Ion beam lithography for Fresnel zone plates in X-ray microscopy

Kahraman Keskinbora; Corinne Grévent; Michael Bechtel; Markus Weigand; Eberhard Goering; Achim Nadzeyka; Lloyd Peto; Stefan Rehbein; Gerd Schneider; Rolf Follath; Joan Vila-Comamala; Hanfei Yan; Gisela Schütz

doi:10.1364/OE.21.011747

Ion beam lithography for Fresnel zone plates in X-ray microscopy

Kahraman Keskinbora, Corinne Grévent, Michael Bechtel, Markus Weigand, Eberhard Goering, Achim Nadzeyka, Lloyd Peto, Stefan Rehbein, Gerd Schneider, Rolf Follath, Joan Vila-Comamala, Hanfei Yan, and Gisela Schütz

Optics Express
Vol. 21,
Issue 10,
pp. 11747-11756
(2013)
•https://doi.org/10.1364/OE.21.011747

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Kahraman Keskinbora, Corinne Grévent, Michael Bechtel, Markus Weigand, Eberhard Goering, Achim Nadzeyka, Lloyd Peto, Stefan Rehbein, Gerd Schneider, Rolf Follath, Joan Vila-Comamala, Hanfei Yan, and Gisela Schütz, "Ion beam lithography for Fresnel zone plates in X-ray microscopy," Opt. Express 21, 11747-11756 (2013)

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Related Topics
Table of Contents Category
- Microscopy
Optics & Photonics Topics
?

The topics in this list come from the OSA Optics and Photonics Topics applied to this article.
Previously assigned OCIS codes
- Diffractive lenses (050.1965)
- Scanning microscopy (180.5810)
- X-ray microscopy (180.7460)
- X-ray optics (340.0340)
- Synchrotron radiation (340.6720)
- X-ray microscopy (340.7460)
- X-rays, soft x-rays, extreme ultraviolet (EUV) (340.7480)

About this Article
History
- Original Manuscript: January 29, 2013
- Revised Manuscript: April 15, 2013
- Manuscript Accepted: April 17, 2013
- Published: May 7, 2013
Virtual Issues
Virtual Journal for Biomedical Optics Vol. 8, Iss. 6

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Open Access

Abstract

Fresnel Zone Plates (FZP) are to date very successful focusing optics for X-rays. Established methods of fabrication are rather complex and based on electron beam lithography (EBL). Here, we show that ion beam lithography (IBL) may advantageously simplify their preparation. A FZP operable from the extreme UV to the limit of the hard X-ray was prepared and tested from 450 eV to 1500 eV. The trapezoidal profile of the FZP favorably activates its 2nd order focus. The FZP with an outermost zone width of 100 nm allows the visualization of features down to 61, 31 and 21 nm in the 1st, 2nd and 3rd order focus respectively. Measured efficiencies in the 1st and 2nd order of diffraction reach the theoretical predictions.

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[Crossref]
J. Gierak, E. Bourhis, G. Faini, G. Patriarche, A. Madouri, R. Jede, L. Bruchhaus, S. Bauerdick, B. Schiedt, A. L. Biance, and L. Auvray, “Exploration of the ultimate patterning potential achievable with focused ion beams,” Ultramicroscopy 109(5), 457–462 (2009).
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[Crossref]

2012 (11)

J. Gelb, “Functionality to failure: Materials Reegineering in the 4th dimension,” Adv. Mater. Process. 170, 14–18 (2012).

T. Popmintchev, M. C. Chen, D. Popmintchev, P. Arpin, S. Brown, S. Alisauskas, G. Andriukaitis, T. Balciunas, O. D. Mücke, A. Pugzlys, A. Baltuska, B. Shim, S. E. Schrauth, A. Gaeta, C. Hernández-García, L. Plaja, A. Becker, A. Jaron-Becker, M. M. Murnane, and H. C. Kapteyn, “Bright Coherent Ultrahigh Harmonics in the keV x-ray Regime from Mid-Infrared Femtosecond Lasers,” Science 336(6086), 1287–1291 (2012).
[Crossref] [PubMed]

S. P. D. Mangles, “Compact X-ray sources: X-rays from self-reflection,” Nat. Photonics 6(5), 280–281 (2012).
[Crossref]

K. Bourzac, “Tabletop X-rays light up,” Nature 486(7402), 172 (2012).
[Crossref] [PubMed]

A. Guilherme, G. Buzanich, and M. L. Carvalho, “Focusing systems for the generation of X-ray micro beam: An overview,” Spectroc. Acta Pt. B-Atom. Spectr. 77, 1–8 (2012).

W. Chao, P. Fischer, T. Tyliszczak, S. Rekawa, E. Anderson, and P. Naulleau, “Real space soft x-ray imaging at 10 nm spatial resolution,” Opt. Express 20(9), 9777–9783 (2012).
[Crossref] [PubMed]

S. Rehbein, P. Guttmann, S. Werner, and G. Schneider, “Characterization of the resolving power and contrast transfer function of a transmission X-ray microscope with partially coherent illumination,” Opt. Express 20(6), 5830–5839 (2012).
[Crossref] [PubMed]

S. R. Wu, Y. Hwu, and G. Margaritondo, “Hard-X-ray zone plates: Recent progress,” Materials 5(12), 1752–1773 (2012).
[Crossref]

A. Nadzeyka, L. Peto, S. Bauerdick, M. Mayer, K. Keskinbora, C. Grevent, M. Weigand, M. Hirscher, and G. Schutz, “Ion beam lithography for direct patterning of high accuracy large area X-ray elements in gold on membranes,” Microelectron. Eng. 98, 198–201 (2012).
[Crossref]

J. E. E. Baglin, “Ion beam nanoscale fabrication and lithography-A review,” Appl. Surf. Sci. 258(9), 4103–4111 (2012).
[Crossref]

L. Bruchhaus, S. Bauerdick, L. Peto, U. Barth, A. Rudzinski, J. Mussmann, J. Klingfus, J. Gierak, and H. Hovel, “High resolution and high density ion beam lithography employing HSQ resist,” Microelectron. Eng. 97, 48–50 (2012).
[Crossref]

2011 (7)

J. Yi, Y. S. Chu, Y.-T. Chen, T.-Y. Chen, Y. Hwu, and G. Margaritondo, “High-resolution hard-x-ray microscopy using second-order zone-plate diffraction,” J. Phys. D Appl. Phys. 44(23), 232001 (2011).
[Crossref]

M. Mayer, C. Grévent, A. Szeghalmi, M. Knez, M. Weigand, S. Rehbein, G. Schneider, B. Baretzky, and G. Schütz, “Multilayer Fresnel zone plate for soft X-ray microscopy resolves sub-39nm structures,” Ultramicroscopy 111(12), 1706–1711 (2011).
[Crossref] [PubMed]

G. E. Ice, J. D. Budai, and J. W. L. Pang, “The race to X-ray microbeam and nanobeam science,” Science 334(6060), 1234–1239 (2011).
[Crossref] [PubMed]

F. Nachtrab, T. Ebensperger, B. Schummer, F. Sukowski, and R. Hanke, “Laboratory X-ray microscopy with a nano-focus X-ray source,” J. Instrum. 6, C11017 (2011).

E. Zschech, C. Wyon, C. E. Murray, and G. Schneider, “Devices, materials, and processes for nanoelectronics: Characterization with advanced X-ray techniques using lab-based and synchrotron radiation sources,” Adv. Eng. Mater. 13(8), 811–836 (2011).
[Crossref]

R. Falcone, C. Jacobsen, J. Kirz, S. Marchesini, D. Shapiro, and J. Spence, “New directions in X-ray microscopy,” Contemp. Phys. 52(4), 293–318 (2011).
[Crossref]

B. Kaulich, P. Thibault, A. Gianoncelli, and M. Kiskinova, “Transmission and emission x-ray microscopy: operation modes, contrast mechanisms and applications,” J. Phys.-Condes. Matter 23,083002 (2011).

2010 (2)

A. Cho, “Materials science. What shall we do with the x-ray laser?” Science 330(6010), 1470–1471 (2010).
[Crossref] [PubMed]

A. Sakdinawat and D. Attwood, “Nanoscale X-ray imaging,” Nat. Photonics 4(12), 840–848 (2010).
[Crossref]

2009 (3)

J. Vila-Comamala, K. Jefimovs, J. Raabe, T. Pilvi, R. H. Fink, M. Senoner, A. Maassdorf, M. Ritala, and C. David, “Advanced thin film technology for ultrahigh resolution X-ray microscopy,” Ultramicroscopy 109(11), 1360–1364 (2009).
[Crossref] [PubMed]

M. Fuchs, R. Weingartner, A. Popp, Z. Major, S. Becker, J. Osterhoff, I. Cortrie, B. Zeitler, R. Horlein, G. D. Tsakiris, U. Schramm, T. P. Rowlands-Rees, S. M. Hooker, D. Habs, F. Krausz, S. Karsch, and F. Gruner, “Laser-driven soft-X-ray undulator source,” Nat. Phys. 5(11), 826–829 (2009).
[Crossref]

J. Gierak, E. Bourhis, G. Faini, G. Patriarche, A. Madouri, R. Jede, L. Bruchhaus, S. Bauerdick, B. Schiedt, A. L. Biance, and L. Auvray, “Exploration of the ultimate patterning potential achievable with focused ion beams,” Ultramicroscopy 109(5), 457–462 (2009).
[Crossref] [PubMed]

2007 (2)

A. Surpi, S. Valizadeh, K. Leifer, and S. Lagomarsino, “Focused ion beam fabrication procedures of x-ray micro Fresnel zone plates,” J. Micromech. Microeng. 17(3), 617–622 (2007).
[Crossref]

H. Yan, J. Maser, A. Macrander, Q. Shen, S. Vogt, G. B. Stephenson, and H. C. Kang, “Takagi-Taupin description of x-ray dynamical diffraction from diffractive optics with large numerical aperture,” Phys. Rev. B 76(11), 115438 (2007).
[Crossref]

2005 (3)

J. Gierak, E. Bourhis, M. N. M. Combes, Y. Chriqui, I. Sagnes, D. Mailly, P. Hawkes, R. Jede, L. Bruchhaus, L. Bardotti, B. Prevel, A. Hannour, P. Melinon, A. Perez, J. Ferre, J. P. Jamet, A. Mougin, C. Chappert, and V. Mathet, “Exploration of the ultimate patterning potential achievable with focused ion beams,” Microelectron. Eng. 78–79, 266–278 (2005).
[Crossref]

A. A. Tseng, “Recent developments in nanofabrication using focused ion beams,” Small 1(10), 924–939 (2005).
[Crossref] [PubMed]

W. L. Chao, B. D. Harteneck, J. A. Liddle, E. H. Anderson, and D. T. Attwood, “Soft X-ray microscopy at a spatial resolution better than 15 nm,” Nature 435(7046), 1210–1213 (2005).
[Crossref] [PubMed]

2002 (2)

D. C. Joy, “SMART - a program to measure SEM resolution and imaging performance,” J. Microsc.-Oxf. 208, 24–34 (2002).

A. Kuyumchyan, A. A. Isoyan, E. V. Shulakov, V. V. Aristov, M. Kondratenkov, A. A. Snigirev, I. Snigireva, A. Souvorov, K. Tamasaku, M. Yabashi, T. Ishikawa, and K. Trouni, “High-efficiency and low-absorption Fresnel compound zone plates for hard X-ray focusing,” Proc. SPIE 4783, 92–96 (2002).

2001 (1)

P. P. Ilinski, B. Lai, N. J. Bassom, J. Donald, and G. Athas, “X-ray zone plate fabrication using a focused ion beam,” Proceedings of SPIE-The International Society for Optical Engineering 4145, 311–316 (2001).
[Crossref]

1994 (2)

M. Baciocchi, R. Maggiora, and M. Gentili, “High resolution fresnel zone plates for soft x-rays,” Microelectron. Eng. 23(1-4), 101–104 (1994).
[Crossref]

R. M. Bionta, K. M. Skulina, and J. Weinberg, “Hard x-ray sputtered-sliced phase zone plates,” Appl. Phys. Lett. 64(8), 945–947 (1994).
[Crossref]

1992 (1)

J. Maser and G. Schmahl, “Coupled wave description of the diffraction by zone plates with high aspect ratios,” Opt. Commun. 89(2-4), 355–362 (1992).
[Crossref]

1988 (1)

Y. Vladimirsky and H. W. P. Koops, “Moire method and zone plate pattern inaccuracies,” J. Vac. Sci. Technol. B 6(6), 2142–2146 (1988).
[Crossref]

1981 (1)

D. Rudolph, B. Niemann, and G. Schmahl, “Status of the sputtered sliced zone plates for x-ray microscopy,” Proc. Soc. Photo Opt. Instrum. Eng. 316, 103–105 (1981).

1967 (1)

D. J. Stiglian, R. Mittra, and R. G. Semonin, “Resolving power of a zone plate,” JOSA 57(5), 610–613 (1967).
[Crossref]

Alisauskas, S.

Anderson, E.

Anderson, E. H.

Andriukaitis, G.

Aristov, V. V.

Arpin, P.

Athas, G.

Attwood, D.

A. Sakdinawat and D. Attwood, “Nanoscale X-ray imaging,” Nat. Photonics 4(12), 840–848 (2010).
[Crossref]

Attwood, D. T.

Auvray, L.

Baciocchi, M.

M. Baciocchi, R. Maggiora, and M. Gentili, “High resolution fresnel zone plates for soft x-rays,” Microelectron. Eng. 23(1-4), 101–104 (1994).
[Crossref]

Baglin, J. E. E.

J. E. E. Baglin, “Ion beam nanoscale fabrication and lithography-A review,” Appl. Surf. Sci. 258(9), 4103–4111 (2012).
[Crossref]

Balciunas, T.

Baltuska, A.

Bardotti, L.

Baretzky, B.

Barth, U.

Bassom, N. J.

Bauerdick, S.

Becker, A.

Becker, S.

Biance, A. L.

Bionta, R. M.

R. M. Bionta, K. M. Skulina, and J. Weinberg, “Hard x-ray sputtered-sliced phase zone plates,” Appl. Phys. Lett. 64(8), 945–947 (1994).
[Crossref]

Bourhis, E.

Bourzac, K.

K. Bourzac, “Tabletop X-rays light up,” Nature 486(7402), 172 (2012).
[Crossref] [PubMed]

Brown, S.

Bruchhaus, L.

Budai, J. D.

G. E. Ice, J. D. Budai, and J. W. L. Pang, “The race to X-ray microbeam and nanobeam science,” Science 334(6060), 1234–1239 (2011).
[Crossref] [PubMed]

Buzanich, G.

A. Guilherme, G. Buzanich, and M. L. Carvalho, “Focusing systems for the generation of X-ray micro beam: An overview,” Spectroc. Acta Pt. B-Atom. Spectr. 77, 1–8 (2012).

Carvalho, M. L.

A. Guilherme, G. Buzanich, and M. L. Carvalho, “Focusing systems for the generation of X-ray micro beam: An overview,” Spectroc. Acta Pt. B-Atom. Spectr. 77, 1–8 (2012).

Chao, W.

Chao, W. L.

Chappert, C.

Chen, M. C.

Chen, T.-Y.

Chen, Y.-T.

Cho, A.

A. Cho, “Materials science. What shall we do with the x-ray laser?” Science 330(6010), 1470–1471 (2010).
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Chriqui, Y.

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Fig. 1 Representation of the fabricated gold FZP (up and cross-sectional side view): Only a few zones are displayed for sake of simplicity. Positive FZP for which the first zone is filled with gold and the last zone is empty; the zone material is polycrystalline gold; the zone height is 500 nm; the diameter is 100 µm; the outermost zone period Λ is 200 nm (corresponding to an outermost zone width Δr of 100 nm); the number of zones N is 251; α is the angle characteristic of the inclination of the walls as a result of ion beam lithography.

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Fig. 2 Local diffraction efficiency as function of the FZP radius (left) and normalized intensity in the 1st and 2nd order focal plane, where the position of the first minimum is the resolution according to the Rayleigh criterion (right) for a trapezoidal FZP with α = 6°. Calculation based on the Takagi-Taupin dynamical diffraction theory.

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Fig. 3 Images of the FZP (a) SEM image recorded with an Everhart Thornley Detector (ETD): overview of the FZP manufactured according to the described procedure and further employed to perform imaging (b) SEM image recorded with a Through Lens Detector (TLD): closed view of the outermost zones, showing the 200 nm period (Λ) of the structure. (c) Ion Beam Image recorded at 45° on a cross section of a FZP manufactured under the same condition than the FZP in (a) and (b) and showing the trapezoidal from of the zones (prior to the cross-sectioning the zones are over coated with Pt to ensure their protection).

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Fig. 4 (a) SEM image of a Siemens-star test object (b) (c) (d) Scanning X-ray microscopy of same test object at the 1st 2nd and 3rd order of diffraction acquired at 900 eV with a pixel size 10 nm and a dwell time of 10ms. The half pitch resolution was determined from the power spectrum of these images and are collected in Table 2

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Fig. 5 Scanning X-ray microscopy image of a certified commercial test sample (BAM L200) recorded at 1200 eV (a) image acquired in the 2nd order focus of the FZP with a pixel size of 5 nm and a dwell time of 10 ms (b) image acquired in the 3rd order focus of the FZP with a pixel size of 5 nm and a dwell time of 15 ms (c) schematic representation of the certified test object (d) width of the features (half pitch)

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Fig. 6 Measured and theoretical efficiencies for the first order focus of the FZP. The theoretical efficiencies for a trapezoidal FZP were calculated for an angle α = 6° within the frame work of the thin grating theory (TG) and the Takagi-Taupin dynamical diffraction theory (TT-DDT). Note that in the real structure the angle α takes value between 4° and 6° which could explain the differences between theoretical and measured values.

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Tables (2)

Table 1 Calculated 1st order diffraction efficiencies for a trapezoidal FZP made out of a 500 nm thick gold layer, Δr = 100 nm and α = 6° within the frame work of the thin grating approximation [19] which is valid as long as the aspect ratio is not too high [35].

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Table 2 Spatial resolution performances obtained with the FZP in the 1st, 2nd and 3rd order focus. Where η is the efficiency $δ_{R a y} / 2$ is the half-pitch (half-period) Rayleigh resolution and $δ_{c u t o f f} / 2$ is the half-pitch cutoff resolution determined from the power spectra of the images [Fig. 4(a) to (c)] and visually from the images [Fig. 5].

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Equations (1)

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δ_{R a y}^{m} = \frac{1.22 Δ r}{m}

Energy [eV]	Efficiency [%]
30	7.6
100	7.6
450	8.2
900	8.1
1200	9.7
1500	16.0
2000	21.9
6000	11.2
8000	7.3

	Theoretical	Measured
Diffraction order	${δ_{R a y} / 2}^{(a)}$ [nm]	$δ_{c u t o f f}^{(b)} / 2$ [nm]
1st order	61.0	44 ^(c)
2nd order	30.5	26 ^(c)
3rd order	20.3	21 ^(d)

Energy [eV]	Efficiency [%]
30	7.6
100	7.6
450	8.2
900	8.1
1200	9.7
1500	16.0
2000	21.9
6000	11.2
8000	7.3

	Theoretical	Measured
Diffraction order	${δ_{R a y} / 2}^{(a)}$ [nm]	$δ_{c u t o f f}^{(b)} / 2$ [nm]
1st order	61.0	44 ^(c)
2nd order	30.5	26 ^(c)
3rd order	20.3	21 ^(d)