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02-12-2016 | Original Paper

In situ hard X-ray transmission microscopy for material science

Authors: Ken Vidar Falch, Daniele Casari, Marco Di Michiel, Carsten Detlefs, Anatoly Snigireva, Irina Snigireva, Veijo Honkimäki, Ragnvald H. Mathiesen

Published in: Journal of Materials Science | Issue 6/2017

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Abstract

Hard X-ray transmission microscopy based on refractive X-ray optics can be employed as a tool in material science to investigate buried-in microstructures in two or three dimensions with spatial resolution approaching 100 nm. Switching from monochromatic to radiation with a broader bandwidth, frame rates down to a few milliseconds can be realized, opening new possibilities for in situ studies of microstructure evolution and response to external fields at spatiotemporal resolutions that go well beyond previous benchmarks, demonstrated by ~200 nm resolution tomograms of eutectic microstructures acquired in less than 2 s. The microscope can also be operated in Zernike phase contrast mode, which expands the range of possible applications to cases which otherwise would produce only very faint contrast. A few possible application areas for the microscope are illustrated by a selection of material science test cases.

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Rack A, Scheel M, Hardy L, Curfs C, Bonnin A, Reichert H (2014) Exploiting coherence for real-time studies by single-bunch imaging. J Synchrotron Radiat 21:815–818. doi:10.1107/S1600577514005852 CrossRef

Rack A, Scheel M, Danilewsky AN (2016) Real-time direct and diffraction X-ray imaging of irregular silicon wafer breakage. Iucrj 3:108–114. doi:10.1107/S205225251502271x CrossRef

Pelliccia D, Rack A, Scheel M, Cantelli V, Paganin DM (2016) Experimental X-ray ghost imaging. Phys Rev Lett 117(11):113902. doi:10.1103/PhysRevLett.117.113902 CrossRef

Douissard PA, Cecilia A, Rochet X, Chapel X, Martin T, van de Kamp T, Helfen L, Baumbach T, Luquot L, Xiao X, Meinhardt J, Rack A (2012) A versatile indirect detector design for hard X-ray microimaging. J Instrum. doi:10.1088/1748-0221/7/09/P09016

Nguyen-Thi H, Reinhart G, Salloum-Abou-Jaoude G, Browne DJ, Murphy AG, Houltz Y, Li J, Voss D, Verga A, Mathiesen RH, Zimmermann G (2014) XRMON-GF experiments devoted to the in situ X-ray radiographic observation of growth process in microgravity conditions. Microgravity Sci Technol 26(1):37–50. doi:10.1007/s12217-014-9370-4 CrossRef

Murphy AG, Browne DJ, Mirihanage WU, Mathiesen RH (2013) Combined in situ X-ray radiographic observations and post-solidification metallographic characterisation of eutectic transformations in Al-Cu alloy systems. Acta Mater 61(12):4559–4571. doi:10.1016/j.actamat.2013.04.024 CrossRef

Hopkins HH, Barham PM (1950) The Influence of the Condenser on Microscopic Resolution. P Phys Soc Lond B 63(370):737–744. doi:10.1088/0370-1301/63/10/301 CrossRef

Schroer CG, Kuhlmann M, Lengeler B, Gunzler TF, Kurapova O, Benner B, Rau C, Simionovici AS, Snigirev AA, Snigireva I (2002) Beryllium parabolic refractive X-ray lenses. Des Microfabr of Novel X-ray Opt 4783:10–18. doi:10.1117/12.451013 CrossRef

Matsuyama S, Emi Y, Kino H, Kohmura Y, Yabashi M, Ishikawa T, Yamauchi K (2015) Achromatic and high-resolution full-field X-ray microscopy based on total-reflection mirrors. Opt Express 23(8):9746–9752. doi:10.1364/Oe.23.009746 CrossRef

10.

Koyama T, Takano H, Konishi S, Tsuji T, Takenaka H, Ichimaru S, Ohchi T, Kagoshima Y (2012) Circular multilayer zone plate for high-energy x-ray nano-imaging. Rev Sci Instrum 83(1):013705. doi:10.1063/1.3676165 CrossRef

11.

Baez AV (1961) Fresnel zone plate for optical image formation using extreme ultraviolet and soft X radiation. J Opt Soc Am 51(4):405–412CrossRef

12.

Kirz J, Rarback H (1985) Soft-X-ray microscopes. Rev Sci Instrum 56(1):1–13. doi:10.1063/1.1138464 CrossRef

13.

Jacobsen C (1999) Soft x-ray microscopy. Trends Cell Biol 9(2):44–47. doi:10.1016/S0962-8924(98)01424-X CrossRef

14.

Wu SR, Hwu Y, Margaritondo G (2012) Hard-X-ray Zone Plates: Recent Progress. Materials 5(10):1752–1773. doi:10.3390/ma5101752

15.

Chao W, Kim J, Rekawa S, Fischer P, Anderson EH (2009) Demonstration of 12 nm resolution Fresnel Zone plate lens based soft X-ray microscopy. Opt Express 17(20):17669–17677. doi:10.1364/Oe.17.017669 CrossRef

16.

Snigireva I, Vaughan GBM, Snigirev A (2011) High-energy nanoscale-resolution X-ray microscopy based on refractive optics on a long beamline. 10th International Conference on X-Ray Microscopy 1365:188–191

17.

Mathiesen RH, Arnberg L, Nguyen-Thi H, Billia B (2012) In situ X-ray video microscopy as a tool in solidification science. Jom-Us 64(1):76–82. doi:10.1007/s11837-011-0213-0 CrossRef

18.

Zabler S, Rueda A, Rack A, Riesemeier H, Zaslansky P, Manke I, Garcia-Moreno F, Banhart J (2007) Coarsening of grain-refined semi-solid Al-Ge32 alloy: X-ray microtomography and in situ radiography. Acta Mater 55(15):5045–5055. doi:10.1016/j.actamat.2007.05.028 CrossRef

19.

Falch KV, Lyubomirskij M, Casari D, Detlefs C, Snigirev A, Snigireva I, Di Michiel M, Mathiesen R (2016) Zernike phase contrast in high-energy X-ray transmission microscopy based on refractive optics. Ultramicroscopy under review.

20.

X-ray chart NTT-AT. http://www.ntt-at.com/product/x-ray_chart/http://www.ntt-at.com/product/x-ray_chart/. Accessed 23 Nov 2016

21.

Huang XJ, Conley R, Bouet N, Zhou J, Macrander A, Maser J, Yan HF, Nazaretski E, Lauer K, Harder R, Robinson IK, Kalbfleisch S, Chu YS (2015) Achieving hard X-ray nanofocusing using a wedged multilayer Laue lens. Opt Express 23(10):12496–12507. doi:10.1364/Oe.23.012496 CrossRef

22.

Niese S, Krueger P, Kubec A, Braun S, Patommel J, Schroer CG, Leson A, Zschech E (2014) Full-field X-ray microscopy with crossed partial multilayer Laue lenses. Opt Express 22(17):20008–20013. doi:10.1364/Oe.22.020008 CrossRef

23.

Nazaretski E, Yan H, Lauer K, Huang X, Xu W, Kalbfleisch S, Yan H, Li L, Bouet N, Zhou J, Shu D, Conley R, Chu YS (2016) Nm-scale spatial resolution X-ray imaging with MLL nanofocusing optics: instrumentational requirements and challenges. AIP Conf Proc 1764(1):040001. doi:10.1063/1.4961143 CrossRef

24.

Nazaretski E, Xu W, Bouet N, Zhou J, Yan H, Huang X, Chu YS (2016) Development and characterization of monolithic multilayer Laue lens nanofocusing optics. Appl Phys Lett 108(26):261102. doi:10.1063/1.4955022 CrossRef

25.

Als-Nielsen J, McMorrow D (2011) Elements of modern X-ray physics. Wiley, HobokenCrossRef

26.

Born MAX, Wolf E (1980) CHAPTER V—geometrical theory of aberrations. In: principles of optics (sixth (corrected) edition). Pergamon, pp 203–232. doi:10.1016/B978-0-08-026482-0.50012-8

27.

Born MAX, Wolf E (1980) chapter VI—Image-FORMING INSTRUMents. In: Principles of Optics (sixth (corrected) edition). Pergamon, pp 233–255. doi: 10.1016/B978-0-08-026482-0.50013-X

28.

Falch KV, Detlefs C, Di Michiel M, Snigireva I, Snigirev A, Mathiesen RH (2016) Correcting lateral chromatic aberrations in non-monochromatic X-ray microscopy. Appl Phys Lett 109(5):054103. doi:10.1063/1.4960193 CrossRef

29.

Dimper RR, H.;Raimondi P, Ortiz LS; Sette F, Susini J (2015) ESRF upgrade programme phase II

30.

Leemann SC, Andersson A, Eriksson M, Lindgren LJ, Wallen E, Bengtsson J, Streun A (2009) Beam dynamics and expected performance of Sweden’s new storage-ring light source: MAX IV. Phys Rev Spec Top-Ac 12(12):120701. doi: 10.1103/PhysRevSTAB.12.120701

31.

Donoghue PCJ, Bengtson S, Dong XP, Gostling NJ, Huldtgren T, Cunningham JA, Yin C, Yue Z, Peng F, Stampanoni M (2006) Synchrotron X-ray tomographic microscopy of fossil embryos. Nature 442(7103):680–683. doi:10.1038/nature04890 CrossRef

32.

Weiss D, Schneider G, Niemann B, Guttmann P, Rudolph D, Schmahl G (2000) Computed tomography of cryogenic biological specimens based on X-ray microscopic images. Ultramicroscopy 84(3–4):185–197. doi:10.1016/S0304-3991(00)00034-6 CrossRef

33.

Zernike F (1942) Phase contrast, a new method for the microscopic observation of transparent objects. Physica 9(7):686–698. doi:10.1016/S0031-8914(42)80035-X CrossRef

34.

Snigirev A, Snigireva I, Kohn V, Kuznetsov S, Schelokov I (1995) On the possibilities of x-ray phase contrast microimaging by coherent high-energy synchrotron radiation. Rev Sci Instrum 66(12):5486–5492. doi:10.1063/1.1146073 CrossRef

35.

Mokso R, Cloetens P, Maire E, Ludwig W, Buffiere JY (2007) Nanoscale zoom tomography with hard X rays using Kirkpatrick-Baez optics. Appl Phys Lett 90(14):144104. doi:10.1063/1.2719653 CrossRef

36.

Cloetens P, Barrett R, Baruchel J, Guigay JP, Schlenker M (1996) Phase objects in synchrotron radiation hard X-ray imaging. J Phys D Appl Phys 29(1):133–146. doi:10.1088/0022-3727/29/1/023 CrossRef

37.

Hegde S, Prabhu KN (2008) Modification of eutectic silicon in Al-Si alloys. J Mater Sci 43(9):3009–3027. doi:10.1007/s10853-008-2505-5 CrossRef

38.

Li JH, Albu M, Ludwig TH, Matsubara Y, Hofer F, Arnberg L, Tsunekawa Y, Schumacher P (2014) Modification of eutectic Si in Al-Si based alloys. Mater Sci Forum 794–796:130–136. doi:10.4028/www.scientific.net/MSF.794-796.130 CrossRef

39.

Ludwig TH, Li JH, Schaffer PL, Schumacher P, Arnberg L (2015) Refinement of Eutectic Si in High Purity Al-5Si Alloys with Combined Ca and P Additions. Metall Mater Trans A 46(1):362–376. doi:10.1007/s11661-014-2585-6 CrossRef

40.

Li JH, Barrirero J, Engstler M, Aboulfadl H, Mucklich F, Schumacher P (2015) Nucleation and Growth of Eutectic Si in Al-Si Alloys with Na Addition. Metall Mater Trans A 46(3):1300–1311. doi:10.1007/s11661-014-2702-6 CrossRef

41.

Barrirero J, Li JH, Engstler M, Ghafoor N, Schumacher P, Oden M, Mucklich F (2016) Cluster formation at the Si/liquid interface in Sr and Na modified Al-Si alloys. Scripta Mater 117:16–19. doi:10.1016/j.scriptamat.2016.02.018 CrossRef

42.

West R, Fredriksson H (1985) On the mechanism of facetted growth. J Mater Sci 20(3):1061–1068. doi:10.1007/Bf00585750 CrossRef

43.

Wang RY, Lu WH, Hogan LM (1999) Growth morphology of primary silicon in cast Al-Si alloys and the mechanism of concentric growth. J Cryst Growth 207(1–2):43–54. doi:10.1016/S0022-0248(99)00347-4 CrossRef

44.

Mathiesen RH, Arnberg L, Li Y, Meier V, Schaffer PL, Snigireva I, Snigirev A, Dahle AK (2011) X-ray videomicroscopy studies of eutectic Al-Si solidification in Al-Si-Cu. Metall Mater Trans A 42(1):170–180. doi:10.1007/s11661-010-0443-8 CrossRef

45.

Jackson KA, Hunt JD (1966) Lamellar and rod eutectic growth. T Metall Soc AIME 236(8):1129–1142

46.

Trivedi R, Magnin P, Kurz W (1987) Theory of eutectic growth under rapid solidification conditions. Acta Metall 35(4):971–980. doi:10.1016/0001-6160(87)90176-3 CrossRef

47.

Magnin P, Trivedi R (1991) Eutectic growth—a modification of the Jackson and Hunt theory. Acta Metall Mater 39(4):453–467. doi:10.1016/0956-7151(91)90114-G CrossRef

48.

Karma A, Sarkissian A (1996) Morphological instabilities of lamellar eutectics. Metall Mater Trans A 27(3):635–656. doi:10.1007/Bf02648952 CrossRef

49.

Ginibre M, Akamatsu S, Faivre G (1997) Experimental determination of the stability diagram of a lamellar eutectic growth front. Phys Rev E 56(1):780–796. doi:10.1103/PhysRevE.56.780 CrossRef

50.

Akamatsu S, Bottin-Rousseau S, Faivre G (2004) Experimental evidence for a zigzag bifurcation in bulk lamellar eutectic growth. Phys Rev Lett 93(17):175701. doi:10.1103/PhysRevLett.93.175701 CrossRef

51.

Akamatsu S, Plapp M, Faivre G, Karma A (2004) Overstability of lamellar eutectic growth below the minimum-undercooling spacing. Metall Mater Trans A 35(6):1815–1828. doi:10.1007/s11661-004-0090-z CrossRef

52.

Akamatsu S, Bottin-Rousseau S, Perrut M, Faivre G, Witusiewicz VT, Sturz L (2007) Real-time study of thin and bulk eutectic growth in succinonitrile-(D)camphor alloys. J Cryst Growth 299(2):418–428. doi:10.1016/j.jcrysgro.2006.11.271 CrossRef

53.

De Wilde J, Froyen L, Witusiewicz VT, Hecht U (2005) Two-phase planar and regular lamellar coupled growth along the univariant eutectic reaction in ternary alloys: an analytical approach and application to the Al-Cu-Ag system. J Appl Phys 97(11):113515. doi:10.1063/1.1906286 CrossRef

54.

Zimmermann G, Hecht U, Mathes M, Mathiesen RH (2010) Time resolved X-ray imaging of eutectic cellular patterns evolving during solidification of ternary Al-Cu-Ag alloys. Int J Mater Res 101(12):1484–1488. doi:10.3139/146.110435 CrossRef

55.

Park JM, Kim DH, Mattern N, Kim KB, Fleury E, Eckert J (2011) Microstructure and mechanical properties of Fe-Si-Ti-(Cu, Al) heterostructured ultrafine composites. J Alloy Compd 509:S367–S370. doi:10.1016/j.jallcom.2010.10.112 CrossRef

56.

Kim TE, Park JM, Kuhn U, Eckert J, Kim WT, Kim DH (2012) In situ martensitic phase reinforced Fe-Nb-Ni-Mn ultrafine composite with enhanced mechanical properties. Mat Sci Eng A-Struct 531:51–54. doi:10.1016/j.msea.2011.10.012 CrossRef

57.

Park JM, Kim TE, Sohn SW, Kim DH, Kim KB, Kim WT, Eckert J (2008) High strength Ni-Zr binary ultrafine eutectic-dendrite composite with large plastic deformability. Appl Phys Lett 93(3):031913. doi:10.1063/1.2952755 CrossRef

58.

Tiwary CS, Mahapatra DR, Chattopadhyay K (2012) Effect of length scale on mechanical properties of Al-Cu eutectic alloy. Appl Phys Lett 101(17):171901. doi:10.1063/1.4761944 CrossRef

59.

Narayanan T (2009) High brilliance small-angle X-ray scattering applied to soft matter. Curr Opin Colloid Interface sc i 14(6):409–415. doi:10.1016/j.cocis.2009.05.005 CrossRef

60.

Petoukhov MV, Svergun DI (2013) Applications of small-angle X-ray scattering to biomacromolecular solutions. Int J Biochem Cell B 45(2):429–437. doi:10.1016/j.biocel.2012.10.017 CrossRef

61.

Ozin GA, Yang SM (2001) The race for the photonic chip: colloidal crystal assembly in silicon wafers. Adv Funct Mater 11(2):95–104. doi:10.1002/1616-3028(200104)11:2<95:Aid-Adfm95>3.0.Co;2-O CrossRef

62.

You JX, Wang LL, Wang ZJ, Li JJ, Wang JC, Lin X, Huang WD (2016) Interfacial undercooling in solidification of colloidal suspensions: analyses with quantitative measurements. Sci Rep-Uk 6:28434. doi:10.1038/srep28434 CrossRef

63.

Schall P, Cohen I, Weitz DA, Spaepen F (2006) Visualizing dislocation nucleation by indenting colloidal crystals. Nature 440(7082):319–323. doi:10.1038/nature04557 CrossRef

64.

Schall P, Cohen I, Weitz DA, Spaepen F (2004) Visualization of dislocation dynamics in colloidal crystals. Science 305(5692):1944–1948. doi:10.1126/science.1102186 CrossRef

65.

Thijssen JHJ, Petukhov AV, ‘T Hart DC, Imhof A, van der Werf CHM, Schropp REI, van Blaaderen A (2006) Characterization of photonic colloidal single crystals by microradian X-ray diffraction. Adv Mater 18(13):1662–1666. doi:10.1002/adma.200502732 CrossRef

66.

Nho HW, Kalegowda Y, Shin HJ, Yoon TH (2016) Nanoscale characterization of local structures and defects in photonic crystals using synchrotron-based transmission soft X-ray microscopy. Sci Rep UK. doi:10.1038/srep24488

67.

Sitters G, Heller I, Broekmans OD, Farge G, Menges C, Wende W, Hell SW, Peterman EJG, Wuite GJ (2014) STED nanoscopy combined with optical tweezers reveals protein dynamics on densely covered DNA. Opt Trapp Opt Micromanip Xi. doi:10.1117/12.2062819

Title: In situ hard X-ray transmission microscopy for material science
Authors: Ken Vidar Falch
Daniele Casari
Marco Di Michiel
Carsten Detlefs
Anatoly Snigireva
Irina Snigireva
Veijo Honkimäki
Ragnvald H. Mathiesen
Publication date: 02-12-2016
Publisher: Springer US
Published in: Journal of Materials Science / Issue 6/2017
Print ISSN: 0022-2461
Electronic ISSN: 1573-4803
DOI: https://doi.org/10.1007/s10853-016-0643-8

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