metals

Article
Effect of Radial Forging on the Microstructure and
Mechanical Properties of Ti-Based Alloys
Lev B. Zuev 1 , Galina V. Shlyakhova 1 and Svetlana A. Barannikova 1,2, *
1 Institute of Strength Physics and Materials Science, Siberian Branch of Russian Academy of Science,
634055 Tomsk, Russia; lbz@ispms.tsc.ru (L.B.Z.); shgv@ispms.tsc.ru (G.V.S.)
2 Physics and Technology Faculty, Tomsk State University, 634050 Tomsk, Russia
* Correspondence: bsa@ispms.tsc.ru; Tel.: +7-3822-286-923




Received: 22 September 2020; Accepted: 6 November 2020; Published: 8 November 2020


Abstract: Radial forging is a reliable way to produce Ti alloy rods without preliminary mechanical
processing of their surface, which is in turn a mandatory procedure during almost each stage
of the existing technology. In the present research, hot pressing and radial forging (RF) of the
titanium-based Ti-3.3Al-5Mo-5V alloy were carried out to study the specifics of plasticized metal
flow and microstructural evolution in different sections of the rods. The structural analysis of these
rods was performed using metallography and X-ray diffraction techniques. The X-ray diffraction
reveals the two-phase state of the alloy. The phase content in the alloy was shown to vary upon radial
forging. Finally, radial forging was found to be a reliable method to achieve the uniform fine-grained
structure and high quality of the rod surface.

Keywords: titanium alloys; structure formation; mechanical properties; radial forging

1. Introduction
The need for increasing strength and reliability of constructions, as well as reducing their
weight, leads to higher demands for structural materials. In particular, titanium-based alloys that are
extensively used in various fields of engineering due to their high specific strength must have high
fatigue resistance, corrosion resistance and wear resistance in addition to excellent strength that can be
achieved whilst retaining high plasticity [1,2].
According to research conducted over recent decades [3–6], the possibilities of improving the
above properties by means of the conventional mechanical and thermal processing methods in order
to modify the chemical composition of titanium-based alloys, aimed at introducing alloying elements
and varying grain size in the parent material, are almost exhausted. On the other hand, it is evident
that strength characteristics along with functional properties of alloys can be noticeably increased via
the formation of micro- and submicrocrystalline phases in the bulk of the alloy under severe plastic
deformation [7–9].
There is a large number of scientific papers [10–14], in which the processes of evolution of the
structure and properties of titanium-based alloys are investigated under deformation by various
methods. It is known [15–17] that the formation of structure in a material is largely determined by
the degree of deformation, and its scheme and conditions. There is a large amount of experimental
data on the effect of deformation on the structural state of titanium-based alloys [18,19]. However, the
evolution of the structure of titanium-based alloys during radial forging (RF) has not been studied
sufficiently. As is known [20–22], a stressed state is implemented in the dynamic deformation site in
the process of compression of a cylindrical rod during radial forging, which is close to the triaxial
compression and makes it possible to obtain large degrees of deformation of rods under dynamic
influence without the formation of cracks.

Metals 2020, 10, 1488; doi:10.3390/met10111488 www.mdpi.com/journal/metals

Metals 2020, 10, 1488 2 of 12

According to [3,10,15–17], thermomechanical processing of titanium-based alloys such as

Ti-Al-Mo-V and containing Mo and V may lead to the changes in X-ray diffraction patterns owing
to texture formation caused by dopant redistribution, forward and backward decomposition of the
β-phase, and partial transformation of the α-phase in a metastable α”-phase. These phenomena
may arise individually or overlap with each other. Elucidating the complex redistributions of XRD
intensities necessitates a careful analysis of XRD ranges with emerging or disappearing uncombined
reflexes from the different phases.
The complex problem of the structural strength of Ti alloys consists in obtaining a homogeneous
material with a fine-grained structure, hardened by a highly dispersed phase and a high-quality surface
of parts. The fine-grained structure and high-quality surface reduce the effect of stress concentrators
and, as a result, increase the resistance to brittle fracture when operating under conditions of alternating
dynamic loads [1,2,4].
Traditional methods for making alloys include heating the billet to a temperature above the
polymorphic transformation temperature in the β-region, rolling at this temperature, cooling to ambient
temperature, heating the rolled stock to a temperature 20–50 ◦ C below the polymorphic transformation
temperature, and final rolling at this temperature. In the case of titanium products, such a technological
scheme does not provide the necessary manufacturability and quality of titanium material due to
its high tendency to grain growth, oxidation and gas saturation during heat treatment and, as a
consequence, to loss of plasticity and embrittlement of the material. The temperature of polymorphic
transformation (TPT) for the Ti-Al-Mo-V alloy is 840–880 ◦ C, at which phase + recrystallization occurs,
which is the basic characteristic for the appointment of heat treatment modes, but it is at TPT and
above that catastrophic grain growth in titanium alloys and coarsening of the intragranular structure
are observed.
It should be noted that, unlike steels, the coarse-grained structure of titanium materials is not
corrected by heat treatment. Therefore, during heat treatment, the hardening temperature is set at
80–150 ◦ C below the TPT of the alloy. However, under these conditions, complete recrystallization
does not occur, which does not provide complete hardening and does not correct the heredity of the
previous processing, as a result of which the material does not have sufficient quality for such critical
parts as bolts and springs. Multiple hot forging and air cooling operations will negatively affect the
surface quality of the bar. In addition, the method requires an expensive abrasive operation to remove
forging defects and surface substandard layers. As a result, the scrap rate rises and the metal yield
decreases, which ultimately leads to an increase in the cost of manufacturing rods.
The problem to be solved by this study is to obtain rods from high quality titanium alloys while
ensuring high process productivity.
A promising method for the formation of an ultrafine-grained structure is RF, the use of which
in the manufacture of products from titanium alloys is still limited. The use of the radial forging
process in the production of pipes from Zr alloys is described in monograph [7]. If the processes
occurring in hcp alloys during cold rolling and subsequent heat treatment are well studied, then there
is still insufficient reliable information regarding the patterns of structure formation and deformation
mechanisms acting during radial forging.
This work aims to characterize the Ti-Al-Mo-V rods with optimal structural and mechanical
properties achieved through severe plastic deformation of a Ti-Al-Mo-V alloy using radial forging
machines (RFMs). Radial forging is a reliable way to produce Ti alloy rods without preliminary
mechanical processing of their surface, which is in turn a mandatory procedure during almost every
stage of the existing technology. In order to meet the technical requirements of semiproducts, the
development of a new technology needs to solve some important problems such as:

- The choice of thermal treatment modes for forged semiproducts, which meet the technical
requirements to the structure and mechanical characteristics;
Metals 2020, 10, 1488 3 of 12

- The elaboration of algorithms for the deformation of rods and alignment of the RFM tool using data
acquired during the analysis of structural and mechanical properties, which obeys requirements
to the geometrical sizes and surface quality.

2. Materials and Methods

High and ultrahigh degrees of deformation and the subsequent or concomitant thermal effect
lead to the implementation of boundary-substructure and dispersion mechanisms of strengthening.
Among the industrial methods that allow us to form a more dispersed structural condition than after
hot forming and heat treatment, including quenching and tempering in a wide temperature range,
is the technology of RF. The billet material is in overall uniform compression in the deformation
center when using four strikers under RF, which leads to the formation of an extremely dispersed and
homogeneous structure [7]. It should be noted that the treatment of the billet is implemented at the
expense of multiple ultrafast simultaneous compressions. This scheme of deformation allows us to
form a high degree of localization of the center of the deformation. Basically, the technology of the
radial forging is used to improve the strength, reliability, and durability of the special pipe billets, the
main task of which is the long-term operation under normal and extreme conditions.
The investigation of structure and properties of the alloys were performed at various stages of
manufacture using mechanical, metallographic, and X-ray diffraction techniques. Samples were rods
with diameters Φ of 25 mm, produced from a Ti-Al-Mo-V alloy via hot pressing, as well as rods with
diameters Φ20, Φ16, Φ12, Φ10.5, and Φ8.5 mm, using the SXP-16 machine of GFM firm (Steyr, Austria).
The chemical composition of a Ti-Al-Mo-V workpiece used in testing the technology is given in Table 1.

Table 1. Chemical composition of Ti-Al-Mo-V alloy (wt %).

Ti Al Mo V C N Fe Si H2 O2
base 3.3 4.6 4.5 0.05 0.01 <0.01 ≤0.10 0.007 0.014

Radial forging of Ti-Al-Mo-V alloy rods, implemented on a SXP-16 machine of GFM firm (Steyr,
Austria), changes their manufacturing technology to a large extent. Radial forging allows one to
achieve the better plastic processing of the material, but also to ensure high quality of the rod surface,
which enables to avoid facing at intermediate stages of the technological process and to facilitate the
process itself. The forging modes applied in this work are given in Table 2. According to the results, the
surface roughness of the rod with a diameter Φ of 10 mm was within a range of 3–9 µm, which met the
technical requirements of less than 10 µm; the ovality of the rod at a length of 2.5 m was below 30 µm.

Table 2. Forging modes of Ti-Al-Mo-V alloy rods.

Transition Number of Beats Per Minute Feed Rate, mm/s

Φ20→Φ16 mm 580 5...7
Φ16→Φ10 mm 580 5...7

The alloy structure in rods exposed to radial forging was inspected in two transition
zones—i.e., Φ20→Φ16 mm and Φ16→Φ10 mm (Figure 1).
Metals 2020, 10, 1488
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Figure 1. Schematics of cutting-out of samples for metallographic analysis in case of Φ20→Φ16 mm

and Φ16→Φ10 mm transitions.
Figure 1. Schematics of cutting-out of samples for metallographic analysis in case of ∅20→∅16 mm
The microstructure of Ti-Al-Mo-V alloy in these zones was probed using a Neophot-21
and ∅16→∅10 mm transitions.
metallographic microscope equipped with a digital camera (Genius VideoCam Smart 300) and a
special
Thesoftware intended for
microstructure of digital image processing.
Ti-Al-Mo-V alloy in theseThe microstructure
zones was probed of the using
alloy was determined
a Neophot-21
via chemical etching
metallographic in a solution
microscope of 3%with
equipped hydrofluoric
a digital acid and (Genius
camera 3% nitricVideoCam
acid in water [23].300) and a
Smart
special software intended for digital image processing. The microstructure of the alloyofwas
To implement the metallographic analysis of metallic state, as well as to assess the efficiency the
used deformation method and to optimize the alignment of strikers of the SXP-16 RFM,
determined via chemical etching in a solution of 3% hydrofluoric acid and 3% nitric acid in water the samples
were
[23]. selected from the deformation center. The schematics of cutting-out of samples for metallographic
tests To
areimplement
shown in Figure 1.
the metallographic analysis of metallic state, as well as to assess the efficiency of
Table 3 contains information about
the used deformation method and to optimize specimens thethat were cutoffrom
alignment deformation
strikers zones RFM,
of the SXP-16 in a cross
the
section according to the scheme in Figure 1, so that each sample corresponds to a
samples were selected from the deformation center. The schematics of cutting-out of samples forcertain degree of
reduction in diameter, which increases
metallographic tests are shown in Figure 1.with increasing number.
Table 3 contains information about specimens that were cut from deformation zones in a cross
Table 3. Tested samples according Figure 1.
section according to the scheme in Figure 1, so that each sample corresponds to a certain degree of
reduction in diameter, which increases with increasingLocation
number. along the
Sample No. Workpiece Diameter, µm Reduction K, %
Workpiece
1 Table
Φ20 3. Tested samples according Figure
Input (initial 1.
state) 0
3 Φ20 Deformation center (RF) 17
5
Sample Workpiece
Φ16
Location alongoutput
the 20
Reduction К, %
7 No. Diameter,
Φ16μm Workpiece
Deformation center (RF) 23
8 1 ∅20
Φ16 Input (initial state)center (RF)
Deformation 0 38
10 3 Φ10
∅20 DeformationOutput
center(final
(RF)state) 17 50
5 ∅16 выход 20
7
X-ray diffraction ∅16
measurements Deformation
of Ti-Al-Mo-V alloycenter (RF)
were conducted 23
on a sample with Φ8.5 mm,
8 ∅16 Deformation center (RF) 38
obtained from the rod exposed to hot pressing, as well as on sample 6 made by radial forging at a
Φ16→Φ10 mm10 ∅10
transition (see Figure 1). The Output (final
data were state) in the Bragg—Brentano
recorded 50 geometry
(Θ-2Θ mode) within a range of angles of 10 ≤ Θ ≤ 125 deg [24] using a DRON-3 (Burevestnik, Russia)
X-ray diffraction
diffractometer and Cumeasurements
Kα radiation withof Ti-Al-Mo-V
the filteredalloy wereThe
Kβ line. conducted were∅8.5
on a sample with
X-ray diffractograms mm,
recorded
obtained frommode
in a stepwise the rod
withexposed to 0.1
a step of hotdeg;
pressing, as well time
the exposure as onwas
sample 6 made
5 s. The XRDby radial
data wereforging at a
processed
∅16→∅10 mm transition (see Figure 1). The data were recorded in the Bragg—Brentano
using a special computational software. The phase analysis was performed in ARFA-7000 software geometry
(Θ-2Θ mode)
(Russia), withinthe
including a range of angles
database ≤ Θ ≤ 125 deg [24] using a DRON-3 (Burevestnik, Russia)
of 10compounds.
for 40,000
diffractometer and Сucharacteristics
The mechanical Kα radiation with the filtered K
of Ti-Al-Mo-V β line.
alloy The studied
were X-ray diffractograms were recorded
on the flat samples, whose
in a stepwise mode with a step of 0.1 deg; the exposure time was 5 s. The XRD data
working element dimensions were 2 mm × 6 mm × 40 mm. Samples were stretched at room temperature were processed
using a special computational
on an Instron-1185 software.
(US) universal testingThe phaseatanalysis
machine a rate ofwas performed
8.3 × 10−5 s−1 . in ARFA-7000 software
(Russia), including the database for 40,000 compounds.
The mechanical characteristics of Ti-Al-Mo-V alloy were studied on the flat samples, whose
working element dimensions were 2 mm × 6 mm × 40 mm. Samples were stretched at room
temperature on an Instron-1185 (US) universal testing machine at a rate of 8.3 × 10−5 s−1.
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3.
3. Results
3. Results
Results

3.1. Mechanical
3.1. Mechanical Properties
Mechanical Properties of
Properties of Ti-Al-Mo-V
of Ti-Al-Mo-V Alloy after
Ti-Al-Mo-V Alloy after Hot
Hot Pressing
Pressing
The mechanical
The mechanicalcharacteristics
mechanical characteristicsofof
characteristics ofTi-Al-Mo-V
Ti-Al-Mo-V
Ti-Al-Mo-V alloy
alloy
alloywere were
were studied
studied
studied on theon the
on the flat samples
flat samples
flat samples for initial
for initial
for initial
state
state
(sample
state (sample
1) with
(sample 1) heads
1) with heads
with heads cut
cut offcut
fromoffthe
off from
from the center
center
the center of the
the workpiece
of the workpiece
of workpiece (1), as
(1), as well
(1), as well
aswell
fromas asthe from
surface
from the surface
the surface
(2) and
(2)
(2) and transition
transition
and transition
(3) layers. (3)The
(3) layers. The appropriate
appropriate
layers. The appropriate
stress–strain stress–strain
diagramsdiagrams
stress–strain diagrams
of the tested of the
of the tested
samples
tested aresamples
given inare
samples are given2.
Figure
given
in
The
in Figure 2.
strength
Figure The
2. The strength
characteristics characteristics of
of all three samples
strength characteristics all three
of all three samples
are quite
samples closeare quite
aretoquite close
each close
other,toto each
aseach
can be other,
seenas
other, as
fromcan be
can the
be
seen
values
seen from
from the values
of strength
the valueslimit
of (σB )1 = 1060
of strength
strength limitMPa,
limit (σВВ))11(σ
(σ )3 = MPa,
== B1060
1060 MPa,
1040 MPa,(σВВ))33 ==and
(σ 1040
1040 B )2 = 980
MPa,
(σMPa, andMPa.
and (σВВ))22 ==At
(σ 980
980 MPa.
theMPa.sameAt Attime,
the
the
same
same time,
the plasticity the plasticity
time, thedrastically drastically
plasticity varies varies
fromvaries
drastically one samplefrom
from one one sample
to the
sample to
other.toSo, the other.
thethe So,
uniform
other. the
So, the uniform
elongation
uniform elongation elongation
(before the
(before
formation
(before theofformation
the formation
the neck) of of
wasthe
the neck)towas
found
neck) was B )1 = 0.06,
found
be (εfound to be
to B )ВВ2))11==
be(ε(ε
(ε =0.08,
0.06,and
0.06, (εВВ))(ε
(ε 2 = 3 = 0.105.
2 =) 0.08,
B 0.08, and (ε
and (εВВ))33 elongation
The == 0.105.
0.105. TheThe
at
elongation
failure was at
evenfailure
more was even
different more
for different
each sample,
elongation at failure was even more different for each sample, for each
being sample,
δ 1 = 0.09,being
δ
being = δ 1 = 0.09,
0.11, and δδ2 == 0.11,
0.16. and
2 δ1 = 0.09, δ2 3= 0.11, and δ3 = 0.16.
δ 3 = 0.16.

Figure 2.
Figure 2. Stress–strain
Stress–strain diagrams
Stress–strain diagrams of
diagrams of Ti-Al-Mo-V
of Ti-Al-Mo-V alloy:
Ti-Al-Mo-V alloy: center
alloy: center of
centerof the
of the workpiece
the workpiece (1),
workpiece (1), surface
(1), surface layer
surface layer (2),
layer (2),
(2),
transition layer (3).
transition layer (3).

This is owing to the large cross-sectional heterogeneity of the alloy structure. AccordingAccording to the
This is owing to the large cross-sectional heterogeneity of the alloy structure. According to the
metallographic data
metallographic data acquired
data acquiredon
acquired onthe
on thecross-section
the cross-sectionofof
cross-section
thethe
of workpiece,
workpiece,
the workpiece,
thethe
phase composition
phase
the phase composition
composition
within the
within
within
scanned area
the scanned from
scanned area the
area from center
from the to
the centerthe
center to surface
to the is presented
the surface
surface is by
is presenteda mixture
presented by of α and
by aa mixture
mixture ofβ
of αphases
α and
and βof titanium,
β phases
phases ofof
the
where thewhere
titanium, volume fraction
the volume offraction
the α-phase
of exceeds
the α-phase that of thethat
exceeds β-phase
of (see
the Figure(see
β-phase 3). Figure 3).
titanium, where the volume fraction of the α-phase exceeds that of the β-phase (see Figure 3).

(a)
(a) (b)
(b) (c)
(c)
Figure 3.
Figure Microstructure
Microstructure of
3. Microstructure of Ti-Al-Mo-V
of Ti-Al-Mo-V alloy
Ti-Al-Mo-V alloy in the
alloy in the initial
initial state
state before
before radial
radial forging: center
forging: center of the
center of the
workpiece (a), surface layer (b), transition layer (c).
workpiece (a), surface layer (b), transition layer (c).

Meanwhile, the
Meanwhile, the average
the averagegrain
average grainsize
grain sizeofof
size ofthe
theα-phase
the α-phase
α-phase
near
near
near
thethe
surface is ~2.7
surface
the surface is ~2.7
is ~2.7 which
µm,µm, is almost
which
µm, which
five
is almost
is almost
times
five lower
times than than
lower in theincenter,
the as seen
center, as in Figure
seen in 3 for initial
Figure 3 for state before
initial state radial radial
before forging. The finest
forging. The grains
finest
five times lower than in the center, as seen in Figure 3 for initial state before radial forging. The finest
attributed
grains to the α-phase
attributed to the were detected
the α-phase
α-phase in the 3-mm-thick
were detected
detected in the surface layer.
the 3-mm-thick
3-mm-thick However,
surface their size gradually
layer. However,
However, their size
size
grains attributed to were in surface layer. their
increased while
gradually moving
increased toward
while movingthe center,
toward attaining
the a value
center, of ~16.5
attaining a µm, which
value of is consistent
~16.5 µm, whichwith
is
gradually increased while moving toward the center, attaining a value of ~16.5 µm, which is
that for pristine
consistent with workpieces.
with that
that for Hence,
for pristine a pronounced
pristine workpieces.
workpieces. Hence, difference
Hence, aa pronounced in plasticity
pronounced difference of
difference in samples cut
in plasticity off
plasticity of from
of samples
samplesthe
consistent
different
cut off parts
from ofdifferent
the the alloyparts
seems of to bealloy
the due seems
to structural
to be heterogeneity
due to structuralof heterogeneity
Ti-Al-Mo-V, which of persists
Ti-Al-Mo-
cut off from the different parts of the alloy seems to be due to structural heterogeneity of Ti-Al-Mo-
under
V, whichhotpersists
pressing of rods.
under hot pressing
pressing of of rods.
rods.
V, which persists under hot
 Metals 2020, 10, 1488 6 of 12
Metals 2020, 10, x FOR PEER REVIEW 6 of 12

The
Themicrohardness
microhardness ofofthe
thealloy
alloywas
wasmeasured
measured ininthe
theindicated
indicatedzones
zonesusing
usinga PMT-3M
a PMT-3M (Russia)
(Russia)
hardness
hardnesstester
testeratata aload
loadofof1 1N.N.InIncomparison
comparisonwith witha acentral
centralpart
partofofthe
thesample,
sample,the
themicrohardness
microhardness
near
nearthe
thesurface
surfaceisisslightly
slightlyreduced
reducedand andcontinues
continuestotodecrease
decreasefrom
from17501750toto1690
1690MPa
MPawhile
whilegoing
going
away
awayfrom
fromthe
thecenter.
center.The Thereason
reasonofofsuch
sucha achange
changeininstructure
structureandandproperties
propertiescan
canbebesurface
surfacelayer
layer
disordering
disorderingcaused
causedbybydegassing
degassingofofsurface
surfacelayers
layersduring
duringprocessing.
processing.

3.2.Structure
3.2. Structure
of of
of of Ti-Al-Mo-V
Ti-Al-Mo-V Alloyafter
Alloy afterRadial
RadialForging
Forging
Radialforging
Radial forgingallows
allowsoneonetotosuppress
suppressporosity
porositythat
thatisisusually
usuallypresent
presentininaxial
axialsections
sectionsofofrods
rods
obtainedvia
obtained viahot
hotpressing.
pressing.According
According totothe
theexperimental
experimentaldata,data,the
thehighest
highestporeporeconcentration
concentrationwas was
foundininsample
found sample1 1(∅20
(Φ20mm)mm)(see(seeFigure
Figure4).4).TheThe poresatat
pores thethe centralpart
central partofofthe
thesample
sampleformformthe
theaxial
axial
porosity.The
porosity. Thesurface
surfacepores
poreshave
havethetheround
roundshape.
shape.The
The pores
pores atat the
the workpiece
workpiece outlet
outlet (Φ20→Φ16
(∅20→∅16 mm)
mm)
(sample5)5)and
(sample andatatthe
theinlet
inlet(∅16→∅10
(Φ16→Φ10mm) mm)(sample
(sample6)6)may
mayformformthethesmall
smalllinear
linearclusters.
clusters.The
The smallest
smallest
density and pore sizes were observed in sample 10 (with the outlet of Φ16→Φ10
density and pore sizes were observed in sample 10 (with the outlet of ∅16→∅10 mm). Figure 4 shows mm). Figure 4 shows
the presence of pores for the initial state (sample 1) and after radial forging (final
the presence of pores for the initial state (sample 1) and after radial forging (final state, sample 10). state, sample 10).

(a) (b)

(c) (d)
Figure
Figure 4. 4.
Microstructure
Microstructureof Ti-Al-Mo-V alloyalloy
of Ti-Al-Mo-V in the
ininitial state before
the initial radial radial
state before forging—sample 1 (a,b) 1
forging—sample
and after
(a,b) andradial forging
after radial in sample
forging 10 (c,d).
in sample FromFrom
10 (c,d). left left
to right: surface
to right: layer
surface (a,b),
layer center
(a,b), of ofthe
center the
workpiece
workpiece(b,d).
(b,d).

Table44 presents data

Table dataon
onthe change
the in the
change in parameters of theofstructure
the parameters depending
the structure on the reduction.
depending on the
reduction.
Table 4. Porosity and grain size (in points) depending on the degree of reduction.
Table 4. Porosity and grain size (in points) depending on the degree of reduction.
Pore Density, mm−2 Maximum Pore Size, µm Grain Score (in Points)
Ti-Al-Mo-V
Ti-Al- Pore Density, mm
Center of
−2
the Surface Maximum
CenterPore Size, μm
of the Surface Grain
CenterScore
of the(in Points)
Surface
Sample No.
Mo-V Center ofWorkpiece Layer Workpiece Layer Workpiece Layer
Surface Center of the Surface Center of the Surface
Sample the
1 771 Layer 325 Workpiece 18 Layer3,5 6
Workpiece 4
Layer
No. Workpiece
1 3 771 542 325 274 18 9 3,5 3 5-4
6 34
3 5 542 362 274 244 9 2.5 3 3 4
5-4 3-2
3
5 7 362 297 244 202 2.5 2 3 2 4
3-2 3-2
2-1
7 297 202 2 2 3-2 2-1
8 183 149 1.5 1 2 1
8 183 149 1.5 1 2 1
10 10 102 102 98 98 <1 <1 1 1 22 11

The metallographic data are illustrated in Figures 5 and 6 for subsequent ∅20→∅16 mm and
∅16→∅10.5 mm transitions. A comparative analysis of images reveals that noticeable structural
Metals 2020, 10, 1488 7 of 12

The metallographic data are illustrated in Figures 5 and 6 for subsequent Φ20→Φ16 mm and
Φ16→Φ10.5
Metals
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2020, 10,
10, transitions.
xx FOR
FOR REVIEWA comparative analysis of images reveals that noticeable77 of
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changes at the deformation center of the workpiece during the Φ20→Φ16 mm transition are manifested
changes at
changes at the
the deformation
deformation center
center of
of the
the workpiece during ∅20→∅16 mm
during the ∅20→∅16 mm transition
transition are
are
by the grain refinement near the surface and workpiece
close to the axis ofthe
the workpiece.
manifested by
manifested by the
the grain
grain refinement
refinement near
near the
the surface
surface and
and close
close to
to the
the axis
axis of
of the
the workpiece.
workpiece.

(a)
(a) (b)
(b) (c)
(c)

(d)
(d) (e)
(e) (f)
(f)
Figure
Figure
Figure 5. Microstructure of
Microstructure
5. 5. Microstructure of Ti-Al-Mo-V
of Ti-Al-Mo-V alloy
Ti-Al-Mo-V alloy atatthe
alloyat the
the Φ20→Φ16
∅20→∅16
∅20→∅16 mmmm
mm transition. From From
transition.
transition. From left to
left to left
right:
to right:
right:
samples
samples 1, and
1, 3,
samples 1, 3, and
3, and 55 (see
(seeFigure
5 (see Figure1);
Figure 1); (a–c)
1); (a–c) surface
(a–c) surface structure;
surfacestructure;
structure;(d–f) structure
(d–f)
(d–f) at the
structure
structure at the central
at central part of
the central
part of the of
part
the rod.
the rod.
rod.

(a)
(a) (d)
(d)

(b)
(b) (e)
(e)

(c)
(c) (f)
(f)
Figure 6. Microstructure of Ti-Al-Mo-V alloy at the ∅16→∅10 mm transition. From top to bottom:
Figure 6. Microstructureof of Ti-Al-Mo-V
Ti-Al-Mo-V alloy ∅16→∅10
Figure 6. Microstructure alloyatatthe
the Φ16→Φ10 mmmm transition. FromFrom
transition. top totop
bottom:
to bottom:
samples 6,
6, 8,
8, and
and 10
10 (see
(see Figure
Figure 1);
1); (a–c)
(a–c) surface
surface structure;
structure; (d–f)
(d–f) structure
structure at
at the
the central
central part
part of
of the
the rod.
samples 6, 8, and 10 (see Figure 1); (a–c) surface structure; (d–f) structure at the central part rod.
samples of the rod.
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Meanwhile, the
Meanwhile, the structural
structural changes
changes at at the
thecentral
centralpart
partofofthe
theworkpiece
workpieceare areless
lesspronounced.
pronounced.AtAta
small rod diameter during the Φ20→Φ16 mm transition it observes
a small rod diameter during the ∅20→∅16 mm transition it observes the drastic refinement of the drastic refinement of the
the
structure and
structure and the
the variation
variation in in grain
grain morphology.
morphology. The The structure
structurenear
nearthe
therod
rodsurface
surfaceisis80%
80%globular.
globular.
The average grain size at the axis of the workpiece is much greater and the amount
The average grain size at the axis of the workpiece is much greater and the amount of globular grains of globular grains
achieves a value of 50–60%. As follows from the metallographic study of
achieves a value of 50–60%. As follows from the metallographic study of samples cut off from the samples cut off from the
Φ16→Φ10 mm
∅16→∅10 mm transition,
transition, thethe alloy
alloy structure
structureat atthis
thisstage
stageofofdeformation
deformationgradually
graduallytransforms
transformsfromfroma
duplex (globular-lamellar) state with a high degree of inhomogeneity (sample
a duplex (globular-lamellar) state with a high degree of inhomogeneity (sample 6) to a more uniform 6) to a more uniform
globular (sample
globular (sample 10)10) state.
state. However,
However,therethereisisstill
stillpartial
partialheterogeneity:
heterogeneity: while
while thethesurface of of
surface sample
sample10
exhibits the uniform and globular structure, the central part of the rod contains
10 exhibits the uniform and globular structure, the central part of the rod contains up to 25% lamellar up to 25% lamellar
grains, which
grains, which results
results inin aa stronger
stronger structural
structural heterogeneity. Nevertheless, the
heterogeneity. Nevertheless, the central
central porosity
porosity inin
samples obtained
samples obtained by by radial
radialforging
forgingisisless
lesspronounced
pronouncedinincomparison
comparisonwith withthetheporosity
porosity near thethe
near axis of
axis
hot-pressed Ti-Al-Mo-V rods. Figure 7 shows the porosity and grain score
of hot-pressed Ti-Al-Mo-V rods. Figure 7 shows the porosity and grain score (in points) depending (in points) depending on
thethe
on degree of reduction.
degree of reduction.

(a) (b) (c)

Figure 7. Changes
Changes in
in pore density
density (a),
(a), maximum
maximum pore
pore size
size (b), and grain score (c) depending on the
degree of reduction in radial forging: 1—center of the workpiece; 2—surface layer.
layer.

The results of transmission electron microscopy showed that in the initial state (sample 1) in the
initially inhomogeneous microstructure, there is a deformation-induced bending of the alpha-plates
and beta-interlayers,
beta-interlayers,as aswell
wellasasthe
theprocess
processof of
destruction of colonies
destruction of the
of colonies of alpha and and
the alpha beta beta
phases with
phases
dispersion of the structure. Solid solutions disintegrate inside the structural elements.
with dispersion of the structure. Solid solutions disintegrate inside the structural elements. At a At a reduction
of 20%, theofmixture
reduction 20%, theofmixture
alpha and beta phases
of alpha and beta occupies most of the
phases occupies near-surface
most layer. The
of the near-surface average
layer. The
transverse
average dimension
transverse of the structural
dimension elements was
of the structural ~0.3 µm.
elements wasThe
~0.3microstructure formed afterformed
µm. The microstructure radial
forging
after as a forging
radial result ofas
a strong deformation
a result of a strongeffect is noticeably
deformation dispersed,
effect homogeneous,
is noticeably dispersed,and is a mixture
homogeneous,
of alpha
and and betaofphases
is a mixture alpha with a size
and beta of 0.05–0.3
phases with aµm.size of 0.05–0.3 µm.

3.3. X-ray
3.3. X-ray Diffraction
Diffraction Analysis
Analysis of
of Ti-Al-Mo-V
Ti-Al-Mo-V Alloy
Alloy
X-ray diffraction
X-ray diffraction measurements
measurements of of Ti-Al-Mo-V
Ti-Al-Mo-V alloy were conducted
alloy were conducted on on aa sample
sample with Φ8.5 mm,
with ∅8.5 mm,
obtained from the rod exposed to hot pressing, as well as on sample 6 made
obtained from the rod exposed to hot pressing, as well as on sample 6 made by radial forging at by radial forging at aa
Φ16→Φ10 mm transition (see Figure 1). Figure 6 displays the X-ray diffractogram
∅16→∅10 mm transition (see Figure 1). Figure 6 displays the X-ray diffractogram that is that is characteristic
of a biphase alloy,
characteristic as seenalloy,
of a biphase fromasthe seenpresence
from theofpresence
reflexes of
from the coexisting
reflexes hcp α-phase
from the coexisting and bcc
hcp α-phase
β-phase.
and bcc β-phase.
The X-ray
The X-ray diffractogram
diffractogramofofsample
sample6 6afterafterradial forging
radial forging a Φ16→Φ10.5
at at a ∅16→∅10.5 mmmm transition (after
transition the
(after
Φ20→Φ16
the ∅20→∅16 mm mmtransition) is given
transition) in Figure
is given 8. The8.observed
in Figure patternpattern
The observed is strongly different
is strongly from that
different for
from
a hot-pressed sample. First of all, there are the differences between the intensities of
that for a hot-pressed sample. First of all, there are the differences between the intensities of the mainthe main peaks
attributed
peaks to the α-phase
attributed and those
to the α-phase andassociated with a quantity
those associated of the β-phase.
with a quantity Moreover,Moreover,
of the β-phase. the (002) and
the
(004) reflexes of the α-phase vanish, indicating the emergence of anisotropy
(002) and (004) reflexes of the α-phase vanish, indicating the emergence of anisotropy in the in the properties along
various crystallographic
properties along various directions, whichdirections,
crystallographic is due to the alloyisprocessing.
which due to the alloy processing.
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Figure
Figure 8.
8. X-ray
X-ray diffraction
diffraction of
of aa hot-pressed biphase Ti-Al-Mo-V
hot-pressed biphase Ti-Al-Mo-V alloy.
alloy.
Figure 8. X-ray diffraction of a hot-pressed biphase Ti-Al-Mo-V alloy.
Toconfirm
To confirmthese
thesechanges,
changes,thetheX-ray
X-raydiffractograms
diffractograms from
from Figures
Figures 8 and
8 and 9 were
9 were merged
merged in Figure
in Figure 10.
One To can
10. One
can confirm
see see these
thatthat
(002) αchanges,
(002) α line
line the
is X-ray
almost
is almost diffractograms
absent
absent in the
in the offrom
casecase Figures
of sample
sample 68after
6 afterand 9 were merged in Figure
forging.
forging.
10. One can see that (002)α line is almost absent in the case of sample 6 after forging.

Figure 9. X-ray diffraction of sample 6 of Ti-Al-Mo-V alloy (see Figure 1).

Figure 9. X-ray diffraction of sample 6 of Ti-Al-Mo-V alloy (see Figure 1).
Figure 9. X-ray diffraction of sample 6 of Ti-Al-Mo-V alloy (see Figure 1).
Metals 2020, 10, 1488 10 of 12
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Figure
Figure 10. Merged X-ray
10. Merged X-ray diffractions
diffractions from
from Figures
Figures 88 and
and 9.
9.
4. Discussion
4. Discussion
As established via X-ray diffraction with regard to the behavior of the fcc β-phase during radial
As established via X-ray diffraction with regard to the behavior of the fcc β-phase during radial
forging, there was no decrease in its reflex intensity, but an increase for all samples. This evidences the
forging, there was no decrease in its reflex intensity, but an increase for all samples. This evidences
absence of the β→α transformation. The analysis of other XRD peaks reveals that some lines from
the absence of the β→α transformation. The analysis of other XRD peaks reveals that some lines from
the β-phase become larger during the processing and lose their intensity as compared with the initial
the β-phase become larger during the processing and lose their intensity as compared with the initial
state. This testifies to a decrease in crystallite size of the β-phase in the VT16 alloy undergoing plastic
state. This testifies to a decrease in crystallite size of the β-phase in the VT16 alloy undergoing plastic
deformation during radial forging.
deformation during radial forging.
An important phenomenon that arises under severe plastic deformation in radial forging can be
An important phenomenon that arises under severe plastic deformation in radial forging can be
the β→α” martensitic transformation, because, as found, there is a small amount of the martensitic
the β→α″ martensitic transformation, because, as found, there is a small amount of the martensitic
α”-phase in all samples. However, in the case of the initial state, there is also a high content of a stable
α″-phase in all samples. However, in the case of the initial state, there is also a high content of a stable
α-phase. The amount of the α-phase is lower in forged samples, where the parent phase is a metastable
α-phase. The amount of the α-phase is lower in forged samples, where the parent phase is a
α”-phase. At the same time, the α-phase has a nonstoichiometric composition, as follows from its
metastable α″-phase. At the same time, the α-phase has a nonstoichiometric composition, as follows
lattice parameter values. Moreover, it appears from the XRD data that the lattice parameters of the hcp
from its lattice parameter values. Moreover, it appears from the XRD data that the lattice parameters
α-phase of Ti-Al-Mo-V alloy are a = b = 0.29487 nm and c = 0.46857 nm, whereas the lattice parameter
of the hcp α-phase of Ti-Al-Mo-V alloy are a = b = 0.29487 nm and c = 0.46857 nm, whereas the lattice
of a metastable β-phase of titanium (bcc) is a = 0.3231 nm [1,2].
parameter of a metastable β-phase of titanium (bcc) is a = 0.3231 nm [1,2].
The most significant change in the phase composition of the alloy caused by radial forging is
The most significant change in the phase composition of the alloy caused by radial forging is the
the change in the volume fraction of the beta-phase shown in the Figure 11 during this process. It is
change in the volume fraction of the beta-phase shown in the Figure 11 during this process. It is
calculated from the ratio of the experimentally determined intensities of the lines (102) of the alpha
calculated from the ratio of the experimentally determined intensities of the lines (102) of the alpha
phase and (200) of the beta phase for various degrees of compression. As can be seen, at the beginning
phase and (200) of the beta phase for various degrees of compression. As can be seen, at the beginning
of radial forging with a reduction of up to 20% by volume, the bulk content of the beta phase remains
of radial forging with a reduction of up to 20% by volume, the bulk content of the beta phase remains
at a level of ~1/3, and then the proportion of the beta phase decreases to ~ 14 at a final reduction of
at a level of ~1/3, and then the proportion of the beta phase decreases to ~¼ at a final reduction of
50%. In the process of radial forging, there is a gradual change in the texture formed during hot
50%. In the process of radial forging, there is a gradual change in the texture formed during hot
pressing. With an increase in the degree of reduction, the ratio of the intensities of the diffraction
pressing. With an increase in the degree of reduction, the ratio of the intensities of the diffraction
maxima approaches the ratio for a fine-grained material after annealing.
maxima approaches the ratio for a fine-grained material after annealing.
Metals 2020, 10, 1488 11 of 12
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Figure 11.
Figure Change in
11. Change in the
the volume
volume fraction
fraction of
of the
the beta
beta phase
phase depending
depending on
on the
the degree
degree of
of reduction
reduction in
in
radial forging.
radial forging.

5. Conclusions
5. Conclusions
- Radial forging of Ti-3.3Al-5Mo-5V alloy workpieces leads to the structural refinement and the
− Radial forging of Ti-3.3Al-5Mo-5V alloy workpieces leads to the structural refinement and the
changes in grain morphology from predominately lamelar to uniform globular, as well as the
changes in grain morphology from predominately lamelar to uniform globular, as well as the
variations in phase composition of the alloy and the supression of powder formation.
variations in phase composition of the alloy and the supression of powder formation.
- The methods of rod deformation and alignment of the RFM working tool, applied in this work,
− The methods of rod deformation and alignment of the RFM working tool, applied in this work,
ensure fulfillment of technical requirements to geometrical sizes and surface quality.
ensure fulfillment of technical requirements to geometrical sizes and surface quality.
- Radial forging is found to allow one to produce semiproducts from titanium-based Ti-Al-Mo-V
− Radial forging is found to allow one to produce semiproducts from titanium-based Ti-Al-Mo-V
alloys without using multiple mechanical processing of workpieces and rods.
alloys without using multiple mechanical processing of workpieces and rods.

Author Contributions: Project

Author Contributions: Project administration,
administration, supervision,
supervision, and
and conceptualization,
conceptualization, L.B.Z.;
L.B.Z.; methodology,
methodology,
investigation, and
andvisualization,
visualization,G.V.S.;
G.V.S.; formal
formal analysis,
analysis, writing—original
writing—original draftdraft preparation,
preparation, and writing—
and writing—review
and editing,
review S.A.B. All
and editing, authors
S.A.B. have read
All authors and
have agreed
read and to the published
agreed version version
to the published of the manuscript.
of the manuscript.
Thework
Funding: The
Funding: workwas
wasperformed
performedaccording
according to
to the
thegovernment
government research
research assignment
assignment for
for ISPMS
ISPMS SB
SB RAS
RAS (project
(project
No. III.23.1.2) and in the framework of the Program of Competitiveness by the National Research Tomsk
No. III.23.1.2) and in the framework of the Program of Competitiveness by the National Research Tomsk State
State University.
University.
Acknowledgments: The authors are gratefully thanks to Danilov Vladimir for the results discussion.
Acknowledgments: The authors are gratefully thanks to Danilov Vladimir for the results discussion.
Conflicts of Interest: The authors declare no conflict of interest.
Conflicts of Interest: The authors declare no conflict of interest.
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