Soft X-ray Multilayer Mirrors Research Articles

Interface evolution of Cr/Ti multilayer films during continuous to discontinuous transition of Cr layer

Cr/Ti multilayers with moderate to low bi-layer thickness have been deposited by Ion beam sputtering system and have been investigated thoroughly by specular grazing incidence X-ray reflectivity (GIXR) and diffused X-ray scattering (both in coplanar and non-coplanar configurations) measurements. The investigation is important for development of Cr/Ti soft X-ray multilayer mirrors for “water window” applications in the wavelength regime of 2.2–4.4 nm. Initially few multilayers have been deposited and the highest reflectivity at first Bragg peak positions of the GIXR plots have been obtained for the Cr layer to bi-layer thickness ratio of 0.4. Subsequently, keeping the ratio fixed a set of five samples with bi-layer thickness varying from 3.8 nm to 2.1 nm have been prepared. For the all five ML samples reported in this communication, Ti layer thickness is greater than 1.3 nm, however, the Cr layer thickness varies from 1.5 to 0.8 nm in the above range of bi-layer thickness and it undergoes continuous-to-discontinuous transition. Cr films undergo significant change in morphology as the thickness changes and thus the interfaces are also evolved differently. Analysis of the diffused X-ray scattering data shows that interface imperfection of Ti-on-Cr interfaces is dominated by interface diffusion at low Cr thickness (discontinuous) regime and by interface roughness at high Cr thickness (continuous) regime, while in case of Cr-on-Ti interfaces, interface roughness dominates throughout the whole thickness regime. For the sample with highest bi-layer thickness of 3.8 nm high Bragg peak reflectivity value close to the ideal case is obtained manifesting high thickness uniformity, very low interface imperfection and high vertical correlation length across the interfaces for this sample which is also confirmed by cross-sectional Transmission Electron Microscopy. A 50 bi-layer sample prepared with the above bi-layer thickness shows high reflectivity of 5.6% at 2.84 nm water window soft X-ray wavelength.

Phase measurement of soft x-ray multilayer mirrors.

We propose a new model enabling the extraction of the phase of a multilayer mirror from photocurrent measurements in the soft x rays. In this range, the effects of the mean free path of the electrons inside the stack can no longer be neglected, which prevents the phase reconstruction by conventional photocurrent measurements. The new model takes into account this phenomenon and thus extends up to the x rays the applicability range of the technique. This approach has been validated through a numerical and experimental study of chromium/scandium multilayers used near 360 eV. To our knowledge, this work constitutes the first measurement of the phase of a multilayer mirror in the soft x-ray range.

Fabrication and Evaluation of Large Area Mo/Si Soft X-Ray Multilayer Mirrors at Indus SR Facilities

Large area Mo/Si multilayer (ML) mirrors with high reflectivity are fabricated using magnetron sputtering deposition system. Thin film growth is optimized for film roughness, density, and interface quality by changing process parameters through fabrication of thin films. Mo/Si MLs are fabricated with varying thickness ratio, number of layer pairs, and periodicity from 0.3 to 0.45, 5 to 65, and 40 to 100 Å, respectively. The samples are characterized using hard X-ray reflectivity and transmission electron microscopy. Soft X-ray performance tests of MLs are done by soft X-ray reflectivity using Indus-1 synchrotron radiation. ML coating with thickness errors of ~0.03% per layer and interface roughness in the range of 2 to 5 Å has been realized. The lateral variation of the periodicity is controlled within 0.5 Å over the mm2 area of the plane substrate by using substrate motion and appropriate masking arrangement. Maximum variation of periodicity from run to run is less than 0.5 Å. Peak reflectivity of ~63% at wavelength of ~127 Å is achieved for incident angle of 71 degree.

Evaluation of Ion Milled Soft X-ray Multilayer Mirrors for Reflection Wavefront Correction

Surface roughness and soft x-ray reflectance of soft x-ray Mo/Si multilayer mirrors ion-milled for physical optical reflection wavefront correction with 0.1 nm accuracy have been measured. The multilayer mirror was milled by Ar ion beam accelerated at 500 V using area-selected mask template with 10×10 mm2 opening. Milled surface at peripheral was rougher than that at center of milling area. Measured maximum roughness of 0.47 nm RMS would cause only under 0.01% reduction of reflectance by theoretical estimation. 44% peak reflectance of the ion-milled multilayer at λ=14.3 nm is practical enough for composing soft x-ray objectives such as Schwarzschild objective. These results prove that ion milling method is effective and gentle milling for precise figure error correction of soft x-ray multilayer mirrors.

Characterization of Mo/Si soft X-ray multilayer mirrors by grazing-incidence small-angle X-ray scattering

The morphology of buried interfaces plays a key role in high performing Mo/Si soft X-ray mirrors. We show that grazing-incidence small-angle X-ray scattering is a highly effective and non-destructive diagnostic technique for analysis of buried interfaces. The parameters of average interface autocorrelation function can be determined unambiguously. Additionally period thickness, roughness of interfaces and an effective number of vertically correlated periods can be extracted. The multilayer mirrors were prepared by e-beam evaporation on heated and unheated substrates, ion beam assisted e-beam evaporation, ion beam sputtering and RF magnetron sputtering. The latter three techniques produce multilayer mirrors with comparable interface roughness. The differences in lateral correlation length and Hurst parameter are found.

Effect of defects on the reflectivity of Cr/C multilayer soft X-ray mirror at 4.48 nm

Cr/C is a promising material combination for multilayer mirror in the “near water window region” (4.4–6.7 nm). In the present paper, the effect of defects on the reflectivity of Cr/C soft X-ray multilayer mirror deposited by magnetron sputtering was studied. Formation of thin interlayer due to the interdiffusion, rough interface due to the non-sharp layer and contamination of O happened during the deposition process were found by a method combined by XPS, soft X-ray reflectivity at 4.48 nm and grazing incidence hard X-ray reflectivity at 0.154 nm. The XPS results show that both interlayers (Cr-on-C and C-on-Cr) are mixture composed of C sp2, C sp3, C O, C O, Cr Cr and Cr O bondings. No chromium carbide was found at the interlayer probably due to the blocking of oxides’ formation. Through the analysis of X-ray reflectivity, we obtained the multilayer structure parameters (thickness and roughness) and optical constants of each layer at 4.48 nm. Based on those results, a further calculation was carried out. The result shows that the formation of the thin interlayer contributes little to the decrease of the reflectivity, the rough interface decreases the reflectivity most and the contaminant (O) not only decreases the reflectivity but also shifts the position of the peak.

Effects of O and N impurities on the nanostructural evolution during growth of Cr/Sc multilayers

Transition metal multilayers are prime candidates for high reflectivity soft x-ray multilayer mirrors. In particular, Cr/Sc multilayers in the amorphous state have proven to give the highest reflectivity in the water window. We have investigated the influence of impurities N and O as residual gas elements on the growth, structure, and optical performance of Cr/Sc multilayers deposited in high vacuum conditions by a dual cathode direct current magnetron sputter deposition. Multilayer structures with the modulation periods in the range of 0.9–4.5 nm and Cr layer to bilayer thickness ratios in the range of 0.17–0.83 were deposited with an intentionally raised base pressure (pB), ranging from 2 × 10−7 to 2 × 10−5 Torr. Compositional depth profiles were obtained by elastic recoil detection analysis and Rutherford backscattering spectroscopy, while the structural investigations of the multilayers were carried out using hard x-ray reflectivity and transmission electron microscopy. By investigating stacked multilayers, i.e., several multilayers with different designs of the modulation periods, stacked on top of each other in the samples, we have been able to conclude that both N and O are incorporated preferentially in the interior of the Sc layers. At pB ≤ 2 × 10−6 Torr, typically <3 at.% of N and <1.5 at.% of O was found, which did not influence the amorphous nanostructure of the layers. Multilayers deposited with a high pB ∼2 × 10−5 Torr, a N content as high as ∼37 at.% was measured by elastic recoil detection analysis. These multilayers mainly consist of understoichiometric face-centered cubic CrNx/ScNy nanocrystalline layers, which could be grown as thin at 0.3 nm and is explained by a stabilizing effect on the ScNy layers during growth. It is also shown that by adding a background pressure of as little as 5 × 10−6 Torr of pure N2 the soft x-ray reflectivity (λ = 3.11 nm) can be enhanced by more than 100% by N incorporation into the multilayer structures, whereas pure O2 at the same background pressure had no effect.

Characterization of ion beam sputter deposited W and Si films and W/Si interfaces by grazing incidence X-ray reflectivity, atomic force microscopy and spectroscopic ellipsometry

An ion beam sputtering system, which uses a commercial ECR microwave based plasma ion source, has been designed and fabricated in-house for deposition of soft X-ray multilayer mirrors. To begin with, in the ion beam sputtering system W, Si thin films, W/Si bi-layer and W/Si/W tri-layer samples have been deposited on c-Si substrates as precursors to W/Si multilayer stack. The samples have been characterized by grazing incidence X-ray reflectivity (GIXR), atomic force microscopy (AFM) and spectroscopic ellipsometry (SE) techniques. By analyzing the results, density, thickness, surface roughness of the single layer samples and interface width of the bi-layer and tri-layer samples have been estimated.

Interface smoothing of soft x-ray Mo/Y multilayer mirror by thermal treatment

A systematic study of structure and thermal stability of a [(Mo/Y/) x 5] soft x-ray multilayer (ML) mirror prepared by electron beam evaporation system has been performed by means of x-ray reflectivity (XRR) and grazing incidence x-ray diffraction (GIXRD). The GIXRD patterns show that the Mo and Y layers are polycrystalline in nature. The obtained XRR patterns confirm the very good quality of the ML stack. Isochronal thermal annealing up to the temperature of 400 °C leads to a decrease in interface roughness which in turn results in sharpening of the ML interfaces. Further elevating the annealing temperature above 400 °C oxidizes the Y layers and the interface roughness increases. Thus increase in interface roughness beyond this temperature can be understood in terms of evolution of yttrium oxide, which significantly affects the ML structural properties. The modulation structure is well maintained even after annealing at 600 °C, which confirms very good thermal stability of the Mo/Y ML mirror. Our results demonstrate that low-temperature annealing (up to 400 °C) is an effective method to improve the quality of an as deposited Mo/Y soft x-ray ML mirror. Diffuse scattering measurements show very good correlation with the XRR fitting parameters.

Si adhesion interlayer effects in hydrogen passivated Si/W soft X-ray multilayer mirrors

The use of hydrogen passivation of the silicon layers in Si/W soft X-ray reflective multilayer mirrors is investigated. Standard passivation, corresponding to Si:H/W structures, led to reduced growth properties of the W layers. The additional use of atomically thin Si adhesion layers, corresponding to Si:H/Si/W, led to improved growth and increased soft X-ray reflectivity. The effects taking place at the interfaces are analysed by bright field planar TEM and in situ X-ray reflectivity, and are described in terms of interface and surface energies, with quantitatively analysis of intermixing, materials density, and geometrical optical effects.

Ion-induced interface layer formation in W/Si and WRe/Si multilayers

The effects of ion-polishing of the metal layers in W/Si and WRe/Si soft X-ray multilayer mirrors has been investigated, essentially distinguishing between effects at the layer directly treated by the ions, and effects at the interface underneath this layer in the stack. Planar transmission electron microscopy (TEM) and calibrated cross-sectional TEM showed counterbalancing effects, in the case of W/Si systems leading to an optimal soft X-ray reflectivity at 100 eV ion energy.

Soft X-ray multilayer mirrors based on depleted uranium

The use of depleted uranium (DU) and DU-based compounds is shown to significantly increase the performance of multilayer mirrors intended for the wavelengths 3–6 nm. In comparison with multilayers based on 3d-elements the increase of peak reflectivity is of a factor 1.3, while the integral reflectivity increases by factor 2. The high chemical reactivity of pure DU hampers its usage. However many DU-compounds are compatible with carbon that makes possible the fabrication of high-quality DU-based multilayer coatings.

Multilayer mirror and foil filter AXUV diode arrays on CDX-U spherical torus

Recent upgrades to CDX-U spherical torus diagnostics include two 10-channel AXUV diode arrays. The multilayer mirror (MLM) array measures the λ150 O VI brightness profile in the poloidal plane using the Mo/B4C synthetic multilayer structures as dispersive elements. The foil filter array has a tangential view and is equipped with interchangeable clear aperture, beryllium and titanium filters. This allows measurements of radiated power, O VI or C V radial distributions, respectively. The O VI and C V emissivity and the radiated power profiles are highly peaked. A Neoclassical impurity accumulation mechanism is considered as an explanation. For radiated power measurements in the Te⩽100 eV plasmas, photon energy dependent corrections must be used in order to account for nonlinear AXUV sensitivity in the range Ephot⩽20 eV. The arrays are also used for characterization of resistive MHD phenomena, such as the low m modes, saw-tooth oscillations and internal reconnection events. Based on the successful operation of the diagnostics, a new ultra soft x-ray multilayer mirror diode AXUV diode array monitoring the 34 Å emissivity distribution of C VI will be built and installed on the National Spherical Torus Experiment.

Review of collisional excitation neon-like and nickel-like soft X-ray lasers pumped by multiple infrared laser pulses at the Institute of Laser Engineering, Osaka University

We report on the soft X-ray laser developments performed at the Institute of Laser Engineering, Osaka University especially for the collisional excitation X-ray lasers at wavelengths between 25 nm and 4 nm. The performance of neon-like and nickel-like ion X-ray lasing pumped by a train of short laser pulses has been investigated. We have also demonstrated double pass amplification using a soft X-ray multi-layer mirror at wavelengths of 19.6 nm and 7.9 nm. Based on these results and experimental technique, two targets were placed in series to double the gain length. Two opposing laser beams irradiated the double targets with a suitable time difference for quasi-traveling wave pumping. The double target amplification was successfully demonstrated with two beam irradiation for Ag, Nd, Yb, Hf and Ta lasing. The estimated absolute photon flux from the saturated amplification Ag X-ray laser was ∼300 μJ. Based on the experimental results, we also discuss the applications of an X-ray laser as a super-high brightness soft X-ray source.

Broadband multilayer mirrors for optimum use of soft x-ray source output

A method of designing soft x-ray multilayer mirrors which maximize the throughput of a system in a given wavelength range is described, where throughput is defined as the product of multilayer reflectivity and source spectral intensity. It is shown that the method can also be used to obtain a flat throughput response in the required wavelength range, and that in either case mirrors which suppress the throughput outside the desired range can be designed. The method is used to optimize multilayers for the wavelength range 13-19 nm, with suppressed throughput in the ranges 12-13 and 19-25 nm. In the latter case the ratio of intensities inside and outside 13-19 nm can be increased from 0.91 to 131 and from 0.70 to 35 for two different source spectra and maximized throughput, or to 67 and 25 for flat throughput.

Characterization of heat-treated CN films fabricated by dual-facing-target sputtering for soft X-ray multilayer mirrors

The structural characterization of heat-treated CN films fabricated by dual-facing-target sputtering for soft X-ray multilayer mirrors was performed by means of X-ray diffraction (XRD), Raman spectroscopy (RS) and X-ray photoelectron spectroscopy (XPS). The XRD analyses indicate a graphization process in the CN films during thermal annealing. The Raman analyses imply that the primary bonding in the CN films is sp2. In other words, the formation of the sp3 bonding in the CN films can be suppressed effectively by doping with N atoms, and thus the thickness expansion resulting from the changes in the density of CN films during annealing can be decreased considerably. This result is also clarified by the increased conductivity measured. The XPS results give the information of the existence of the strong covalent bonding between N and C atoms, which can slow down the tendency of the structural relaxation during annealing. These results suggest that CN films suitable for soft X-ray multilayers used at high-temperature environments can be obtained by reactive dual-facing-target sputtering. With the low-angle X-ray diffraction measurements, we do observe the enhanced thermal stability of CoN/CN multilayers.

Aging effect of Co/C soft X-ray multilayer mirrors

We have investigated the aging effect of Co/C soft X-ray multilayers prepared by dualfacing-target sputtering. It was found that phase-separation phenomena exist in the Co/C multilayers, which causes the reflectivity at grazing incidence to increase with time, and can be interpreted as positive enthalpy of Co-C mixing. It is evident that oxidation of the outermost layer of Co/C multilayers with Co deposited last is a potential problem in applications where the highest possible reflectivity is required.

Aging effect of Co/C soft x-ray multilayer mirrors

The effect of aging on Co/C multilayer x-ray mirrors is presented. One significant result is the enhancement of the reflectivity at grazing incidence with time for the Co/C multilayers with C-on-top stored in air or argon and Co-on-top stored in argon. This can be interpreted in terms of a Co–C phase-separation at Co–C interfaces due to the positive enthalpy of Co–C mixing. Results also show that oxidation of the surface of Co-on-top Co/C multilayers plays an important role in the decrease of reflectivity. The oxidation can be prevented by storing the multilayers in an oxygen-free atmosphere or by depositing amorphous carbon as the top layer. The reflectivity of tarnished multilayers can be restored by removing the oxides by wet chemical methods.

Fabrication of Soft .CHI.-Ray Multilayer Mirrors by Excimer Laser-Induced Chemical Vapor Deposition.

An argon-fluoride (ArF) excimer laser-induced chemical vapor deposition (LCVD) technique has been developed for fabrication of soft X-ray multilayer mirrors. Film thickness distribution is controlled by scanning a laser beam on the substrate. Tungsten-carbon (W/C) and tungsten-silicon (W/Si) multilayers with a uniform film thickness are deposited and characterized from soft X-ray reflectivity measurement. Furthermore, a W/Si multilayer with laterally varying film thicknesses is successfully fabricated, and the feasibility of LCVD was demonstrated for fabricating multilayer mirrors for high performance soft X-ray focusing systems.

Enhanced reflectivity of soft x-ray multilayer mirrors by reduction of Si atomic density

We report a significant increase of the reflectivity of a soft x-ray Mo/Si multilayer mirror after low energy hydrogen ion beam bombardment of each of the Si layers after deposition. Cross section transmission electron microscopy pictures indicate no significant qualitative difference in interface roughness between the two samples. Elastic recoil detection and Rutherford backscattering spectrometry reveal a concentration of 22 at. % of H in the ion beam bombarded Si layers and a 12% reduction of the Si atomic density. Calculations using the measured atomic density and a very simple roughness model agree with the measured reflectivities. This is the first report of the modification of atomic density of Si in order to change the x-ray optical constants of the Si layer.