This work reports on a pump–probe laser-based heating and sensing metrology to study the failure mechanisms of materials during extreme heat fluxes localized near surfaces, the localization of which is controlled by the focus of the laser beam and sensed by the reflection of a secondary probe laser. We focus the demonstration of these power density at failure tests on the damage mechanisms of commercially pure titanium metal during and after high heat fluxes induced from the absorbed laser energy. Using this steady-state thermoreflectance pump–probe metrology, a localized region of the material was irradiated at a low modulated frequency, while the average change in the thermoreflectance signal was monitored. We observe surface and cross-sectional oxidation of the titanium, revealing correlations between microstructural evolution events and shifts in thermoreflectance trends as a function of absorbed power density. Furthermore, the damage morphology was shown to be heavily influenced by the size of the heater (dictated by the radius of the pump laser beam), which controlled the relative degree of thermomechanical, melting, and oxidative decohesion failure mechanisms in the samples. The analysis of the temperature distribution coupled with the observed microstructural damage gives rise to a high-throughput experimental technique to induce desired deformation modes through cyclic thermal testing.
REFERENCES
1.
W. G.
Fahrenholtz
and G. E.
Hilmas
, “Ultra-high temperature ceramics: Materials for extreme environments
,” Scr. Mater.
129
, 94
–99
(2017
). 2.
M. M.
Opeka
, I. G.
Talmy
, and J. A.
Zaykoski
, “Oxidation-based materials selection for 2000 °C+ hypersonic aerosurfaces: Theoretical considerations and historical experience
,” J. Mater. Sci.
39
, 5887
–5904
(2004
). 3.
X.
Zhang
, P.
Hu
, J.
Han
, and S.
Meng
, “Ablation behavior of ZrB2-SiC ultra high temperature ceramics under simulated atmospheric re-entry conditions
,” Compos. Sci. Technol.
68
, 1718
–1726
(2008
). 4.
L.
Pienti
, D.
Sciti
, L.
Silvestroni
, A.
Cecere
, and R.
Savino
, “Ablation tests on HfC- and TaC-based ceramics for aeropropulsive applications
,” J. Eur. Ceram. Soc.
35
, 1401
–1411
(2015
). 5.
M.
Azadi
, G. H.
Farrahi
, G.
Winter
, and W.
Eichlseder
, “Thermo-mechanical behaviours of light alloys in comparison to high temperature isothermal behaviours
,” Mater. High Temp.
31
, 12
–17
(2014
). 6.
R. H.
Cook
and R. P.
Skelton
, “Environment-dependence of the mechanical properties of metals at high temperature
,” Int. Metall. Rev.
19
, 199
–222
(1974
). 7.
M.
Bache
, “A review of dwell sensitive fatigue in titanium alloys: The role of microstructure, texture and operating conditions
,” Int. J. Fatigue
25
, 1079
–1087
(2003
). 8.
D.
Lee
and E. W.
Hart
, “Stress relaxation and mechanical behavior of metals
,” Metall. Trans.
2
, 1245
–1248
(1971
). 9.
Y.
Li
, Y.
Guo
, H.
Hu
, and Q.
Wei
, “A critical assessment of high-temperature dynamic mechanical testing of metals
,” Int. J. Impact Eng.
36
, 177
–184
(2009
). 10.
D. R.
Chichili
, K. T.
Ramesh
, and K. J.
Hemker
, “The high-strain-rate response of alpha-titanium: Experiments, deformation mechanisms and modeling
,” Acta Mater.
46
, 1025
–1043
(1998
). 11.
U.
Diebold
, The Surface Science of Titanium Dioxide
(North-Holland
, 2003
), see https://www.sciencedirect.com/science/article/pii/S0167572902001000 (accessed March 8, 2018).12.
C.
Leyens
and M.
Peters
, Titanium and Titanium Alloys
(Wiley
, 2003
).13.
P.
Kofstad
, “High-temperature oxidation of titanium
,” J. Less-Common Met.
12
, 449
–464
(1967
). 14.
R.
Bansal
, J. K.
Singh
, V.
Singh
, D. D. N.
Singh
, and P.
Das
, “Optimization of oxidation temperature for commercially pure titanium to achieve improved corrosion resistance
,” J. Mater. Eng. Perform.
26
, 969
–977
(2017
). 15.
M. V.
Diamanti
, S.
Codeluppi
, A.
Cordioli
, and M. P.
Pedeferri
, “Effect of thermal oxidation on titanium oxides’ characteristics
,” J. Exp. Nanosci.
4
, 365
–372
(2009
). 16.
J.
Dai
, J.
Zhu
, C.
Chen
, and F.
Weng
, “High temperature oxidation behavior and research status of modifications on improving high temperature oxidation resistance of titanium alloys and titanium aluminides: A review
,” J. Alloys Compd.
685
, 784
–798
(2016
). 17.
Y.
Mizuno
, F. K.
King
, Y.
Yamauchi
, T.
Homma
, A.
Tanaka
, Y.
Takakuwa
, and T.
Momose
, “Temperature dependence of oxide decomposition on titanium surfaces in ultrahigh vacuum
,” J. Vac. Sci. Technol. A
20
, 1716
–1721
(2002
). 18.
R. R.
Boyer
, “An overview on the use of titanium in the aerospace industry
,” Mater. Sci. Eng., A.
213
, 103
–114
(1996
). 19.
J. A.
Daleo
, K. A.
Ellison
, and D. H.
Boone
, “Metallurgical considerations for life assessment and the safe refurbishment and requalification of gas turbine blades
,” J. Eng. Gas Turbines Power
124
, 571
–579
(2002
). 20.
B.
Fischer
, S.
Vorberg
, R.
Völkl
, M.
Beschliesser
, and A.
Hoffmann
, “Creep and tensile tests on refractory metals at extremely high temperatures
,” Int. J. Refract. Met. Hard Mater.
24
, 292
–297
(2006
). 21.
S.
Siddique
, M.
Imran
, and F.
Walther
, “Very high cycle fatigue and fatigue crack propagation behavior of selective laser melted AlSi12 alloy
,” Int. J. Fatigue
94
, 246
–254
(2017
). 22.
A. J.
Schmidt
, X.
Chen
, and G.
Chen
, “Pulse accumulation, radial heat conduction, and anisotropic thermal conductivity in pump-probe transient thermoreflectance
,” Rev. Sci. Instrum.
79
, 114902
(2008
). 23.
C. A.
Paddock
and G. L.
Eesley
, “Transient thermoreflectance from thin metal films
,” J. Appl. Phys.
60
, 285
–290
(1986
). 24.
D. G.
Cahill
, “Analysis of heat flow in layered structures for time-domain thermoreflectance
,” Rev. Sci. Instrum.
75
, 5119
–5122
(2004
). 25.
J. L.
Braun
, C. J.
Szwejkowski
, A.
Giri
, and P. E.
Hopkins
, “On the steady-state temperature rise during laser heating of multilayer thin films in optical pump-probe techniques
,” J. Heat Transfer
140
, 052801
(2018
). 26.
J. L.
Braun
, D. H.
Olson
, J. T.
Gaskins
, and P. E.
Hopkins
, “A steady-state thermoreflectance method to measure thermal conductivity
,” Rev. Sci. Instrum.
90
, 024905
(2019
). 27.
L.
Lavisse
, D.
Grevey
, C.
Langlade
, and B.
Vannes
, “The early stage of the laser-induced oxidation of titanium substrates
,” Appl. Surf. Sci.
186
, 150
–155
(2002
). 28.
G. V.
Chertihin
and L.
Andrews
, “Reactions of laser ablated titanium, zirconium, and hafnium atoms with oxygen molecules in condensing argon
,” J. Phys. Chem.
99
, 6356
–6366
(1995
). 29.
T. N.
Baker
, “Laser surface modification of titanium alloys
,” in Surface Engineering of Light Alloys: Aluminium, Magnesium and Titanium Alloys
(CRC Press, 2010
), Vol. 12, pp. 398
–443
. 30.
L.
Lavisse
, J. M.
Jouvard
, L.
Imhoff
, O.
Heintz
, J.
Korntheuer
, C.
Langlade
, S.
Bourgeois
, and M. C. M.
de Lucas
, “Pulsed laser growth and characterization of thin films on titanium substrates
,” Appl. Surf. Sci.
253
, 8226
–8230
(2007
). 31.
Y. S.
Tian
, C. Z.
Chen
, D. Y.
Wang
, and T. Q.
Lei
, “Laser surface modification of titanium alloys—A review
,” Surf. Rev. Lett.
12
, 123
–130
(2005
). 32.
B.
Baufeld
, E.
Brandl
, and O.
Van Der Biest
, “Wire based additive layer manufacturing: Comparison of microstructure and mechanical properties of Ti-6Al-4V components fabricated by laser-beam deposition and shaped metal deposition
,” J. Mater. Process. Technol.
211
, 1146
–1158
(2011
). 33.
G.
Kasperovich
and J.
Hausmann
, “Improvement of fatigue resistance and ductility of TiAl6V4 processed by selective laser melting
,” J. Mater. Process. Technol.
220
, 202
–214
(2015
). 34.
J. L.
Braun
and P. E.
Hopkins
, “Upper limit to the thermal penetration depth during modulated heating of multilayer thin films with pulsed and continuous wave lasers: A numerical study
,” J. Appl. Phys.
121
, 175107
(2017
). 35.
W. E.
Frazier
, “Metal additive manufacturing: A review
,” J. Mater. Eng. Perform.
23
, 1917
–1928
(2014
). 36.
Y.
Kok
, X. P.
Tan
, P.
Wang
, M. L. S.
Nai
, N. H.
Loh
, E.
Liu
, and S. B.
Tor
, “Anisotropy and heterogeneity of microstructure and mechanical properties in metal additive manufacturing: A critical review
,” Mater. Des.
139
, 565
–586
(2018
). 37.
B.
Dutta
and F. H. S.
Froes
, “The additive manufacturing (AM) of titanium alloys
,” Met. Powder Rep.
72
, 96
–106
(2017
). 38.
W.-H.
Wu
, C.-C.
Yang
, and J.-W.
Yeh
, “Industrial development of high-entropy alloys
,” Ann. Chim. Sci. Mater.
31
, 737
–747
(2006
). 39.
E.
Castle
, T.
Csanádi
, S.
Grasso
, J.
Dusza
, and M.
Reece
, “Processing and properties of high-entropy ultra-high temperature carbides
,” Sci. Rep.
8
, 8609
(2018
). 40.
D.
Miracle
, J.
Miller
, O.
Senkov
, C.
Woodward
, M.
Uchic
, and J.
Tiley
, “Exploration and development of high entropy alloys for structural applications
,” Entropy
16
, 494
–525
(2014
). 41.
A. H.
Firester
, M. E.
Heller
, and P.
Sheng
, “Knife-edge scanning measurements of subwavelength focused light beams
,” Appl. Opt.
16
, 1971
(1977
). 42.
P. E.
Hopkins
, “Influence of electron-boundary scattering on thermoreflectance calculations after intra- and interband transitions induced by short-pulsed laser absorption
,” Phys. Rev. B
81
, 035413
(2010
). 43.
S.
Dilhaire
, S.
Grauby
, and W.
Claeys
, “Calibration procedure for temperature measurements by thermoreflectance under high magnification conditions
,” Appl. Phys. Lett.
84
, 822
–824
(2004
). 44.
B. F.
Donovan
, J. A.
Tomko
, A.
Giri
, D. H.
Olson
, J. L.
Braun
, J. T.
Gaskins
, and P. E.
Hopkins
, “Localized thin film damage sourced and monitored via pump-probe modulated thermoreflectance
,” Rev. Sci. Instrum.
88
, 054903
(2017
). 45.
F.
Cverna
, ASM Ready Reference: Thermal Properties of Metals
(ASM International
, Materials Park
, OH
, 2002
).46.
C. J.
Boxley
, H. S.
White
, C. E.
Gardner
, and J. V.
Macpherson
, “Nanoscale imaging of the electronic conductivity of the native oxide film on titanium using conducting atomic force microscopy
,” J. Phys. Chem. B.
107
, 9677
–9680
(2003
). 47.
R.
Dutton
, A Review of the Low-Temperature Creep Behaviour of Titanium
(Whiteshell Laboratories
, 1996
).48.
A.
Takano
and K.
Ueda
, “A study of the oxygen adsorption process on a titanium single crystal surface by electron stimulated desorption
,” Surf. Sci.
242
, 450
–453
(1991
). 49.
D. P.
Adams
, R. D.
Murphy
, D. J.
Saiz
, D. A.
Hirschfeld
, M. A.
Rodriguez
, P. G.
Kotula
, and B. H.
Jared
, “Nanosecond pulsed laser irradiation of titanium: Oxide growth and effects on underlying metal
,” Surf. Coat. Technol.
248
, 38
–45
(2014
). 50.
G.
Bertrand
, K.
Jarraya
, and J. M.
Chaix
, “Morphology of oxide scales formed on titanium
,” Oxid. Met.
21
, 1
–19
(1984
). 51.
C. J.
Beevers
, M. R.
Warren
, and D. V.
Edmonds
, “Fracture of titanium-hydrogen alloys
,” J. Less Common Met.
14
, 387
–396
(1968
). 52.
T.
Furuhara
, H. J.
Lee
, E. S. K.
Menon
, and H. I.
Aaronson
, “Interphase boundary structures associated with diffusional phase transformations in Ti-base alloys
,” Metall. Trans. A.
21
, 1627
–1643
(1990
). 53.
X.
Feng
, X.
Huang
, and X.
Wang
, “Thermal conductivity and secondary porosity of single anatase TiO2 nanowire
,” Nanotechnology
23
, 185701
(2012
). 54.
N.
Okinaka
and T.
Akiyama
, “Latent property of defect-controlled metal oxide: Nonstoichiometric titanium oxides as prospective material for high-temperature thermoelectric conversion
,” Jpn. J. Appl. Phys.
45
, 7009
–7010
(2006
). 55.
Y. S.
Touloukian
, Thermal Conductivity: Nonmetallic Solids
, Thermophysical Properties of Matter Vol. 2 (Plenum
, 1970
), pp. 183
–193
.56.
B. F.
Donovan
, D. M.
Long
, A.
Moballegh
, N.
Creange
, E. C.
Dickey
, and P. E.
Hopkins
, “Impact of intrinsic point defect concentration on thermal transport in titanium dioxide
,” Acta Mater.
127
, 491
–497
(2017
). 57.
E. A.
Scott
, J. T.
Gaskins
, and S. W.
King
, “Thermal conductivity and thermal boundary resistance of atomic layer deposited high-k dielectric aluminum oxide, hafnium oxide, and titanium oxide thin films on silicon on silicon
,” APL Mater.
6
, 058302
(2018
). 58.
Y.
Wang
, J. Y.
Park
, Y. K.
Koh
, and D. G.
Cahill
, “Thermoreflectance of metal transducers for time-domain thermoreflectance
,” J. Appl. Phys.
108
, 043507
(2010
). 59.
S.
Zimmermann
, U.
Specht
, L.
Spieß
, H.
Romanus
, S.
Krischok
, M.
Himmerlich
, and J.
Ihde
, “Improved adhesion at titanium surfaces via laser-induced surface oxidation and roughening
,” Mater. Sci. Eng., A
558
, 755
–760
(2012
). 60.
M. N.
Ghazzal
, N.
Chaoui
, M.
Genet
, E. M.
Gaigneaux
, and D.
Robert
, “Effect of compressive stress inducing a band gap narrowing on the photoinduced activities of sol-gel TiO2 films
,” Thin Solid Films
520
, 1147
–1154
( 2011
). 61.
G.
Rajender
and P. K.
Giri
, “Strain induced phase formation, microstructural evolution and bandgap narrowing in strained TiO2 nanocrystals grown by ball milling
,” J. Alloys Compd.
676
, 591
–600
(2016
). 62.
A.
Moridi
, H.
Ruan
, L. C.
Zhang
, and M.
Liu
, “International journal of solids and structures residual stresses in thin film systems: Effects of lattice mismatch, thermal mismatch and interface dislocations
,” Int. J. Solids Struct.
50
, 3562
–3569
(2013
). 63.
M.
Seifi
, A.
Salem
, D.
Satko
, J.
Shaffer
, and J. J.
Lewandowski
, “Defect distribution and microstructure heterogeneity effects on fracture resistance and fatigue behavior of EBM Ti–6Al–4V
,” Int. J. Fatigue
94
, 263
–287
(2017
). 64.
T.
Lee
, J. H.
Kim
, S. L.
Semiatin
, and C. S.
Lee
, “Internal-variable analysis of high-temperature deformation behavior of Ti-6Al-4V: A comparative study of the strain-rate-jump and load-relaxation tests
,” Mater. Sci. Eng., A
562
, 180
–189
(2013
). 65.
R. E.
Reed-Hill
, C. V.
Iswaran
, and M. J.
Kaufman
, “A power law model for the flow stress and strain-rate sensitivity in CP titanium
,” Scr. Metall. Mater.
33
, 157
–162
(1995
). 66.
L. B.
Freund
and S.
Suresh
, Thin Film Materials: Stress, Defect Formation and Surface Evolution
(Cambridge University Press
, Cambridge
, 2004
).67.
L. H.
Chong
, K.
Mallik
, C. H.
de Groot
, and R.
Kersting
, “The structural and electrical properties of thermally grown TiO2 thin films related content
,” J. Phys.: Condens. Matter
18
, 645
–657
(2006
). 68.
C.-C.
Ting
, S.-Y.
Chen
, and D.-M.
Liu
, “Preferential growth of thin rutile TiO2 films upon thermal oxidation of sputtered Ti films
,” Thin Solid Films
402
, 290
–295
(2002
). 69.
C.-C.
Ting
, S.-Y.
Chen
, and D.-M.
Liu
, “Structural evolution and optical properties of TiO2 thin films prepared by thermal oxidation of sputtered Ti films
,” J. Appl. Phys.
88
, 4628
–4633
(2000
). 70.
A. K.
Vijh
, “Relationship between activation energies for the thermal oxidation of metals and the semiconductivity of the oxides
,” J. Mater. Sci.
9
, 985
–988
(1974
). 71.
S.
Yu
and H.-S. P.
Wong
, “A phenomenological model for the reset mechanism of metal oxide RRAM
,” IEEE Electron Device Lett.
31
, 1455
–1457
(2010
). 72.
L. B.
Freund
, “Substrate curvature due to thin film mismatch strain in the nonlinear deformation range
,” J. Mech. Phys. Solids
48
, 1159
–1174
(2000
). 73.
H.
Gao
, “Some general properties of stress-driven surface evolution in a heteroepitaxial thin film structure
,” J. Mech. Phys. Solids
42
, 741
–772
(1994
). © 2022 Author(s). Published under an exclusive license by AIP Publishing.
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