Accepted Manuscript

Letter

Precipitation behavior and tensile properties of new high strength beta titanium
alloy Ti-1300

Jinwen Lu, Yongqing Zhao, Peng Ge, Yusheng Zhang, Hongzhi Niu, Wei
Zhang, Pingxiang Zhang

PII: S0925-8388(15)00690-8
DOI: http://dx.doi.org/10.1016/j.jallcom.2015.02.222
Reference: JALCOM 33617

To appear in: Journal of Alloys and Compounds

Received Date: 15 January 2015

Revised Date: 28 February 2015
Accepted Date: 28 February 2015

Please cite this article as: J. Lu, Y. Zhao, P. Ge, Y. Zhang, H. Niu, W. Zhang, P. Zhang, Precipitation behavior and
tensile properties of new high strength beta titanium alloy Ti-1300, Journal of Alloys and Compounds (2015), doi:
http://dx.doi.org/10.1016/j.jallcom.2015.02.222

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 Precipitation behavior and tensile properties of new high
strength beta titanium alloy Ti-1300

Jinwen Lu, Yongqing Zhao*, Peng Ge, Yusheng Zhang, Hongzhi Niu, Wei Zhang, Pingxiang Zhang

Northwest Institute for Nonferrous Metal Research, Xi'an 710016, China

Abstract: A study on the relationship between microstructure and tensile properties of new high

strength titanium alloy Ti-1300 is investigated systematically. The result shows that the tensile

properties are strongly determined by their microstructure characteristics, such as the aspect ratio,

volume fraction and size of precipitated plates ( primary phase and secondary phase ).

Transmission electron microscopic (TEM) examination reveals that, in the aged samples,

secondary plates are intersected each other and dispersed in the matrix, but not

homogeneously enough. Comparing with conventional near beta-alloys, Ti-1300 alloy achieves an

excellent combination of high strength and good ductility based on the multi-component

strengthening, which results in a high strength above 1350 MPa with elongation over 13.5%.

Keywords: Metals and alloy, Microstructure, Precipitation, Tensile properties

1. Introduction

Near and metastable alloys have been significantly attracted to use in aerospace,

petrochemical and orthopedic implant applications due to their unique combination of high

specific strength, deep hardenability and excellent corrosion resistance [1-3]. Near alloy is

possessed of a broad range of mechanical properties depending on the changing of microstructure,

and excellent mechanical properties can be achieved in these alloys by solution treatment or aging

metastable phase to precipitate a fine dispersion of plates within -matrix [4-6]. The

precipitation of phase is a key strengthening mechanism, so it is essential to understand its

Corresponding author. Tel.: +86 29 86221498; fax: +86 29 86231103

E-mail address: lujwen@163.com (Jinwen Lu); trc@c-nin.com (Yongqing Zhao)

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nucleation and growth mechanism. The morphology, volume fraction, size and distribution of

phase have an important influence on properties, especially for strength, ductility and fatigue

performance [7]. The growth of phase is influenced by a range of factors, and one of important

ways is to adjust thermomechanical processing parameters. Many investigations have revealed

that even if a small change in heating or cooling rates and heat treatment temperatures can result

in very different precipitation microstructures and consequently very different properties [8, 9]. As

a result, producing an optimum set of properties ( the balancing of strength and ductility ) can be

obtained by perfect processing parameters.

A new beta titanium alloy Ti-1300 suitable for heavy section structural aerospace applications,

has been developed by Northwest Institute for Nonferrous Metal Research (China). In addition,

Ti-1300 alloy belongs to six-component system, and the nominal composition is

Ti-5Al-3Zr-4Mo-4Cr-4V. Comparing with these of Ti-1023 [10, 11], Ti-6554 [12] and Ti-5553

[13-15] alloys, Ti-1300 alloy is to achieve an excellent combination of high strength and good

ductility based on the multi-component strengthening, and its microstructure and properties are

sensitive to hot working technology. Previous research efforts have focused on hot deformation

behavior[16, 17], hot processing techniques[18] and the thick-walled cylinder techniques[19, 20]

of the alloys. However, more extensive details of microstructure and mechanical properties are

essential to utilize the alloy and also broaden its range of uses. Therefore, the intention of present

study is to investigate the microstructure characteristics and mechanical properties, and try to

reveal the effect of the precipitation phase on the mechanical properties of Ti-1300.

2. Experimental

Ti-1300 alloy used for this study was prepared by vacuum consumable arc-remelting furnace,

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and the melting chamber was firstly evacuated and purged with argon. The alloy was re-melted

three times to ensure chemical and microstructural homogeneity, and then double forged at around

950C to square billets with 50mm in each dimension. The square billets were then hot rolled at

750C to round bars with 11mm in diameter. Chemical analysis method was carried out to

determine the actual alloying composition and it was found to be ( in wt.% ): 5.15Al, 2.96Zr,

3.96Cr, 3.79Mo, 3.95V with the balance Ti. The transus temperature of the alloy was

metallographically measured to be approximately 830C. The details of quantitative

metallography was as follow: cylindrical specimens ( 11mm10mm ) were spark machined from

round bars and were solution treated at various temperature both above and below the estimated

transus temperature and examined metallographically. The -transus temperatures of the Ti-1300

alloys was identified by solution treating specimens in the temperature range of 800 - 860 C and

soaked for 1 h in an electric heat treatment furnace and then water quenched to examine the

microstructure ( metallographic techniques ). When the solution temperature was above 830C,

the microstructure was completely in the phase regime. Therefore, the transus temperature of

the alloy is 830 5C. Solution and aging heat treatment were conducted in a box electrical

furnace in air. The specimens were solution treated at 750C ( below transus temperature ) for 1h

by placing them directly into the preheated furnace, followed by air cooling. Aging treatment were

conducted at 500C, and then held for 6 h followed by air cooling.

Microstructure characterization was performed on scanning electron microscopy (SEM) and

transmission electron microscopy (TEM). The phase identification was made by X-ray diffraction

(XRD) analysis operating at 30 kV and 30 mA, the phases were identified by matching each

characteristic peak with the JCPDS files. Standard cylindrical tensile specimens with a gage length

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of 25mm and a cross section of 5mm in diameter were machined from both the solution treated

and aged specimens, and the cross-head speed was 1 mm/min at room temperature. In order to

confirm the validity of tensile test result, tensile test of each heating treatment condition was

repeated twice, and the ultimate tensile strength, yield strength, elongation and the area of

reduction at fracture were accordingly obtained from the average of two tensile results in

conventionality. The error range also has been added in the experimental data, and showed in

Table 1.

3. Results and Discussion

The XRD patterns of the solution treated and aging treated Ti-1300 alloys are shown in Fig.1.

The solution treated and aging treated Ti-1300 alloys are comprised of a mixture of and phases,

but the intensity of diffraction peak of phase is stronger than the adjacent phase in contrast

with the aging treated one. This phenomenon can be explained by the precipitation of quantity of

secondary phases during aging treatment, the primary and secondary phase have the same

diffraction peak in XRD patterns and are considered to be the phase.

Fig. 1. X-ray diffraction patterns showing the phase structure of Ti-1300 alloys under different heat processing

The microstructure of the solution treated Ti-1300 alloy as shown in Fig.2 consists with the

XRD results. It can be seen from Fig.2 that the micrograph of the solution treated alloy presents

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fine equiaxed grains with an average diameter of 8 m, many primary phases with strip shape

are intersected each other at grain boundaries, and others with sphericity or short-strips shape

non-homogeneously precipitates within matrix. From Fig.2(a), it is noted that the prior grain

boundaries are not straight, the recrystallization of the grain has not occurred during rolling

process and solution treatment. Besides, because of relatively smaller thickness and length-width

ratio ( Fig.2(b) ), the primary phase can pin the prior grain boundaries and suppress the

dislocation slipping and grain growth.

Fig. 2. SEM micrographs showing the precipitated primary phases in matrix of Ti-1300 after solution treatment
at 750C for 1 h

Fig. 3 shows SEM micrographs of the morphology of primary phases after solution

treatment plus aging at 500 C for 6 h. The grain boundary of primary phase and secondary

phase, as well as the size, can be clearly seen in Fig.3(a) and (b). As show in Fig.3, the region with

dark contrast is identified as primary phase ( the coarse strip shape plates ) and secondary

phase ( platelets with fine acicular within matrix precipitates during aging ) whereas region

with light gray contrast is the retained matrix. The distribution of primary phase in aged alloy

is non-homogeneous and considerably coarser as compared to the solution treated alloy, and the

morphology characteristic is quantified by means of the image analysis software. When the alloy

is under aging condition, the volume fraction is above 23.3% and the width reaches 320nm. The

increasing volume fraction of primary phase can be increased the stability of matrix and

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reduced the driving force of the secondary phase formation during subsequent aging process,

besides, the increasing of the width of primary phase can suppress the size of the secondary

phase, which have been reported earlier [21].

Fig. 3. SEM micrographs of the aged sample: (a) low magnification and (b) fine acicular- secondary phases

Fig. 4. Bright field TEM micrographs show coarse primary phases (a) and fine secondary phases (b) for

Ti-1300 under aging condition, insets show the corresponding diffraction pattern taken from the circled area

For the sake of investigation the different precipitation behavior, samples aged at

intermediate temperatures were examined by TEM. Fig. 4 shows the bright field TEM

micrographs of coarse primary phases and fine secondary phase for Ti-1300 alloy, insets show

the corresponding diffraction pattern taken from the circled area. Selected area diffraction (SAD)

pattern confirms the presence of primary phases ( brigth coarse strip shape in Fig. 4(a) ),

secondary phase ( brigth fine acicular shape in Fig. 4(b) ) and phase ( darker contrast ). Finer

acicular secondary phase in matrix, as compared to the coarse primary phases, is also visible.

The fine platelets between the coarse primary phases are formed in aging process which have

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been defined to secondary phase. The overall precipitation of secondary phase appears much

finer than adjacent primary phase, which with acicular shape around 40~80 nm in width

precipitates and distributes in matrix during aging. Besides, many secondary phases intersect

each other, and exhibit the occurrence of several variants of plates. It is accepted that the

primary and secondary phase are possess of the same crystal structure ( hexagonal structure

( HCP ) ), and the main difference of the primary and secondary phase may be the lattice

parameter and the orientation relationships between matrix and precipitating phase. As a result, the

microstructure of the aging treated alloy is possessed of the Bi-modal microstructure [22], which

is composed of a mixture of primary phase, secondary phase and phase.

In order to understand the influence of precipitation behavior on the mechanical properties,

tensile tests were conducted on the solution and aging samples. Table 1 shows mechanical

properties of the Ti-1300 alloy under different heat processing. In the solution treated condition,

the alloy has lower strength ( 1034 MPa for yield strength ( YS ) and 1075 MPa for ultimate

tensile strength ( UTS ) ) and higher plastic property ( 21% for elongation ( E ) ) than the aged one.

When the alloy is under aging condition, the yield strength and ultimate tensile strength are

1310MPa and 1370MPa, respectively, and the alloy ruptures at the elongation of 17%. It is well

known that the properties of Ti alloy are sensitive to their phases/crystal structure, and certain

phases may be stabilized by the addition of alloying elements. In the composition of 1300 alloy, Al

is belong to -stabilizing elements, and which can obtain the required percentage of platelets for

strengthening or bimodal microstructures for fatigue property improvement. Zr can reduce the

volume percentage of phase in aging by stabilizing -phase in near and metastable alloys,

and strengthens phase and improves thermostability and welding performance. Two types of

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stabilizer are added to the 1300 alloy in present study. The -isomorphous, Mo and V are included,

while -eutectic elements, Cr is chosen. Adding Mo in titanium alloys can increase the strength

and improve the plastic property, while V can decrease the distortion of lattice and also improve

the structure stability. In addition, the titanium alloy with Cr can improve processability. The strip

secondary phase had a significant effect on the strength of beta titanium alloys, but the ductility

of the alloy was kept on the higher levels due to the growth of sphericity primary phase.

Therefore, the Ti-1300 alloy has achieved an excellent combination of high strength and good

ductility based on precipitation behavior of phase comparable with Ti-5553 alloy (1200 MPa for

ultimate tensile strength and 10% for elongation [13-15] ).

Table 1 Mechanical properties of the Ti-1300 alloy under different heat processing

Condition UTS / MPa YS /MPa E /% A /%

ST 10753 10343 210.2 630.2
STA 13700.5 13100.5 170.2 590.5

In titanium alloy, the widely accepted strengthening mechanism is precipitation strength of

fine phase, and the precipitated phase creates a high number of / interfaces that act as

dislocation barriers. Work by some researchers [23-25] was found that the dislocation

multiplication in defect-free phase and phase after deformation was hardly inhibited by the /

interfaces. Therefore, the interfacial effect of precipitation behavior is limited to strength effect.

On the other hand, the secondary precipitates formed during aging in the matrix is hard phase

in titanium alloy, and the primary precipitates formed during solution processing and phase

are soft ones. The solution treated alloy has a moderate strength with an excellent ductility due to

the acceleration of primary phase precipitation with strip shape and the fine grain strengthening

of grain. As comparing with the solution treated alloy, the aging alloy exhibits high strength of

above 1350MPa with an excellent elongation above 15%, the strength is increased sharply due to

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the fine distributed secondary phase with the mean size of 50nm in width, which exhibits the

best strengthening effect. The excellent ductility is attributed to the relatively small sized prior

grains restrained by primary phase and the increasing interfacial effect of precipitation behavior

[22, 26, 27]. As a result, the Ti-1300 alloy can be controlled by slightly adjusting the heat

processing to obtain a desired combination of the strength and the ductility for any given

engineering structure applications.

4. Conclusions

The new high strength titanium alloy Ti-1300 exhibits excellent tensile elongation along with

superior strength, by means of controlling the precipitation behavior of phase. The distribution

of primary phase in the aging alloy is non-homogeneous and considerably coarser as compared

to the solution alloy, and the overall precipitation of secondary phase appears much fine and

intersects each other. The strength is increased sharply due to the fine distributed secondary

phase, but the improvement of the ductility attributes to the relatively small sized prior grains

restrained by primary phase and the increasing interfacial effect of precipitation behavior.

Acknowledgements

This work is performed partially under the support of the the Nation Natural Science

Foundation of China ( Grant No. 51471136, 51301140 and 51271152) and the Scientific and

Technical Research Team Program of Shaanxi Province ( Grant No. 2012KCT-23 ).

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