电子能谱法研究锡铅合金镀层的表面状态及其与可焊性的关系

本文用X射线光电子能谱(XPS)和俄歇电子能谱(AES)研究了Sn-Pb合金镀层的表面氧化物膜状态并用润湿称量法测定了可焊性。结果表明,Sn-Pb合金镀层表面生成的氧化物膜主要由四价锡的氧化物(SnO_2·XH_2O和SnO_2)组成,铅的氧化物只占很少部分。这说明Sn-Pb合金镀层中锡组分较铅容易氧化。 Sn-Pb合金镀层经155℃加热16小时后,表面氧化物膜的厚度增长很大,同时可焊性明显下降。当Sn-Pb合金镀层经过热熔后,表面变得致密光亮;经155℃加热16小时后生成氧化物膜的厚度较未经热熔的在相同条件下要薄。同时可焊性也较未热熔的好。这说明Sn-Pb合金表面生成氧化物膜的厚度是影响可焊性的重要因素,热熔使Sn-Pb镀层均匀的再结晶改变了镀层结构,使之成为致密的细晶结构,增加了镀层表面的抗氧化能力。故经热熔处理的Sn-Pb合金镀层具有较长的贮存期仍能保持良好的可焊性。     

超高真空俄歇电子能谱原位加热和GaN热效应研究

An in situ heating system was built for the Auger electron spectroscopy to investigate the thermal effect of Auger lines. A GaN sample was studied in this system. The kinetic energy of Ga LMM and MVV Auger lines were observed to shift negatively with temperature increasing. By using ab initio calculation, the theoretical Ga MVV Auger line shape was fit, which well reflects the inner property of the line. The Auger shift with heating is related with the valence electron rearrangement in the thermal expansion of the local bonds.     

薄膜CdSe及CdSexTe1-x电极的光电子能谱研究

用X射线光电子能谱(XPS)研究了不同含氧气氛中烧结的薄膜CdSe及Cdse_xTe_1-x电极表面,以及薄膜与Ti底基之间的界面。研究中发现,二种薄膜电极的表面形成了CdO,SeO₂及TeO₂氧化物,与薄膜接触的Ti底基表面上形成了TiO₂。用俄歇电子能谱(AES)对在电极表面及Ti表面所生成的氧化层分别进行了深度分析。结果表明,各种氧化物形成的程度有很大的不同,氧化层厚度也存在差异。对影响薄膜电极的光电性能的因素进行了讨论。     

化学镀镍诱发过程的研究 II.用电子能谱研究诱发过程

In the previous paper, it was reported that a sudden decrease down to -0.6V and lower in stationary potential was observed from the stationary potential-time curve and the reaction of electroless nickeling could be induced by metallic iron catalyst when it was in contact with substrate metallic copper. In this paper, AES and XPS surface analysis and depth profile technique was employed to investigate the surface and depth distribution of Ni, Cu, Fe and P in the nickel coating deposited on the substrate metal. The experimental results showed that there was a thin adsorption layer consisting of C, S and Cl. The pure electroless nickel deposition, its Ni/P ratio being about two, existed under the adsorption layer. A layer with rapidly changed Ni/P ratio occurred close to the surface of substrate metal, under this layer the substrate metal was alloyed with Ni and P, thus becoming Cu-Ni-P alloy. The ratio of components in this alloy was found to be Cu:Ni:P=56:36:5. This fact explained why the electroless nickel deposition can preferably adhered to the substrate metal. In inducing process, Fe was not detected by AES from the substrate metal and nickel deposition. Thus it showed that the inducing reaction takes place without the deposition of inducing metal.     

用俄歇能谱和X射线能谱研究板状碘溴化银微晶中的碘离子的空间分布

本文制备了一系列不同碘含量的板状碘溴化银微晶(微晶大小约为3微米)。运用扫描透射电镜和X射线能谱仪(EDS)对单个微晶进行了分析和研究,半定量地测定了碘离子在板状微晶中的面分布;运用扫描俄歇微区棵针(SAM)和二次电子像、离子溅射剥层技术对微晶进行了表面及其纵深的碘离子的点分析,根据EDS和SAM的结果,可以得到板状碘溴化银微晶中的碘离子的空间分布。实验结果表明在板状缺溴化银微晶中,在其中心部位的碘含量最高;越靠近横向边缘的位置,碘含量越低。且在制备碘溴化银微晶时,如果pAg值较高,将会使在制备早期加入的碘离子通过不断的重结晶向微晶表面扩散,得到的微晶不是夹心结构的碘溴化银微晶。     

X光电子能谱分析中光电子峰和俄歇峰的干扰及消除

X光电子能谱(XPS)在分析多元素材料时,光电子峰可能受到其它元素俄歇谱的干扰.在AlKα激发CrZnSi合金样品时,光电子峰Cr2p和俄歇峰ZnLMM相互干扰,而换用双阳极中的MgKα源激发,虽可消除此相互干扰,但样品表面的Cls和Nls又会受到ZnLMM干扰.类似地,AlKα激发的GaN样品中Nls受俄歇峰GaLMM的严重干扰,而换用MgKα源激发时,Cls峰又受到的GaLMM的干扰.交替使用Mg/Al双阳极激发源,可改变XPS分析中的俄歇谱及其背景对光电子峰的干扰位置,并用未受干扰的峰互相校正2组谱图能量位置,以对样品谱峰作出正确的分析.     

砷化镓半导体表面自然氧化层的X射线光电子能谱分析

用X射线光电子能谱(XPS),测量了Ga3d和As3d光电子峰的结合能值,指认了砷化镓(GaAs)晶片表面的氧化物组成,计算了表面氧化层的厚度,定量分析了表面的化学组成;比较了几种不同的砷化镓晶片表面的差异。结果表明：砷化镓表面的自然氧化层主要由Ga2O3、As2O5、As2O3和单质As组成,表面镓砷比明显偏离理想的化学计量比,而且,氧化层的厚度随镓砷比的增大而增加;溶液处理后,砷化镓表面得到了改善。讨论了可能的机理。     

成像X射线光电子能谱定量分析研究

探索了直接用实验测得的XPS图像强度来做元素或化学态相对定量分析的可能性。以AgCl和Na2S2O3样品为例,实验结果表明：XPS图像强度与成像时间有良好的线性关系,根据图像强度对两种元素或化学态进行相对定量是可能的。     

稀土富勒烯电子结构的XPS研究

采用Ｘ射线光电子能谱（ＸＰＳ）对富含稀土富勒烯Ｐｒ、Ｇｄ、Ｔｂ、Ｄｙ、Ｅｒ＠Ｃ２ｎ的吡啶提取液的固态沉积膜进行了研究，检测到明确的稀土元素的ＸＰＳ谱峰，表明富勒烯笼内嵌入的稀土元素具有特征的ＸＰＳ谱峰。通过对谱峰的分析，发现稀土富勒烯具有较为稳定的结构。嵌入的Ｐｒ、Ｇｄ、Ｔｂ、Ｄｙ、Ｅｒ等稀土元素与富勒烯球笼间存在电子的迁移。     

用固体核磁共振和电子能谱研究我国高硫煤的结构

用固体ＮＭＲ和ＸＰＳ技术研究了我国三种（广西合山煤、湖南辰溪煤、浙江长广煤）高硫煤的结构特征。由固体ＮＭＲ测试结果计算出煤的十二种结构参数和芳香簇团的大小，获得了三个样品的结构特征及变化规律，由ＸＰＳ测试结果得到了煤中各种不同形态硫、氮的结合能数值。根据前入所做的模型化合物的结果，得知三咱煤中硫元素主要以噻吩硫形态存在，氮元素主要以吡啶和中的形态存在。     

Quantitative surface analysis by X-ray photoelectron spectroscopy and X-ray excited auger electron spectroscopy

It is shown that X-ray excited KLL Auger electron spectra allow it to describe measured signal strengths similarly to X-ray photoelectron signals, thus offering valuable information on the quantitative surface composition of a solid sample. The principal equation and corresponding fundamental parameters are discussed. As a result Auger spectra of C, N, O, F, and Na can be easily used in a multiline approach for quantitative analysis. LMM and MNN spectra give rise to more problems, due to their more complicated structure, uncertainties with regard to the background and the influence of Coster-Kronig transitions. These problems are overcome by the use of empirical ratios of the strongest lines of 2p/LMM or 3d/MNN. Since these ratios are independent of sample composition, they allow it to transform the Auger signal into the corresponding photoelectron signal, provided that a standard sample has been measured. Thus a true additional information is obtained and moreover difficulties in cases of photoelectron spectra with overlapping lines from other chemical elements can be overcome.Dedicated to Professor Günther Tölg on the occasion of his 60th birthday     

Analysis of the antitarnish film on a tin surface by x-ray photoelectron spectroscopy and Auger electron spectroscopy

A corrosion-resistant complex film formed in ethylenediaminetetra(methylidenephosphonic acid) (EDTMP) solution was determined by x-ray photoelectron spectroscopy and Auger electron spectroscopy to consist of 48.0% O, 11.7% Sn, 7.7% N, 22.1% C and 10.5% P. From the differences in the binding energies of Sn, N and O before and after film formation and the RPO^2?₃ and SnN vibrations in the Raman spectrum of the film, it was deduced that N and O in EDTMP were coordinated with Sn in the film.     

Polyaniline Nanofibrils Array Synthesized within the Anodic Aluminum Oxide Template

Introduction Many methods for the fabrication of nanoparticles have been developed ranging from lithographic techniques to chemical methods. The method termed template synthesis for preparation of a variety of micro- and nano-materials has been explored1-3. The template membranes employed contain cylindrical pores with mono-disperse diameters, that extend through the entire thickness of the membrane. The diameter of this nanocylinder is determined by the diameter of the pores of the template m…     

Analysis of PPMMA films from oxygen plasma using X-ray photoelectron spectroscopy

Plasma polymerized methyl methacrylate (PPMMA) films have been synthesised on silicon substrates in RF glow discharge using oxygen plasma. The electron beam delineation sensitivity of the PPMMA films has been studied systematically by varying oxygen and monomer flow rates. X-ray photoelectron spectroscopy (XPS) analysis clearly illustrates how C/O ratio in the films determines the properties of PPMMA films as electron beam resist. © 1994 John Wiley & Sons, Inc.     

Surface properties of the Ni-Cu-Cr oxide catalyst for dehydrogenative hydrolysis of amines

Catalysts for dehydrogenative hydrolysis of amines, prepared by sorption of copper ions from a solution on a preformed Ni-Cr oxide system, were studied by Auger electron spectroscopy, X-ray photoelectron spectroscopy, and IR spectroscopy of adsorbed CO and NH₃ probe molecules. It was shown that on adsorption copper blocked the chromium ions in the Ni-Cr catalyst with concomitant stabilization as Cu⁺. The incorporation of copper into the Ni-Cr system increased the ability of nickel to reduce water with the formation of oxygen-containing complexes.Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 2, pp. 288–291, February, 1993.     

Immobilization of Biomolecules on NH3, H2/NH3 Plasma-Treated Nitrocellulose Films

Detectors with covalently immobilized bioactive compounds able to interact with selected analytes are needed for various kinds of biosensors. Protein macromolecules can be immobilized covalently on surfaces with appropriate functional groups such as amine groups. Low pressure plasmas of NH₃ and NH₃/H₂ mixtures were used to incorporate a maximum of 2.4 amine functions per nm² of porous surface under specific conditions. A mechanism of the functionalization process was proposed using on-line emission spectroscopy and mass spectrometry analysis to monitor the reaction process. The physico-chemical modifications created on the plasma-treated material were investigated by surface analytical techniques such as X-ray photoelectron spectroscopy (XPS) and Scanning Electron Microscopy (SEM).     

Combined analysis methods for investigating titanium and nickel surface contamination after plasma deep etching

Plasma etching techniques can result in damage and contamination of materials, which, if not removed, can interfere with further processing. Therefore, characterisation of the etched surface is necessary to understand the basic mechanisms involved in the etching process and enable process control and cleaning procedures to be developed. A detailed investigation by means of the combined use of scanning electron microscopy coupled with energy-dispersive X-ray spectrometry (SEM/EDS), X-ray photoelectron spectroscopy (XPS) and optical microscopy (OM) has been carried out on deep titanium trenches etched by plasma. This innovative approach has provided a further insight into the microchemical structure of the surface contamination layer on both the titanium and the nickel hard mask surfaces. The described experiments were conducted on 25 to 100-μm wide trenches, first etched in bulk titanium by an optimised Cl₂/SF₆/O₂-based inductively coupled plasma process, through an electroplated nickel hard mask. The results allow to identify chlorine, fluorine and carbon as the main contaminating agents of the nickel mask and to associate three oxidation states around the etched trenches highlighting certain specific aspects related to the passivation mechanism. These observations reinforce the scientific relevance of the combined use of complementary optical and imaging analytical techniques.     

Low-energy electrons and X-ray irradiation effects on plasma-polymerized allylamine bioactive coatings for stents

Radiation used in biomedical applications causes chemical changes to biomedical materials. This work is an ex situ simulation of the influence of low-energy electron (LEE) impact and X-ray irradiation on the chemical properties of plasma-polymerized allylamine (PPA) bioactive and biocompatible stent coatings. Preliminary X-ray photoelectron spectroscopy (XPS) results show that PPA coatings oxidize in contact with ambient air by the detection of C-O and CO bonds which are typical of polymer oxidation. Chemical changes after LEE and X-ray irradiation are mainly a loss of oxygen, assuming a surface deoxidizing and not a complete destruction of the surface. XPS survey analyses show that the amine groups remain stable during irradiation. LEE impact measurements by TOF mass spectrometry show that the main ionic losses are H⁻ ions. It appears that CN groups are stable under irradiation and we observe a loss of hydrogen and oxygen as the main chemical modifications. In conclusion, these results suggest that PPA coatings are stable under biomedical radiation, and they can therefore be used for bioactive and biocompatible stent coatings.