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Soft X-ray Multilayer Mirrors
Linköping University, Department of Physics, Measurement Technology, Biology and Chemistry. Linköping University, The Institute of Technology.
2004 (English)Doctoral thesis, comprehensive summary (Other academic)
Abstract [en]

This thesis is focused on the design, growth and characterization of soft x-ray multilayer mirrors with the emphasis on the wavelength region called the water window (λ=2.4-4.4 nm). The main application in mind is condenser mirrors for a high resolution compact soft x-ray microscope using a droplet-target laser-produced plasma (LPP) source operating at λ=3.374 nm. However, other applications, utilizing other wavelengths, have also been considered.

The design of the multilayers which involves understanding of the details of the optical properties of the elements and the interaction between multilayer and electromagnetic radiation is reviewed. To design the multilayers, e.g., to determine the material system, the individual layer thicknesses, and the total number of layers, the simulation software package IMD was used. From the simulations it was also found that in order to realize high-reflectivity multilayer mirrors, interface imperfections, like roughness and intermixing need to be minimized.

In particular the material systems W/B4C, Cr/Sc, and Ni/V grown by ion-assisted dualtarget magnetron sputter deposition, have been studied. The effect of various process parameters, especially the energy and flux of low-energy ion bombardment have been investigated in order to increase the understanding of the ion-surface interactions and the materials science of the multilayers.

To characterize the multilayers mainly different x-rays techniques have been used; hard x-ray reflectivity, LPP soft x-ray reflectivity and also soft x-ray synchrotron reflectivity measurements at BESSY in Berlin and at the Advanced Light Source (ALS) in Berkeley. Both specular reflectivity and diffuse scattered intensity has been measured to assess the lateral and vertical structure of the multilayers.

With an increased knowledge and understanding of the effects of the ion-surface interaction on the structure of the multilayers, advances were made in the development, with a following improvement in performance. The first multilayer material system investigated was W /B,C. However, because of a naturally high absorption of x-rays in W, the theoretically achievable reflectivity is very low, only about 12%.

Cr/Sc, on the other hand, has potentially a much higher reflectivity of about 60%. Here different energies, but also fluxes, of ion assistance was investigated. It was found that, for a low ion flux, the ion energy, providing the optimum compromise between reduced roughness and induced intermixing, was rather high. By increasing the ion flux,the energy could be lowered, which in turn decreased the intermixing with a subsistent surface smoothening. This resulted in an improved reflectivity, where maximum nearnormal incidence reflectivities of R=5.5% and R=14.5% were achieved at λ=3.374 nm and at the Sc absorption edge (λ=3.115 nm), respectively.

However, although fairly high reflectivities were obtained, the trade-off between roughness reduction and interface mixing persisted. Analytical calculations, based on a binary collision approximation, revealed that an interface mixing of ±1 atomic distance is unavoidable when a continuous flux of assisting ions is used. To overcome this limitation, a sophisticated interface engineering technique was employed, where the first part of each layer was grown using a high-flux of low energy ions, and the remaining part with a slightly higher ion energy. This method was demonstrated to largely eliminate the intermixing while maintaining the smoothening effect of ion-assistance.

Using this novel modulated low-energy and high-flux ion-assistance technique extremely flat and abrupt interfaces were obtained. Soft x-ray Cr/Sc and Ni/V multilayer mirrors with near-normal incidence reflectivities of 20.7% and 2.7% at the Sc and V(λ=2.43 nm) absorption edges, respectively, were realized. Multilayer optimized for the Brewster angle showed a reflectance of R=26.7% and a polarizing power of Rs/Rp=5450 for Cr/Sc and R=l0% and Rs/Rp=4190 for Ni/V, when realized with engineered interfaces.

Finally, also the long-term goal of producing a large-area, spherically-shaped, normalincidence soft x-ray multilayer condenser mirror for a compact soft x-ray microscope was accomplished.

Place, publisher, year, edition, pages
Linköping: Linköping University , 2004. , p. 116
Series
Linköping Studies in Science and Technology. Dissertations, ISSN 0345-7524 ; 875
National Category
Atom and Molecular Physics and Optics
Identifiers
URN: urn:nbn:se:liu:diva-179113Libris ID: 9473040ISBN: 9173739502 (print)OAI: oai:DiVA.org:liu-179113DiVA, id: diva2:1594313
Public defence
2004-05-14, hörsal Planck, Fysikhuset, Linköpings universitet, Linköping, 10:15
Opponent
Note

All or some of the partial works included in the dissertation are not registered in DIVA and therefore not linked in this post.

Available from: 2021-09-16 Created: 2021-09-15 Last updated: 2023-02-23Bibliographically approved
List of papers
1. Compact soft x-ray reflectometer based on a line-emitting laser-plasma source
Open this publication in new window or tab >>Compact soft x-ray reflectometer based on a line-emitting laser-plasma source
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2001 (English)In: Review of Scientific Instruments, ISSN 0034-6748, E-ISSN 1089-7623, Vol. 72, no 1 I, p. 58-62Article in journal (Refereed) Published
Abstract [en]

We describe a compact soft x-ray reflectometer for in-house characterization of water-window multilayer optics. The instrument is based on a line-emitting, liquid-jet, laser-plasma source in combination with angular scanning of the studied multilayer optics. With a proper choice of target liquid and thin-film filters, one or a few lines of well-defined wavelength dominate the spectrum and multilayer periods are measured with an accuracy of 0.003 nm using a multi-line calibration procedure. Absolute reflectivity may also be estimated with the instrument. The typical measurement time is currently 10 min. Although the principles of the reflectometer may be used in the entire soft x-ray and extreme ultraviolet range, the current instrument is primarily directed towards normal-incidence multilayer optics for water-window x-ray microscopy, and is thus demonstrated on W/B4C multilayers for this wavelength range. © 2001 American Institute of Physics.

National Category
Engineering and Technology
Identifiers
urn:nbn:se:liu:diva-47494 (URN)10.1063/1.1327307 (DOI)
Available from: 2009-10-11 Created: 2009-10-11 Last updated: 2021-12-29
2. Enhanced soft x-ray reflectivity of Cr/Sc multilayers by ion-assisted sputter deposition
Open this publication in new window or tab >>Enhanced soft x-ray reflectivity of Cr/Sc multilayers by ion-assisted sputter deposition
2002 (English)In: Optical Engineering: The Journal of SPIE, ISSN 0091-3286, E-ISSN 1560-2303, Vol. 41, no 11, p. 2903-2909Article in journal (Refereed) Published
Abstract [en]

Cr/Sc multilayers have been grown on Si substrates using dc magnetron sputtering. The multilayers are intended as condenser mirrors in a soft x-ray microscope operating at the wavelength 3.374 nm. They were designed for normal reflection of the first and second orders, with multilayer periods of 1.692 and 3.381 nm, and layer thickness ratios of 0.471 and 0.237, respectively. At-wavelength soft-x-ray reflectivity measurements were carried out using a reflectometer with a compact soft-x-ray laser-plasma source. The multilayers were irradiated during growth with Ar ions, varying both in energy (9 to 113 eV) and flux, in order to stimulate the adatom mobility and improve the interface flatness. It was found that to obtain a maximum soft x-ray reflectivity with a low flux (Cr=0.76, Sc=2.5) of Ar ions a rather high energy of 53 eV was required. Such energy also caused intermixing of the layers. By the use of a solenoid surrounding the substrate, the arriving ion-to-metal flux ratio could be increased 10 times and the required ion energy could be decreased. A high flux (Cr=7.1, Sc=23.1) of low-energy (9 eV) Ar ions yielded the most favorable growth condition, limiting the intermixing with a subsistent good surface flatness. © 2002 Society of Photo-Optical Instrumentation Engineers.

Keywords
Cr/Sc, Ion energy, Ion flux, Ion-assisted sputter deposition, Multilayer, Reflectivity, Soft-x-ray microscopy, Water window
National Category
Engineering and Technology
Identifiers
urn:nbn:se:liu:diva-46863 (URN)10.1117/1.1510750 (DOI)
Available from: 2009-10-11 Created: 2009-10-11 Last updated: 2021-12-29
3. Recent advances in ion-assisted growth of Cr/Sc multilayer X-ray mirrors for the water window
Open this publication in new window or tab >>Recent advances in ion-assisted growth of Cr/Sc multilayer X-ray mirrors for the water window
2002 (English)Conference paper, Published paper (Refereed)
Abstract [en]

Cr/Sc multilayer X-ray mirrors intended for normal incidence reflection in the water window wavelength range, ?=[2.4-4.4nm], have been grown by ion-assisted sputter deposition and characterized using soft and hard X-ray reflectivity. By extracting low-energy ions, with energies, Eion, ranging from 9 to 113eV and with ion-to-metal flux ratios, F, between 0.76 and 23.1, from the sputtering plasma to the growing film, the nano-structure of the multilayer interfaces could be modified. A significantly increased soft X-ray reflectivity, using ?=3.374nm, for Cr/Sc multilayers with layer thicknesses in the range 0.4-2.8nm, was obtained when high ion-to-metal flux ratios, FCr=7.1 and FSc=23.1, and low energy ions, Eion=9eV, were used. An experimental reflectivity of 5.5% was obtained at 76° for a multilayer with 400 bi-layers. Simulations of the reflectivity data showed that the interface widths are <0.425nm. It could be concluded that roughness of low spatial frequency is reduced at lower ion energies than the high spatial frequency which was eliminated at the expense of intermixing at the interfaces at higher ion energies. The predicted performance of normal incidence multilayer mirrors grown at optimum conditions and designed for ?=3.374 and 3.115nm indicates possible reflectivities of 6.5% and 14%, respectively. © 2002 Elsevier Science Ltd. All rights reserved.

Keywords
Chromium, Ion-assisted growth, Multilayer, Scandium, Sputtering, Water window, X-ray mirror
National Category
Engineering and Technology
Identifiers
urn:nbn:se:liu:diva-46853 (URN)10.1016/S0042-207X(02)00457-8 (DOI)
Available from: 2009-10-11 Created: 2009-10-11 Last updated: 2021-12-29
4. 14.5% near-normal incidence reflectance of Cr/Sc x-ray multilayer mirrors for the water window
Open this publication in new window or tab >>14.5% near-normal incidence reflectance of Cr/Sc x-ray multilayer mirrors for the water window
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2003 (English)In: Optics Letters, ISSN 0146-9592, E-ISSN 1539-4794, Vol. 28, no 24, p. 2494-2496Article in journal (Refereed) Published
Abstract [en]

Cr/Sc multilayer mirrors, synthesized by ion-assisted magnetron sputter deposition, are proved to have a high near-normal reflectivity of R = 14.5% at a grazing angle of 87.5degrees measured at the wavelength A = 3.11 nm, which is an improvement of more than 31% compared with previously published results. Elastic recoil detection analyses show that the mirrors contained as much as 15 at. % of N and traces of C and O. Soft x-ray reflectivity simulations reveal interface widths of sigma = 0.34 nm and an exceptionally small layer thickness drift of similar to1.6 X 10(-5) nm/multilayer period throughout the stack. Simulations show that a reflectivity of R = 25.6% is attainable if impurities and layer thickness drift can be eliminated. The abrupt interfaces are achieved with ion assistance with a low ion energy of 24 eV and high ion-to-metal flux ratios of 7.1 and 23.1 during Cr and Se sputter deposition, respectively. In addition, a near-normal incidence reflectivity of 5.5% for the C VI emission line (lambda = 3.374 nm) from a laser plasma source was verified. (C) 2003 Optical Society of America.

National Category
Engineering and Technology
Identifiers
urn:nbn:se:liu:diva-48449 (URN)
Available from: 2009-10-11 Created: 2009-10-11 Last updated: 2021-12-29
5. Interface engineering of short-period Ni/V multilayer X-ray mirrors
Open this publication in new window or tab >>Interface engineering of short-period Ni/V multilayer X-ray mirrors
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2006 (English)In: Thin Solid Films, ISSN 0040-6090, E-ISSN 1879-2731, Vol. 500, no 1-2, p. 84-95Article in journal (Refereed) Published
Abstract [en]

Low-energy ion-assisted magnetron sputter deposition has been used for the synthesis of highly reflective Ni/V multilayer soft X-ray mirrors. A low ion energy and a high ion-to-metal flux ratio were employed in order to stimulate the adatom mobility while minimizing ion-induced intermixing at the interfaces. An analytic model, based on the binary collision approximation, was used in order to gain insight into low-energy ion-surface interactions as a function of ion energy and ion-to-metal flux ratio. The model predicted a favorable region in the ion energy-flux parameter space where only surface atomic displacements are stimulated during growth of Ni and V for multilayers. For a series of Ni/V multilayer mirrors with multilayer periods about Λ = 1.2 nm, grown with a continuous ion assistance using energies in the range 7-36 eV and with ion-to-metal flux ratios ΦNi = 4.7 and ΦV=20.9, specular and diffuse X-ray scattering analyses revealed that ion energies of ∼27-31 eV produced the best trade-off between reduced interfacial roughness and intermixing. However, it was also concluded that an interface mixing of about ± 1 atomic distance is unavoidable when a continuous flux of assisting ions is used. To overcome this limitation, a sophisticated interface engineering technique was employed, where the first 0.3 nm of each layer was grown with a high-flux low-energy ion assistance and the remaining part was grown with a slightly higher ion energy. This method was demonstrated to largely eliminate the intermixing while maintaining the smoothening effect of ion assistance. Two Ni/V multilayer soft X-ray mirror structures, one with 500 periods designed for near-normal incidence and one 150 periods reflecting polarizer at the Brewster angle, were grown utilizing the interface engineering concept. Both the near-normal incidence reflectivity as well as polarizability were improved by a factor of 2 as compared to previously reported data for an X-ray energy of E = 511 eV. © 2005 Elsevier B.V. All rights reserved.

National Category
Natural Sciences
Identifiers
urn:nbn:se:liu:diva-30903 (URN)10.1016/j.tsf.2005.11.019 (DOI)16568 (Local ID)16568 (Archive number)16568 (OAI)
Available from: 2009-10-09 Created: 2009-10-09 Last updated: 2021-12-29

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Eriksson, Fredrik

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