Applicability of focused Ion beam (FIB) milling with gallium, neon, and xenon to the fracture toughness characterization of gold thin films
Source abstract
Abstract
Abstract Focused ion beam (FIB) milling is an increasingly popular technique for fabricating micro-sized samples for nanomechanical characterization. Previous investigations have cautioned that exposure to a gallium ion beam can significantly alter the mechanical behavior of materials. In the present study, the effects of gallium, neon, and xenon ions are scrutinized. We demonstrate that fracture toughness measurements on freestanding gold thin films are unaffected by the choice of the ion species and milling parameters. This is likely because the crack initiation is controlled by the local microstructure and grain boundaries at the notch, rather than by the damaged area introduced by FIB milling. Additionally, gold is not susceptible to chemical embrittlement by common FIB ion species. This confirms the validity of microscale fracture measurements based on similar experimental designs. Graphical abstract
Source: crossref · Quality: baseline
Research context
OpenAlex topics: Integrated Circuits and Semiconductor Failure Analysis · Hydrogen embrittlement and corrosion behaviors in metals · Non-Destructive Testing Techniques
SciVX discovery tags are terminology-based. OpenAlex topics are source-provided classifications.
References (72)
Show source-provided references
1. D.S. Gianola, A. Sedlmayr, R. Mnig, C.A. Volkert, R.C. Major, E. Cyrankowski, S.A.S. Asif, O.L. Warren, O. Kraft, In situ nanomechanical testing in focused ion beam and scanning electron microscopes. Rev. Sci. Instrum. 82(6), 063901 (2011)10.1063/1.3595423 ↗
2. G. Dehm, B.N. Jaya, R. Raghavan, C. Kirchlechner, Overview on micro- and nanomechanical testing: new insights in interface plasticity and fracture at small length scales. Acta Mater. 142, 248 (2018)10.1016/j.actamat.2017.06.019 ↗
3. D. Kiener, C. Motz, T. Schoeberl, M. Jenko, G. Dehm, Determination of mechanical properties of copper at the micron scale. Adv. Eng. Mater. 8(11), 1119 (2006)10.1002/adem.200600129 ↗
4. D. Kiener, C. Motz, W. Grosinger, D. Weygand, R. Pippan, Cyclic response of copper single crystal micro-beams. Scr. Mater. 63(5), 500 (2010)10.1016/j.scriptamat.2010.05.014 ↗
5. P.J. Imrich, C. Kirchlechner, D. Kiener, G. Dehm, Internal and external stresses: In situ TEM compression of Cu bicrystals containing a twin boundary. Scr. Mater. 100, 94 (2015)10.1016/j.scriptamat.2014.12.023 ↗
6. S.H. Oh, M. Legros, D. Kiener, G. Dehm, In situ observation of dislocation nucleation and escape in a submicrometre aluminium single crystal. Nat. Mater. 8(2), 95 (2009)10.1038/nmat2370 ↗
7. F. Mompiou, M. Legros, A. Sedlmayr, D.S. Gianola, D. Caillard, O. Kraft, Source-based strengthening of sub-micrometer Al fibers. Acta Mater. 60(3), 977 (2012)10.1016/j.actamat.2011.11.005 ↗
8. D.S. Gianola, S. Van Petegem, M. Legros, S. Brandstetter, H. Van Swygenhoven, K.J. Hemker, Stress-assisted discontinuous grain growth and its effect on the deformation behavior of nanocrystalline aluminum thin films. Acta Mater. 54(8), 2253 (2006)10.1016/j.actamat.2006.01.023 ↗
9. G. Dehm, C. Motz, C. Scheu, H. Clemens, P.H. Mayrhofer, C. Mitterer, Mechanical size-effects in miniaturized and bulk materials. Adv. Eng. Mater. 8(11), 1033 (2006)10.1002/adem.200600153 ↗
10. D. Kiener, W. Grosinger, G. Dehm, R. Pippan, A further step towards an understanding of size-dependent crystal plasticity: in situ tension experiments of miniaturized single-crystal copper samples. Acta Mater. 56(3), 580 (2008)10.1016/j.actamat.2007.10.015 ↗
11. C. Kirchlechner, D. Kiener, C. Motz, S. Labat, N. Vaxelaire, O. Perroud, J.-S. Micha, O. Ulrich, O. Thomas, G. Dehm, J. Keckes, Dislocation storage in single slip-oriented Cu micro-tensile samples: new insights via X-ray microdiffraction. Philos. Mag. 91(7–9), 1256 (2011)10.1080/14786431003785639 ↗
12. J.P. Liebig, M. Göken, G. Richter, M. Mackovic, T. Przybilla, E. Spiecker, O.N. Pierron, B. Merle, A flexible method for the preparation of thin film samples for in situ TEM characterization combining shadow-FIB milling and electron-beam-assisted etching. Ultramicroscopy 171, 82 (2016)10.1016/j.ultramic.2016.09.004 ↗
13. B. Merle, H.W. Höppel, Microscale high-cycle fatigue testing by dynamic micropillar compression using continuous stiffness measurement. Exp. Mech. 58(3), 465 (2018)10.1007/s11340-017-0362-3 ↗
14. S. Gabel, B. Merle, Small-scale high-cycle fatigue testing by dynamic microcantilever bending. MRS Commun. 10(2), 332 (2020)10.1557/mrc.2020.31 ↗
15. J.R. Greer, W.D. Nix, Nanoscale gold pillars strengthened through dislocation starvation. Phys. Rev. B Condens. Matter Mater. Phys. 73(24), 245410 (2006)10.1103/PhysRevB.73.245410 ↗
16. S.C. Pun, W. Wang, A. Khalajhedayati, J.D. Schuler, J.R. Trelewicz, T.J. Rupert, Nanocrystalline Al-Mg with extreme strength due to grain boundary doping. Mater. Sci. Eng. A 696, 400 (2017)10.1016/j.msea.2017.04.095 ↗
17. S. Korte, W.J. Clegg, Micropillar compression of ceramics at elevated temperatures. Scr. Mater. 60(9), 807 (2009)10.1016/j.scriptamat.2009.01.029 ↗
18. J. Schwiedrzik, R. Raghavan, A. Bürki, V. Lenader, U. Wolfram, J. Michler, P. Zysset, In situ micropillar compression reveals superior strength and ductility but an absence of damage in lamellar bone. Nat. Mater. 13(7), 740 (2014)10.1038/nmat3959 ↗
19. Y. Xiao, Y. Zou, A.S. Sologubenko, R. Spolenak, J.M. Wheeler, Size-dependent strengthening in multi-principal element, face-centered cubic alloys. Mater. Des. 193, 108786 (2020)10.1016/j.matdes.2020.108786 ↗
20. D. Kiener, P. Hosemann, S.A. Maloy, A.M. Minor, In situ nanocompression testing of irradiated copper. Nat. Mater. 10(8), 608 (2011)10.1038/nmat3055 ↗
21. N.V. Malyar, H. Springer, J. Wichert, G. Dehm, C. Kirchlechner, Synthesis and mechanical testing of grain boundaries at the micro and sub-micro scale. Mater. Test. 61(1), 5 (2019)10.3139/120.111286 ↗
22. J.P. Liebig, S. Krauß, M. Göken, B. Merle, Influence of stacking fault energy and dislocation character on slip transfer at coherent twin boundaries studied by micropillar compression. Acta Mater. 154, 261 (2018)10.1016/j.actamat.2018.05.037 ↗
23. S. Krauß, T. Schieß, M. Göken, B. Merle, Revealing the local fatigue behavior of bimodal copper laminates by micropillar fatigue tests. Mater. Sci. Eng. A 788, 139502 (2020)10.1016/j.msea.2020.139502 ↗
24. N.V. Malyar, J.S. Micha, G. Dehm, C. Kirchlechner, Dislocation-twin boundary interaction in small scale Cu bi-crystals loaded in different crystallographic directions. Acta Mater. 129, 91 (2017)10.1016/j.actamat.2017.02.067 ↗
25. P.J. Imrich, C. Kirchlechner, C. Motz, G. Dehm, Differences in deformation behavior of bicrystalline Cu micropillars containing a twin boundary or a large-angle grain boundary. Acta Mater. 73, 240 (2014)10.1016/j.actamat.2014.04.022 ↗
26. E.I. Preiß, B. Merle, M. Göken, Understanding the extremely low fracture toughness of freestanding gold thin films by in-situ bulge testing in an AFM. Mater. Sci. Eng. A 691, 218 (2017)10.1016/j.msea.2017.03.037 ↗
27. E.I. Preiß, H. Lyu, J.P. Liebig, G. Richter, F. Gannott, P.A. Gruber, M. Göken, E. Bitzek, B. Merle, Microstructural dependence of the fracture toughness of metallic thin films: a bulge test and atomistic simulation study on single-crystalline and polycrystalline silver films. J. Mater. Res. 34(20), 3483 (2019)10.1557/jmr.2019.262 ↗
28. E.I. Preiß, F. Gannott, M. Göken, B. Merle, Scaling of the fracture toughness of freestanding metallic thin films with the yield strength. Mater. Res. Lett. 6(10), 607 (2018)10.1080/21663831.2018.1520749 ↗
29. T. Kondo, K. Hiramine, H. Hirakata, K. Minoshima, Fracture toughness of freestanding copper films with a thickness of 39 nm. Eng. Fr. 200, 521 (2018)
30. H. Hirakata, Y. Takeda, T. Kondo, K. Minoshima, Direct observation of the thickness effect on critical crack tip opening displacement in freestanding copper submicron-films by in situ electron microscopy fracture toughness testing. Int. J. Fract. 192(2), 203 (2015)10.1007/s10704-015-0003-8 ↗
31. I. Issa, A. Hohenwarter, R. Fritz, D. Kiener, Fracture properties of ultrafine grain chromium correlated to single dislocation processes at room temperature. J. Mater. Res. 34(13), 2370 (2019)10.1557/jmr.2019.140 ↗
32. D. Kiener, C. Motz, M. Rester, M. Jenko, G. Dehm, FIB damage of Cu and possible consequences for miniaturized mechanical tests. Mater. Sci. Eng. A 459(1), 262 (2007)10.1016/j.msea.2007.01.046 ↗
33. S. Shim, H. Bei, M.K. Miller, G.M. Pharr, E.P. George, Effects of focused ion beam milling on the compressive behavior of directionally solidified micropillars and the nanoindentation response of an electropolished surface. Acta Mater. 57(2), 503 (2009)10.1016/j.actamat.2008.09.033 ↗
34. H. Bei, S. Shim, M.K. Miller, G.M. Pharr, E.P. George, Effects of focused ion beam milling on the nanomechanical behavior of a molybdenum-alloy single crystal. Appl. Phys. Lett. 91(11), 111915 (2007)10.1063/1.2784948 ↗
35. Y. Xiao, J. Wehrs, H. Ma, T. Al-Samman, S. Korte-Kerzel, M. Göken, J. Michler, R. Spolenak, J.M. Wheeler, Investigation of the deformation behavior of aluminum micropillars produced by focused ion beam machining using Ga and Xe ions. Scr. Mater. 127, 191 (2017)10.1016/j.scriptamat.2016.08.028 ↗
36. Y. Xiao, V. Maier-Kiener, J. Michler, R. Spolenak, J.M. Wheeler, Deformation behavior of aluminum pillars produced by Xe and Ga focused ion beams: Insights from strain rate jump tests. Mater. Des. 181, 107914 (2019)10.1016/j.matdes.2019.107914 ↗
37. T. Vermeij, E. Plancher, C.C. Tasan, Preventing damage and redeposition during focused ion beam milling: the “umbrella” method. Ultramicroscopy 186, 35 (2018)10.1016/j.ultramic.2017.12.012 ↗
38. D. Kiener, Z. Zhang, S. Šturm, S. Cazottes, P.J. Imrich, C. Kirchlechner, G. Dehm, Advanced nanomechanics in the TEM: effects of thermal annealing on FIB prepared Cu samples. Philos. Mag. 92(25–27), 3269 (2012)10.1080/14786435.2012.685966 ↗
39. S. Lee, J. Jeong, Y. Kim, S.M. Han, D. Kiener, S.H. Oh, FIB-induced dislocations in Al submicron pillars: annihilation by thermal annealing and effects on deformation behavior. Acta Mater. 110, 283 (2016)10.1016/j.actamat.2016.03.017 ↗
40. J.A. Liddle, H.A. Huggins, P. Mulgrew, L.R. Harriott, H.H. Wade, K. Bolan, Fracture strength of thin ceramic membranes. Mater. Res. Soc. Symp. Proc. 338, 501 (1994)10.1557/PROC-338-501 ↗
41. Y. Xiang, J. McKinnell, W.-M. Ang, J.J. Vlassak, Measuring the fracture toughness of ultra-thin films with application to AlTa coatings. Int. J. Fract. 144(3), 173 (2007)10.1007/s10704-007-9095-0 ↗
42. B. Merle, M. Göken, Fracture toughness of silicon nitride thin films of different thicknesses as measured by bulge tests. Acta Mater. 59(4), 1772 (2011)10.1016/j.actamat.2010.11.043 ↗
43. J.I. Bluhm, A model for the effect of thickness on fracture toughness. ASTM Proc. 61, 1324 (1961)
44. J.F. Knott, Fundamentals of Fracture Mechanics (Butterworth and Co., London, 1973).
45. H. Hirakata, T. Yoshida, T. Kondo, K. Minoshima, Effects of film thickness on critical crack tip opening displacement in single-crystalline and polycrystalline submicron Cu films. Eng. Fract. Mech. 159, 98 (2016)10.1016/j.engfracmech.2016.03.031 ↗
46. S. Jaddi, M. Coulombier, J.-P. Raskin, T. Pardoen, Crack on a chip test method for thin freestanding films. J. Mech. Phys. Solids 123, 267 (2019)10.1016/j.jmps.2018.10.005 ↗
47. H.D. Espinosa, B. Peng, A new methodology to investigate fracture toughness of freestanding MEMS and advanced materials in thin film form. J. Microelectromech. Syst. 14(1), 153 (2005)10.1109/JMEMS.2004.839013 ↗
48. E. Hosseinian, S. Gupta, O.N. Pierron, M. Legros, Size effects on intergranular crack growth mechanisms in ultrathin nanocrystalline gold free-standing films. Acta Mater. 143, 77 (2018)10.1016/j.actamat.2017.10.004 ↗
49. D. Picard, D. Leguillon, C. Putot, A method to estimate the influence of the notch-root radius on the fracture toughness measurement of ceramics. J. Eur. Ceram. Soc. 26(8), 1421 (2006)10.1016/j.jeurceramsoc.2005.02.016 ↗
50. M.D. Drory, R.H. Dauskardt, A. Kant, R.O. Ritchie, Fracture of synthetic diamond. J. Appl. Phys. 78(5), 3083 (1995)10.1063/1.360060 ↗
51. J.F. Ziegler, M.D. Ziegler, J.P. Biersack, SRIM—the stopping and range of ions in matter (2010). Nucl. Instrum. Methods Phys. Res. Sect. B Beam Interact. Mater. At. 268(11), 1818 (2010)10.1016/j.nimb.2010.02.091 ↗
52. J. Guénolé, A. Prakash, E. Bitzek, Atomistic simulations of focused ion beam machining of strained silicon. Appl. Surf. Sci. 416, 86 (2017)10.1016/j.apsusc.2017.04.027 ↗
53. T.C. Pekin, F.I. Allen, A.M. Minor, Evaluation of neon focused ion beam milling for TEM sample preparation. J. Microsc. 264(1), 59 (2016)10.1111/jmi.12416 ↗
54. S. Tan, R. Livengood, P. Hack, R. Hallstein, D. Shima, J. Notte, S. McVey, Nanomachining with a focused neon beam: A preliminary investigation for semiconductor circuit editing and failure analysis. J. Vac. Sci. Technol. B Nanotechnol. Microelectron. Mater. Process. Meas. Phenom. 29(6), 0604 (2011)
55. W.J. MoberlyChan, D.P. Adams, M.J. Aziz, G. Hobler, T. Schenkel, Fundamentals of focused ion beam nanostructural processing: below, at, and above the surface. MRS Bull. 32(5), 424 (2007)10.1557/mrs2007.66 ↗
56. D.J. Barber, Radiation damage in ion-milled specimens: characteristics, effects and methods of damage limitation. Ultramicroscopy 52(1), 101 (1993)10.1016/0304-3991(93)90025-S ↗
57. J. Ast, M. Ghidelli, K. Durst, M. Göken, M. Sebastiani, A.M. Korsunsky, A review of experimental approaches to fracture toughness evaluation at the micro-scale. Mater. Des. 173, 107762 (2019)10.1016/j.matdes.2019.107762 ↗
58. S. Schmidt, W. Sigle, W. Gust, M. Rühle, Gallium segregation at grain boundaries in aluminium. Z. Für Met. 93(5), 428 (2002)10.3139/146.020428 ↗
59. R.P. Elliott, F.A. Shunk, The Au-Ga (Gold-Gallium) system. Bull. Alloy Phase Diagr. 2(3), 356 (1981)10.1007/BF02868293 ↗
60. A.D. Norton, S. Falco, N. Young, J. Severs, R.I. Todd, Microcantilever investigation of fracture toughness and subcritical crack growth on the scale of the microstructure in Al2O3. J. Eur. Ceram. Soc. 35(16), 4521 (2015)10.1016/j.jeurceramsoc.2015.08.023 ↗
61. J.P. Best, J. Zechner, I. Shorubalko, J.V. Oboňa, J. Wehrs, M. Morstein, J. Michler, A comparison of three different notching ions for small-scale fracture toughness measurement. Scr. Mater. 112, 71 (2016)10.1016/j.scriptamat.2015.09.014 ↗
62. C.M. Lauener, L. Petho, M. Chen, Y. Xiao, J. Michler, J.M. Wheeler, Fracture of Silicon: Influence of rate, positioning accuracy, FIB machining, and elevated temperatures on toughness measured by pillar indentation splitting. Mater. Des. 142, 340 (2018)10.1016/j.matdes.2018.01.015 ↗
63. R. Estivill, G. Audoit, J.-P. Barnes, A. Grenier, D. Blavette, Preparation and analysis of atom probe tips by xenon focused ion beam milling. Microsc. Microanal. 22(3), 576 (2016)10.1017/S1431927616000581 ↗
64. K. Wittmaack, H. Oppolzer, Quantitative characterization of xenon bubbles in silicon: Correlation of bubble size with the damage generated during implantation. Nucl. Instrum. Methods Phys. Res. Sect. B Beam Interact. Mater. At. 269(3), 380 (2011)10.1016/j.nimb.2010.11.025 ↗
65. J. Hütsch, E.T. Lilleodden, The influence of focused-ion beam preparation technique on microcompression investigations. Scr. Mater. 77, 49 (2014)10.1016/j.scriptamat.2014.01.016 ↗
66. B.N. Jaya, C. Kirchlechner, G. Dehm, Can microscale fracture tests provide reliable fracture toughness values? A case study in silicon. J. Mater. Res. 30(5), 686 (2015)10.1557/jmr.2015.2 ↗
67. J. Ast, B. Merle, K. Durst, M. Göken, Fracture toughness evaluation of NiAl single crystals by microcantilevers—a new continuous J-integral method. J. Mater. Res. 31(23), 3786 (2016)10.1557/jmr.2016.393 ↗
68. I. Utke, P. Hoffmann, J. Melngailis, Gas-assisted focused electron beam and ion beam processing and fabrication. J. Vac. Sci. Technol. B Microelectron. Nanometer Struct. Process. Meas. Phenom. 26(4), 1197 (2008)10.1116/1.2955728 ↗
69. C.R.M. Grovenor, H.T.G. Hentzell, D.A. Smith, The development of grain structure during growth of metallic films. Acta Metall. 32(5), 773 (1984)10.1016/0001-6160(84)90150-0 ↗
70. J.A. Thornton, Influence of apparatus geometry and deposition conditions on the structure and topography of thick sputtered coatings. J. Vac. Sci. Technol. 11(4), 666 (1974)10.1116/1.1312732 ↗
71. J.J. Vlassak, W.D. Nix, New bulge test technique for the determination of Young’s modulus and Poisson’s ratio of thin films. J. Mater. Res. 7(12), 3242 (1992)10.1557/JMR.1992.3242 ↗
72. G.R. Irwin, Fracture, in Handbook of Physics (Springer, Berlin, 1958), p. 551.10.1007/978-3-642-45887-3_5 ↗