Ion irradiation induced evolution of nanostructure in a graded multi-trilayer system

Nanostructural modifications in a double-graded Pt/Ni/C multi-trilayer, due to irradiation by an energetic ion-beam, have been analyzed using X-ray reflectivity (XRR), X-ray standing wave (XSW) and cross-sectional transmission electron microscopy (X-TEM) techniques. 2 MeV Au²⁺ ions were rastered on Pt/Ni/C multi-trilayer samples producing a uniformly irradiated area at ion-fluences ranging from 1 × 10¹⁴ ions/cm² to 2 × 10¹⁵ ions/cm². Ion irradiation induced modifications of microstructural parameters, e.g., layer thicknesses and electron densities of individual layers and interface roughnesses have been obtained from XRR analysis. Pt- and Ni-fluorescence yield from the as-deposited sample under the XSW condition show the distinct existence of Pt and Ni layers. The almost indistinguishable Pt- and Ni-fluorescence data over the first order Bragg peak from the sample irradiated at the highest ion-fluence, suggest complete mixing of Pt and Ni. Strong mixing between Pt and Ni in the ion irradiated samples is also corroborated by XRR results. X-TEM studies reveal the individual layer structure in the as-deposited sample. This layer structure is lost in the sample irradiated at the highest ion fluence indicating a complete mixing between Pt and Ni layers and nanoscale grain growth of Pt-Ni alloys. Additionally, formation of Pt-Ni alloy nano-clusters in the C-layers is observed. The results are understood in the light of the positive heat of mixing between Pt and C, and Ni and C and the negative heat of mixing between Pt and Ni. The effect of heat of mixing becomes dominant at high fluence irradiation.     

Atomic-scale X-ray structural analysis of self-assembled monolayers on Silicon

Two related self-assembled monolayers (SAMs), 4-bromostyrene (BrSty) and 4-bromophenylacetylene (BPA), are photochemically grown from solution on to the monohydride-terminated Si(111) surface. The atomic-scale structures of the resulting SAMs are examined by X-ray standing waves (XSW), X-ray reflectivity (XRR), X-ray fluorescence, atomic-force microscopy (AFM), X-ray photoelectron spectroscopy (XPS), and density functional theory (DFT). The coverage is 0.5 ML. The results show that in each case the molecule covalently bonds to a single Si T₁ site and stands up-right with a slight molecular tilt of 17^○ that leaves the Br terminal end over a neighboring T₄ site. The Br height is 8.5?Å (BrSty) and 8.6?Å (BPA) above the top surface Si atom. The combined XSW and XRR results rule-out two alternative bonding models predicted by DFT that have the root of the molecule bonded to two neighboring top Si surface atoms. Based on the XSW 111 and 333 coherent fractions, the BPA/Si(111) has a reduced vertical Br distribution width in comparison to BrSty. This greater rigidity in the molecular structure is correlated to a C=C bond at the root.     

Analysis of periodic Mo/Si multilayers: Influence of the Mo thickness

A set of Mo/Si periodic multilayers is studied by non-destructive analysis methods. The thickness of the Si layers is 5 nm while the thickness of the Mo layers changes from one multilayer to another, from 2 to 4 nm. This enables us to probe the effect of the transition between the amorphous and crystalline state of the Mo layers near the interfaces with Si on the optical performances of the multilayers. This transition results in the variation of the refractive index (density variation) of the Mo layers, as observed by X-ray reflectivity (XRR) at a wavelength of 0.154 nm. Combining X-ray emission spectroscopy (XES) and XRR, the parameters (composition, thickness and roughness) of the interfacial layers formed by the interaction between the Mo and Si layers are determined. However, these parameters do not evolve significantly as a function of the Mo thickness. It is observed by diffuse scattering at 1.33 nm that the lateral correlation length of the roughness strongly decreases when the Mo thickness goes from 2 to 3 nm. This is due to the development of Mo crystallites parallel to the multilayer surface.     

多层膜软X光反射镜的研制

本文介绍了镍-碳多层膜软X光反射镜的设计与制造方法,特别是膜厚监控法.用俄歇谱仪分析了一个样品的剖面情况;对一些样品在1.54(?)的衍射特性和在软X光区的反射率进行了测量并与理论计算结果作了比较.     

Thin film and surface characterization by specular X-ray reflectivity

We review the use of specular X-ray reflectivity (XRR) for the characterization of thin-film and surface structures. Specular X-ray scattering at small scattering vectors allows characterization of electron density profiles perpendicular to the surface on the length scale of 0.1 to 100 nm. This allows measurement of surface morphology, thin films, multilayer structures, and buried interfaces. The technique is nondestructive and can be applied in situ in a variety of processing environments. In the first half of the article, we review the theory and methods of XRR, including analysis of XRR spectra by a multilayer optical approach and a discussion of surface roughness measurements by XRR and other techniques. In the second half, we present a wide range of examples of XRR applications in thin-film structures, dynamic processes, liquid surfaces, and macromolecular structures.     

Probing atomic migration in nanostructured multilayers: application of X-ray standing wave fields

X-ray standing wave fields, excited in periodic nanostructured multilayers during Bragg diffraction, have been used to probe atomic migration in multilayers. Ion beam induced migration of Fe impurity atoms from the C layers to the Pt layers in a Pt(Fe)/C(Fe) multilayer, where each layer is about 2 nm thick, has been detected. With a depth resolution better than 0.2 nm of this technique, the direction of Fe migration (here outward) and the change of Fe concentration in C (also Pt) layers have been determined. The results of such measurements are important for understanding the properties of multilayers, for example, the evolution of ferromagnetism in the present example [Dev, Microelectron. Eng. 83, 1721 (2006)10.1016/j.mee.2006.01.230].     

All-optical switching device for infrared based on PbTe quantum dots

Multilayers of PbTe quantum dots embedded in SiO₂ were fabricated by alternate use of Pulsed Laser Deposition (PLD) and Plasma Enhanced Chemical Vapor Deposition (PECVD) techniques. The morphological properties of the nanostructured material were studied by means of High Resolution Transmission Electron Microscopy (HRTEM), Grazing-Incidence Small-Angle X-ray scattering (GISAXS) and X-ray Reflectometry (XRR) techniques. A preliminary analysis of the GISAXS spectra provided information about the multilayer periodicity and its relationship to the size of the deposited PbTe nanoparticles. Finally multilayers were fabricated inside a Fabry–Perot cavity. The device was characterized by means of Scanning Electron Microscopy (SEM). Transmittance measurements show the device functionality in the infrared region.     

4.48 nm正入射软X射线激光用Cr/C多层膜高反射镜的研制

针对4.48nm类镍钽软X射线激光及其应用实验,设计制备了工作于这一波长的近正入射多层膜高反射镜。选择Cr/C为制备4.48nm高反射多层膜的材料对,通过优化设计,确定了多层膜的周期、周期数以及两种材料的厚度比。模拟了多层膜非理想界面对高反射多层膜性能的影响。采用直流磁控溅射方法在超光滑硅基片上实现了200周期Cr/C多层膜高反射镜的制备。利用X射线衍射仪测量了多层膜结构,在德国BessyⅡ同步辐射上测量了在工作波长处多层膜反射率,测量的峰值反射率达7.5%。对衍射仪测量的掠入射反射曲线和同步辐射测量的反射率曲线分别进行拟合,得到的粗糙度和厚度比的结果相近。测试结果表明,所制备的Cr/C多层膜样品结构良好,在指定工作波长处有较高的反射峰,达到了设计要求。     

Structure and magnetic properties of magnetron-sputtered [(Fe/Pt/Fe)/Au]n multilayer films

Using dc magnetron sputtering, Fe/Pt/Au multilayer films were prepared, and the effects of Au layer thickness and annealing temperature on structure and magnetic properties of the Fe/Pt/Au multilayer films were investigated. The as-deposited Fe/Pt/Au multilayer films have good periodic structure with composition modulation along the growth direction. The stress stored in the as-deposited films promoted the ordering of the films annealed at 400 °C. When the films were annealed at 500 °C, the thicker Au layer could restrain the order-disorder transformation region volume and lead to the decrease of the ordered volume fraction with Au layer thickness increasing.     

利用透射光谱与X射线反射谱精确测量溶胶-凝胶TiO2薄膜厚度和光学常数

在洁净K9玻璃基底上沉积TiO2薄膜,将透射光谱和X射线反射光谱相结合分析获得膜层的厚度和光学常数。X射线反射谱拟合能精确得到膜层的厚度、电子密度及表面和界面粗糙度,其中膜层厚度的数值为透射光谱的分析提供了重要参考。基于Forouhi-Bloomer色散模型拟合膜层透射光谱,得到薄膜折射率和消光系数,理论曲线和实验曲线吻合良好。对于同一样品,两种光谱拟合分析得到的厚度数值非常接近,差值最大为4.9nm,说明两种方法的结合能够提高光学分析结果的可靠性。     

X-ray reflectivity study of hydrogen implanted silicon

The X-ray reflectivity (XRR) technique was used to study monocrystalline silicon samples implanted with H₂ ions at an energy of 31 keV and to the dose of 2 × 10¹⁶ hydrogen atoms/cm². All samples were subsequently isochronally annealed in vacuum at different temperatures in the range from 100 to 900 °C. Although the hydrogen depth distribution was expected to be smooth initially, fringes in the XRR spectra were observed already in the implanted but not annealed sample, revealing the presence of a well-defined film-like structure. Annealing enhances the film top to bottom interface correlation due to structural relaxation, resulting in the appearance of fringes in the larger angular range, already at low annealing temperatures. The thickness of the film decreases slowly up to 350 °C where substantial changes in the roughness are observed, probably due to the onset of larger clusters formation. Further annealing at higher temperatures restores the high correlation of the film interfaces, while the thickness decreases with the temperature more rapidly.     

2,7-二辛基[1]苯并噻吩并[3,2-b]苯并噻吩/Ni(100)的界面能级结构随薄膜厚度的演化

利用紫外光电子能谱、X射线光电子能谱以及原子力显微镜系统研究了2,7-二辛基[1] 苯并噻吩并[3,2-b]苯并噻吩(C8-BTBT)生长在单晶Ni(100)上的能级结构随着薄膜厚度的演化以及薄膜的生长方式. 发现第一层C8-BTBT平躺生长且与Ni基底发生了化学吸附反应. 从第二层起分子直立生长且呈现岛状生长模式. 这种平躺至直立的分子取向转变, 导致薄膜的能级结构在第一层与第二层间发生阶梯式的变化, 真空能级与最高占据能级同步下降. 此后能带结构随着薄膜厚度的增加逐渐向下弯曲, 功函数随着膜厚的增加而减小. 同时还发现由于直立生长的C8-BTBT其层间电导率较差导致实验中的能级未能收敛. 实验结果提示对基于Ni和C8-BTBT的自旋器件需要插入缓冲层并尽可能减少C8-BTBT的层数.     

X射线反射法测量α:CH薄膜的密度和厚度

 利用低压等离子体化学气相沉积法制备厚度不同的非晶碳氢薄膜，采用X射线反射法测量了非晶碳氢薄膜的密度和厚度。实验中分别采用曲线拟合法和周期估算法计算薄膜的厚度，两种方法测得的厚度平均差别为5.5%，一致性较好。利用X射线反射谱的临界角计算所得的7个样品的密度差别较小，在8%之内。     

Magnetostatic interaction in electrodeposited Ni/Au multilayer nanowire arrays

Ordered Ni/Au multilayer nanowire arrays are successfully fabricated inside the nanochannels of anodic aluminum oxide template by pulse electrodeposition method. The thickness of the alternating layers is controlled to examine the magnetostatic interaction in Ni/Au multilayer nanowires. The magnetic easy axis parallel to the nanowires indicates that here the magnetostatic coupling along the wire axis dominates over the interactions perpendicular to the nanowires. However,the magnetostatic interaction between adjacent nanowires with larger magnetic layers is enhanced, leading to the existence of an optimum coercivity value.     

In situ XPS investigation of Pt(Sn)/Mg(Al)O catalysts during ethane dehydrogenation experiments

Calcined hydrotalcite with or without added metal (Mg(Al)O, Pt/Mg(Al)O and Pt,Sn/Mg(Al)O) have been investigated with in situ X-ray photoelectron spectroscopy (XPS) during ethane dehydrogenation experiments. The temperature in the analysis chamber was 450 °C and the gas pressure was in the range 0.3-1 mbar. Depth profiling of calcined hydrotalcite and platinum catalysts under reaction, oxidation and in hydrogen-water mixture was performed by varying the photon energy, covering an analysis depth of 10-21 Å. It was observed that the Mg/Al ratio in the Mg(Al)O crystallites does not vary significantly in the analysis depth range studied. This result indicates that Mg and Al are homogeneously distributed in the Mg(Al)O crystallites. Catalytic tests have shown that the initial activity of a Pt,Sn/Mg(Al)O catalyst increases during an activation period consisting of several cycles of reduction-dehydrogenation-oxidation. The Sn/Mg ratio in a Pt,Sn/Mg(Al)O catalyst was followed during several such cycles, and was found to increase during the activation period, probably due to a process where tin spreads over the carrier material and covers an increasing fraction of the Mg(Al)O surface. The results further indicate that spreading of tin occurs under reduction conditions.A PtSn₂ alloy was studied separately. The surface of the alloy was enriched in Sn during reduction and reaction conditions at 450 °C. Binding energies were determined and indicated that Sn on the particle surface is predominantly in an oxidised state under reaction conditions, while Pt and a fraction of Sn is present as a reduced Pt-Sn alloy.     

Thickness-dependent magnetic properties in Pt/[Co/Ni]n multilayers with perpendicular magnetic anisotropy

We systematically investigated the Ni and Co thickness-dependent perpendicular magnetic anisotropy (PMA) coefficient, magnetic domain structures, and magnetization dynamics of Pt(5 nm)/[Co($t_{\rm Co}$)/Ni($t_{\rm Ni}$)]$_{5}$/Pt(1 nm) multilayers by combining the four standard magnetic characterization techniques. The magnetic-related hysteresis loops obtained from the field-dependent magnetization $M$ and anomalous Hall resistivity (AHR) $\rho_{{xy}}$ showed that the two serial multilayers with $t_{\rm Co} = 0.2$ nm and 0.3 nm have the optimum PMA coefficient $K_{\rm U}$ as well as the highest coercivity $H_{\rm C}$ at the Ni thickness $t_{\rm Ni}= 0.6 $ nm. Additionally, the magnetic domain structures obtained by magneto-optic Kerr effect (MOKE) microscopy also significantly depend on the thickness and $K_{\rm U}$ of the films. Furthermore, the thickness-dependent linewidth of ferromagnetic resonance is inversely proportional to $K_{\rm U}$ and $H_{\rm C}$, indicating that inhomogeneous magnetic properties dominate the linewidth. However, the intrinsic Gilbert damping constant determined by a linear fitting of the frequency-dependent linewidth does not depend on the Ni thickness and $K_{\rm U}$. Our results could help promote the PMA [Co/Ni] multilayer applications in various spintronic and spin-orbitronic devices.     

Determination of the K adsorption site on Fe(1 1 0) with XSW

We have used X-ray standing waves (XSW) in near normal incidence to determine the K–Fe bond length and the adsorption site of K at the saturation coverage at room temperature on the Fe(1 1 0) surface. Three different scattering geometries were used to enable the determination of the adsorption site by triangulation. From the results we conclude that the potassium atoms adsorb in a distorted hexagonal overlayer. The Fe–K distance, as determined from the measurements in the (2 2 0) Bragg reflection, is 3.4±0.2 Å. The long bridge site seems to be the preferred adsorption site for the potassium atoms in the distorted hexagonal overlayer. This geometry not only fits all the XSW data, but also explains all spots in the LEED pattern without the need to introduce multiple scattering. Comparison of the measured and simulated XSW data, based on the distorted hexagonal overlayer, enables a more accurate determination of the Fe–K bond length to 3.36±0.14 Å. This corresponds to a potassium hard sphere radius of r_K=2.12±0.14 Å. This radius is among the largest reported for potassium on a metal, which is attributed to the high coverage and coordination of the K atoms in this overlayer arrangement.     

Spin reorientation transition in Fe/CeH2 multilayers probed by soft X-ray resonant magnetic scattering

The magnetic domain configurations of Fe 3d spins in Fe/CeH₂ multilayers were measured by soft X-ray resonant magnetic scattering. The interface region could be probed by setting up X-ray standing waves due to the multilayer periodicity. By resolving first- and second-order magnetic scattering contributions, we show that the latter probe directly the magneto-crystalline anisotropy which is dominated by the Fe interface layers causing a spin reorientation transition when the temperature is lowered. Received: 30 May 2001 / Accepted: 4 July 2001 / Published online: 5 October 2001