High-resolution X-ray imaging—a powerful nondestructive technique for applications in semiconductor industry

The availability of high-brilliance X-ray sources, high-precision X-ray focusing optics and very efficient CCD area detectors has contributed essentially to the development of transmission X-ray microscopy (TXM) and X-ray computed tomography (XCT) with sub-50 nm resolution. Particularly, the fabrication of high aspect ratio Fresnel zone plates with zone widths approaching 15 nm has contributed to the enormous improvement in spatial resolution during the previous years. Currently, Fresnel zone plates give the ability to reach spatial resolutions of 15 to 20 nm in the soft and of about 30 to 50 nm in the hard X-ray energy range. X-ray microscopes with rotating anode X-ray sources that can be installed in an analytical lab next to a semiconductor fab have been developed recently. These unique TXM/XCT systems provide an important new capability of nondestructive 3D imaging of internal circuit structures without destructive sample preparation such as cross sectioning. These lab systems can be used for failure localization in micro- and nanoelectronic structures and devices, e.g., to visualize voids and residuals in on-chip metal interconnects without physical modification of the chip. Synchrotron radiation experiments have been used to study new processes and materials that have to be introduced into the semiconductor industry. The potential of TXM using synchrotron radiation in the soft X-ray energy range is shown for the nondestructive in situ imaging of void evolution in embedded on-chip copper interconnect structures during electromigration and for the imaging of different types of insulating thin films between the on-chip interconnects (spectromicroscopy).     

软X射线显微成像位相型波带片浅析

软X射线显微成像技术是研究超微观世界的有力工具,而位相型波带片则以其高分辨率的优势,目前已成为实现软X射线成像的理想光学元件.本文简要介绍位相型波带片的特性及其在软X射线显微成像技术中的应用.     

上海光源硬X射线相干衍射成像实验方法初探

相干X射线衍射成像方法是一种先进的成像技术,分辨率可达纳米量级.国际上大多数的同步辐射装置和自由电子激光装置都建立了该成像方法,并有将其作为主要成像技术的趋势.上海光源作为目前国内唯一的一台第三代同步辐射光源,尚未建立基于硬X射线的相干衍射成像实验平台.随着一批以波荡器为光源的光束线站投入使用,使得该方法的建立成为了可能.本文基于上海光源BL19U2生物小角散射线站,通过有效的光路设计,搭建了相干衍射实验平台,在12 keV和13.5 keV能量点均获得了硬X射线相干光束,并基于小孔衍射测量了入射光束的空间相干长度.该平台支持常规和扫描相干衍射实验模式,对小孔衍射图样及波带片扫描衍射图样实现了正确的相位重建,证明了该平台初步具备开展硬X射线相干衍射成像实验的能力.硬X射线相干衍射成像实验平台为国内首次建立,将为国内该实验方法的发展和应用提供有效的软硬件支持.     

One-dimensional Wolter optics with a sub-50 nm spatial resolution

We studied an imaging system consisting of an elliptical mirror and a hyperbolic mirror [i.e., one-dimensional (1D) Wolter optics] to realize an achromatic full-field hard x-ray microscopy with a resolution better than 50 nm. We report the performance of this 1D Wolter optical system when the mirrors were ultraprecisely figured by elastic emission machining. Experiments to form a demagnified image (demagnification factor of 385) of a 10 μm slit were conducted at an x-ray energy of 11.5 keV at BL29XUL of SPring-8. The system could form a demagnified image with a resolution better than 50 nm over a 12.1 μm field.     

Fabrication of high‐aspect‐ratio Fresnel zone plates by e‐beam lithography and electroplating

The fabrication of gold Fresnel zone plates, by a combination of e‐beam lithography and electrodeposition, with a 30 nm outermost zone width and a 450 nm‐thick structure is described. The e‐beam lithography process was implemented with a careful evaluation of applied dosage, tests of different bake‐out temperatures and durations for the photoresist, and the use of a developer without methylisobutylketone. Electrodeposition with a pulsed current mode and with a specially designed apparatus produced the desired high‐aspect‐ratio nanostructures. The fabricated zone plates were examined by electron microscopy and their performances were assessed using a transmission X‐ray microscope. The results specifically demonstrated an image resolution of 40 nm.     

Imaging Properties of Hard X-Ray Zone Plates with Corrugated Boundary Roughness

The imaging properties of hard X-ray multilayer zone plates with corrugated roughness along circular zone boundaries are investigated. First, the transmission function for zone plates with the roughness is derived using a geometric optical approach, and based on the Fresnel-Kirchhoff diffraction theory formulas are developed to calculate the point spread function (PSF) efficiently, assuming that the roughness increases with radius. Then, the PSFs for various magnitudes and angular configurations of the roughness are presented, and the imaging properties are discussed particularly in terms of the focusing efficiency (or the Strehl ratio) and the resolution. Tolerances for the maximum magnitude of the roughness, and the relationship between the angular configuration of the roughness and the symmetry of the PSF are also discussed.     

电子束和X射线双曝光制作大高宽比高分辨率的X射线波带片

介绍了利用电子束和 X射线束双曝光技术制作大高宽比高分辨率的 X射线聚焦或色散元件的新方法 (波长范围为 1～ 5 nm )。所制做的厚度为 10μm的 Au波带片具有 30个波带 ,最外环的宽度为 0 .5μm。实验表明 :对 8ke V的X射线来说 ,波带片的衬度大于 10 ,分辨率为 0 .5 5μm,焦距为 2 1.3cm。     

Fourier treatment to the diffractive optical element composed of Fresnel zone and pinholes

Currently, the minimum feature size fabricated is about 15-40 nm. The resolution of Fresnel zone plates is limited by the width of the outermost zone. Although the photon sieves make it possible to focus soft X-rays to spot sizes smaller than the diameter of the smallest pinhole they have low diffraction efficiency. In order to foster strengths and circumvent weaknesses of them, we propose a new model which is composed of Fresnel zone and pinholes and give its fast Fourier algorithm. The simulation results demonstrate that the resolution of photon sieves is not better than that of Fresnel zone plates in low order of local rings. In this case, we can substitute pinholes for Fresnel zone in photon sieves. Resolution is nearly a constant, and also the diffraction efficiency improves.     

Penetrating view of nano-structures in Aleochara verna spermatheca and flagellum by hard X-ray microscopy

A penetrating view of the three-dimensional nanostructure of female spermatheca and male flagellum in the species Aleochara verna is obtained with 100-nm resolution using a hard X-ray microscope, which provides a fast noninvasive imaging technology for insect morphology. Through introducing Zernike phase contrast and heavy metal staining, images taken at 8 keV displayed sufficient contrast for observing nanoscale fine structures, such as the spermatheca cochleate duct and the subapex of the flagellum, which have some implications for the study of the sperm transfer process and genital evolution in insects. This work shows that both the spatial resolution and the contrast characteristic of hard X-ray microscopy are quite promising for insect morphology studies and, particularly, provide an attractive alternative to the destructive techniques used for investigating internal soft tissues.     

Hard X ray holographic diffraction imaging

We determine the absolute electron density of a lithographically grown nanostructure with 25 nm resolution by combining hard x-ray Fourier transform holography with iterative phase retrieval methods. While holography immediately reveals an unambiguous image of the object, we deploy in addition iterative phase retrieval algorithms for pushing the resolution close to the diffraction limit. The use of hard (8 keV) x rays eliminates practically all constraints on sample environment and enables a destruction-free investigation of relatively thick or buried samples, making holographic diffraction imaging a very attractive tool for materials science. We note that the technique is ideally suited for subpicosecond imaging that will become possible with the emerging hard x-ray free-electron lasers.     

Three‐dimensional coherent diffractive imaging on non‐periodic specimens at the ESRF beamline ID10

The progress of tomographic coherent diffractive imaging with hard X‐rays at the ID10 beamline of the European Synchrotron Radiation Facility is presented. The performance of the instrument is demonstrated by imaging a cluster of Fe₂P magnetic nanorods at 59 nm 3D resolution by phasing a diffraction volume measured at 8 keV photon energy. The result obtained shows progress in three‐dimensional imaging of non‐crystalline samples in air with hard X‐rays.     

菲涅耳波带板应用于聚变靶的高分辨X射线成像分析

在惯性约束核聚变研究中,为了实现1μm高空间分辨keV-X射线成像,文中发展了菲涅耳波带板(FZP)直接成像的分析方法,并通过数值计算研究了FZP的成像特性.针对钛K_α线(光子能量4.51 keV,波长0.275 nm),提出了FZP参数,对制作技术的要求较低.研究了靶尺度的影响.FZP的有效视场使它能够对数毫米大尺度靶实现高分辨成像.还研究了入射光的光谱带宽对成像的影响.FZP的色差有助于单色成像,但是带宽超过限度会导致像的反衬度降低.这些结果表明FZP应用于聚变点火靶的高空间分辨X射线成像的能力,也为应用提出了要求. 关键词： X射线成像 惯性约束核聚变 菲涅耳波带板     

Design and performance of an X‐ray scanning microscope at the Hard X‐ray Nanoprobe beamline of NSLS‐II

A hard X‐ray scanning microscope installed at the Hard X‐ray Nanoprobe beamline of the National Synchrotron Light Source II has been designed, constructed and commissioned. The microscope relies on a compact, high stiffness, low heat dissipation approach and utilizes two types of nanofocusing optics. It is capable of imaging with ～15 nm × 15 nm spatial resolution using multilayer Laue lenses and 25 nm × 26 nm resolution using zone plates. Fluorescence, diffraction, absorption, differential phase contrast, ptychography and tomography are available as experimental techniques. The microscope is also equipped with a temperature regulation system which allows the temperature of a sample to be varied in the range between 90 K and 1000 K. The constructed instrument is open for general users and offers its capabilities to the material science, battery research and bioscience communities.     

Aspects of nanometer scale imaging with extreme ultraviolet (EUV) laboratory sources

Imaging systems with nanometer resolution are instrumental to the development of the fast evolving field of nanoscience and nanotechnology. Decreasing the wavelength of illumination is a direct way to improve the spatial resolution in photon-based imaging systems and motivated a strong interest in short wavelength imaging techniques in the extreme ultraviolet (EUV) region. In this review paper, various EUV imaging techniques, such as 2D and 3D holography, EUV microscopy using Fresnel zone plates, EUV reconstruction of computer generated hologram (CGH) and generalized Talbot self-imaging will be presented utilizing both coherent and incoherent compact laboratory EUV sources. Some of the results lead to the imaging with spatial resolution reaching 50 nm in a very short exposure time. These techniques can be used in a variety of applications from actinic mask inspection in the EUV lithography, biological imaging to mask-less lithographic processes in nanofabrication.     

Coherent x-ray diffraction imaging with nanofocused illumination

Coherent x-ray diffraction imaging is an x-ray microscopy technique with the potential of reaching spatial resolutions well beyond the diffraction limits of x-ray microscopes based on optics. However, the available coherent dose at modern x-ray sources is limited, setting practical bounds on the spatial resolution of the technique. By focusing the available coherent flux onto the sample, the spatial resolution can be improved for radiation-hard specimens. A small gold particle (size <100 nm) was illuminated with a hard x-ray nanobeam (E=15.25 keV, beam dimensions approximately 100 x 100 nm2) and is reconstructed from its coherent diffraction pattern. A resolution of about 5 nm is achieved in 600 s exposure time.     

自支撑二值化Beynon-Gabor波带片的制备及其单级聚焦特性

Gabor波带片是一种理想的单级聚焦光学元件,但制备困难.本文采用聚焦离子束直写技术成功制备出30环、20扇区的二值化Beynon-Gabor波带片,其有效面积半径为700μm,第一环半径90μm.利用各向异性腐蚀液对硅基底进行开孔,实现了Beynon-Gabor波带片二值化、自支撑、镂空的结构特征.在波长为355 nm的激光下测试其光学性能,结果表明所制备的Beynon-Gabor波带片主光轴上只存在1级衍射叠加后的焦点,不存在高级衍射焦点,具有优异的单级聚焦性能.     

软X射线激光背光阴影成像技术的空间分辨研究

软X射线激光阴影成像技术是一种诊断高温稠密等离子体临界面附近阴影轮廓的诊断技术,具有测量视场大、空间分辨能力高的特点,具有重要的应用前景.对该技术的空间分辨具体能够达到什么程度则没有进行过系统研究.本文分别从光路几何、衍射极限、成像像差三个方面进行了仔细分析,结果表明目前采用该技术的诊断系统能够达到约2μm的空间分辨.主要受限是光路几何因素,通过增加放大倍数、选择单元尺寸更小的接收元器件等方式,有希望达到优于1μm的空间分辨.     

X射线菲涅耳波带板成像和投影式相衬成像的数值模拟比较

通过解析分析和数值模拟,比较了钛K线（4.5 keV）与铜K线（8.0 keV）等X射线源背光透视物体情况下,菲涅耳波带板直接成像与投影式相衬成像对被透视物体的空间分辨能力。结果表明,波带板成像可实现优于1 m的高空间分辨能力,而且使用较大尺度背光源更有利于成像。对于高透射或弱吸收的透视物体,波带板难以成像,可采用投影式相衬成像实现m级空间分辨。计入了以前文献没有考虑到的更高阶影响后,解析给出了点光源照射下相衬像的强度分布与对比度。模拟了微焦点X射线源照射存在厚度起伏的薄膜靶以及密度空间调制靶的相衬成像,点光源情况下模拟结果和解析结果相符。讨论了光源大小、成像距离等参数对相衬成像对比度和空间分辨能力的影响,结果表明,通过减小光源尺度和调节物体到探测面的距离,空间分辨能力可优化到1～4 m。     

Wet-etched diffractive lenses for hard X-rays

A method for the fabrication of linear transmission Fresnel zone plates for X-rays in the 8-15 keV photon energy range is presented. The diffractive elements are generated by electron-beam lithography and chemical wet etching of (110)-oriented silicon membrane substrates. Diffractive structures with aspect ratios of more than 30 for 300 nm-wide structures were obtained. The diffraction efficiency of such a lens was measured for 13.3 keV radiation to be 20%.     

Performances of a metallic magnetic calorimeter for the measurement of hard X‐ray emission intensities

The energy spectrum analysis of X‐ray intensities with semiconductor detectors is often difficult because their energy resolution is usually not good enough to separate the different X‐ray lines. Metallic magnetic calorimeters (MMCs) can be an alternative; they can offer both high energy resolution and high intrinsic detection efficiency from 0 to 100 keV. MMCs are thermal detectors; that is to say, the energy of each absorbed photon is measured as a temperature elevation. At very low temperature, typically few tens of mK, a very large pulse height‐to‐noise ratio can be obtained that is an essential condition for high energy resolution. We are involved in the development of MMCs for metrology applications such as the determination of hard X‐ray emission intensities. For that purpose, we conceived an MMC with an energy resolution of 57 eV around 30 keV. The absorber is made of gold providing high intrinsic detection efficiency even for a small volume, greater than 90% below 60 keV. We will describe the physical principle and the practical realisation of this detector and discuss its performances by analysing the energy spectrum obtained from a ¹³³Ba source. Preliminary outcomes of relative emission intensities of the K X‐ray of cesium are presented and compared with other experimental data and theoretical calculations. Copyright © 2012 John Wiley & Sons, Ltd.