查看完整版本: 纳米Ag基材料的XPS表征

纳米Ag基材料的XPS表征

Ag和Ag的氧化物由于结合能的差异较小，在材料表面分析特别是XPS分析上存在一定难点。而且一些文献给出的Ag的芯能级结合能差别比较大，希望这个帖子把这方面的资料总结一下。可能对大家有用。`JeB-a9un

(]2Cru(s JHK [img]http://www.lasurface.com/design/lasurface.gif[/img]的Ag3dXPS谱和O1sXPS谱o5SC8S [
[img]http://www.lasurface.com/database/spectres/Ag_3d.gif[/img]:OV1T e9}&JQ U)R'yF\
[img]http://www.lasurface.com/database/spectres/O_1s.gif[/img]

老大这是什么意思？氧化银的纳米颗粒？纳米线？9[|{Mf7e:^g @F
找nanoquebec帮你分析分析。。。？呵呵呵

回复 #2 lsly 的帖子

最近分析Ag颗粒的XPS遇到这方面的知识 向nanoquebec老师请教了下 @3?,g6R0r R^(Oim1_
这里给出些文章方便大家查找

[color=Purple][size=4][b]Size selectivity for CO-oxidation of Ag nanoparticles on highly ordered pyrolytic graphite (HOPG)[/b][/size]
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d@P9g Surface Science 598 (2005) 96–103{1@8E;^Ny[
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Dong Chan Lim, Ignacio Lopez-Salido, Young Dok Kim *
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The Ag nanoparticles on HOPG were oxidized using atomic oxygen environments under ultrahigh-vacuum conditions,
u6yK/{QSd and the nature of the oxidized Ag particles, and their interactions with CO were studied using X-ray photoelectrone@;h(VT
spectroscopy (XPS). The oxygen uptake of a smaller Ag nanoparticle is significantly higher than that of a larger3_7d8B(qM
particle and bulk-like Ag. For the Ag nanoparticles larger than 3 nanometers (nm), two different oxygen species wereRg%`c}[:_(E0I;C
identified, one of which readily reacts with CO to form CO2 at room temperature. Based on our XPS studies, the catalytically
!FU;X7D1rq9b,} active oxygen species is assigned to be in Ag2O and/or AgO. For the smaller Ag nanoparticles, only a singleUj.g/?qf7H
oxygen species can form upon reacting with oxygen atoms in the gas phase, which is inert towards CO-oxidation. The
W2Y*rHY,Wl nature of the catalytically inert oxygen species is discussed. The formation of different oxide species as a function of
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~i3q particle size can be responsible for the size selectivity in chemical reactions catalyzed by Ag nanoparticles.
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%x bm9tx [b][size=4]Characterization of Ag nanoparticles on Si wafer prepared using Tollen’s reagent and acid-etching[/size][/b]
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Applied Surface Science 253 (2006) 959–965
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Dong Chan Lim , Ignacio Lopez-Salido, Young Dok Kim*9Ww ?~n'`Z/Eq

#A/t{ f#k/U Ag nanoparticles on SiO2/Si surfaces synthesized using the Tollen’s reagent and a subsequent acid-etching were characterized using X-ray photoelectron spectroscopy (XPS). Combining the reduction of the Tollen’s reagent and the chemical etching, one can create naked Ag nanoparticles with various sizes in the size range below  10 nanometers (nm). The reduced particle size by the chemical etching was identified using positive core level shifts with increasing etching time. Ag nanoparticles smaller than  3 nm undergo a reversible oxidation and reduction cycle by reacting with H2O2/H2O and a subsequent heating under vacuum to 150 8C, which was not found for the bulk counterparts and larger particles, demonstrating unique chemical properties of nanoparticles compared to the bulk counterparts.k8MNZ HjGQ
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[color=Purple][b][size=4]On the mechanism of Ag(111) sub-monolayer oxidation: a combined electrochemical, in situ SERS and ex situ XPS study[/size][/b]
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ibd;B(G(P#t.B:H Electrochimica Acta 46 (2000) 175–183 (Sciencedirect Database)
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E.R. Savinova *, D. Zemlyanov , B. Pettinger , A. Scheybal , R. Schlo¨gl ,K. Doblhofer+Z9cxLR r`
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In the present work in situ surface enhanced Raman spectroscopy (SERS), ex situ X-ray photoelectron spectroscopy (XPS) and ultraviolet photoelectron spectroscopy (UPS) are used to study the interface between a Ag(111)electrode and an alkaline electrolyte. Formation of a number of potential-dependent adsorbates is observed above the point of zero charge (Epzc) of the Ag electrode. These are: OH groups (OHadsg ) and oxide-like species (Oadsd ).Electrochemisorbed hydroxide species show by the appearance of Raman bands at 540–560 cm 1 and at 803–819 cm 1, attributed to Ag–OH stretching and AgO–H bending vibrations respectively. Strong isotope shift of the Raman bands towards lower frequencies is observed in D2O solutions, proving their assignment. The Oadsd  and OHadsg  species are characterised by the O 1s peaks at ca. 529.5 and 531.6, respectively. Formation of the above-mentioned species is verified also by the UP spectra of the emersed electrodes, showing the bands at 3.0 eV typical for the oxide-like adsorbates and 9.0 and 11.1 eV for hydroxo-groups. The OHadsg  and Oadsd  species are negatively charged,as evidenced by the adsorption of Na  on the Ag electrode positive to the Epzc. A mechanism of the Ag(111)sub-monolayer oxidation is suggested on the basis of combined evidence from cyclic voltammetry, in situ SERS, ex situ XPS and UPS.1E5yS'L4Q~/U

.j,mq ?p ~L3G [b][size=4]Preparation and characterization of nanostructured silver thin films deposited by radio frequency magnetron sputtering[/size][/b]X D~1~,a)m!W
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Thin Solid Films 375(2000)300-303
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Yuqing Xiong*, Hao Wu, Yan Guo, Yan Sun, Dequan Yang, Daoan Da
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Nanostructured silver thin films were prepared by radio frequency magnetron sputtering at room and liquid nitrogen substrate temperatures. Atomic force microscopy and X-ray photoelectron spectroscopy were employed to study the ft1bZH^,J;ia
topography and chemical composition, respectively, of the thin films. The AFM results indicate a significant difference in the morphology of the thin films when argon or nitrogen ions were used as sputtering ions. For argon ion sputtering, a difference also exists in the microstructure and topography of the thin films for ambient and liquid nitrogen substrate temperatures. The XPS results show a high purity of nanostructured silver thin films for sputtering by both argon ions and nitrogen ions, but with some oxygen and carbon contamination. For argon ion sputtering, the content of oxygen and carbon is less than 6.9% and 4.5%, and for nitrogen ion sputtering, less than 4.7% and 3.6%.[/color]*Wa"Fc)q
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[color=Purple][size=4][b]Surface characterization study of Ag, AgO, and Ag2O using x-ray photoelectron spectroscopy and electron energy-loss spectroscopy [/b]
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[b]Phys. Rev. B 62, 11126 - 11133 (2000)[/b]*\1@.c&P\Js4hg

MDK(mU|#K^-u Gar B. Hoflund,  and et al.
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p ?e7Z1w3MbG+\#K*j Electron energy-loss spectra (ELS) have been obtained from polycrystalline Ag metal, AgO powder, and Ag2O powder using primary electron-beam energies ranging from 100 to 2000 eV. These samples were characterized using x-ray photoelectron spectroscopy (XPS) to determine the compositions and chemical species in their near-surface regions. The ELS spectra obtained from these three materials are significantly different, implying that ELS is a useful technique for distinguishing between Ag metal, AgO, and Ag2O or analyzing mixtures of these species. Such an analysis is difficult using techniques including XPS or Auger-electron spectroscopy because spectral features of these species are quite similar and closely spaced. The ELS spectral features consist of losses due to the formation of surface and bulk plasmons and interband transitions. An attempt has been made in this study to assign the processes responsible for the ELS features observed in the spectra. This interpretation will be improved as the electronic structures of Ag metal, AgO, and Ag2O are better understood.[/color])c5pTRG
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}*r~8V [size=4][color=Purple][b]AgO investigated by photoelectron spectroscopy:  Evidence for mixed valence [/b][/color][/size]ho9qf/mi.L ^
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[color=Purple][b]Phys. Rev. B 65, 235431 (2002) [/b]@e-q1kP
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M. Bielmann, and et al.[/color]&h#R p6M |eo+q

u)^2ZB{FN [color=Purple]We present photoelectron spectroscopy investigations of in-situ prepared AgO. The sample was prepared by room temperature oxidation of Ag in an electron cyclotron resonance O2 plasma. In contrast to other measurements based on ex situ prepared AgO powder samples, our investigations show a distinct double peak structure of the O 1s signal with a remarkable chemical shift of 2.9 eV between the two O 1s components. These two components can not be motivated from a crystallographic point of view as the oxygen sites are all equivalent in the unit cell. We interpret this double peak structure as a characteristic feature of AgO and discuss it in terms of mixed valences.[/color]
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[color=Purple]Phys. Rev. Lett. 94, 047403 (2005)
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[size=4][b]Optical Absorption and Photoluminescence Spectroscopy of the Growth of Silver Nanoparticles[/b][/size]r htmLD8F0m
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P. Gangopadhyay, and et al.
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v(z]A Results obtained from the optical absorption and photoluminescence (PL) spectroscopy experiments have shown the formation of excitons in the silver-exchanged glass samples. These findings are reported here for the first time. Further, we investigate the dramatic changes in the photoemission properties of the silver-exchanged glass samples as a function of postannealing temperature. Observed changes are thought to be due to the structural rearrangements of silver and oxygen bonding during the heat treatments of the glass matrix. In fact, photoelectron spectroscopy does reveal these chemical transformations of silver-exchanged soda glass samples caused by the thermal effects of annealing in a high vacuum atmosphere. An important correlation between temperature-induced changes of the PL intensity and thermal growth of the silver nanoparticles has been established in this Letter through precise spectroscopic studies.
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t/Rk5N!A*Eft-\a [color=Purple]Japanese Journal of Applied Physics 43( 2004)267[/color]
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[b][size=4][color=Purple]The Characteristics of Reactively Sputtered AgOx Films Prepared at Different Oxygen Flow Ratios and Its Effect on Super-Resolution Near-Field Properties[/color][/size][/b]}'p;_(}'y2[$oj
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Yung-Chiun Her and et al.

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o*b]mg1\k The characteristics of several reactively sputtered AgOx films, prepared at different oxygen flow ratios, with and without ZnS-SiO2 protective layers have been examined. For the as-deposited AgOx films, the amount and size of Ag clusters decreased, and the constituent phase of AgOx gradually transferred from pure Ag2O, to a mixture of Ag2O and AgO, then to pure AgO, as the oxygen flow ratio was increased. After annealing, the reduction of AgO into Ag2O and decomposition of Ag2O into Ag and O2 took place, and the decomposed Ag elements would diffuse outward and precipitate small silver particles on the surface of ZnS–SiO2 protective layers. The chemical decomposition of AgOx film confined by ZnS–SiO2 protective layers was confirmed to be an irreversible process. The super-resolution near field effect becomes significant only when the super-resolution near-field structure (super-RENS) disk with an AgOx mask layer prepared at oxygen flow ratios above a threshold value, where AgOx film consists of Ag2O or AgO phase.[/color]
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回复 1# 的帖子

好东西，就要看看！好东西，就要看看！