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International Journal of Fatigue 23 (2001) S319S323 www.elsevier.

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The fatigue crack propagation resistance of Ti6Al4V under aqueous saline environments
M.R. Bache *, W.J. Evans
IRC in Computer Aided Materials Engineering, Department of Materials Engineering, University of Wales, Swansea, SA2 8PP, UK

Abstract Fatigue crack propagation rates are characterised for the titanium alloy Ti 6/4 in atmospheric air and under complete immersion in 3.5% salt solution. The alloy is assessed in three microstructural forms: mill annealed, bimodal and fully transformed lamellar. Through the employment of a corner crack specimen geometry containing a part through crack with a maximum length of 2.5 mm, the lamellar variant demonstrates microstructurally sensitive growth for cracks shorter than 1 mm. The growth rate response is highly dependent on both environment and mean stress. Relative to this, both the mill annealed and bimodal microstructures are shown to be insensitive to salt solution conditions. 2001 Elsevier Science Ltd. All rights reserved.
Keywords: Saline environment; Microstructure; Mean stress; Defect tolerance

1. Introduction Commercially pure titanium and its alloys are often employed for high performance engineering applications where components are subject to aqueous saline environments. Corrosion studies of these materials dating back over the past fty years have conrmed their credentials as relatively corrosion resistant systems when compared to the majority of competitive steels and aluminium alloys. Combined with their low density and intermediate to high strength, the titanium alloys offer great potential to the aerospace, offshore, biomedical and chemical processing industries. In support of an expanding range of applications, titanium producers have developed specic alloy compositions to meet a variety of environmental needs. For example, extra low interstitial (ELI) variants of the Ti 6Al4V system are now recommended by ASTM standards as implant materials [1] and offer reduced toxicity levels to the body. Alternative alpha+beta alloys have been derived with improved hot brine corrosion resistance for geothermal applications through minor additions of ruthenium or palladium [2]. The same elements incorporated into the beta alloys again increase

* Corresponding author. E-mail address: m.bache@swansea.ac.uk (M.R. Bache).

resistance to reducing acids whilst the inherently high content of molybdenum, typically used as the beta stabilising element, also retards corrosion from the decomposition of hydraulic uids commonly utilised in aircraft assemblies [2]. Such improvements in corrosion resistance must be accompanied by a comparable, if not improved, mechanical performance relative to the standard atmospheric LCF or HCF response. Stresscorrosion and corrosion fatigue studies of the common titanium alloys in salt solutions appear to demonstrate a degree of inconsistency in their ndings. Some authors demonstrate negligible effects by comparing to data generated in air, whilst others report evidence for an acceleration in fatigue crack growth rates together with a marked sensitivity to the frequency of loading [3,4]. The majority of these studies have tended to concentrate on laboratory investigations of physically long cracks employing a variety of testpiece geometries. One possible reason for the reported variations in behaviour, therefore, may be the different response of microstructurally small and long cracks to environmentally assisted crack growth. The present paper will consider the effects of a saline environment on fatigue crack growth in a conventional Ti6Al4V alloy. In particular, the role of microstructure will be investigated and through the use of a suitably sized, corner crack specimen geometry, the crack growth rate data will span the transition from short to long crack

0142-1123/01/$ - see front matter 2001 Elsevier Science Ltd. All rights reserved. PII: S 0 1 4 2 - 1 1 2 3 ( 0 1 ) 0 0 1 4 1 - 4

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growth. This is an essential consideration for aerospace applications where, due to the relatively severe in-service loading of components, a fundamental understanding of the very early stages of crack development is vitally important. This regime will account for a large proportion of the potential life of the component, i.e. the life to rst engineering crack, typically dened as a surface crack of 0.75 mm length. Since corrosion fatigue interactions are known to be sensitive to mean stress, data are presented for a range of R values from 0.01 to 0.7. The implications for component ling under corrosive environments will be addressed.

2. Experimental details The + titanium alloy Timetal 318 (Ti6Al4V) is a mid-strength titanium alloy with a recommended maximum operating capability of approximately 300C. Specic combinations of strength and ductility are achieved via different heat treatment routines. The microstructures assessed during the present study cover the two most popular forms used in engineering components (i.e. mill annealed and bi-modal) together with a coarse, fully transformed lamellar structure for comparison, Fig. 1. The mill annealed material contains over 90% primary alpha phase, consisting of equi-axed grains with an average diameter of approximately 10 m, with beta phase material surrounding the -grain boundaries. The bimodal microstructure contains approximately 30% equiaxed primary alpha grains within a transformed alpha+beta matrix. The fully transformed variant was produced via heat treatment above the beta transus followed by slow cooling. Individual grains, often exceeding 0.5 mm, contain sub colonies of aligned alpha laths. Specimen blanks were taken from 30 mm diameter round bar stock and heat treated prior to machining. Full details of the heat treatment routines are specied in Table 1. Fatigue crack propagation measurements were taken using a corner crack specimen design, Fig. 2. Cracks were initiated from a starter slit, 0.35 mm in depth from the specimen edge, and growth terminated at a maximum crack length of approximately 2.5 mm. Crack growth was monitored using a pulsed DC potential drop system utilising a constant current setting of 30 A. Previous calibration trials and comparisons with data obtained using optical systems have established that the DC system has no measurable effect on the rate of propagation in these alloys in the aqueous salt solution environment under investigation. Data were generated at laboratory temperature either in atmospheric air or under complete immersion in a salt solution (3.5% NaCl by mass). The solution was contained within in a small cell (approximate volume 250 ml) surrounding the specimen and was not replenished during the course of an individ-

Fig. 1. Ti 6/4 microstructures: (a) mill annealed; (b) bi-modal +; (c) tramsformed lamellar.

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Table 1 Ti 6/4 heat treatments Heat treatment Mill annealed at 700C (as received bar stock) 960C for 30 min + water quench annealed for 2 h at 700C air cool 1030C for 30 min + furnace cool aged for 8 h at 550C, air cool Microstructural form Primary alpha (90%), plus retained beta (= average 10 m diameter) Fig. 1(a) Primary alpha (30%), plus transformed beta (=1520 m diameter) Fig. 1(b) Coarse aligned colonies of transformed beta (prior grain size =750 m colony width =200 m) Fig. 1(c) Fig. 3. Fatigue crack growth rates in mill annealed material.

Fig. 4.

Fatigue crack growth rates in bimodal material.

Fig. 2.

Corner crack specimen design.

ual test. Employing a sinusoidal loading waveform of 1 Hz frequency and a peak stress of 300 MPa provided tests with a maximum duration of approximately 48 h. Stress ratios spanning the range R=0.010.7 are reported. 3. Results Fatigue crack propagation data measured from corner crack test pieces machined from the + titanium alloy Timetal 318 in the three microstructural forms of interest are included in Figs. 35. In each graph, the da/dN versus K data encompass a range of stress ratio (R=0.01 0.7) in the salt solution environments. Data from similar tests performed on each microstructure in atmospheric air at R=0.1 are also included in each gure for comparison. Figs. 3 and 4 demonstrate that both the mill annealed and bimodal microstructures are relatively in-

Fig. 5. Fatigue crack growth rates in fully transformed lamellar material.

sensitive to environment with only a marginal increase in growth rates noted under the inuence of the salt solution as the stress ratio R is increased. In contrast, crack growth rates measured in the relatively coarse lamellar form, Fig. 5, demonstrate a marked inuence of environment. Comparable tests performed under effectively zero to maximum tension conditions (i.e. R=0.01 and 0.1, respectively) illustrate a signicant increase in

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growth rate under the saline condition compared to air. Data at each R value in the saline environment also indicate an extremely erratic growth response marked by periods of relatively rapid acceleration and deceleration.

4. Discussion Titanium alloys are renowned for their for their resistance to corrosive, oxidising media due to the formation of a protective, passive oxide surface lm. Specic aerospace, offshore and automotive applications currently employ variants of the Ti 6/4 alloy for this very reason. Early examples of biomedical prostheses also utilised Ti 6/4, although more recent concerns over the introduction of aluminium and heavy metal ions such as vanadium into the human body have led to development of specic alloys for the medical community. Because of strength and fatigue endurance requirements, virtually all these applications will employ the alloy in the mill annealed or bimodal microstructural forms. Therefore, it is encouraging to note that both of these variants illustrate no adverse response under fatigue crack propagation experiments performed in saline solutions as compared to laboratory air. Similar FCG rates were noted in the corner crack specimens tested in air and salt solution irrespective of stress ratio, Figs. 3 and 4. Further, comparisons made between these two gures show that the rates measured in both microstructures are virtually identical. Due to the microstructural scale of all these alloy variants, it is argued that the cracks produced in the corner crack geometry, ranging from 0.35 to 2.5 mm, are essentially long cracks which are known to be less sensitive to stress range and environmental inuence. In sharp contrast, the data for the fully transformed lamellar microstructure show a strong dependence between FCG and environment which is further affected by stress ratio, Fig. 5. By re-plotting these data using a crack length criterion instead of stress intensity range, Fig. 6, it is noted that under the salt solution condition,

Fig. 6. Growth rates in lamellar microstructure characterised using a crack length criterion.

the early episodes of rapid acceleration measured under each R value relate to the growth of cracks of the order of 1 mm or less. Beyond this length the rates of propagation appear to be more consistent during the remainder of the individual tests. It is interesting to note that cracks of this magnitude in the transformed variant are still on average within the scale of two grain diameters. Despite the formation of physically long cracks, irregular subsurface crack proles and the uneven appearance of the fracture surfaces both indicate that growth remains strongly inuenced by microstructure for cracks of this size in the lamellar structure. The crack paths were highly tortuous when viewed on the external surface of the specimens and evidence of crack branching was noted, clearly different to the forms of cracking found in the annealed and bimodal variants. The earliest stages of crack development appear transgranular with intergranular fracture evident at a later stage. Careful examination of the data for the atmospheric air tests in this microstructure, Fig. 5, also supports the argument for microstructuarally sensitive growth since these also demonstrate erratic growth rate behaviour. The exact mechanisms behind the accelerated FCG rates for the transformed microstructure in salt solution are not clear. However, a process of hydrogen embrittlement is often argued as the cause of similar behaviour in alternative materials (e.g. steels). It is perhaps signicant in the present case that the transformed microstructure is characterised by colonies of aligned, elongated alpha plates separated by a near continuous network of retained phase. Hydrogen acts as a stabilising element in titanium alloys, where concentrations in the order of thousands of parts per million can be held in solid solution. Previous research has inferred that such concentrations can lead to a process of hydride-induced fracture along / interfaces under fatigue loading in similar coarse grained titanium alloys with an aligned microstructure, e.g. Timetal 685 [5]. During the present environmental tests on Ti 6/4, a process of chemical dissociation would have been active as the fatigue crack advanced to expose fresh titanium alloy at the crack tip. The newly formed crack surfaces eventually oxidise to form a passive layer offering an improved chemical resistance. However, simultaneous with this reaction, hydrogen is generated and absorbed by the bulk metal. Whatever the mechanism, the effect is clearly enhanced by high R values. This is consistent with both well-established [6] and contemporary [7] models for environmentally assisted crack growth since under high R the crack is not allowed to close during the unloading half cycle, therefore, a constant supply of the aggressive chemical species is fed to the crack tip and any reaction products are readily transported away. Despite the greater engineering requirement for Ti 6/4 in the mill annealed and bimodal microstructural forms, examples of fully transformed lamellar regions could be

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5. Conclusions Evidence for environmentally assisted crack growth has been presented in the titanium alloy Ti 6/4 when heat treated to produce a fully transformed, coarse grained lamellar microstructure. The mill annealed and bimodal microstructural variants, which are more commonly employed for high strength engineering components, were by contrast largely insensitive to the effects of aqueous saline solution. In general, the potential role of aggressive environments must be considered when designing laboratory experiments in support of component design.

Fig. 7. Ti 6/4 plates with bimodal microstructure joined by electron beam welding.

encountered in large components and structures which employ welding. An example of an electron beam weld joint made between two plates of Ti 6/4 originally in the bimodal microstructural form is illustrated in Fig. 7. The weld region is clearly distinguished by a region of coarse lamellar grains. It is argued that structures fabricated using similar technology and intended for service in aqueous saline environments must take into account the potential for environmentally assisted short fatigue crack growth as dened in the present study. In the absence of data generated in the relevant environmental conditions, design methodologies relying on laboratory information generated under atmospheric air conditions can clearly, under some circumstances, compromise fatigue life predictions. Laboratory testing remains a cost effective method for the generation of materials property data. However, the designer must demand that, as far as practically possible, the conditions applied during testing are fully representative of the inservice environment.

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