Accepted Manuscript

Influence of grain boundary misorientations on the mechanical behavior of a

near-α Ti-6Al-7Nb alloy processed by ECAP

V.V. Polyakova, I.P. Semenova, A.V. Polyakov, D.K. Magomedova, Y. Huang,

T.G. Langdon

PII: S0167-577X(16)31967-X
DOI: http://dx.doi.org/10.1016/j.matlet.2016.12.083
Reference: MLBLUE 21895

To appear in: Materials Letters

Received Date: 11 November 2016

Revised Date: 23 December 2016
Accepted Date: 27 December 2016

Please cite this article as: V.V. Polyakova, I.P. Semenova, A.V. Polyakov, D.K. Magomedova, Y. Huang, T.G.
Langdon, Influence of grain boundary misorientations on the mechanical behavior of a near-α Ti-6Al-7Nb alloy
processed by ECAP, Materials Letters (2016), doi: http://dx.doi.org/10.1016/j.matlet.2016.12.083

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 Influence of grain boundary misorientations on the mechanical behavior of a

near-α Ti-6Al-7Nb alloy processed by ECAP

V.V. Polyakovaa, I.P. Semenovaab, A.V. Polyakov ab*, D.K. Magomedovab, Y. Huangc,

T.G. Langdonc
a
Ufa State Aviation Technical University, 12 K.Marx street, 450008, Ufa, Russia
b
Saint Petersburg State University, 28 Universitetsky pr., 198504, Peterhof, Saint

Petersburg, Russia
c
University of Southampton, Southampton, SO17 1BJ, UK

*Corresponding author: [email protected]

Abstract

A near-α Ti-6Al-7Nb alloy was processed by equal-channel angular pressing

(ECAP) and the features of microstructural transformation were studied using EBSD

analysis and transmission electron microscopy. The results show a non-monotonic

variation in the density of low-angle and high-angle boundaries of the α-phase grains

with increasing strain during ECAP. The relationship between the misorientations of the

grain boundaries and the mechanical properties of the alloy were examined.

Keywords: titanium alloy; ultrafine-grained structure; grain boundaries; strength;

ductility.

1
Introduction

The Ti-6Al-7Nb alloy was designed especially for medical applications as a more inert

analogue of the Ti-6Al-4V alloy [1]. However, unlike the Ti-6Al-4V, the Ti-6Al-7Nb

alloy is practically not hardened by conventional heat treatment (HT), since it belongs to

the near-α Ti alloys in which the content of the β-phase is not more than 5% [2]. As is

well known, severe plastic deformation (SPD) techniques enable the fabrication of bulk

nanostructured billets having ultrafine-grained (UFG) structures with grain sizes below

1 µm and excellent mechanical properties [3]. An enhancement in the strength of the Ti-

6Al-7Nb alloy due to UFG structure formation will enable, in many cases, a successful

replacement of Ti-6Al-4V and stainless steels which are traditionally used in

osteosynthesis and orthopedics.

In practice, the grain boundaries (GB) in UFG materials play a key role in their

mechanical behavior [4] and there is a possibility of controling the mechanical behavior

through the use of grain boundary engineering [5]. The UFG structure formation in

metals under SPD depends on the processing regimes, which leads to establishing

various types of boundaries such as high-angle, low-angle, special and random,

equilibrium and non-equilibrium boundaries [4,5].

The aim of the investigation was to study the deformation mechanisms of the

formation of new intergranular and inter-phase boundaries and to reveal the relationship

between the microstructural evolution and the mechanical properties of the Ti-6Al-7Nb

alloy.

Experimental methods

The Ti-6Al-7Nb (IMI 367) rods in a diameter of 22 mm were subjected to HT at

985°С for 1h, quenched, then annealed at 750°С for 4h for the formation of a duplex

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(equiaxed-lamellar) structure. The ECAP was conducted at 600°C using Вс route in a

die-set with a channel intersection angle of 120°. The numbers of ECAP passes (n) were

from 1 to 6 and, according to the equation [6], the strain (ε) for 1 pass is

0.67.

A study of GB misorientations was conducted by automatic analysis of electron

backscattered diffraction (EBSD) obtained using a scanning electron microscope Philips

XL40 FESEM with field emission and TSL OIM 6 (EDAX) software. The step sizes

were 200 and 30 nm. From the ratio of the total length of the low-angle boundaries

(LAB <15º) and high-angle boundaries (HABs) to the scanned area, the values of the

densities of boundaries were defined [7]. The microstructure was studied using a JEM

2100 electron microscope.

Tensile mechanical testing was performed at RT with a strain rate of 1×10 -3 s-1.

The specimens had cylindrical sections of 3 mm in diameter with gauge lengths of 15

mm.

Results and discussion

Figure 1a shows an EBSD grain map of the initial structure after HT consisting

of primary α-phase grains and colonies of α-phase plates. After 2 passes ECAP in Fig.

1b, the microstructure consists of fragments of severely distorted plates which appear to

be broken by LAB in addition to small globular grains of the α- and β-phases. The

larger grains of the primary α-phase are characterized by a developed substructure in

Fig. 1b.

Figure 2a,b shows typical TEM images of the fragmented primary α-phase at

different magnifications after 2 passes of ECAP. As a result of the SPD, there is an

increase in the dislocation density in the bodies of larger grains with the formation of

3
weakly misoriented structures of a cellular type. The lamellar structure has transformed

with the formation of subgrain boundaries with a high dislocation density.

After reaching strain 2.68 and 4.02, the structure forms a GB ensemble from

fully spheroidized grains/subgrains of the α- and β-phases where two types of grains can

be noted: new grains with equilibrium boundaries and those with non-equilibrium

boundaries of deformation origin (Fig. 3a). The average sizes of the α- and β-phases

grains/subgrains after 4 and 6 passes are similar and reached values of 350 and 330 nm,

respectively (Fig. 3b). Fig. 3c shows the distribution of the β-phase in the EBSD phase

contrast map after 6 passes of ECAP. The β-phase (bright contrast) is distributed in the

form of separate grains with sizes from 300 to 500 nm and therefore it has

approximately the same size as the α-phase grains.

Using the EBSD analysis, the dependencies the LABs and HABs densities (ρB)

on strain of ECAP are shown in Fig. 4a. It can be seen that in the initial state the density

of LABs is on average to 0.15±0.04 µm-1 whereas the density of HABs is 1.2±0.3 µm-1.

With an increase in strain from 1.34 to 4.02, the density of HABs monotonically

increases, thereby indicating an increase in the length of the boundaries and the

formation of smaller grains. The density of HABs at strain 4.02 was 6.5±0.8 µm-1. It is

important to note that, under the same strains, the fraction of LABs does not change

significantly and even slightly decreases after 6 passes, amounting to 2.4±0.43 µm-1.

Therefore, it can be seen in Fig. 4a that the incremental rate of HABs is noticeably

higher than the growth of LABs. As the accumulated strain increases, this difference

becomes significant due to the predominant transformation of subgrain boundaries into

HABs although the formation of new LABs also continues. The increase in the amount

of HABs with increase in the dispersion degree of the structure in the Ti-6Al-7Nb

4
facilitates the occurrence of grain boundary sliding (GBS), which eventually becomes

manifest in a reduction of the plastic flow stress and thereby in an increase of the

ductility as observed after 6 passes of ECAP [8].

Figure 4b shows the change in the strength and ductility of the Ti-6Al-7Nb alloy

during ECAP. An increase in the dislocation density and the formation of a developed

dislocation ensemble in the plates and primary α-phase grains after 2 passes is the main

reason for the sharp increase in the density of LABs (Fig. 4a). This leads to a significant

enhancement of the strength (1050 MPa) due to the cumulative action of the

strengthening mechanisms caused by irregular dislocation tangles and the organized

substructures. Such structural changes correspond to a decrease in ductility (δ ∼ 9%).

However, with a further increase in strain up to 4.02, the strength increases up to 1200

MPa, the ductility also grows and the elongation reaches 12% (Fig. 4b). Thus, the

average size of the α-phase grains after 4 and 6 passes does not change significantly

(350 and 330 nm, respectively), while the density of HABs grows visibly as in Fig. 4a.

Thus, the enhancement in the strength with increasing fraction of HABs may be related

to the Hall-Petch relation, since with decreasing grain size the total length of boundaries

increases. At the same time, HABs promote the mechanisms of GBS and/or contribute

to strain hardening during plastic deformation which leads to ductility enhancement

[4,5]. LABs or subgrains make a contribution to strength due to the mechanism of

dislocation hardening which is less efficient than the grain-boundary mechanism (due to

HABs).

The present results show that SPD provide new opportunities for GB design

through the fabrication of UFG and nanocrystalline metals and alloys [4]. Therefore, the

research results obtained in this study for the Ti-6Al-7Nb alloy confirm that the

5
structure of boundaries of new grains, formed after SPD, has a significant effect on the

mechanical behavior of these UFG materials.

Conclusions

Microstructure evolution in the Ti-6Al-7Nb alloy subjected to ECAP was

studied. Fragmentation of the primary α-phase grains is realized through the slip and

accumulation of dislocations with the formation of predominantly subgrain boundaries.

A transformation of the initial lamellar fraction leads to the formation of high-angle

boundaries. The dependence of the density of LABs and HABs on the strain has a stage

character. The formation of an UFG structure in the Ti-6Al-7Nb alloy with a mean size

of 330 nm leads to an increase in the UTS up to 1210 MPa, where this is 20% higher

than for the hot-rolled counterpart.

Acknowledgements

ECAP and mechanical testing was supported by the Russian Science Foundation

№ 16-19-10356 in «USATU», the TEM analyses – by the RFBR grant №16-58-

1006116. The work of two authors was supported by the European Research Council

under ERC Grant Agreement No. 267464-SPDMETALS (YH and TGL). The authors

thank V.N. Anumalasetty for help with the EBSD analysis.

6
References.

[1] D.M. Brunette, P. Tengvall, M. Textor, P. Thomsen, Titanium in Medicine,

Springer-Verlag Berlin Heidelberg, Germany, 2001.

[2] R. Boyer, G. Welsch, E. Collings, Materials Properties Handbook: Titanium

Alloys, ASM International, Metals Park, OH, USA, 1998.

[3] R.Z. Valiev, Y. Estrin, Z. Horita, T.G. Langdon, M.J. Zehetbauer, Y.T. Zhu,

Producing Bulk Ultrafine-Grained Materials by Severe Plastic Deformation, JOM 58, 4

(2006) 33–39.

[4] R.Z. Valiev, On grain boundary engineering of UFG metals and alloys for

enhancing their properties, Mater Sci Forum 584-586 (2008) 22-28.

[5] I.P. Semenova, G.H. Salimgareeva, G.Da Costa, W. Lefebvre, R.Z. Valiev,

Enhanced strength and ductility of ultra-fine grained Ti processed by severe plastic

deformation, Adv Eng Mater 12 (2010) 803-807.

[6] V.M. Segal, Materials processing by simple shear, Mater Sci Eng. A197 (1995)

157-164.

[7] V.N Anumalasetty, G. Colombo, G. McIntosh, Yu. Mardakhayeva, D. Yu,

Microstructure and mechanical properties of coarse and ultrafine grain titanium with

different iron contents, In: Proceeding of PRICM-8, Wiley (2013) 3265-3273.

[8] S. Mironov, M. Murzinova, S. Zherebtsov, G.A. Salishchev, S.L. Semiatin,

Microstructure evolution during warm working of Ti–6Al–4V with a colony-α

microstructure, Acta Mater 57 (2009) 2470–2481.

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Figure captions

Fig. 1 EBSD grain map of the Ti-6Al-7Nb alloy: (a) initial microstructure; (b) 2 passes

ECAP.

Fig. 2 TEM images after 2 passes ECAP: (a) primary α-phase grains (region A) and

deformed α- grains (region B); (b) deformed (α+β)- region.

Fig. 3 Microstructure of the Ti-6Al-7Nb alloy after 6 passes ECAP: (а) bright-field

TEM image; b) EBSD grain map; c) EBSD phase contrast map (β-phase).

Fig. 4 Dependence of LABs and HABs density (a) and UTS with elongation (b) on the

strain value (ε) of ECAP Ti-6Al-7Nb alloy.

8
Fig. 1

9
Fig. 2

10
Fig. 3

11
Fig. 4

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*Highlights (for review)

• The microstructure evolution of equiaxed and lamellar fraction of near-α Ti-6Al-7Nb

alloy during the ECAP processing was studied.
• The low- and high-angle boundaries have a non-monotonic variation in density during
the ECAP processing.
• An increase in the fraction of high-angle boundaries in the ultrafine-grained structure
as strain reaches ε ≈ 4 leads to an enhancement in both the strength and the ductility.

13