Characterizing nanoscale precipitation in a titanium alloy by laser-assisted atom probe tomography

Abstract Atom-probe tomography was performed on the metastable β-Ti alloy, Ti-5Al-5Mo-5V-3Cr wt% (Ti-5553), aged at 300 °C for 0 to 8 h, to precipitate the embrittling isothermal ω phase. Accurate precipitate quantification requires monitoring and controlling suitable charge-state ratios in the mass spectrum, which in turn are closely related to the laser pulse energy used. High ultraviolet laser pulse energies result in significant complex molecular ion formation during field-evaporation, causing mass spectral peak overlaps that inherently complicate data analyses. Observations and accurate quantification of the ω-phase under such conditions are difficult. The effect is minimized or eliminated by using smaller laser pulse energies. With a small laser pulse energy, Ti-rich and solute depleted precipitates of the isothermal ω phase with an oxygen enriched interface are observed as early as after 1 h aging time utilizing the LEAP 5000X S (77% detection efficiency). We note that these precipitates were not detected below a 2 h aging time with the LEAP 4000X Si (58% detection efficiency). The results are compared to the archival literature. The Al concentration in the matrix/precipitate interfacial region increases during aging. Nucleation of the α-phase at longer aging times may be facilitated by the O and Al enrichment at the matrix/precipitate interface (both strong α-stabilisers). The kinetics and compositional trajectory of the ω-phase with aging time are quantified, facilitating direct correlation of the APT data to previously published mechanical testing.

[1]  D. Dye,et al.  Effect of precipitation on mechanical properties in the β-Ti alloy Ti-24Nb-4Zr-8Sn , 2016 .

[2]  Tien T. Tsong,et al.  Atom‐Probe Field Ion Microscopy , 1990 .

[3]  Baptiste Gault,et al.  Atom Probe Microscopy , 2012 .

[4]  D. Seidman,et al.  Atom-Probe Tomographic Analyses of Hydrogen Interstitial Atoms in Ultrahigh Purity Niobium , 2015, Microscopy and Microanalysis.

[5]  Dieter Isheim,et al.  Analysis of Three-dimensional Atom-probe Data by the Proximity Histogram , 2000, Microscopy and Microanalysis.

[6]  David N. Seidman,et al.  Application software for data analysis for three-dimensional atom probe microscopy , 2002 .

[7]  D. Seidman,et al.  Doubly- and Triply- Charged Diatomic Molybdenum Cluster Ions As Observed in Pulsed-Laser Assisted Local-Electrode Atom-Probe (LEAPTM) Tomography , 2007, Microscopy and Microanalysis.

[8]  Harald Leitner,et al.  Impact of directional walk on atom probe microanalysis , 2012 .

[9]  B. Gault,et al.  Determination of the tip temperature in laser assisted atom-probe tomography using charge state distributions , 2008 .

[10]  T. Tsong Observation of doubly charged diatomic cluster ions of a metal , 1986 .

[11]  D Lawrence,et al.  In situ site-specific specimen preparation for atom probe tomography. , 2007, Ultramicroscopy.

[12]  Yufeng Zheng,et al.  The indirect influence of the ω phase on the degree of refinement of distributions of the α phase in metastable β-Titanium alloys , 2016 .

[13]  H. W. Rosenberg,et al.  TITANIUM ALLOYING IN THEORY AND PRACTICE , 1970 .

[14]  D. Seidman,et al.  Atom-by-atom chemistry of internal interfaces: simulations and experiments , 2001 .

[15]  Richard Dashwood,et al.  Thermomechanical processing of Ti-5Al-5Mo-5V-3Cr , 2008 .

[16]  David J. Larson,et al.  Local Electrode Atom Probe Tomography: A User's Guide , 2013 .

[17]  Olof C Hellman,et al.  Efficient sampling for three-dimensional atom probe microscopy data. , 2003, Ultramicroscopy.

[18]  Yufeng Zheng,et al.  Role of ω phase in the formation of extremely refined intragranular α precipitates in metastable β-titanium alloys , 2016 .

[19]  D. Seidman,et al.  Isothermal omega formation and evolution in the Beta-Ti alloy Ti-5Al-5Mo-5V-3Cr , 2016 .

[20]  P. De Bièvre,et al.  Isotopic Compositions of the Elements, 2001 , 2005 .

[21]  D. Seidman,et al.  Three-dimensional Investigation of Ceramic/Metal Heterophase Interfaces by Atom-probe Microscopy , 2000, Microscopy and Microanalysis.

[22]  D. Seidman,et al.  Atomic-Scale Structure and Chemistry of Segregation at Matrix/Precipitate Heterophase Interfaces , 2001 .

[23]  P. Bagot,et al.  Precipitation of the ordered α2 phase in a near-α titanium alloy , 2016 .

[24]  P. Bagot,et al.  Precipitation processes in the Beta-Titanium alloy Ti-5Al-5Mo-5V-3Cr , 2015 .

[25]  G. Lütjering,et al.  Mechanical properties of age-hardened titanium-aluminum alloys , 1970 .

[26]  S. Semiatin,et al.  Thermomechanical processing of beta titanium alloys—an overview , 1998 .

[27]  D. Seidman,et al.  Microstructural evolution in a superelastic metastable beta-Ti alloy , 2017 .

[28]  M. Mills,et al.  Phenomenological and microstructural analysis of room temperature creep in titanium alloys , 2000 .

[29]  David J. Larson,et al.  Local Electrode Atom Probes , 1998, Microscopy and Microanalysis.

[30]  C. Leyens,et al.  Titanium and titanium alloys : fundamentals and applications , 2005 .

[31]  D. Kent,et al.  The role of ω in the precipitation of α in near-β Ti alloys , 2016 .

[32]  D. Dye,et al.  Nanoprecipitation in a beta-titanium alloy , 2015 .

[33]  D. Kent,et al.  New insights into the phase transformations to isothermal ω and ω-assisted α in near β-Ti alloys , 2016 .

[34]  B. P. Geiser,et al.  Developing detection efficiency standards for atom probe tomography , 2014, Optics & Photonics - NanoScience + Engineering.

[35]  H. Fraser,et al.  Elemental partitioning between α and β phases in the Ti–5Al–5Mo–5V–3Cr–0.5Fe (Ti-5553) alloy , 2009 .

[36]  M. Jackson,et al.  β Phase decomposition in Ti–5Al–5Mo–5V–3Cr , 2009 .

[37]  H. Fraser,et al.  ω-Assisted nucleation and growth of α precipitates in the Ti–5Al–5Mo–5V–3Cr–0.5Fe β titanium alloy , 2009 .

[38]  D. Kent,et al.  The mechanism of ω-assisted α phase formation in near β-Ti alloys , 2015 .

[39]  P. Bagot,et al.  The formation of ordered clusters in Ti-7Al and Ti-6Al-4V , 2016 .