Energy‐resolved electron‐yield XAS studies of nanoporous CoAlPO‐18 and CoAlPO‐34 catalysts

Energy‐resolved electron‐yield X‐ray absorption spectroscopy is a promising technique for probing the near‐surface structure of nanomaterials because of its ability to discriminate between the near‐surface and bulk of materials. So far, the technique has only been used in model systems. Here, the local structural characterization of nanoporous cobalt‐substituted aluminophosphates is reported and it is shown that the technique can be employed for the study of open‐framework catalytically active systems. Evidence that the cobalt ions on the surface of the crystals react differently to those in the bulk is found.     

Augmentation of the step‐by‐step Energy‐Scanning EXAFS beamline BL‐09 to continuous‐scan EXAFS mode at INDUS‐2 SRS

An innovative scheme to carry out continuous‐scan X‐ray absorption spectroscopy (XAS) measurements similar to quick‐EXAFS mode at the Energy‐Scanning EXAFS beamline BL‐09 at INDUS‐2 synchrotron source (Indore, India), which is generally operated in step‐by‐step scanning mode, is presented. The continuous XAS mode has been implemented by adopting a continuous‐scan scheme of the double‐crystal monochromator and on‐the‐fly measurement of incident and transmitted intensities. This enabled a high signal‐to‐noise ratio to be maintained and the acquisition time was reduced to a few seconds from tens of minutes or hours. The quality of the spectra (signal‐to‐noise level, resolution and energy calibration) was checked by measuring and analysing XAS spectra of standard metal foils. To demonstrate the energy range covered in a single scan, a continuous‐mode XAS spectrum of copper nickel alloy covering both Cu and Ni K‐edges was recorded. The implementation of continuous‐scan XAS mode at BL‐09 would expand the use of this beamline in in situ time‐resolved XAS studies of various important systems of current technological importance. The feasibility of employing this mode of measurement for time‐resolved probing of reaction kinetics has been demonstrated by in situ XAS measurement on the growth of Ag nanoparticles from a solution phase.     

The measurement of differential EXAFS modulated by high pressure

Differential EXAFS (DiffEXAFS) is able to detect subtle atomic perturbations in the local area of the absorbing atom. Here a new method of performing DiffEXAFS experiments under the modulation of high pressure has been developed. Periodic pressure was achieved in the gasket with the help of a dynamic diamond anvil cell, and the measurements were conducted in common energy‐scanning mode. This technique has been utilized on ZnSe at 4.8 GPa. The present results have demonstrated a good agreement with the equation of state of ZnSe, and revealed sensitivity to atomic displacements of one order higher in magnitude than that of conventional EXAFS.     

The SAMBA quick‐EXAFS monochromator: XAS with edge jumping

Results and performances of the QEXAFS double monochromator of the SAMBA beamline (Synchrotron SOLEIL) are presented. The device is capable of speeds of up to 40 Hz, while giving the user the possibility to choose the amplitude of the scan from 0.1° to 4° in a few seconds. The device is composed of two independent units and it is possible to perform scans alternating between two different crystals, literally jumping from low (4 keV) to high (37 keV) energies.     

金属二次电子发射系数表达式

根据二次电子发射的主要物理过程,推导出二次电子发射系数和单位背散射电子产生的内二次电子数与原电子产生的内二次电子数之比、原电子入射能量、参数、最大二次电子发射系数、背散射系数之间的关系式。根据实验结果,给出了2~10 keV比率的表达式。根据推导的关系式,用实验数据分别计算出6种金属的平均参数。发现6种金属的平均参数都近似为一个常数11.89(eV)0.5。根据推导的关系式和计算的参数,推导出以背散射系数、原电子入射能量和最大二次电子发射系数为变量的二次电子发射系数通式。用该通式计算出二次电子发射系数,并与相应的实验值进行了比较,最后成功地推导出金属2~10 keV的二次电子发射系数通式。     

金属二次电子发射系数表达式

根据二次电子发射的主要物理过程,推导出二次电子发射系数和单位背散射电子产生的内二次电子数与原电子产生的内二次电子数之比、原电子入射能量、参数、最大二次电子发射系数、背散射系数之间的关系式。根据实验结果,给出了2~10 keV比率的表达式。根据推导的关系式,用实验数据分别计算出6种金属的平均参数。发现6种金属的平均参数都近似为一个常数11.89(eV)0.5。根据推导的关系式和计算的参数,推导出以背散射系数、原电子入射能量和最大二次电子发射系数为变量的二次电子发射系数通式。用该通式计算出二次电子发射系数,并与相应的实验值进行了比较,最后成功地推导出金属2~10 keV的二次电子发射系数通式。     

电子入射角度对聚酰亚胺二次电子发射系数的影响

采用具有负偏压收集极的二次电子发射系数测试系统, 对聚酰亚胺样品的二次电子发射系数与入射电子角度和入射电子能量的关系进行了测量. 测量结果表明, 在电子小角度入射样品的情况下, 随着入射角度的增加, 二次电子发射系数单调增加, 并符合传统的规律, 但是在电子大角度入射时, 却与此不符合. 测量显示, 出现偏差时对应的临界电子入射角度随着入射电子能量的降低而减小. 采用简化的电子弹性散射过程和卢瑟福弹性散射截面公式对这种偏差的出现进行了分析, 并推导出修正后的二次电子发射系数的计算公式. 修正后的二次电子发射系数的计算结果更加符合实验结果.     

高能电子辐照绝缘厚样品的表面电位动态特性

采用数值计算和实验测量相结合的方法, 阐明了高能电子束照射下绝缘厚样品的表面电位和电子产额动态特性. 结果表明: 由于电子在样品内部的散射和输运, 沿着深度方向, 空间电位先缓慢下降到最小值, 然后逐渐升高并趋近于零; 随着电子束照射, 样品的表面电位逐渐下降, 可至负千伏量级, 电子总产额逐渐增大至一个接近于1的稳定值; 电子束停止照射后, 长时间放置下, 表面电位将逐渐升高, 但带电并不会消除; 表面电位随电子束能量的升高近似线性下降, 随入射角的增大而升高, 而随样品厚度的增大仅略有下降.     

Effect of Cu doping on the secondary electron yield of carbon films on Ag-plated aluminum alloy

Reducing the secondary electron yield (SEY) of Ag-plated aluminum alloy is important for high-power microwave components. In this work, Cu doped carbon films are prepared and the secondary electron emission characteristics are studied systematically. The secondary electron coefficient δ_max of carbon films increases with the Cu contents increasing at first, and then decreases to 1.53 at a high doping ratio of 0.645. From the viewpoint of surface structure, the higher the content of Cu is, the rougher the surface is, since more cluster particles appear on the surface due to the small solid solubility of Cu in the amorphous carbon network. However, from viewpoint of the electronic structure, the reduction of the sp² hybrid bonds will increase the SEY effect as the content of Cu increases, due to the decreasing probability of collision with free electrons. Thus, the two mechanisms would compete and coexist to affect the SEY characteristics in Cu doped carbon films.     

Secondary electron yield measurements of carbon covered multilayer optics

Carbon contamination on extreme ultraviolet (EUV) optics has been observed in EUV lithography. In this paper, we performed in situ monitoring of the build-up and removal of carbon contamination on Mo/Si EUV multilayers by measuring the secondary electron yield as a function of primary electron energy. An electron beam with an energy of 2 keV was used to simulate the EUV radiation induced carbon contamination. For a clean EUV multilayer, the maximum secondary electron yield is about 1.5 electrons per primary electron at a primary electron energy of 467 eV. The maximum yield reduced to about 1.05 at a primary electron energy of 322 eV when the surface was covered by a non-uniform carbon layer with a maximum thickness of 7.7 nm. By analyzing the change in the maximum secondary electron yield with the final carbon layer thickness, the limit of detection was estimated to be less than 0.1 nm.     

绝缘体二次电子发射系数测量装置的研制

成功研制了测量绝缘体二次电子发射系数的测量装置,该装置主要由栅控电子枪系统、真空系统和电子采集系统组成,测量装置产生的原电子流的能量范围为0.8~60 keV。采用单脉冲电子枪法,测量了原电子能量范围为0.8~45 keV的多晶MgO的二次电子发射系数。测量中,收集极(偏置盒)离材料表面设置为约35 mm,偏置电压设置为 45 V。测量得到：用磁控溅射法制备的MgO的二次电子发射系数最大值约为2.83,处于 2~26范围内,其对应的原电子能量约为980 eV。这表明该装置测量的绝缘体二次电子发射系数是可信的,但用磁控溅射法制备的MgO的二次电子发射系数较低,这可能是制备MgO时引入了过多的杂质在MgO二次电子发射体里面所引起的。     

绝缘体二次电子发射系数测量装置的研制

 成功研制了测量绝缘体二次电子发射系数的测量装置，该装置主要由栅控电子枪系统、真空系统和电子采集系统组成，测量装置产生的原电子流的能量范围为0.8~60 keV。采用单脉冲电子枪法，测量了原电子能量范围为0.8~45 keV的多晶MgO的二次电子发射系数。测量中，收集极(偏置盒)离材料表面设置为约35 mm，偏置电压设置为 45 V。测量得到：用磁控溅射法制备的MgO的二次电子发射系数最大值约为2.83，处于 2~26范围内，其对应的原电子能量约为980 eV。这表明该装置测量的绝缘体二次电子发射系数是可信的，但用磁控溅射法制备的MgO的二次电子发射系数较低，这可能是制备MgO时引入了过多的杂质在MgO二次电子发射体里面所引起的。     

Secondary electron emission yield from vertical graphene nanosheets by helicon plasma deposition

The secondary electron emission yields of materials depend on the geometries of their surface structures.In this paper,a method of depositing vertical graphene nanosheet(VGN)on the surface of the material is proposed,and the secondary electron emission(SEE)characteristics for the VGN structure are studied.The COMSOL simulation and the scanning electron microscope(SEM)image analysis are carried out to study the secondary electron yield(SEY).The effect of aspect ratio and packing density of VGN on SEY under normal incident condition are studied.The results show that the VGN structure has a good effect on suppressing SEE.     

铝阳极氧化的多孔结构抑制二次电子发射的研究

针对空间大功率微波部件中的二次电子倍增效应影响微波部件性能的问题,基于铝阳极氧化产生大深宽比、高孔隙率均匀纳米级多孔结构的特性,结合蒸发镀银技术,提出一种有效降低表面二次电子发射系数的方法.结果表明,相比于未阳极氧化的铝样片,在不清洗样片的情况下(实际的样片表面都会存在吸附或沾污),测试得到二次电子发射系数曲线的第一能量交叉点E1从45 eV增加到77 eV,最大二次电子发射系数SEY_(max)从2.68减小到1.52;在清洗样片的情况下(清洗是为了去除吸附或沾污,获得理想的表面),测试得到第一能量交叉点E_1从40 eV增加到211 eV,最大二次电子发射系数SEY_(max)从2.55减小到1.36.为了验证本文所提方法对抑制空间大功率微波部件二次电子倍增效应的有效性,分别将获得的未阳极氧化和阳极氧化后的二次电子发射系数数据用于一个X频段阻抗变换器设计中,结果显示,使用本文所提方法后,阻抗变换器的微放电阈值从7000 W提高到125000 W.本文研究的方法不仅对解决空间大功率微波部件的微放电问题有指导意义,而且对真空电子器件、加速器等领域的研究也具有重要参考价值.     

金属规则表面形貌影响二次电子产额的解析模型

表面形貌是影响二次电子发射特性的重要因素, 但目前仍缺乏刻画这一影响规律的解析模型. 本文通过分析发现表面结构的遮挡作用是影响二次电子发射特性的主要因素. 基于二次电子以余弦角分布出射的规律, 提出了建立表面形貌参数与二次电子产额之间定量关系的方法, 并以矩形槽和三角槽为例, 建立了电子正入射和斜入射时的一代二次电子产额的解析模型. 将推导的解析模型与Monte Carlo模拟结果和实验结果进行了比较, 结果表明本文建立的模型能够正确反映规则表面形貌的二次电子产额. 本文的模型对于反映常用规则结构影响二次电子出射的规律以及指导通过表面结构调控二次电子发射特性都具有参考价值.     

低温二次电子产额测试系统设计与研究

在合肥先进光源（HALF）建设中,由低温超导材料组成的真空部件被大量使用,尤其是超导高频腔。超导腔以高加速梯度、低束流阻抗、高无载品质因数和低运行成本等特点,成为21世纪国际上拟建的大型加速器的首选。而超导腔和低温真空室内表面的二次电子发射可能会引发电子云（EC）现象。超剂量的二次电子倍增功率沉积会引起低温区域热负载增加、超导腔失超等现象,因此降低超导高频腔内二次电子发射成为合肥先进光源设计过程中的巨大挑战。在常温材料二次电子产额（SEY）测试系统的基础上,作者自主研发设计低温样品架结构,使液氦流经样品台并通过热传导冷却样品,计算漏热来反推所需要的制冷量和液氦的消耗速率。在系统集成调试后进行降温性能测试,搭建了低温材料二次电子测试系统。     

Atomic absorption background of Ba in EXAFS analysis of BaFe12O19 nanoparticles

The approximate barium X‐ray atomic absorption in the energy region of L‐edges is reconstructed from the absorption spectrum of an aqueous solution of BaCl₂. The result is corroborated by comparison with pure atomic absorption spectra of neighbour elements Xe and Cs. The application of the atomic absorption signal as a proper EXAFS background is demonstrated and discussed in the analysis of Ba hexaferrite nanoparticles with a very weak structural signal. The essential gain is found in the decrease of uncertainty intervals of structural parameters and their correlations. A simple analytical model of the absorption background for the practical EXAFS analysis is demonstrated.     

Polycapillary‐optics‐based micro‐XANES and micro‐EXAFS at a third‐generation bending‐magnet beamline

A focusing system based on a polycapillary half‐lens optic has been successfully tested for transmission and fluorescence µ‐X‐ray absorption spectroscopy at a third‐generation bending‐magnet beamline equipped with a non‐fixed‐exit Si(111) monochromator. The vertical positional variations of the X‐ray beam owing to the use of a non‐fixed‐exit monochromator were shown to pose only a limited problem by using the polycapillary optic. The expected height variation for an EXAFS scan around the Fe K‐edge is approximately 200 µm on the lens input side and this was reduced to ～1 µm for the focused beam. Beam sizes (FWHM) of 12–16 µm, transmission efficiencies of 25–45% and intensity gain factors, compared with the non‐focused beam, of about 2000 were obtained in the 7–14 keV energy range for an incoming beam of 0.5 × 2 mm (vertical × horizontal). As a practical application, an As K‐edge µ‐XANES study of cucumber root and hypocotyl was performed to determine the As oxidation state in the different plant parts and to identify a possible metabolic conversion by the plant.     

The charging stability of different silica glasses studied by measuring the secondary electron emission yield

This paper reports that the charging properties of lead silica,Suprasil silica and Infrasil silica are investigated by measuring the secondary electron emission(SEE) yield.At a primary electron beam energy of 25 keV,the intrinsic SEE yields measured at very low injection dose are 0.54,0.29 and 0.35,respectively for lead silica,Suprasil and Infrasil silica glass.During the first e-beam irradiation at a high injection current density,the SEE yields of lead silica and Suprasil increase continuously and slowly from their initial values to a steady state.At the steady state,the SEE yields of lead silica and Suprasil are 0.94 and 0.93,respectively.In Infrasil,several charging and discharging processes are observed during the experiment.This shows that Infrasil does not reach its steady state.Two hours later,all samples are irradiated again in the same place as the first irradiation at a low current density and low dose.The SEE yields of lead silica,Suprasil and Infrasil are 0.69,0.76 and 0.55,respectively.Twenty hours later,the values are 0.62,0.64 and 0.33,respectively,for lead silica,Suprasil and Infrasil.These results show that Infrasil has poor charging stability.Comparatively,the charging stability of lead silica is better,and Suprasil has the best characteristics.