Fabrication of multi-scale structures with multiple X-ray masks and synchrotron hard X-ray irradiations

Synchrotron hard X-ray irradiation can be utilized in lithography processes to manufacture precise structures. Due to the difficulty of precise X-ray mask fabrication in hard X-ray lithography, this X-ray process has been used mainly to fabricate precise microstructures. In this study, a technology is proposed for fabricating novel multi-scale patterns that include submicron-scale structures using hard X-rays. The required X-ray masks for submicron-sized patterning are fabricated by a simple UV lithography process and sidewall metal deposition. Above all, thanks to the high penetration capability of hard X-rays with sub-nanometer wavelengths, it is possible to employ multiple masks to fabricate a variety of patterns. By combining each sub-micron X-ray mask with typical micro-sized X-ray masks, a unique X-ray lithography is performed, and various multi-scale structures are fabricated. The usefulness of the proposed technology is demonstrated by the realization of these structures.     

Multilayer mirror systems to form hard X-ray beams

This paper is an overview of the research activities carried out in the past five years at the Institute for Physics of Microstructures RAS and “X-ray” Company towards the manufacture of multilayer mirror systems capable of forming X-ray beams in the subnanometer range of wavelengths. The systems fabrication technology is presented, including techniques for producing supersmooth surfaces of specified shape, methods of graded multilayer structure deposition on such surfaces, and the principles of designing optimal mirror parameters. The characteristics of a quadrelliptical reflector—a novel high light-gathering power four-corner focusing system—are reported.     

X-ray masks based on epoxygraphite

A simple fabrication technology of hard X-ray masks with thin (50–150μm thick) X-ray transparent bearing membranes made of a new material, i.e., polymerized epoxy resin with graphite filler (hereafter, epoxygraphite), is described. The first results of using such masks in pattern scanning synchrotron X-ray lithography in the exposing radiation wavelength range λ ≈ 0.5–3 Å are presented. The prospects of applications of such masks in the softer spectral range λ ≈ 3–7 Å are considered.     

Fabrication of quasi-optical selective elements for the terahertz range in the form of pseudometallic structures via deep X-ray lithography

A technique for fabricating self-bearing pseudometallic structures, which hold promise for utilization as quasi-optical frequency-selective elements in the terahertz range of the electromagnetic spectrum, is discussed. The technique is based on microstructuring a continuous dielectric layer via stencilled X-ray lithography involving synchrotron radiation with subsequent metallization of the entire structure surface. The main manufacturing schemes are described, including fabrication of the initial substrates and X-ray masks. Examples of samples of the produced selective elements, such as frequency filters and flat lenses, as well as their operating characteristics, are presented.     

The effect of the chemical environment on theKβ/Kα X-ray intensity ratio

Summary Chemical effects on theKβ/Kα X-ray intensity ratios were investigated for different constitutions of Ti, V, Fe, Se, Br, Zr and Ce by a Ge(Li) X-ray detector. The vacancies were produced by heavily filtered²⁴¹Am gamma-rays. It is found that theKβ/Kα X-ray intensity ratios measured with compounds deviated up to 12% from the corresponding values of the pure elements (Ti, V, Fe) are larger than for the others (Se, Br, Zr and Ce).     

Calcium in ancient glazes and glasses: a XAFS study

Ceramic tiles used to manufacture artistic panels during the XVI to the XVIII centuries were decorated with high-lead soda-lime glazes, incorporating a diversity of chromophore cations, as ascertained by SRXRF (synchrotron radiation X-ray fluorescence). Previous X-ray absorption spectroscopy (XAS) studies have shown that sodium and lead are hosted by the glassy matrix in those glazes. However, the possible role of calcium as a modifier of the tetrahedral silica network is not fully clarified, despite being recognized that calcium cations alter some fundamental properties of glazes, namely transparency. An X-ray absorption fine structure (XAFS) study of glazes with varied colorings was therefore undertaken at Ca K- and L-edges. Well crystallized oxide minerals were used to model distinct coordination environments by oxygen atoms – close to octahedral geometry in calcite and dodecahedral in gypsum – while fluorite was chosen to mimic ideal cubic coordination. A first XAS approach suggested a minor variation in the energy separation between L₂–L₃ absorption edges when comparing blue and yellow glazes, irrespective of the period of manufacture. A further study on the X-ray absorption near-edge structure (XANES) carried out at the K-edge corroborated this difference and, along with the theoretical spectra modeling performed with the FEFF code, allowed interpreting of the Ca 1s absorption spectra of glazes as arising from a non-regular high-coordination environment within the silica matrix. PACS  61.43.Fs; 41.60.Ap; 61.10.Ht     

Multilayer optics for XUV spectral region: technology fabrication and applications

We present research investigations in the field of multilayer optics in X-ray and extreme ultra-violet ranges (XUV), aimed at the development of optical elements for applications in experiments in physics and in scientific instrumentation. We discuss normal incidence multilayer optics in the spectral region of “water window”, multilayer optics for collimation and focusing of hard X-ray, multilayer dispersing elements for X-ray spectroscopy of high-temperature plasma, multilayer dispersing elements for analysis of low Z-elements. Our research pays special attention to optimization of multilayer optics for projection EUV-lithography (ψ-13nm) and short period multilayer optics.     

Simulation of Reciprocal Space Maps with the Use of Spectral Angular Diagrams in the Triple Crystal X-Ray Diffraction Scheme

An approach to the simulation of reciprocal space maps corresponding to the maps obtained experimentally by the triple crystal X-ray diffractometry (TXD) is proposed. A specific feature of the approach is the use of spectral angular distribution diagrams of X-ray radiation, which allows one to visualize the two-dimensional pattern of the spectral angular “composition” of an X-ray beam after its interaction with each element of the scheme and thus to take into account the contribution of the hardware function of the experimental setup. The algorithms developed allow calculations for a wide class of radiation sources (from an X‑ray tube with any material of the anode to a synchrotron radiation source) and X-ray optical elements (slits, X-ray mirrors of monochromators, and analyzers). The results of simulation are compared with the experimental data for dispersive diffraction geometry, which confirms the adequacy of the proposed approach and its applicability to the simulation of a diffraction pattern corresponding to a real experiment in the triple crystal scheme.     

Measurement of the K shell X-ray production cross-sections and fluorescence yields for Nd,Eu, Gd,Dy and Ho using radioisotope X-ray fluorescence in the external magnetic field

The effect of external magnetic field on the K_α and K_β X-ray production cross-sections and K shell fluorescence yields for ferromagnetic elements Nd, Gd and Dy and paramagnetic elements Eu and Ho have been measured at the excitation energy of 59.5 keV γ -rays from ²⁴¹Am radioactive source of strength 100 mCi in the external magnetic field of intensities ±0.75 T. Furthermore, I_Kβ /I_Kα intensity ratios for these elements have been measured in the external magnetic field. The K X-rays from different targets were detected using a high resolution Si(Li) semiconductor detector. For B = 0, the measured K X-ray production cross-sections, K shell fluorescence yields and the I_Kβ /I_Kα intensity ratios were compared with the experimental and theoretical data in literature. The results have shown that the fluorescence parameters as photoionization cross section, fluorescence yield, radiation rates and spectral linewidth can change when the irradiation is conducted in a magnetic field.     

The X-ray fluorescence cross-section for bromide and iodide compounds

The K_α and K_β X-ray fluorescence cross-sections for the bromide and the iodide compounds were measured by a high-resolution Si(Li) X-ray detector. The vacancies were produced by heavily filtered ²⁴¹Am gamma rays. We found that K_α and K_β X-ray fluorescence cross-sections are changed by chemical effect for different Br and I compounds. Experimental results were compared with the calculated values of Br and I elements. Received 15 May 2001 and Received in final form 8 July 2001     

Synchrotron-based X-ray fluorescence,imaging and elemental mapping from biological samples

The present study utilized the new hard X-ray microspectroscopy beamline facility, X27A, available at NSLS, BNL, USA, for elemental mapping. This facility provided the primary beam in a small spot of the order of ∼10 μm, for focussing. With this spatial resolution and high flux throughput, the synchrotron-based X-ray fluorescent intensities for Mn, Fe, Zn, Cr, Ti and Cu were measured using a liquid-nitrogen-cooled 13-element energy-dispersive high-purity germanium detector. The sample is scanned in a ‘step-and-repeat’ mode for fast elemental mapping measurements and generated elemental maps at 8, 10 and 12 keV, from a small animal shell (snail). The accumulated trace elements, from these biological samples, in small areas have been identified. Analysis of the small areas will be better suited to establish the physiology of metals in specific structures like small animal shell and the distribution of other elements.     

Chemical effects on the K<Subscript>β</Subscript>/K<Subscript>α</Subscript> X-ray intensity ratios of Mn,Ni and Cu complexes

Chemical effects on the K_β/K_α X-ray intensity ratios for some Mn, Ni, and Cu complexes of a new schiff-base with salen N₂H₂ type were investigated. The samples were excited by 59.543 keV γ-rays from a ²⁴¹Am annular radioactive source. K X-rays emitted by samples were counted by a Si(Li) detector with resolution 157 eV at 5.9 keV. We observed the chemical effect on the K_β/K_α X-ray intensity ratios for Mn, Ni and Cu complexes. The experimental results showed that the K_β/K_α X-ray intensity ratios for compounds with complexes are generally larger than those with salt form. The experimental values have been compared with the other experimental and the theoretically calculated values of pure elements. The results are in very good agreement with the others.     

聚合物阵列波导光栅的制作技术

研究了聚合物阵列波导光栅AWG制作的几个关键技术.首先,为了克服反应离子刻蚀过程中单独使用光刻胶作掩膜而导致的光波导形状和尺寸偏离设计的缺点,采用了光刻胶与金属掩膜相结合的双掩膜技术进行器件制作.详细介绍了双掩膜技术制备聚合物AWG的过程,并得出铝膜作为掩膜的最佳厚度为100nm左右.测试给出了使用和没有使用双掩膜的对比结果,该结果表明使用双掩膜技术制作的波导质量明显好于单独使用光刻胶作掩膜制作的结果.其次,采用蒸气回溶技术来减小反应离子刻蚀产生的波导表面和侧壁的起伏,从而降低了波导的散射损耗.结果表明,蒸气回溶技术使所制作的波导表面的均方根粗糙度从41.307nm降低到24.564nm.     

组合材料芯片技术及其应用

组合材料芯片技术是用一系列掩膜在同一块基片上获得含不同参数单元样品面阵的方法．文章介绍了它在量子阱特性、碲镉汞零偏电阻值、三元合金制备、半导体深能级捕获截面的研究以及在波分复用器件、滤光片式分光元件制作方面的一些新应用．作为一种新的材料功能操控或制备技术，它在研究材料性质变化规律、建立材料性能数据库、筛选优良材料和制作面阵型元件等方面表现出高效、快捷等特点．     

Nonequilibrium laser-produced plasma of volume-structured media and inertial-confined-fusion applications

We review the results of experimental and theoretical studies of the properties of a nonequilibrium plasma produced from volume-structured media, containing micro- and nano-size internal elements, under laser-pulse irradiation. We consider two types of materials, i.e., regularly and stochastically structured materials. The first type is either a set of flat layers or cylindrical and spherical shells of micrometer thickness, and the second type is either foams of light elements or light foams containing clusters of heavy elements with dimensions in the range of 10–100 nm. We study the properties of high-temperature laser-produced plasmas of such materials and applications directed to developing the design of inertial confinement fusion (ICF) targets and creating powerful sources of thermonuclear neutron and soft X-ray emission initiated by the laser pulse. The foam materials can be used as absorbers capable of providing homogeneity of laser-energy absorption by the target. A neutron yield up to 1014−1015 DT neutrons per shot can be achieved by heating regularly structured materials using a laser pulse in the regime of the consequent thermal explosions of solid elements containing isotopes of hydrogen. Laser-radiation conversion into soft X-ray emission with the efficiency controlled in a wide range may be realized in laser-produced plasmas of porous media doped with clusters of heavy elements. In particular, such a material can be used as an absorber–converter of laser radiation in inertial confinement fusion targets. Under direct irradiation of an ICF target by a laser pulse, such a converter can provide transformation of 20–30% of the absorbed laser energy into the energy of X-ray radiation transferred to thermonuclear capsules.     

软X射线投影光刻技术及其发展

软X射线投影光刻的研究近年来取得了突破性进展，所采用的新型光学系统由于无污染激光等离子光源及分辨率大视场投影光刻系统组成，该技术多采用无应力光学装调工艺、深亚纳米级的镜面加工和多层膜制备技术及低缺陷反射式掩摸技术，该技术还采用表面成像光刻胶技术并涉及到精密扫描机构等技术，本文介绍了这一技术的发展历史，关键技术以及研究进展。     

Uncooled microbolometer detector: recent developments at ULIS

Uncooled infrared focal plane arrays are being developed for a wide range of thermal imaging applications. Fire-fighting, predictive maintenance, process control and thermography are a few of the industrial applications which could take benefit from uncooled infrared detector. Therefore, to answer these markets, a 35-μm pixel-pitch uncooled IR detector technology has been developed enabling high performance 160×120 and 384×288 arrays production. Besides a wide-band version from uncooled 320×240/45 μm array has been also developed in order to address process control and more precisely industrial furnaces control. The ULIS amorphous silicon technology is well adapted to manufacture low cost detector in mass production. After some brief microbolometer technological background, we present the characterization of 35 μm pixel-pitch detector as well as the wide-band 320×240 infrared focal plane arrays with a pixel pitch of 45 μm. The paper presented there appears in Infrared Photoelectronics, edited by Antoni Rogalski, Eustace L. Dereniak, Fiodor F. Sizov, Proc. SPIE Vol. 5957, 59570M (2005).     

Study of ZnO and Ni-doped ZnO synthesized by atom beam sputtering technique

Zinc oxide (ZnO) and Ni-doped zinc oxide (ZnO:Ni) films are prepared by atom beam sputtering with an intent of growing transparent conducting oxide (TCO) material and understanding its physical properties. The crystalline phases of the films are identified by the grazing angle X-ray diffraction (GAXRD) technique. Thicknesses of the films are measured by ellipsometry. Chemical states of the elements present in the films are investigated by X-ray photoelectron spectroscopy (XPS), which indicates the presence of Ni in the ZnO environment in a divalent state. Average transmission across the ZnO:Ni film was determined to be ∼83% in the visible region, which is less than that (∼90%) of undoped ZnO films. The resistivity measured by van der Pauw technique of the ZnO:Ni film (∼9×10^-3 Ω cm) is two orders of magnitude smaller as compared to its undoped counterpart (1 Ω cm). For ZnO:Ni film an average carrier concentration of ∼1.4×10¹⁹ cm^-3 was observed by Hall measurements. Two important mechanisms reported in the literature viz. influence of d–d transition bands and electron scattering from crystallites/grains are discussed as the possible causes for the increase in conductivity on Ni doping in ZnO. PACS 73.50.Bk; 78.66.Li; 79.60.Dp; 61.05.cp     

Estimation of InN phase inclusion in InGaN films grown by MOVPE

The amount of InN included in InGaN films grown by MOCVD (metalorganic chemical vapor deposition) was estimated by X-ray diffraction measurement technology. The In compositions in our InGaN films are measured as 0.1–0.34 by X-ray 2θ scan using Vegard’s law. The inclusion of InN in InGaN layers was obtained as 0.0684–2.6396% by measuring the ratio of the integrated intensity of the InN (0002) peak to that of the InGaN (0002) peak in X-ray rocking curves. The theoretical diffraction intensities from InN and InGaN have been calculated according to the X-ray-diffraction theory. The values of the InN inclusion for all our samples were less than 3%, which indicated that the degree of phase separation of the samples was low. It was also found that the flow rate of N₂ carrier gas and the operation pressure strongly affected the InN inclusion in InGaN. Received: 20 November 2000 / Accepted: 16 May 2001 / Published online: 27 June 2001     

Characterisation of baroque tin amalgam mirrors of the historical Green Vault in Dresden

The historical Green Vault, one of Europe’s most sumptuous treasure chambers, has reopened in September 2006 in the Dresden Royal Palace. For the baroque presentation of the artworks the special properties of tin amalgam mirrors are of great importance. A comprehensive analytic characterisation was necessary for restoration and reconstruction. The different original casting glasses were analysed in respect of chemical composition, roughness, waviness and optical properties like chromaticity coordinates and transmittance. The microstructure of the tin amalgam layers were investigated on metallographic cross-sections and by X-ray diffraction. The investigations reveal that the tin amalgam layers are composed of γ-HgSn_6-10 phase with a grain size between 5 and 50 μm surrounded by a thin mercury phase with about 2 wt. % tin. However the most important property of the baroque tin amalgam mirrors is a relative low reflectivity of about 59% which is drastically lower than for silver mirrors with a reflectivity of about 96%. According to the characterisation results a suitable glass for reconstruction was selected. The mirror layers were produced by historical tin amalgam technology for the rooms not destroyed by bombarding of Dresden in February 1945. For the completely destroyed Jewel Room pure tin layers were deposited by magnetron sputtering. The results show that this new technology enables an adequate substitute for the original tin amalgam layers. PACS  61.66.-f; 74.25.Gz; 61.10.Nz; 68.37.Hk