Nitriding molybdenum: Effects of duration and fill gas pressure when using 100-Hz pulse DC discharge technique

Molybdenum is nitrided by a 100-Hz pulsed DC glow discharge technique for various time durations and fill gas pressures to study the effects on the surface properties of molybdenum. X-ray diffractometry(XRD), scanning electron microscopy(SEM), and atomic force microscopy(AFM) are used for the structural and morphological analysis of the nitrided layers. Vickers’ microhardness tester is utilized to investigate surface microhardness. Phase analysis shows the formation of more molybdenum nitride molecules for longer nitriding durations at fill gas pressures of 2 mbar and 3 mbar(1 bar = 105Pa). A considerable increase in surface microhardness(approximately by a factor of 2) is observed for longer duration(10 h) and 2-mbar pressure. Longer duration(10 h) and 2-mbar fill gas pressure favors the formation of homogeneous, smooth, hard layers by the incorporation of more nitrogen.     

Mass Spectrometric Analysis of Water-soluble Gold Nanoclusters

Batches of water-soluble gold nanoclusters of nominal 2.0 or 3.5-nm diameter were prepared to evaluate particle size determinations by a number of techniques such as transmission electron microscopy or atomic force microscopy and to validate estimates derived by mass spectrometric analysis using matrix-assisted laser desorption ionization (MALDI). Good agreement was found and MALDI lends itself to analyses even in the presence of aggregates.     

Dopant profiling in silicon nanowires measured by scanning capacitance microscopy

Silicon nanowires (SiNWs) with axial doping junctions were synthesized via the Au‐catalyzed vapor–liquid–solid growth method with the use of HCl. In this work, dopant profiling from three axially doped SiNWs with p–i, p–n and n–i–p junctions were investigated using both scanning electron microscopy (SEM) and scanning capacitance microscopy (SCM). It turns out that observed doping contrasts in SEM are also affected by the surface roughness and sample charging. In contrast, SCM allows us to delineate with sub‐10 nm resolution the electrical junctions and provides a relative value of the doping concentration in each segment of the NW. SCM clearly evidences the expected doping regions within these SiNWs thanks to the addition of HCl during the growth that strongly prevents shell overgrowth. (© 2014 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Local thermal conductivity of polycrystalline AlN ceramics measured by scanning thermal microscopy and complementary scanning electron microscopy techniques

The local thermal conductivity of polycrystalline aluminum nitride (AlN) ceramics is measured and imaged by using a scanning thermal microscope (SThM) and complementary scanning electron microscope (SEM) based techniques at room temperature. The quantitative thermal conductivity for the AlN sample is gained by using a SThM with a spatial resolution of sub-micrometer scale through using the 3ω method. A thermal conductivity of 308 W/m·K within grains corresponding to that of high-purity single crystal AlN is obtained. The slight differences in thermal conduction between the adjacent grains are found to result from crystallographic misorientations, as demonstrated in the electron backscattered diffraction. A much lower thermal conductivity at the grain boundary is due to impurities and defects enriched in these sites, as indicated by energy dispersive X-ray spectroscopy.     

A Raman spectroscopic and combined analytical approach to the restoration of severely damaged frescoes: the Palomino project

The deterioration of art objects is normally relatively minor, controllable and attributable to environmental changes or bacterial invasion, and until now there has not been any recorded attempt to analyse an artwork that has been deliberately and significantly destroyed. The analytical problems are correspondingly larger but the potential reward from any information that can be forthcoming is thereby proportionately greater. The 17th Century Palomino frescoes on the vaulted ceiling of the Church of Sant Joan del Mercat in Valencia were largely destroyed by insurgents in the Spanish Civil War in 1936. The ensuing gunfire and a series of seven conflagrations inside the church had a devastating effect upon the artwork, and the surviving areas were also rendered unstable with respect to their detachment from the substrate. During the current restoration project being undertaken on these frescoes, an opportunity was provided for the application of several analytical techniques to secure information about the original pigment palette employed, the technology of application used by Palomino and the changes consequent upon the destruction process. Here, we report for the first time the use of analytical Raman spectroscopy, supported by scanning electron microscopy (SEM) and voltammetry of microparticles, for the combined identification of pigments, binders, substrate treatments and pigment alteration in an important, although badly damaged, wall painting for the informing of the ongoing conservation and restoration strategy. Copyright © 2008 John Wiley & Sons, Ltd.     

Identification of pigments from the Shrine of Kaiping Diaolou by micro‐Raman spectroscopy

Shrines (or altars) are constructed in China for worshiping ancestors, Bodhisattva, and God of Wealth. In this work, pigments from the shrine of Kaiping Diaolou tower were analyzed by micro‐Raman spectroscopy, in conjunction with other analytical methods including scanning electron microscopy (SEM) with energy dispersive X‐ray spectroscopy (EDX) and X‐ray fluorescence (XRF). Paintings of the shrine were composed of 2–3 pigment layers and the total thickness was determined as about 200–300 µm by optical microscopy and SEM, indicating the fine painting skills applied in the construction of the shrine. The green pigments on the surface layer of the green fragment were identified as a mixture of lead phthalocyanine (PbPc) and cornwallite (Cu₅(AsO₄)₂(OH)₄) by XRF and micro‐Raman spectroscopy with two different excitation wavelengths (488 and 785 nm). Underneath the green layer, red and yellow ochre were found. The pigments on the surface layer of red and blue fragments were identified as hematite (Fe₂O₃) and lazurite or synthetic ultramarine [(Na₈(Al₆Si₆O₂₄)S₃)], respectively. Finally, the pigments under the two surface layers were identified by EDX and micro‐Raman spectroscopy as chromium oxide (Cr₂O₃), gypsum (CaSO₄·2H₂O) and calcite (CaCO₃). Copyright © 2011 John Wiley & Sons, Ltd.     

二维原子晶体的低电压扫描透射电子显微学研究

二维原子晶体材料,如石墨烯和过渡金属硫族化合物等,具有不同于其块体的独特性能,有望在二维半导体器件中得到广泛应用.晶体中的结构缺陷对材料的物理化学性能有直接的影响,因此研究结构缺陷和局域物性之间的关联是当前二维原子晶体研究中的重要内容,需要高空间分辨率的结构研究手段.由于绝大部分二维原子晶体在高能量高剂量的电子束辐照下容易发生结构损伤,利用电子显微方法对二维原子晶体缺陷的研究面临诸多挑战.低电压球差校正扫描透射电子显微(STEM)技术的发展,一个主要目标就是希望在不损伤结构的前提下对二维原子晶体的本征结构缺陷进行研究.在STEM下,多种不同的信号能够被同步采集,包括原子序数衬度高分辨像和电子能量损失谱等,是表征二维原子晶体缺陷的有力工具,不但能对材料的本征结构进行单原子尺度的成像和能谱分析,还能记录材料结构的动态变化.通过调节电子束加速电压和电子辐照剂量,扫描透射电子显微镜也可以作为电子刻蚀二维原子晶体材料的平台,用于加工新型纳米结构以及探索新型二维原子晶体的原位制备.本综述主要以本课题组在石墨烯和二维过渡金属硫族化合物体系的研究为例,介绍低电压扫描透射电子显微学在二维原子晶体材料研究中的实际应用.     

Integration of correlative Raman microscopy in a dualbeam FIB SEM

We present an integrated confocal Raman microscope in a focused ion beam scanning electron microscope (FIB SEM). The integrated system enables correlative Raman and electron microscopic analysis combined with focused ion beam sample modification on the same sample location. This provides new opportunities, for example the combination of nanometer resolution with Raman advances the analysis of sub‐diffraction‐sized particles. Further direct Raman analysis of FIB engineered samples enables in situ investigation of sample changes. The Raman microscope is an add‐on module to the electron microscope. The optical objective is brought into the sample chamber, and the laser source, and spectrometer are placed in a module attached onto and outside the chamber. We demonstrate the integrated Raman FIB SEM function with several experiments. First, correlative Raman and electron microscopy is used for the investigation of (sub‐)micrometer‐sized crystals. Different crystals are identified with Raman, and in combination with SEM the spectral information is combined with structurally visible polymorphs and particle sizes. Analysis of sample changes made with the ion beam is performed on (1) structures milled in a silicon substrate and (2) after milling with the FIB on an organic polymer. Experiments demonstrate the new capabilities of an integrated correlative Raman–FIB–SEM. Copyright © 2016 John Wiley & Sons, Ltd.     

单层FeSe薄膜/氧化物界面高温超导

单层FeSe/SrTiO₃界面增强超导的发现为理解高温超导机理提供了一个新的途径,也为实现新的高温超导体开拓了新思路.本文通过在SrTiO₃（001）表面高温沉积Mg进而沉积单层FeSe薄膜,制备出了FeSe/MgO双层/SrTiO₃异质结.利用扫描隧道显微镜研究了异质结的电学及超导特性,观测到约14–15 meV的超导能隙,比体相FeSe超导能隙值增大了5–6倍,与K掺杂双层FeSe/SrTiO₃的超导能隙值相当.这一结果可理解为能带弯曲造成的界面电荷转移和界面处电声耦合共同作用导致的超导增强.FeSe/MgO界面是继FeSe/TiO₂之后的一个新界面超导体系,为研究界面高温超导机理提供了新载体.     

Scanning probe microscope with interchangeable AFM-FFM and STM heads

Summary A scanning probe microscope operating in air with interchangeable atomic force-friction force (AFM-FFM) and electronic-tunnelling (STM) heads is presented. Our AFM operates in the so-called contact mode and utilizes the optical-lever detection method which allows simultaneous measurement of the topography as well as the lateral force. The set-up also contains an optical microscope to control both the sample and the probe laser spot on the cantilever. The experimental method to change from AFM to STM operation is based on the use of the probe laser beam and the optical microscope. The maximum scanning area is (24×24) μm² and it is well embraced in the optical-microscope visual field. The microscope attains atomic resolution in air in both AFM and STM configuration. Its performance is demonstrated on the surface of different samples. In honour of Prof. Fausto Fumi on the occasion of his retirement from teaching.     

The transport and switching of Xe atoms on the Ni-W interface of a scanning tunnelling microscope

Summary The transport and switch of Xe atoms on the Ni-W interface of a scanning tunnelling microscope have been analysed for different geometries as a function of the tip position with respect to the Ni(110) surface. Our results show that the control of the different experimental results can only be achieved by a precise control of the position of the tip on the sample. In particular, the tip-sample Xe switch can only be obtained within tip heights of 0.2?. In honour of Prof. Fausto Fumi on the occasion of his retirement from teaching.     

Preparation,structural and magnetic characterization of synthetic anti-ferromagnetic (SAF) nanoparticles

Synthetic anti-ferromagnetic nanoparticles (SAFs) are a novel type of magnetic nanoparticle (MNP) fabricated using nanoimprint lithography, direct deposition of multilayer films and retrieval in liquid phase via an ‘etching’ release process. Such physical fabrication techniques enable accurate control of particle shape, size and composition. We systematically varied the processing conditions to produce different configurations of SAF nanoparticles and performed extensive characterization using transmission electron microscopy (TEM) and alternating gradient magnetometry (AGM) to study their corresponding structural and magnetic behavior. A key focus of this paper is the preparation of TEM cross-section specimens of SAF nanoparticles for their structural characterization. This is not a trivial task, but is useful and revealing in terms of structural features. A major finding from our study shows that the introduction of oxygen during deposition of the copper release layer gives significantly improved flatness of the multilayer structure but no significant change in the magnetic properties. Magnetic measurements show that these nanoparticles have nearly zero magnetic remanence, a linear response of magnetization and more than twice the saturation magnetization compared to iron oxide nanoparticles.     

Electrochemical tip-enhanced Raman Spectroscopy for microscopic studies of electrochemical interfaces

The review describes electrochemical applications of tip-enhanced Raman spectroscopy (TERS). These applications combine the merits of both scanning probe microscopy (SPM) and Raman spectroscopy, which enables us to simultaneously obtain high-resolution images of surface morphology and chemical information under the electrochemical environment. This review, first summarizes the pioneering work done on the TERS systems that operate in liquid and electrochemical environments, and then gives an overview of the typical instrumentation of electrochemical TERS (EC-TERS) based on electrochemical scanning tunneling microscopy (EC-STM). Furthermore, this review summarizes the advancements in EC-TERS studies of events that occur at the interfaces. These include potential dependent structural changes and electrochemical reactions. Finally, we discuss the current issues and future prospects of EC-TERS for microscopic studies of electrochemical interfaces.     

扫描电子显微镜法测定金属衬底上石墨烯薄膜的覆盖度

利用化学气相沉积法生长在金属衬底上的石墨烯薄膜,由于其尺寸的可控性和转移的便利性,被广泛用作各种透明电极.石墨烯薄膜的方块电阻是衡量其品质的重要指标之一,而石墨烯覆盖完全是保证薄膜拥有优良导电性能的基本前提.本文通过研究评估不确定度的分量,提出利用扫描电子显微镜像素计算微区和宏观覆盖度的方法.考虑到石墨烯薄膜覆盖区域与未覆盖区域边界的确定,以及晶畴数目的选取这两个因素对覆盖度测定造成的误差.通过微区有效扫描电子显微镜图像的确定、宏观石墨烯薄膜有效扫描电子显微镜图像的测量数目以及宏观石墨烯薄膜覆盖均匀性的表达,系统研究了化学气相沉积法生长在金属衬底上的石墨烯薄膜的微区覆盖度、宏观覆盖度和覆盖均匀性.该方法通过获得有限次微区扫描电子显微镜图像,不仅可以计算宏观石墨烯薄膜的覆盖度,还可以给出覆盖均匀性,既节省了测量时间,同时也能保证测量有效性.     

Spectroscopic Investigation of the Adsorption of Nitrophenol Isomers on Ammonium Zeolite of Type “Y”

In this study, nitrophenol isomers were adsorbed on synthetic ammonium Y zeolite and the samples acquired were examined with infrared spectroscopy and scanning electron microscopy. The aim of the work is to investigate whether isomeric effects can be monitored after adsorption process. Theoretical calculations of isomers had been performed and the data acquired show that adsorption occurred via bonding from the sites of zeolite.     

Synthesis of large-scale GaN nanowires by ammoniating Ga2O3 films on Co layer deposited on Si（111） substrates

A mass of GaN nanowires has been successfully synthesized on Si（111） substrates by magnetron sputtering through ammoniating Ga2O3/Co films at 950℃. X-ray diffraction, scanning electron microscopy, high resolution transmission electron microscope and Fourier transformed infrared spectra are used to characterize the samples. The results demonstrate that the nanowires are of single-crystal GaN with a hexagonal wurtzite structure and possess relatively smooth surfaces. The growth mechanism of GaN nanowires is also discussed.     

Adsorption geometry of glycine on Cu（001） determined with low—energy electron diffraction and scanning tunnelling microscopy

Using low-energy electron diffraction (LEED) and scanning tunnelling microscopy (STM) it has been found that glycine molecules adsorbed on Cu(001) can form but only the (2×4) and c(2×4) superstructures. On the basis of the missing LEED spots of the surface, it has been concluded that: each (2×4) unit cell consists of two molecules, one being the mirror image of the other; the C－C axis of both molecules lies in the mirror plane of the Cu substrate without a significant shift and twist from the plane; and the two O atoms of the carboxylate group of both molecules locate at the same height level without significant buckling. According to these conclusions, a structural model has been proposed for the (2×4) superstructure (a model for the c(2×4) superstructure already exists). We argue that the (2×4) and c(2×4) superstructures must have similar specific surface free energy, that their hydrogen bonds must be of N-H-O_II type, and that their local adsorption geometry must be similar or even the same. The advantage of combining STM with LEED to determine surface structures is clearly demonstrated.     

High-resolution electron microscopy and X-ray diffraction study of intergrowth structures in α- and β-type YbAlB4 single crystals

Structural features of layered boride YbAlB₄ single crystals with YCrB₄-type (α-type) and ThMoB₄-type (β-type) phases derived from a hexagonal AlB₂-type structure were investigated by electron diffraction, high-resolution electron microscopy and X-ray diffraction. X-ray diffraction experiments indicate the existence of some structural motifs. High-resolution images clearly show that the structural motifs build the intergrown lamellar structures in the matrix. The lamellar structures can be characterized by a coherent tiling of deformed Yb hexagons, which are a common structure unit in the α- and β-type structures. The characteristic intergrown nanostructure is similar to that observed in the β-type TmAlB₄ polycrystalline sample.