表面热处理研究石墨及含杂质单壁碳纳米管的C 1s X射线吸收谱

用表面敏感光电子能谱全电子产额模式(TEY)对石墨及含杂质单壁碳纳米管的C 1s X射线吸收谱进行了研究.在高真空里表面退火处理后,石墨C 1s X射线吸收谱中未占据π^{*和σ*态特征峰之间的小峰消失,证实此峰不是来自于一直被认为的所谓的类自由电子态,而来自于样品表面态,即表面结构扭曲或吸附气体所引起的结构变化.而且π*和σ*峰强度有明显的变化,提示着在研究不同纳米管未占据态的态密度对比研究中,原位温度处理是关键的.我们通过对含杂质不同单壁碳纳米管的态密度对比研究来说明这种处理过程的必要性.}     

X射线光电子能谱辅助Raman光谱分析类金刚石碳膜的结构细节

分别采用具有和不具有弯曲弧磁过滤器的两种真空阴极弧离子镀方法,在不同工艺参量下制备了类金刚石碳膜.采用Raman光谱和X射线光电子能谱(XPS),分析了不同工艺参量下的类金刚石碳膜的键结构,通过对Raman光谱的D峰、G峰和C1s电子结合能峰位、强度的对比,详细讨论了沉积工艺参量对类金刚石碳膜结构的影响.研究发现,不同工艺下具有高强度D峰Raman光谱的类金刚石碳膜,其C1s电子结合能却分别位于284.15,285.50eV,表明高度石墨化和高度金刚石化两种状态类金刚石碳膜,都可以形成具有高强度D峰Raman光谱曲线 关键词： 类金刚石碳膜 Raman光谱 X射线光电子能谱     

C+离子注入Si单晶形成SiC埋层中Si2p的特征能量损失谱

利用metal vapor vacuum arc离子源产生的C⁺离子，注入单晶Si衬底，得到了SiC埋层.利用X射线光电子能谱，研究了SiC埋层中Si2p的特征能量损失谱.结果表明：Si2p的特征能量损失谱依赖于SiC埋层中C原子的浓度分布，并且与SiC埋层的有序度对应. 关键词：     

纳米Al2O3表面接枝修饰的XPS研究

在纳米Al2O3表面接枝聚缩醛可在粒子表面建立起空间位阻稳定层, 不但提高了纳米粒子的分散稳定性, 还可以增强纳米粒子与树脂基体的相容性. X射线光电子能谱(XPS)的分析结果表明, 经过聚缩醛接枝改性的纳米Al2O3的Al(2p)峰几乎消失, O(1s)峰也相应降低, 与之相对应的是C(1s)峰有了明显的增长, 对C(1s)峰精细扫描及分峰拟合表明, 纳米Al2O3表面碳元素中有61.92%属于接枝物聚缩醛的有机碳, 接枝物聚缩醛与纳米Al2O3形成了Al-O-C键, 两者产生化学结合. 同时对比XPS和热失重分析(TG)的数据结果, 可以推测聚缩醛主要分布在纳米Al2O3的表面, 而在体相中独立存在的概率较小.     

SiC外延层表面化学态的研究

用高分辨X射线光电子能谱仪(XPS)和傅里叶变换红外(FTIR)光谱仪研究了SiC外延层表面的组分结构. XPS宽扫描谱,红外掠反射吸收谱及红外镜面反射谱的解析结果说明SiC外延层表面是由Si—O—Si和Si—CH₂—Si聚合体构成的非晶SiC_xO_y:H. SiC外延层表面的化学态结构为Si(CH₂)₄,SiO(CH₂)₃,SiO₂(CH₃)₂,SiO₃(CH₃),Si—Si,游离H₂O,缔合OH,Si—OH,O和O₂. 根据化学态结构和元素电负性确定了化学态的各原子芯电子束缚能顺序,并与XPS窄扫描谱拟合结果相对比,建立了化学态与其束缚能的对应关系,进而用Si(CH₂)₄的实际C 1s束缚能值进行校正,确定了各化学态的束缚能. 结果发现,除了SiC_xO_y(x=1,2,3,4,x+y=4)的Si 2p束缚能彼此不同外,其C 1s和O 1s彼此也不相同,其中SiO₂(CH₃)₂和SiO₃(CH₃)的C 1s束缚能与CH_m和C—O中C 1s的相近,对此从化学态结构,元素电负性和邻位效应进行了解释. 关键词： SiC 化学态 XPS FTIR     

碳硅共掺杂p型AlN的光电性能研究

在SiC衬底上生长了碳硅共掺杂p型AlN晶体,通过X射线衍射、X射线光电子能谱(XPS)、光致发光(PL)光谱、霍尔测试对碳硅共掺杂p型AlN晶体的结构、光学及电学性能进行了综合研究。通过XPS测试分析(尤其是对样品中Si 2p和C 1s的XPS谱分析)发现,样品中C替代N成为受主,而Si替代Al成为施主。样品的PL谱主要包括两个特征发射峰,分别来自于C、Si在AlN中形成的复合物V N-C N和C N-Si Al。     

ITO/Rubrene表面及界面的AFM和XPS研究

采用原子力显微镜（AFM）和X射线光电子能谱仪（XPS）研究了氧化铟锡（ITO）/红荧烯（Rubrene）的形貌和表面、界面的电子态。AFM结果显示,ITO上的Rubrene膜有良好的均匀性。XPS结果表明:C1s谱有3个峰,位于282.50,284.70,289.30 eV,对应于C-Si、C O和C-C键。用氩离子束溅射表面,芳香碳对应的峰值逐渐增大,其他两个峰值迅速消失。随着表面O污染的去除,O1s峰先快速减弱然后逐渐增强。界面附近的O原子与C原子结合构成O C、C-O-C和醛基。In3d和Sn3d峰则缓慢增强,在界面附近峰值变得稳定。C1s、In3d、Sn3d谱峰都向低束缚能发生化学位移,表明ITO与Rubrene在界面发生了相互作用,形成一个互扩散层。     

ITO/Rubrene表面及界面的AFM和XPS研究

采用原子力显微镜(AFM)和X射线光电子能谱仪(XPS)研究了氧化铟锡(ITO)/红荧烯(Rubrene)的形貌和表面、界面的电子态。AFM结果显示,ITO上的Rubrene膜有良好的均匀性。XPS结果表明:C1s谱有3个峰,位于282.50,284.70,289.30 eV,对应于C—Si、CO和C—C键。用氩离子束溅射表面,芳香碳对应的峰值逐渐增大,其他两个峰值迅速消失。随着表面O污染的去除,O1s峰先快速减弱然后逐渐增强。界面附近的O原子与C原子结合构成OC、C—O—C和醛基。In3d和Sn3d峰则缓慢增强,在界面附近峰值变得稳定。C1s、In3d、Sn3d谱峰都向低束缚能发生化学位移,表明ITO与Rubrene在界面发生了相互作用,形成一个互扩散层。     

微波等离子体化学汽相沉积法沉积CNx膜的研究

对用微波等离子体化学汽相沉积法沉积在Si基片上的CN_x膜分别进行Raman散射、X射线光电子能谱、X射线衍射和扫描电子显微镜等技术的分析与测试. Raman散射的研究结果表明在CH₄与N₂的流量比低于1∶8时，CN_x膜的散射谱中以非晶石墨峰的形式出现.当流量比为1∶8时，则表现为较尖锐的C≡N键(2190cm^-1)的特征峰；从X射线光电子能谱的分析结果可以看出C，N成键的方式主要是C≡N键和C—N 关键词：     

X射线衍射多相谱中某一物相点阵参数的直接求解方法

介绍了一种新的求解点阵参数的方法--不涉及结构的谱峰拟合方法.该方法适用于单一物相或多个物相衍射谱中某一物相点阵参数的直接求解,可以避免外推函数的不同选择而造成的差异,且快速准确.根据此方法编写的应用程序已在实际工作中得到应用.程序中还包括了调整样品表面离轴偏差和零度偏差以提高拟合精确度的功能. 关键词： X射线衍射 谱峰拟合 点阵参数     

Influence of surface structure of SiC nano-sized powder analyzed by X-ray photoelectron spectroscopy on basic powder characteristics

SiC nano-sized powder with high specific surface area is potentially of considerable interest to form fully dense SiC ceramics at lower sintering conditions (temperature/pressure). Surface structure of six kinds of commercially available SiC nano-sized powders produced by three different venders was analyzed in detail by X-ray photoelectron spectroscopy (XPS). The overall XPS spectra of all nano-sized powders detected O-based bond (O1s peak), C-based bond (C1s peak) and Si-based bond (Si2s and Si2p peak). Surface structure of nano-sized powders included one of three impurity phases: (1) free carbon, (2) silica and (3) silicon oxycarbide. Furthermore, the influences of surface structure by XPS were systematically investigated on basic powder characteristics, such as chemical composition, morphology, particle density and primary particle size. It was revealed that the basic powder characteristics had a close relationship to the surface structure of nano-sized powder each impurity.     

Resolving surface chemical states in XPS analysis of first row transition metals, oxides and hydroxides: Cr, Mn, Fe, Co and Ni

Chemical state X-ray photoelectron spectroscopic analysis of first row transition metals and their oxides and hydroxides is challenging due to the complexity of their 2p spectra resulting from peak asymmetries, complex multiplet splitting, shake-up and plasmon loss structure, and uncertain, overlapping binding energies. Our previous paper [M.C. Biesinger et al., Appl. Surf. Sci. 257 (2010) 887-898.] in which we examined Sc, Ti, V, Cu and Zn species, has shown that all the values of the spectral fitting parameters for each specific species, i.e. binding energy (eV), full wide at half maximum (FWHM) value (eV) for each pass energy, spin-orbit splitting values and asymmetric peak shape fitting parameters, are not all normally provided in the literature and data bases, and are necessary for reproducible, quantitative chemical state analysis. A more consistent, practical and effective approach to curve fitting was developed based on a combination of (1) standard spectra from quality reference samples, (2) a survey of appropriate literature databases and/or a compilation of literature references and (3) specific literature references where fitting procedures are available. This paper extends this approach to the chemical states of Cr, Mn, Fe, Co and Ni metals, and various oxides and hydroxides where intense, complex multiplet splitting in many of the chemical states of these elements poses unique difficulties for chemical state analysis. The curve fitting procedures proposed use the same criteria as proposed previously but with the additional complexity of fitting of multiplet split spectra which has been done based on spectra of numerous reference materials and theoretical XPS modeling of these transition metal species. Binding energies, FWHM values, asymmetric peak shape fitting parameters, multiplet peak separation and peak area percentages are presented. The procedures developed can be utilized to remove uncertainties in the analysis of surface states in nano-particles, corrosion, catalysis and surface-engineered materials.     

4H-SiC同质外延的绿带发光与缺陷的关系

利用室温光致发光谱(PL)对CVD法生长的4H-SiC同质外延特性进行研究,发现有绿带发光(GL)特性.用扫描电子显微镜(SEM) 、二次离子质谱(SIMS)和X射线光电子谱(XPS)技术获得了4H-SiC样品纵截面形貌和元素相对含量分布.结果表明,GL与4H-SiC晶体中碳空位(V_C)及络合体缺陷相关,V_C和缓冲层的扩展缺陷(点缺陷和刃位错等)是GL微观来源.GL的半峰宽(FWHM) 反映了参与复合发光的V_C及其络合缺陷能级分散的程度.室温下获得的样品GL强度和光谱波长度可用于分析4H-SiC外延中缺陷分布和晶体质量. 关键词： 绿带发光 4H-SiC同质外延 晶体缺陷     

Photoemission studies of pulsed-RF plasma nitrided ultra-thin SiON dielectric layers

Results are presented of a photoemission study of the electronic structure of SiON layers formed by a pulsed-RF decoupled plasma nitration (DPN) of ultra-thin SiO₂ grown base layers approximately 1.0 nm thick. The optical thickness of these device grade nitrided dielectric layers was in the range 1.4-1.6 nm. X-ray photoelectron spectroscopy (XPS) studies indicate that the nitrogen is incorporated in a single chemical environment at concentration levels in the range 15-17%. Angle resolved XPS measurements show that the nitrogen is distributed through the layer, with the binding energy of the N 1s peak at 398.3 eV which is indicative of a Si₃N₄-like chemical species in an oxide environment. High resolution core level photoemission studies of the spin orbit stripped Si 2p⁴⁺ peak revealed full width half maximum values in the range 1.4-1.55 eV, which are significantly larger than the 1.15 eV value reported for SiO₂ layers. Synchrotron radiation photoemission studies of the valence band spectra enable the valence band off-set at the Si/SON interface to be evaluated as 2.3 eV and to infer a conduction band off-set of 2.1 eV.     

X-ray photoelectron spectroscopic study of nitrogen incorporated amorphous carbon films embedded with nanoparticles

The effect of substrate bias on X-ray photoelectron spectroscopy (XPS) study of nitrogen incorporated amorphous carbon (a-C:N) films embedded with nanoparticles deposited by filtered cathodic jet carbon arc technique is discussed. High resolution transmission electron microscope exhibited initially the amorphous structure but on closer examination the film was constituted of amorphous phase with the nanoparticle embedded in the amorphous matrix. X-ray diffraction study reveals dominantly an amorphous nature of the film. A straight forward method of deconvolution of XPS spectra has been used to evaluate the sp³ and sp² contents present in these a-C:N films. The carbon (C 1s) peaks have been deconvoluted into four different peaks and nitrogen (N 1s) peaks have been deconvoluted into three different peaks which attribute to different bonding state between C, N and O. The full width at half maxima (FWHM) of C 1s peak, sp³ content and sp³/sp² ratio of a-C:N films increase up to −150 V substrate bias and beyond −150 V substrate bias these parameters are found to decrease. Thus, the parameters evaluated are found to be dependent on the substrate bias which peaks at −150 V substrate bias.     

Resolving overlapping peaks in ARXPS data: The effect of noise and fitting method

Peak-fitting of X-ray photoelectron spectroscopy (XPS) data can be very sensitive to noise when the difference on the binding energy among the peaks is smaller than the width of the peaks. This sensitivity depends on the fitting algorithm. Angle-resolved XPS (ARXPS) analysis offers the opportunity of employing the combined information contained in the data at the various angles to reduce the sensitivity to noise. The assumption of shared peak parameters (center and width) among the spectra for the different angles, and how it is introduced into the analysis, plays a basic role. Sequential fitting is the usual practice in ARXPS data peak-fitting. It consist on first estimating the center and width of the peaks from the data acquired at one of the angles, and then using those parameters as a starting approximation for fitting the data for each of the rest of the angles. An improvement of this method consists of averaging the centers and widths of the peaks obtained at the different angles, and then employing these values to assess the areas of the peaks for each angle. Another strategy for using the combined information is by assessing the peak parameters from the sum of the experimental data. The complete use of the combined information contained in the data-set is optimized by the simultaneous fitting method. It consists of the assessment of the center and width of the peaks by fitting the data at all the angles simultaneously. Computer-generated data was employed to compare the sensitivity with respect to noise between the sequential, averaged-sequential, sum, and simultaneous fitting methods. It is shown that the latter is significantly more robust and could provide reliable results even for noisy data and small peak separation. The fundamentals for the robustness of the simultaneous method are discussed, as well as the possibility of fitting many parameters at the same time. As an added feature of ARXPS, it was found that the estimation of the error intervals on the peak parameters is done remarkably more precisely by employing XPS data at various angles.     

Growth of LiNbO3 epitaxial films by oxygen radical-assisted laser molecular beam epitaxy

LiNbO₃ films were epitaxially grown on c-sapphire substrates using oxygen radical-assisted laser molecular beam epitaxy (MBE). X-ray diffraction-based structural analysis showed that the films were epitaxial. Triple-axis rocking curve measurements of the LiNbO₃ (0 0 0 6) reflection revealed that the film was highly c-oriented with an extremely narrow mosaic; the full width at half maximum of the LiNbO₃ (0 0 0 6) rocking curve was 0.0036°, comparable to the value of high-quality bulk crystals. The surface of the film was very smooth, with a surface roughness r.m.s. value, measured by atomic force microscope, of 0.4 nm for a film of thickness 15 nm. The chemical composition of the film measured by X-ray photoelectron spectroscopy (XPS) was stoichiometric within the accuracy of XPS measurement.     

PIIID复合强化处理轴承钢表面TiN膜层的XPS表征

用等离子体浸没离子注入与沉积(PIIID)复合强化新技术在AISI52100轴承钢基体表面成功合成了硬而耐磨的氮化钛薄膜。膜层表面的化学组成和相结构分别用X射线衍射(XRD)和X射线光电子能谱(XPS)表征;膜层表面的原子力显微镜(AFM)形貌显示出TiN膜结晶完整,结构致密均匀。XRD测试结果表明,TiN在(200)晶面衍射峰最强,具有择优取向。Ti(2p)的XPS谱峰泰勒拟合分析揭示出,Ti(2p_1/2)峰和Ti_2p3/2峰均有双峰出现,表明氮化物中的Ti至少存在不同的化学状态;N(1s)的XPS谱峰在396.51, 397.22和399.01 eV附近出现了三个分峰,分别对应于TiNO_y,TiN和N—N键中的氮原子。结合O(1s)的XPS结果,证实膜层中除生成有稳定的TiN相外,还有少量钛的氧化物和未参与反应的单质氮。整个膜层是由TiN,TiO₂,Ti—O—N化合物和少量单质氮组成的复合体系。     

Optimizing accuracy and precision in spectral data

Parameters derived by computer fitting of Gaussian or Lorentzian curves to spectral data suffer from inaccuracies derived by the data gathering strategy, by instrumental errors and by the inherent statistical fluctuation of the measurements. When measurements of extreme quality are required, minimum uncertainty for peak centroid and linewidth for a given data collection time is obtained by proper choice of the number of ‘channels’ in the peak. The optimum conditions that are derived analytically are supported by results of fitting spectra with Gaussian curves. Fittings were done with the simplex procedure yielding precise values of the centroid and linewidth. Data used were x‐ray fluorescence signals and computer‐simulated spectral peaks. Results of the theoretical calculations and of computer fittings to both empirical data and simulated spectra indicate that the optimum number of channels in a peak, for the best quality of measurements of the peak centroid and its linewidth, is independent of the peak integral and has full width at half‐maximum in the neighborhood of 2.5 channels. Copyright © 2005 John Wiley & Sons, Ltd.