Wolter type I x-ray focusing mirror using multilayer coatings

A multilayer coating is a useful addition to a mirror in the x-ray region and has been applied to normal incidence mirrors used with soft x rays. When a multilayer coating is used on grazing incidence optics, higher performance can be achieved than without it. Cr/Sc multilayers coated on a Wolter type I mirror substrate for a soft x-ray microscope are considered. The reflectivity and effective solid angle are calculated for Wolter type I mirrors with uniform and laterally graded multilayer coatings. The laterally graded multilayer mirror showed superior x-ray performance, and the multilayer tolerances were relaxed. This multilayer mirror could be especially useful in the soft x-ray microscope intended for biological applications.     

Chromium-scandium multilayer mirrors for the nitrogen K(alpha) line in the water window region

Chromium-scandium (Cr-Sc) is a promising material combination for multilayer mirrors in the water window region. A possible x-ray source for laboratory use in this wavelength range is the nitrogen K(alpha) line at 3.16 nm. High reflectivities at this wavelength can be achieved with Cr-Sc multilayer mirrors if the interfaces between adjacent layers are smooth. The growth parameters of the magnetron sputtering process for these materials have been optimized. It is shown that the reflectivity of such mirrors can be considerably improved by the application of a proper bias voltage during film growth. The high quality of the multilayer films is demonstrated with copper K(alpha) x-ray reflection and transmission electron microscopy. The reflective properties of the multilayers close to the nitrogen K(alpha) line were measured with synchrotron radiation for different angles of incidence. Reflectivities between R = 5.9% for near-normal incidence (theta = 1.5 degrees) and R = 29.6% for theta = 59.9 degrees were measured.     

Metal-substituted organic Cd-arachidate multilayers as soft-x-ray mirrors

Multilayers for soft x rays, lambda > 4.5 nm, have been made with Cd arachidate, a metal-substituted fatty acid. The multilayer period is found to be 5.53 nm, double the normal length of a Cd-arachidate molecule. The interfaces have a low roughness value of < 0.3 nm, which does not reduce the long-wavelength reflectance significantly. The soft-x-ray reflectance at 3.0 nm has been measured to be 0.13% for this prototypical multilayer that has 12 bilayers. The theoretical reflectance of these multilayers determined at a wavelength of 10.0 nm, suitable for x-ray lithography, is found to saturate at approximately 43% for approximately 150 bilayers.     

Interface engineered ultrashort period Cr-Ti multilayers as high reflectance mirrors and polarizers for soft x rays of lambda = 2.74 nm wavelength

Cr-Ti multilayers with ultrashort periods of 1.39-2.04 nm have been grown for the first time as highly reflective, soft-x-ray multilayer, near-normal incidence mirrors for transition radiation and Cherenkov radiation x-ray sources based on the Ti-2p absorption edge at E = 452 eV (lambda = 2.74 nm). Hard, as well as soft, x-ay reflectivity and transmission electron microscopy were used to characterize the nanostructure of the mirrors. To achieve minimal accumulated roughness, improved interface flatness, and to avoid intermixing at the interfaces, each individual layer was engineered by use of a two-stage ion assistance process during magnetron sputter deposition: The first 0.3 nm of each Ti and Cr layer was grown without ion assistance, and the remaining 0.39-0.72 nm of the layers were grown with high ion-neutral flux ratios phi (phiTi = 3.3, phiCr = 2.2) and a low energy Eion (ETi = 23.7 and ECr = 21.2), ion assistance. A maximum soft-x-ray reflectivity of R = 2.1% at near-normal incidence (approximately 78.8 degrees) was achieved for a multilayer mirror containing 100 bilayers with a modulation period of 1.379 nm and a layer thickness ratio of tau = 0.5. For a polarizing multilayer mirror with 150 bilayers designed for operation at the Brewster angle, 45 degrees, an extinction ratio, Rs/Rp, of 266 was achieved with an absolute reflectivity of R = 4.3%.     

Structure and normal incidence soft-x-ray reflectivity of Ni-Nb/C amorphous multilayers

Multilayers for the water window region of the soft x rays have been prepared by pulsed laser ablation with amorphous Ni(50) Nb(50) and amorphous C. The structural characterization of the multilayers, period d = 2.41 nm, shows that the interfaces are sharp with a roughness of only 0.4 nm that is chemical, not morphological, in origin. The interface roughness was found to be uncorrelated in the direction normal to the plane of the film. The normal incidence soft-x-ray reflectivity of the multilayer at 4.85-nm wavelength is 0.06%, 1 order of magnitude lower than the theoretically predicted value. However, the resolution limit lambda/Dlambda of the multilayer was found to be 16.7, close to the theoretically predicted value.     

Survey of Ti-, B-, and Y-based soft x-ray-extreme ultraviolet multilayer mirrors for the 2- to 12-nm wavelength region

We have performed an experimental investigation of Ti-, B(4)C-, B-, and Y-based multilayer mirrors for the soft x-ray?extreme ultraviolet (XUV) wavelength region between 2.0 and 12.0 nm. Eleven different material pairs were studied: Ti/Ni, Ti/Co, Ti/Cu, Ti/W, B(4)C/Pd, B/Mo, Y/Pd, Y/Ag, Y/Mo, Y/Nb, and Y/C. The multilayers were sputter deposited and were characterized with a number of techniques, including low-angle x-ray diffraction and normal incidence XUV reflectometry. Among the Ti-based multilayers the best results were obtained with Ti/W, with peak reflectances up to 5.2% at 2.79 nm at 61° from normal incidence. The B(4)C/Pd and B/Mo multilayer mirrors had near-normal incidence (5°) peak reflectances of 11.5% at 8.46 nm and 9.4% at 6.67 nm, respectively, whereas a Y/Mo multilayer mirror had a maximum peak reflectance of 25.6% at 11.30 nm at the same angle. The factors limiting the peak reflectance of these different multilayer mirrors are discussed.     

W/SiC x-ray multilayers optimized for use above 100 keV

We have developed a new depth-graded multilayer system comprising W and SiC layers, suitable for use as hard x-ray reflective coatings operating in the energy range 100-200 keV. Grazing-incidence x-ray reflectance at E = 8 keV was used to characterize the interface widths, as well as the temporal and thermal stability in both periodic and depth-graded W/SiC structures, whereas synchrotron radiation was used to measure the hard x-ray reflectance of a depth-graded multilayer designed specifically for use in the range E approximately 150-170 keV. We have modeled the hard x-ray reflectance using newly derived optical constants, which we determined from reflectance versus incidence angle measurements also made using synchrotron radiation, in the range E = 120-180 keV. We describe our experimental investigation in detail compare the new W/SiC multilayers with both W/Si and W/B4C films that have been studied previously, and discuss the significance of these results with regard to the eventual development of a hard x-ray nuclear line telescope.     

Extreme-ultraviolet Mo/Si multilayer mirrors deposited by radio-frequency-magnetron sputtering

Mo/Si multilayer mirrors with a high reflectance at normal incidence in the 130-135-? spectral region have been deposited by rf magnetron sputtering. A new and quick technique was used to calibrate the deposition rates. Characterization by transmission electron microscopy (TEM) and grazing-incidence x-ray diffraction (XRD) indicated good thickness control of the deposition process and low interface roughness. However, the TEM and, indirectly, the XRD reflectance measurements, indicated that the interfaces are asymmetric. A brief review discussing the origin of the modulation of the Bragg peak intensities in the XRD reflectance is given. An analytical formula was derived for periodic multilayers that describes the effect of asymmetric interfaces on the amplitude of the Bragg peak modulation. Theoretically, in XRD reflectance measurements, any asymmetry in the interdiffusion of the Mo-Si interfaces results in a decrease of the usual amplitude modulation of the Bragg peaks. Extreme-ultraviolet (XUV) reflectance measurements were also made with synchrotron radiation on a new high-resolution reflectometer. The near-normal-incidence peak reflectances measured at λ = 134 ? were ~ 59% for the best multilayer mirrors. Good fits to both XRD and XUV reflectance measurements have been obtained with a model that allows for interface asymmetry.     

Carbon/Titanium multilayers as soft-x-ray mirrors for the water window

C/Ti multilayers with a period thickness of 2.1-2.7 nm were produced by electron-beam evaporation in ultrahigh vacuum as soft-x-ray mirrors in the water window (lambda = 2.3-4.4 nm). For smoothing the individual interfaces and thus enhancing the total reflectance, each layer was ion polished with an Ar(+) ion beam after deposition. For a multilayer of 85 bilayers, a reflectance of approximately 11% at an angle of incidence of 59 degrees (with respect to the surface normal) by use of s-polarized radiation at a wavelength of 2.77 nm was achieved.     

Fabrication of multilayer mirrors consisting of oxide and nitride layers for continual use across the K-absorption edge of carbon

The development of multilayer mirrors for continual use around the K-absorption edge of carbon (4.4 nm) has been begun. Cobalt oxide (Co3O4), silicon oxide (SiO2), and boron nitride (BN) are found to be suitable for multilayer mirrors on the basis of theoretical calculations for wavelengths around the carbon K-absorption edge region. X-ray reflectivity curves with CuKalpha1 x rays of the fabricated Co3O4/SiO2 multilayers have sharp Bragg peaks, and the layer structures evaluated from transmission electron microscopy (TEM) observations are uniform. On the other hand, the Bragg peaks of Co3O4/BN multilayers split, and aggregated Co3O4 is observed. To improve the Co3O4 layer structure, chromium oxide (Cr2O3) was mixed into Co3O4. The mixed oxide layer structure in the Mix/BN multilayer (Mix = Co3O4 + Cr2O3) is relatively uniform, and the Bragg peaks do not split.     

Study of normal incidence of three-component multilayer mirrors in the range 20-40 nm

We study theoretically and experimentally the increase of normal incidence reflectivity generated by addition of a third material in the period of a standard periodic multilayer, for wavelengths in the range 20 to 40 nm. The nature and thickness of the three materials has been optimized to provide the best enhancement of reflectivity. Theoretical reflectivity of an optimized B4C/Mo/Si multilayer reaches 42% at 32 nm. B4C/Mo/Si multilayers have been deposited with a magnetron sputtering system and a reflectivity of 34% at 32 nm has been measured on a synchrotron radiation source.     

Production and performance of multilayer-coated conical x-ray mirrors

A method of fabricating replica figured x-ray optics with integral multilayer coatings is presented. With the intact electroforming multilayer process (IEMP) technique, we sputter multilayers onto a reusable superpolished mandrel, electroform nickel over the multilayers, and remove the multilayer-coated nickel shell intact from the mandrel. This approach offers advantages over more traditional, original, and segmented-replica fabrication techniques, including low cost; compatibility with a wide range of mirror designs, diameters, and focal lengths; simple integration with multilayer sputtering processes; and the ability to produce complete shells of revolution. The fabrication of W/Si multilayer-coated 10-cm-diameter conical x-ray mirrors is described, as are reflectivity measurements at 10 and 30 keV. The measured reflectivity of the IEMP multilayers at the 10-keV primary Bragg peak was 17%. Measurements of multiple points on the cone showed multilayer uniformity to within a few percent around the mirror.     

Preparation and characterization of superhard TiC/Mo multilayers

Nanometer scale TiC/Mo multilayers have been prepared by ion beam assisted deposition (IBAD) at nearly ambient temperature. The modulation wavelength was in the range of 2 nm to 14 nm and the individual layer thickness was maintained to be equal. Two series (series A and series B) were prepared which were bombarded with different bombarding energy (0 eV and 50 eV) in order to investigate the bombardment effect on the nano-hardness of the multilayers. Low angle X-ray diffraction (LXRD) was used to analyzed the layered structure of multilayers. Mechanical properties of these multilayers were thoroughly studied using a nanoindentation facility. The nanohardness showed a strong dependence on the sharpness of the interlayer and the modulation wavelength. It was found that the multilayer hardness was greater than the volume weighted mean of the component hardness. With the modulation wavelength adjusted, the multilayer can be even harder than its hard component (TiC). A maximum hardness of 47.62 GPa, about 1.5 times larger than that of the TiC values, was found at = 8 nm multilayer deposited without ion beam bombardment. It was also found that the films without ion bombardment were much harder than those bombarded by 50 eV Ar⁺ ion beam.     

General theory of sub-quarterwave multilayers with highly absorbing materials

A general theory of multilayers with enhanced reflectance has been developed based on the superposition of sub-quarterwave layers of various highly radiation-absorbing materials. The theory has been developed by second-order expansion of the multilayer reflectance with respect to the optical-constant differences between the materials in the multilayer. The current paper completes and improves the theory that was developed in a previous paper [J. Opt. Soc. Am. A 18, 1406 (2001)] by including the case of nonnormal incidence and general radiation polarization and by providing more-accurate film thickness values of the optimized multilayer than with the previous theory. The theory provides an accurate approach to the design of a new concept of multilayer coatings with more than two materials. The new multilayers are adequate to enhance the reflectance of the materials particularly in the far and the extreme ultraviolet.     

Fast imaging of hard x rays with a laboratory microscope

An improved x-ray microscope with a fully electronic CCD detector system has been constructed that allows improved laboratory-based microstructural investigations of materials with hard x rays. It uses the Kirkpatrick-Baez multilayer mirror design to form an image that has a demonstrated resolution of 4 mum at 8 keV (Cu K(alpha) radiation). This microscope performs well with standard sealed-tube laboratory x-ray sources, producing digital images with 20-s exposure times for a 5-mum Au grid (a thickness of two absorption lengths).     

New layer-by-layer multilayer design method

A new layer-by-layer multilayer design method is presented. The method is demonstrated mathematically and makes possible the optimization of the multilayer for the highest possible reflectance either at normal incidence or at nonnormal incidence for s- or p-polarized radiation. With the current method multilayers can be designed regardless of the number of different materials used. The optimum layer thickness is determined by means of functions suitable for implementation in a computer code. The new multilayer design method is fast and accurate.     

Mo/Si multilayers for EUV lithography by ion beam sputter deposition

Mo/Si multilayers for applications in extreme ultraviolet (EUV) lithography have been prepared on Si wafer substrates using ion beam deposition. The multilayers were characterised by transmission electron microscopy, secondary ion mass spectroscopy, atomic force microscopy, photoelectron spectroscopy, X-ray reflectometry at grazing incidence, and EUV-reflectivity measurements at nearly normal incidence. The surface and the interfaces of the multilayers are rather smooth with only small roughness. The material properties of the layers are characterised by some intermixing and silicide formation at the Mo-Si interfaces and a polycrystalline grain structure of the Mo layers, which is in agreement with prior studies. Appearance of multilayer diffraction spots, well-resolved Kiessig fringes and other diffraction evidence indicate very good coherence of the wave fields and in this manner a good reproducibility of the multilayer period of 6.7 nm. Normal incidence peak reflectivities of 64-65% in the EUV spectral range were routinely obtained at 13.4 nm wavelength. This reflectivity value and the formation of an EUV standing wave field are confirmed using photoelectron spectroscopy, and an application for defect particle analysis is proposed. The obtained results are discussed in comparison to literature data of multilayers prepared by other deposition techniques and considering new attempts of interface engineering.     

Micromechanical analysis of effective properties of magneto-electro-thermo-elastic multilayer composites

An exact matrix method, originally proposed for evaluating effective elastic constants of generally anisotropic multilayer composites, is further developed for a micromechanical analysis of multilayers with various coupled physical effects including piezoelectricity, piezomagnetism, thermoelasticity (in consideration of entropy), and the Biot’s poroelasticity. The results for a BaTiO₃-CoFe₂O₄ magneto-electro-thermo-elastic (METE) multilayer coincide with those calculated using other micromechanical models based on the Mori-Tanaka method and the asymptotic homogenization method. It is shown that the present method can efficiently handle the most general type of multilayers with an arbitrary number of general anisotropic layers. Analytical expressions for effective material properties of a transversely isotropic METE multilayer composite are derived, from which those for functionally graded METE multilayers can be directly obtained. The effects of crystallographic orientations and volume fractions of constituting layers on the magnetoelectric coefficients are investigated for BaTiO₃-CoFe₂O₄ and LiNbO₃-CoFe₂O₄ multilayer composites. It is thus demonstrated that the present model can be used for the layout/material optimization of these METE multilayers to obtain a maximum product property such as the magnetoelectric, pyroelectric, and pyromagnetic coefficients. It is also shown that the same method can be used to predict the effective properties of poroelastic multilayers.     

High reflectivity multilayer for He-II radiation at 30.4 nm

SiC/Mg and B(4)C/Mo/Si multilayers were designed for He-II radiation at 30.4 nm. These multilayers were prepared by use of a direct current magnetron sputtering system and measured at the National Synchrotron Radiation Laboratory, China. The measured reflectivities were 38.0% for the SiC/Mg multilayer at an incident angle of 12 deg and 32.5% for the B(4)C/Mo/Si multilayer at 5 deg, respectively. A dual-function multilayer mirror was also designed by use of the aperiodic SiC/Mg multilayer. Annealing experiments were performed to investigate the thermal stability of the SiC/Mg multilayer. The interface of the SiC/Mg multilayer before and after annealing was studied by electron-induced x-ray emission spectra, which evidences the absence of thermal reaction products at the interfaces after annealing.     

X-ray-ultraviolet beam splitters for the Michelson interferometer

With the aim of realizing a Michelson interferometer working at 13.9 nm, we have developed a symmetrical beam splitter with multilayers deposited on the front and back sides of a silicon nitride membrane. On the basis of the experimental optical properties of the membrane, simulations have been performed to define the multilayer structure that provides the highest reflectivity-transmission product. Optimized Mo-Si multilayers have been successfully deposited on both sides of t he membrane by use of the ion-beam sputtering technique, with a thickness-period reproducibility of 0.1 nm. Measurements by means of synchrotron radiation at 13.9 nm and at an angle of 45 degrees provide a reflectivity of 14.2% and a transmission of 15.2% for a 60% s-polarized light, close to the simulated values. Such a beam splitter has been used for x-ray laser Michelson interferometry at 13.9 nm. The first interferogram is discussed.