held at the HIPping temperature for
5 hours, i.e., for 1 hour longer using the new procedure
than during a conventional HIPping cycle.
Some samples were partially HIPped, by reducing the
HIP temperature to 1123 K (850
C) and cooling the
sample as soon as it had reached 1123 K (850
C).
In this case, the temperature and pressure were ramped
in phase. These experiments were carried out so that the
microstructural and morphological changes that occur
during HIPping could be followed at the early stages of
consolidation. These observations were compared both
with conventionally HIPped samples and with observa-
tions made on individual powder particles that were
simply heated to the HIPping temperature and held
there for 2 hours, without the application of pressure.
Three cylindrical M8 tensile samples were machined
from HIPped compacts for each HIP condition in order
Fig. 1—Graph showing the temperature dependence during HIPping
of the 0.2 pct proof stress of powder Ti64, together with the flow
stress of the mild steel tooling and of fully HIPped Ti64. The macro-
scopic density of the partially HIPped powder is seen to increase
from about 70 pct full density at 873 K (600
C) to >99.9 pct at
temperatures above 1173 K (900
C), which results in an initial in-
crease in proof stress, followed by the expected decrease at high tem-
peratures. Note that the individual partially HIPped samples are
tested at the temperature at which they have been HIPped.
Fe Al V Ti
0.006 0.17 6.42 3.88 balance
METALLURGICAL AND MATERIALS TRANSACTIONS A
to assess the tensile properties of HIPped samples (i.e.,
of samples from which the as-HIPped surface had been
removed). One sample, which was HIPped using the new
HIP procedure and which contained the as-HIPped
surface, was tested in tension. The complex method
required to manufacture such a sample has been
described earlier.[14] In this method, the gage length of
the sample was produced to net shape but the rest was
produced to near net shape, at successively increasing
diameters (in a series of steps). Final machining was
done on the near net-shape sections to produce the
conventionally tapered section and threaded ends of the
tensile sample. This method was used because it is very
difficult to produce the tapered geometry of a tensile
sample directly by HIPping, but it is straightforward to
produce to net shape the parallel-sided cylindrical gage
length and the stepped contour at either end.
To investigate the influence of the as-HIPped surface
on the fatigue properties, flat HIPped plates 120 mm in
length, 60 mm in width, and 10 mm in thickness were
cut by EDM along their length, after removing the mild
steel can by acid pickling in 20 pct nitric acid. The EDM
cut surfaces were final machined by reciprocating
surface grinding (RSG) to generate the side surfaces of
the samples, and the original plate surfaces, which had
been in contact with the mild steel can during HIPping,
became the top and bottom surfaces of the test pieces.
Some of these specimens with as-HIPped surfaces were
electropolished (using 60 vol pct Methanol, 35 vol pct
1-Butanol, and 5 vol pct HClO4, at a temperature of
238 K (–35
C) and a current of 0.8 to 1 A) for 15 to
20 minutes so that fatigue data could be obtained for the
bulk sample without any influence of surface machining.
Compact tension specimens were machined from
HIPped bars to conduct fracture toughness tests accord-
ing to the relevant British Standard.[15]
Tensile tests were carried out using a Zwick
(Leominster, UK) testing machine at an initial strain
rate of 10 3 s 1 in air at room temperature. Three
specimens were used for each HIPping condition in
order to obtain some indication of the repeatability of
the properties. Four-point bending fatigue tests were
carried out using an Amsler Vibrophore electromagnetic
resonance testing machine for fatigue life evaluation.
Typically, ten specimens were used to determine the
fatigue limit. Tests were conducted at room tempera-
ture, at a stress ratio R of 0.1 and a frequency of ~95 Hz.
A stress that corresponded to a life beyond 1.0 9 107
cycles was defined as the fatigue limit, i.e., the runout of
the specimen.
For fracture toughness testing, specimens were
precracked at room temperature, using an Amsler
Vibrophore (Stratford upon Avon, UK) testing
machine, via fatigue to give starter crack lengths within
the range set out in the standard. The maximum applied
loads during precracking were reduced from 8 to 2 kN
during cycling; the stress ratio was 0.1 and the frequency
was 60 to 70 Hz. The final fracture toughness testing
was carried out on a servohydraulic testing machine
manufactured by ESH Ltd (Telford, Shropshire, UK)
with a ramp rate of 0.5 mm/min to obtain load vs crack
opening displacement curves.
METALLURGICAL AND MATERIALS TRANSACTIONS A
A JEOL* 7000 scanning electron microscope (SEM)
*JEOL is a trademark of Japan Electron Optics Ltd., Tokyo.
was used to examine the powder particles’ morphology
and cross sections and the solid specimens’ cross
sections. The fracture surfaces of failed tensile and
fatigue samples were examined using a PHILIPS**
**PHILIPS is a trademark of FEI Company, Hillsboro, OR.
XL30 SEM or JEOL 6060 SEM. The Inca (Oxford
Instruments, Abingdon, Oxfordshire, UK) electron
backscattered diffraction (EBSD) system was an integral
part of the JEOL 7000 SEM, which was used to provide
information about the crystallographic orientation in
original powders and in HIPped samples. The operating
parameters were as follows: specimen tilt angle of
70 deg, accelerating voltage of 20 kV, and working
distance of 12 to 16 mm. The step size for the mapping
was 0.4 lm, the pixel area was 0.05 lm2, and the low-
angle boundaries (<5 deg) were not counted.
Hardness tests using a Vickers hardness with a 20-kg
load were carried out on the as-HIPped surface and on
cross sections of HIPped samples. In addition, taper
sections were prepared from HIPped samples so that the
rate of change of hardness with distance from the
as-HIPped surface could be assessed. The taper sections
were spark machined from the as-HIPped sample and
were lightly hand polished to 1200 grit. These polished
taper sections were examined using the JEOL 7000 SEM
to assess the microstructure and to determine if any
significant changes in composition were detectable as a
function of distance from the as-HIPped surface.
III. RESULTS
X-ray diffraction patterns show that the powder is
martensitic, as would be expected from the rapid cooling
rates associated with the production of PREP
powder,[16,17] between about 103 and 104 K s 1 (103 and
104
C s 1). The spherical morphology of the as-received
powder is shown in Figures 2(a) and (b). Cross sections
of these powder particles (e.g., Figure 2(c)) confirm that
they are composed entirely of martensitic alpha-prime
phase. The powders are mostly polycrystalline, as seen
in Figure 2(d).
A. Effect of HIPing Temperature on Microstructure
and Mechanical Properties
1. Microstructure of samples HIPped using different
temperatures
The effect of HIPping temperature was investigated
using a range of temperatures, and Figure 3 shows the
microstructure and EBSD maps of samples HIPped at
1153 K (880
C), 1203 K (930
C), 1293 K (1020
C),
and 1313 K (1040
C). These conventionally HIPped
samples were found to be fully dense, as judged by the
VOLUME 41A, APRIL 2010—1035
Fig. 2—(a) and (b) SEM SE micrographs showing the morphology of as-received PREP Ti-6Al-4V powders; (c) SEM BSE micrograph of cross
section of the powder showing martensitic alpha-prime phase; and (d) EBSD map showing orientations of the martensite laths.
absence of any visible porosity in conventional SEM
images, and in the case of samples HIPped at 1203 K
(930
C), tomography showed that the porosity was less
than 0.02 pct. The as-HIPped microstructures, obtained
for samples HIPped below the transus, are composed of
equiaxed grains, which appear to have formed both at
the former powder particle boundaries and at grain
boundaries inside the powders, together with a mainly
lathlike structure in the central part of the original
particles. The sample HIPped above the transus at
1313 K (1040
C) shows a beta-transformed microstruc-
ture, with alpha formation strongly influenced by the
beta boundaries, as would be expected.[18,19] This
microstructure is obviously very different from those
of samples HIPped below the transus
In order to understand the as-HIPped microstructure,
powders were either heat treated at a selected subtransus
HIPping temperature (with no pressure applied) or were
1036—VOLUME 41A, APRIL 2010
only partially HIPped. In Figure 4(a), taken from a
powder particle heat treated at 1203 K (930
C) for
2 hours, it is clear that the martensitic structure of the
original powder particle has transformed to alpha and
beta, effectively on the same scale as the original alpha
prime martensite. No equiaxed grains are obvious at the
prior particle surface, although some may be present
within the original powder particle. In contrast, in the
partially HIPped samples shown in Figures 4(b) and (c),
the development of equaixed microstructure is obvious
where particles are in contact. Hence, it is suggested that
the equiaxed phases in fully HIPped samples (Figure 3)
are formed at prior particle boundaries (PPBs) during
HIPping, because sufficient deformation occurs locally
to cause recystallization. The limited amount of equi-
axed grains formed within particles are formed at prior
beta boundaries, perhaps because diffusion is faster in
these regions than within grains.
METALLURGICAL AND MATERIALS TRANSACTIONS A
Fig. 3—SEM BSE micrographs in which the dark phase is a and EBSD map of Ti-6Al-4V samples HIPped at (a) and (b) 1153 K (880
C),
(c) and (d) 1203 K (930
C), (e) and (f) 1293 K (1020
C), and (g) BSE micrograph of sample HIPped at 1313 K (1040
C) showing
(transformed microstructure. (h) EBSD map of b phase of sample HIPped at 1293 K (1020
C) (cf. (f)).

The microstructures simply coarsen as the tempera- very close to the b transus, the microstructure coarsened
ture is increased below the b transus. When the HIPping significantly, as shown in Figures 3(e) and (f), but still
temperature was increased to 1293 K (1020
C), i.e., retained the same microstructural features of laths and

METALLURGICAL AND MATERIALS TRANSACTIONS A VOLUME 41A, APRIL 2010—1037

Fig. 3—Continued.
equiaxed grains. When the sample was HIPped at
1313 K (1040
C), a b transformed microstructure was
obtained, as shown in Figure 3(g).
It should be noted that these EBSD maps in Figure 3
and elsewhere show the orientation of the alpha phase
and the limited volume of beta appears as unindexed
volumes. An example of a beta EBSD is shown in
Figure 3(h), where it is clear that the volume fraction of
the beta is small. These regions will be ignored in the
following description of the microstructure.
2. Tensile properties and examination of fracture
surfaces
A summary of the tensile data obtained from the
HIPped samples is given in Table II. Samples HIPped at
1153 K (880
C) had the highest 0.2 pct proof stress and
a relatively low elongation of about 10 pct. Samples
HIPped at 1293 K (1020
C) were shown to have the
lowest proof stress and tensile strength, and an elonga-
tion similar to that of samples HIPped at 1153 K
(880
C). The samples HIPped at 1203 K (930
C) had
proof stresses intermediate between those of samples
HIPped at 1153 K (880
C) and 1293 K (1020
C) but
had the largest elongation up to 21 pct.
Fracture surfaces of the tensile specimens were
examined, as shown in Figure 5. Figure 5(a) shows the
fracture surface of a specimen HIPped at 1153 K
(880
C), where groups of transgranular facets can be
seen. The crack appears to have propagated along a PPB
(indicated by the arrow in Figure 5(a)). There were no
obvious crack initiation sites in samples HIPped at
1203 K (930
C); a typical ductile fracture surface can
be seen in Figure 5(b). In the specimens HIPped at
1293 K (1020
C), cracking was characterized by flat
transgranular facets (Figure 5(c)), which were on the
scale of the coarser lamellar colonies in this sample
(Figures 3(e) and (f)).
The tensile properties of a sample that contained the
as-HIPped surface made using the new HIPping proce-
dure were also measured, and it was found that the
1038—VOLUME 41A, APRIL 2010
0.2 pct proof stress was slightly higher (900 MPa) than
that found for a similarly HIPped sample (886 MPa),
which had the HIPped surface machined off, and the
elongation was further reduced from 12 pct to about 8 pct.
3. Fatigue properties and observations of fracture
surfaces of fatigued samples machined from HIPped bars
Figure 6 shows a plot of stress amplitude vs number of
cycles to failure (SN curve) for the samples machined
from bars HIPped at different temperatures. The samples
HIPped at 1203 K (930
C) exhibited the highest fatigue
limit of 500 MPa (at 1.5 9 107 cycles). The fatigue limit
of specimens HIPped at 1153 K (880
C) was 400 MPa,
whereas for samples HIPped at 1293 K (1020
C), the
fatigue limit was decreased further to 300 MPa.
The SEM micrographs of fracture surfaces near crack
initiation sites are shown in Figure 7. It can be seen that
fatigue cracks originated from the surface in all speci-
mens. In the fractured surfaces, river patterns could be
seen. The main mode of fatigue failure of the samples is
transgranular. For samples HIPped at 1153 K (880
C)
and 1203 K (930
C), groups of transgranular facets
can be identified as the fatigue crack initiation sites
(Figures 7 (a) and (b)). This form of faceting is also
typical of the early stages of fatigue fractures in wrought
forms of Ti-6Al-4V, in other a/b alloys, and in near a
titanium alloys in general.[20]
For samples HIPped at 1293 K (1020
C), large facets
are seen, as shown in Figure 7(c). These large facets can
be formed[21] when the crack extends through a packet
of aligned alpha laths (indicated by the arrow) that have
similar orientations.
4. Fracture toughness of HIPped samples
Room-temperature fracture toughness testing was
conducted to further assess the properties of powder
Ti-6Al-4V samples HIPped at 1203 K (930
C) and
1293 K (1020
C). Values of fracture toughness are
shown in Table III, which shows that there is no
significant difference.
METALLURGICAL AND MATERIALS TRANSACTIONS A
Fig. 4—SEM BSE images of PREP powder of Ti-6Al-4V showing (a) an isolated powder particle that has been held for 2 h at 1203 K (930
C)
under ambient pressure (no equaixed region is obvious) and (b) and (c) partially HIPped samples where the development of equiaxed structure at
PPBs is apparent (as indicated by the arrow).

Table II. Room-Temperature Tensile Properties for Powder Ti-6Al-4V HIPped at Different Temperatures; Results Shown are for
the Three Samples Which Were Tested for Each Condition; Typical Data for Forged Samples are Also Shown as a Comparison

Processing Conditions 0.2 Pct Proof Stress (MPa) UTS (MPa) Elongation (Pct)
HIPping at 1153 K (880
C)/100 MPa/4 h 925, 927, 931 989, 994, 998 9, 10,11
HIPping at 1203 K (930
C)/100 MPa/4 h 899, 901 904 970, 971, 972 18, 19, 21
HIPping at 1293 K (1020
C)/100 MPa/4 h 836, 839, 840 913, 913, 913 10, 11, 12
Sample forged at 1193 K (920
C) to 1213 K (940
C)[19] 875 965 15

The best balance of properties (tensile, fatigue, and
fracture toughness) was obtained for samples HIPped at
1203 K (930
C), and this temperature was therefore
chosen as the HIPping temperature for subsequent tests
where the effects of surface finish and of the influence
of the as-HIPped surface on fatigue properties were
investigated.
B. Effect of HIP Schedule and of Post HIP Surface
Treatments on Mechanical Properties
1. Nature of as-HIPped surfaces
Figure 8 shows secondary electron micrographs of
cross sections of HIPped Ti-6Al-4V surfaces. It is clear
that the as-HIPped surface, made using the conventional

METALLURGICAL AND MATERIALS TRANSACTIONS A VOLUME 41A, APRIL 2010—1039

Fig. 5—SEM SE micrographs showing the fracture surfaces of tensile failed samples HIPped at (a) 1153 K (880
C) (crack propagating along a
PPB is indicated by the arrow), (b) 1203 K (930
C), and (c) 1293 K (1020
C).
Fig. 6—SN fatigue curves for powder Ti-6Al-4V samples with
machined surface HIPped at different temperatures showing that the
fatigue limit of samples HIPped at 1203 K (930
C) was higher
than those obtained at 1153 K (880
C) and 1293 K (1020
C). The
arrows indicate that the tests were interrupted without the failure of
the samples.
procedure (Figure 8(a)), is quite rough with the rough-
ness being on the scale of the original powder particle
size.[14] A much smoother surface is obtained using the
new procedure, as shown in Figure 8(b).
Figure 9(a) compares the surface and interior hard-
ness of a sample HIPped using the new procedure and
also shows the rate of change of hardness from the
as-HIPped surface measured on taper sections cut at an
angle of 2.5 deg. It is clear that there is a small, but
significant hardness difference between the as-HIPped
1040—VOLUME 41A, APRIL 2010
surface and the interior and that the hardness change
extends to a depth of about 200 lm into the sample, as
indicated in Figure 8(a). The WDX analysis showed
(Figure 9(b)) the rate of change of C count measured on
taper sections, which follows the hardness change.
Metallographic examination and image analysis of the
taper sections showed a small increase in alpha content
at the surface of the as-HIPped sample, as shown in
Figure 9(c).
2. Influence of HIPping procedure on the tensile
properties of HIPped samples
Test samples, which were machined from HIPped
billets made using the new HIPping procedure, had a
proof stress of 886 MPa and an elongation of 12 pct.
These properties are somewhat lower than those
obtained using the conventional HIPping process shown
in Table II (yield of 901 MPa and elongation of 19 pct)
and are associated with the slight coarsening of the
microstructure caused by the longer time at the HIP
temperature (compare Figures 8(c) and (d)) even though
oxygen content of this HIPped sample (2300 ppm) is
higher. The fracture surfaces of failed tensile sample
HIPped at 1203 K (930
C) using the new procedure
show transgranular facets formed by clusters of lamellae
with similar orientations around the crack initiation site
(Figure 10). The properties lie between those of samples
conventionally HIPped at 1203 K (930
C) and 1293 K
METALLURGICAL AND MATERIALS TRANSACTIONS A
Fig. 7—Secondary electron SEM micrographs of fracture surfaces of fatigue failed samples HIPped at (a) 1153 K (880
C), (b) 1203 K (930
C),
and (c) 1293 K (1020
C). The fatigue failure of the samples is associated with transgranular facets.
Table III. Room-Temperature Fracture Toughness Values
Obtained from Powder Ti-6Al-4V Samples HIPped
at Different Temperatures
Fracture
Toughness,
Specimen KQ (MPaÆm)
HIPped Ti-6Al-4V at 1203 K (930
C) 71/74/76/77
HIPped Ti-6Al-4V at 1293 K (1020
C) 77/80
(1020
C), as would be expected from the microstructure
that is intermediate between these.
3. Influence of surface finish on the fatigue strength
of HIPped samples
Four sets of samples with different surface finishes
were produced to assess the influence on the fatigue
properties for samples HIPped at 1203 K (930
C). The
first three types of sample were made using the conven-
tional HIPping procedure and were samples (a) with the
as-HIPped surface; (b) HIPped and electropolished, as
described in the experimental section; (c) HIPped and
machined by RSG; and (d) containing the as-HIPped
surface made using the new HIPping cycle. Table IV
shows the surface roughness of the four surface condi-
tions. It is obvious that the as-HIPped surface made
using the conventional HIPping procedure had the
METALLURGICAL AND MATERIALS TRANSACTIONS A
highest roughness with Ra = 9.1 lm, as noted
earlier,[14] and the machined surface had the lowest with
Ra = 0.4 lm. The roughness values of the electropo-
lished surface and of the as-HIPped surface made using
the new HIPping procedure were between these two
extremes.
The SN curves for HIPped Ti-6Al-4Vsamples with the
four different surface finishes are shown in Figure 11.
Samples with as-HIPped surfaces made using the new
HIPping procedure had the highest fatigue limit
(at N > 107 cycles) of 620 MPa. The fatigue limit
of samples with as-HIPped surfaces made using the
conventional HIPping procedure[14] was confirmed as
much lower, at 350 MPa. Conventionally HIPped
samples that were machined or electropolished after
HIPping have fatigue limits between these two.
The fracture surfaces of samples failed in fatigue were
examined to investigate the crack initiation characteris-
tics and the crack initiation; all are associated with
transgranular facets consisting of a cluster of a and b
laths with a similar orientation, as seen in Figure 7(b).
IV. DISCUSSION
There are two aspects of the experimental results
obtained in this work on HIPping of Ti-6Al-4V, which
will be the main focus of this discussion. These aspects
VOLUME 41A, APRIL 2010—1041
Fig. 8—Secondary electron SEM images of cross sections of HIPped Ti-6Al-4V surface: (a) rough surface obtained using conventional HIPping
procedure and (b) smooth surface obtained using the new HIPping procedure. SEM BSE images of PREP powder of Ti-6Al-4V HIPped using
(c) the conventional procedure and (d) the new procedure showing coarser microstructure in the HIPped sample.
are (1) the influence of the nature of the surface on the
fatigue and tensile properties of samples and (2) the
influence of HIPping temperature and HIPping proce-
dure on the tensile and fatigue properties of HIPped
samples where any influence of the HIPped surface is
removed by machining samples from larger HIPped
samples. These two aspects are discussed, in turn, before
discussing the factors that influence the microstructure
of the HIPped samples.
A. Influence of the Nature of the Surface of As-HIPped
Samples on Fatigue and Tensile Properties
The fatigue response of samples HIPped using the
conventional HIPping schedule, and the response of
samples HIPped using the new procedure, which devel-
ops a smoother surface, show the importance of surface
finish on fatigue life, which is of course well docu-
mented. In the HCF regime, the total fatigue life
depends principally on fatigue crack initiation and early
growth behavior.[22] The sharp grooves formed by
powder particles on the conventional as-HIPped surface
serve as sites of stress concentration and promote crack
initiation, and the reproducibility of these data probably
reflects the fact that these stress concentrations are
present on every sample. Electropolishing removes
about 15 to 20 lm, and the sharp grooves were turned
1042—VOLUME 41A, APRIL 2010
into blunt undulations and, thus, result in a decrease in
the magnitude of the stress concentration. The machined
surface has a low roughness, but some surface damage
was produced during the machining process.
In the samples HIPped using the new procedure,
flatter surfaces are formed, because no longer do the
particles penetrate the steel to form sharp features. It
should be noted that the scatter observed in these
samples is larger than that found in the samples that
have been HIPped conventionally. It is suggested that
this larger scatter could be associated with the presence
of some remnant surface dimples; samples with grooves
will fail earlier than those without grooves. Further
work on optimizing surface quality is thus of interest.
The combined effect of low surface roughness and the
absence of any significant surface damage can lead to
the improved fatigue life of the sample.[14] This is an
important observation because it means that compo-
nents made by net-shape HIPping do not require
any surface machining, and indeed the fatigue limit
of 620 MPa obtained with samples containing the
as-HIPped surface obtained when using the new HIP
schedule is within the range of those reported for
wrought samples.[23–25]
In the earlier work on conventionally HIPped
samples,[14] the elongation was slightly degraded from
about 21 pct for samples machined from the HIPped
METALLURGICAL AND MATERIALS TRANSACTIONS A

Fig. 9—(a) Values of Vickers hardness, (b) carbon counts obtained
by WDX analysis, and (c) fraction of alpha taken from taper
sections of a sample of Ti-6Al-4V HIPped using the new HIPping
procedure. The x-axis is the approximate distance from the as-HIPped
surface obtained from the measured positions of the data points.
Values of hardness obtained from measurements on the as-HIPped
surface (S) and on a cross section (X) are also indicated in (a).
samples to 19 pct for samples that were tested with the
as-HIPped surface present. Thus, in the earlier work, the
presence of the as-HIPped surface was found to decrease
the ductility slightly. In the present work, the lower
value of elongation of 12 pct, found in samples HIPped
using the new HIPping procedure and that were
machined from the bulk, is associated with a signifi-
cantly higher oxygen content of 2300 ppm compared
with 1700 to 2000 ppm in the earlier work and coarser
microstructure in the samples HIPped using the new
HIPping procedure. The further decrease in elongation
to 8 pct, found in samples that contained the as-HIPped
surface, is slightly larger than the decrease found in the
METALLURGICAL AND MATERIALS TRANSACTIONS A
earlier work, but it is still only a small, although
significant decrease. This slight reduction in elongation
and the significant improvement in fatigue properties
are associated with the smooth as-HIPped surface
(Figure 8) and with the increase in hardness (Figure 9(a))
observed in the near-surface region of the as-HIPped
sample, but the relative importance of these two
independent factors in increasing the fatigue limit is
not clear. This hardness increase is coupled with a
detectable increase in the carbon counts near the surface
(Figure 9(b)), which would be expected since diffusion
of carbon from the mild steel casing would occur during
HIPping. The activation energy for diffusion of carbon
into beta titanium is reported as between 150 and
200 kJ/mol[26,27] and diffusion constant (Do) at 1223 K
(950
C) as 108 cm2/s,[27] which would lead to a value of
Dt during the 3 hours of HIPping at 1203 K (930
C)
within a factor of 2 of 500 lm. This calculation, which is
of course approximate, has ignored diffusion through
alpha. The observed increase in carbon (an alpha
stabilizer) counts also results in a small increase in the
proportion of alpha phase near the surface (Figure 9(c)),
which may also account for the slight reduction in
elongation observed. According to the measurements in
Figure 9, the hardness and microstructural changes
extend to a depth of about 200 lm, which is compatible
with the distance over which the change in C count is
observed. Increase of surface carbon content and
consequent hardness can increase the fatigue strength
as long as no obvious alpha case forms. Apparently, in
the present study, the 1 to 2 pct increase in alpha volume
fraction does not form a deleterious alpha case. It would
be of interest to carry out a study where the diffusion of
C could be significantly reduced using the low C iron
(0.01 wt pct C) as a tooling material,[28] but it would be
necessary to assess its strength at the HIPping temper-
ature since if it is softer than the Ti64 indentations of the
sort shown in Figure 8 could form. A comparison of
fatigue limit between the as-HIPped samples obtained
using mild steel and ultralow C steel under the new
HIPping procedure will clarify whether the smooth
surface or diffusion of C is the key for improving the
fatigue property.
B. Influence of HIPping Temperature and HIPping
Procedure on the Tensile and Fatigue Properties
of Machined Samples
The fracture surfaces of the tensile specimens in the
specimens HIPped at 1153 K (880
C) show that the
crack appears to have propagated along a PPB, sug-
gesting that inadequate bonding occurs at the HIPping
temperature of 1153 K (880
C). In the specimens
HIPped at 1293 K (1020
C), cracking was character-
ized by flat transgranular facets that were on the scale of
the coarser lamellar colonies in this sample and the
corresponding clusters of these coarser regions. It thus
appears that the temperature of 1203 K (930
C) is an
optimum between the limited bonding at 1153 K
(880
C) and the coarsening of the microstructure at
1293 K (1020
C). The tensile properties of samples
HIPped at 1203 K (930
C) using the new HIPping
VOLUME 41A, APRIL 2010—1043
Fig. 10—SEM secondary electron micrographs showing the fracture surfaces of failed tensile sample HIPped at 1203 K (930
C) using the new
procedure. Transgranular facets formed by clusters of lamellae can be seen in the crack initiation site (elongation = 13 pct).
Fig. 11—SN fatigue curves for HIPped Ti-6Al-4V samples with four
different surface finishes. Samples with the as-HIPped surfaces
formed using the new HIPping procedure had the highest fatigue
limit. The arrows indicate that the tests were interrupted without the
failure of the samples.
procedure are intermediate between the properties of the
samples conventionally HIPped at 1203 K (930
C) and
1293 K (1020
C), which is reasonable in view of the
scale of the microstructure, which is intermediate
between these samples. In view of this observation, it
may be that the tensile properties could be improved if a
slightly lower HIPping temperature were used when
using the new HIP procedure, and this may lead to a
further improvement in fatigue properties.
The fatigue response of the machined samples, which
were HIPped at three different temperatures using the
conventional HIPping schedule, shows that samples
HIPped at 1203 K (930
C) have significantly better
fatigue properties than samples HIPped either at 1153 K
(880
C) or 1293 K (1020
C). In these samples, it was
Table IV. Arithmetic Mean Surface Roughness (Ra) and Maximum Peak to Valley Height (Rmax) of HIPped Four Point Bending
Fatigue Samples with Different Surface Conditions
Conventionally HIPped Electropolished
Ra (lm) 9.08 4.69
Rmax (lm) 41.4 28.24
1044—VOLUME 41A, APRIL 2010
shown that fatigue cracks initiate from clusters of a laths
that have similar grain orientation. Such clusters could
fail as a large individual grain. For samples HIPped at
1293 K (1020
C), a cluster of coarser alpha laths, which
have similar crystallographic orientations (Figures 3(e)
and (f)), can be formed, with fine beta laths between the
coarse alpha laths. Such a large size cluster can result in
earlier crack initiation and rapid crack propagation. For
samples HIPped at 1153 K (880
C), the beta grains and
laths are fine, which cannot deflect or blunt a crack, so
the crack will cut through the beta laths and propagate
more easily than through a coarser structure.[26]
In addition, the imperfect bonding illustrated in
Figure 5(a) will also reduce the fatigue life if a crack
nucleates close to a region where bonding is inadequate.
The sample HIPped at 1203 K (930
C) has a coarser
microstructure than the samples HIPped at 1153 K
(880
C), but finer than that those HIPped at 1293 K
(1020
C), and it appears that this structure offers an
optimum balance for fatigue when using conventional
HIPping.
The increase of fracture toughness with the increase of
HIPping temperature from 1203 K (930
C) to 1293 K
(1020
C) is likely to be associated with the coarsened
HIPped microstructure, which can lead to more marked
deflection of cracks.[26]
The overall scale of the microstructure in the
as-HIPped samples clearly contributes to the balance
of properties, and the origin of this fine microstructure is
the fact that the microstructure of the as-received
powder particles is martensitic. Overall, the mechanical
properties that have been investigated here are within
the large range obtainable in thermomechanically
processed samples.[11,29]
Machined Surface Improved As-HIPped Surface
0.4 1.05
3.75 9.85
METALLURGICAL AND MATERIALS TRANSACTIONS A
 V. CONCLUSIONS
1. The fatigue limit of the as-HIPped surface is signifi-
cantly improved by using a HIPping schedule,
which results in a much smoother as-HIPped
surface than is obtained with conventional HIP
schedules. Diffusion of C from the tooling may con-
tribute to the high fatigue limit of samples contain-
ing the smooth, as-HIPped surface.
2. A HIPping temperature of 1203 K (930
C) results
in the best balance of properties for the conditions
investigated here, and these properties are compara-
ble with those reported in forged samples.
3. The origin of the properties obtained in HIPped
samples is the martensitic structure within the powder
particles, which gives rise to a fine microstructure.
ACKNOWLEDGMENTS
The authors acknowledge the financial support of
this work by ORS and Rolls-Royce plc. Tremendous
thanks are due to Professor M.H. Loretto for many
stimulating discussions and thoughtful suggestions.
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