Interfacial reactions in Mo-Zr multilayer structure: an X-ray reflectivity study

The effect of elevated temperature on the structural stability and alloy formation in Mo-Zr multilayers is investigated. Mo-Zr multilayers deposited by the electron beam evaporation technique under ultra-high vacuum conditions are annealed up to 650 °C. The changes induced due to thermal treatment are observed using X-ray reflectivity (both specular and off-specular) and X-ray diffraction techniques. The Mo-Zr multilayers remained as an insoluble layered structure even after annealing as revealed from X-ray reflectivity measurements. The interfacial roughness is found to be very similar at all interfaces and decreases on annealing. The multilayer structure remains intact on annealing with expansion of the multilayer period and a marginal increase in X-ray reflectivity.     

Interface engineering of short-period Ni/V multilayer X-ray mirrors

Low-energy ion-assisted magnetron sputter deposition has been used for the synthesis of highly reflective Ni/V multilayer soft X-ray mirrors. A low ion energy and a high ion-to-metal flux ratio were employed in order to stimulate the adatom mobility while minimizing ion-induced intermixing at the interfaces. An analytic model, based on the binary collision approximation, was used in order to gain insight into low-energy ion–surface interactions as a function of ion energy and ion-to-metal flux ratio. The model predicted a favorable region in the ion energy-flux parameter space where only surface atomic displacements are stimulated during growth of Ni and V for multilayers. For a series of Ni/V multilayer mirrors with multilayer periods about Λ = 1.2 nm, grown with a continuous ion assistance using energies in the range 7–36 eV and with ion-to-metal flux ratios Φ_Ni = 4.7 and Φ_V=20.9, specular and diffuse X-ray scattering analyses revealed that ion energies of 27–31 eV produced the best trade-off between reduced interfacial roughness and intermixing. However, it was also concluded that an interface mixing of about ± 1 atomic distance is unavoidable when a continuous flux of assisting ions is used.

To overcome this limitation, a sophisticated interface engineering technique was employed, where the first 0.3 nm of each layer was grown with a high-flux low-energy ion assistance and the remaining part was grown with a slightly higher ion energy. This method was demonstrated to largely eliminate the intermixing while maintaining the smoothening effect of ion assistance. Two Ni/V multilayer soft X-ray mirror structures, one with 500 periods designed for near-normal incidence and one 150 periods reflecting polarizer at the Brewster angle, were grown utilizing the interface engineering concept. Both the near-normal incidence reflectivity as well as polarizability were improved by a factor of 2 as compared to previously reported data for an X-ray energy of E = 511 eV.     

Interfacial electron density profile in Nb/Si bilayer films: an X-ray reflectivity study

This article describes a systematic study of the nature of interfaces involved in a Nb layer deposited on Si (Nb-on-Si) and Si layer deposited on Nb (Si-on-Nb) bilayer films by using a UHV electron beam evaporation technique, having individual layer thickness of 35 and 100 Å each. By using Grazing angle X-ray reflectivity and adopting a proper modelling technique the electron density profile (EDP) as a function of depth has been determined in the samples. EDP determined in as-deposited 35 Å Nb and 35 Å Si bilayer films show that the width of Si-on-Nb and Nb-on-Si interfaces are 20 Å and 40 Å, respectively. The difference observed in the width of two interfaces is attributed to the different growth morphology of 35 Å Nb and 35 Å Si single-layer films as revealed by atomic force microscopy (AFM) investigations. EDP determined from measured XRR data for 100 Å Nb and 100 Å Si deposited bilayer film shows that the width of Si-on-Nb interface is 10 Å. This observed width is smaller than the similar interface in the case of samples having an individual layer thickness of 35 Å. The corresponding interface width of Nb-on-Si is found to be 45 Å and marginally more than the similar interface in the case of the 35 Å Nb/35 Å Si bilayer samples. AFM studies carried out on 100 Å Nb and Si layers deposited separately on float glass substrate indicate similar gross as well as subtle morphological features and cannot be attributed to the observed asymmetry in this case. The observed asymmetry in EDP of two interfaces in this case is due to the enhanced diffusion of Si into the formed metal layer relative to the diffusion into the already deposited metal layer.     

Characterization of Mo/Si soft X-ray multilayer mirrors by grazing-incidence small-angle X-ray scattering

The morphology of buried interfaces plays a key role in high performing Mo/Si soft X-ray mirrors. We show that grazing-incidence small-angle X-ray scattering is a highly effective and non-destructive diagnostic technique for analysis of buried interfaces. The parameters of average interface autocorrelation function can be determined unambiguously. Additionally period thickness, roughness of interfaces and an effective number of vertically correlated periods can be extracted. The multilayer mirrors were prepared by e-beam evaporation on heated and unheated substrates, ion beam assisted e-beam evaporation, ion beam sputtering and RF magnetron sputtering. The latter three techniques produce multilayer mirrors with comparable interface roughness. The differences in lateral correlation length and Hurst parameter are found.     

Nano-scaled Pt/Ag/Ni/Au contacts on p-type GaN for low contact resistance and high reflectivity

We synthesized the vertical-structured LED (VLED) using nano-scaled Pt between p-type GaN and Ag-based reflector. The metallization scheme on p-type GaN for high reflectance and low was the nano-scaled Pt/Ag/Ni/Au. Nano-scaled Pt (5 A) on Ag/Ni/Au exhibited reasonably high reflectance of 86.2% at the wavelength of 460 nm due to high transmittance of light through nano-scaled Pt (5 A) onto Ag layer. Ohmic behavior of contact metal, Pt/Ag/Ni/Au, to p-type GaN was achieved using surface treatments of p-type GaN prior to the deposition of contact metals and the specific contact resistance was observed with decreasing Pt thickness of 5 A, resulting in 1.5 x 10(-4) ohms cm2. Forward voltages of Pt (5 A)/Ag/Ni contact to p-type GaN showed 4.19 V with the current injection of 350 mA. Output voltages with various thickness of Pt showed the highest value at the smallest thickness of Pt due to its high transmittance of light onto Ag, leading to high reflectance. Our results propose that nano-scaled Pt/Ag/Ni could act as a promising contact metal to p-type GaN for improving the performance of VLEDs.     

Resonant anomalous X-ray reflectivity as a probe of ion adsorption at solid-liquid interfaces

We discuss new opportunities to understand processes at the solid-liquid interface using resonant anomalous X-ray reflectivity (RAXR). This approach is illustrated by determination of element-specific density profiles at mica surfaces in aqueous electrolyte solutions containing Rb⁺ and Sr²⁺. The total interfacial electron density profile is determined by specular reflectivity (i.e., reflected intensity vs. momentum transfer, q, at an energy, E, far from any characteristic absorption edge). RAXR spectra (i.e., intensity vs. E at fixed q) reveal element-specific ion distributions. Key differences in the interaction of Rb⁺ and Sr²⁺ with mica are observed using resonant anomalous X-ray reflectivity: Rb⁺ adsorbs in a partially hydrated state, but Sr²⁺ adsorbs in both fully and partially hydrated states.     

Oxidation study of Co/Cu multilayers by resonant X-ray reflectivity

The outer oxide layer of magnetron-sputtered Co/Cu multilayers has been studied by means of resonant and classical X-ray reflectometry. The variation of the oxide layer thickness has been monitored versus the upper-Co layer thickness. The surface oxidation seems to stop at the Co/Cu interface and hence no Cu oxide is produced. The contact potential at the Co/Cu interface may be at the basis of this effect. In addition, the dependence of the oxide layer roughness with its thickness has been studied, varying the roughness inversely to the oxide layer thickness, something which results comprehensible on the basis of the low temperature oxidation process.     

X-ray reflectivity study on TiN/Ti/Si structures before and after annealing

X-ray reflectivity was employed as a powerful tool for studying the surface and interface roughness and thickness, as well as density, of TiN/Ti/Si layers. X-ray reflectivity of the as-deposited samples, with nominal thickness of 17.5 nm of Ti and 3.0 nm of TiN, shows uniform oscillations. When the samples are annealed at 710°C, residual strongly attenuated oscillations are still observed, while the 850°C-annealed sample does not show oscillations, indicating high surface and interface roughness of the formed nitride and silicide layers. It is demonstrated that increased interface roughness, even for a layer with a larger average electron density difference, reduces the oscillations in the reflectivity curve very rapidly. For comparison, cross sectional transmission electron microscopy was employed to find the thickness of the surface and interface layers in silicide structures, which are in good agreement with the X-ray reflectivity results. The work was also supported by tapping mode atomic force microscopy observations, where we have observed nearly flat structures for the as-deposited sample surface and needle-like protrusions for the annealed samples. The surface roughness of the top TiN layer was used to obtain simulated X-ray reflectivity spectra in good agreement with the experimental results. Preliminarily, the crystallography of the layers in the samples was determined by the grazing angle X-ray diffraction technique, to acquire knowledge on the Ti and Si compounds formed in the samples after the annealing.     

Temperature treatment of semiconducting polymers: An X-ray reflectivity study

The influence of temperature treatment on three types of conjugated polymer thin films, named poly(3-hexylthiophene) (P3HT), polyarylamine (PAA) and octylfluorene-bithiophene copolymer (F8T2) is studied. A detailed knowledge of the film morphology and crystalline structure is important since the performance of organic thin film transistors is extremely sensitive to small changes of morphology and structure. Samples are prepared via a spin-casting process on thermal oxidized silicon wafers. The influence of heat treatment in the range from ambient temperatures to 600 K is studied with specular X-ray reflectivity, X-ray diffraction and differential scanning calorimetry. The morphological parameters like layer thicknesses, electron densities and roughnesses of the interface and of the surface are calculated from the XRR measurements. The maximum change of layer thickness due to heat treatment is 15% of the initial layer thicknesses. The maximum variation of the mean electron densities are about 20% and the rms surface roughness vary from 2 Å up to 20 Å as a result of annealing. Interface roughness show variation of about 1 Å. Strong variations of the morphological parameters next to phase transition temperatures are observed as well.     

Crystallization of Au-Si/glass thin film: a real-time synchrotron X-ray scattering study

The crystallization of amorphous, Si-rich, Au28Si72/glass thin film was studied in real-time synchrotron X-ray scattering experiments. The amorphous film crystallizes first into Au and Si phases at a low temperature of 206 degrees C. At annealing temperatures above eutectic temperature (T(E) = 360 degrees C), the Au phase melts while the Si phase rapidly grows further. The crystallized Au28Si72 thin film has nanowire-type grains with 1000-nm-length and 10-nm-diameter. We confirm that the Au liquid phase contributes to the low-temperature crystallization of the Si solid phase for Si-nanowire growth.     

Structure and scattering properties of Ni80Nb20-MgO water-window multilayer mirrors

Ni80Nb20-MgO multilayers with d spacing that varies from 2.50 to 3.07 nm were prepared by pulsed laser deposition under conditions of ultrahigh vacuum (UHV) and argon. The morphological and atomic structure in the multilayers was determined by hard-x-ray scattering. It was found that the interface roughness in both cases, UHV and argon deposition, is <0.4 nm, whereas the lateral and longitudinal correlation lengths in the case of argon deposition, 5.0 and 1.0 nm, respectively, are an order of magnitude lower. This is due to a reduction in kinetic energy of the condensing species in argon by orders of magnitude due to multiple collisions, which reduces the lateral relaxation probability. Hence the soft-x-ray reflectance of [Ni80Nb20-MgO]10 multilayers deposited in argon was determined at 413 eV (3.00 nm), middle of the water window. The reflectance has a peak at approximately 35.2 degrees with a half-width of 3.5 degrees and 0.19% maximum value. These results agree well with the simulation results performed by use of the structural parameters obtained from hard-x-ray scattering. The atomic structure determined by high-angle x-ray diffraction shows that both Ni80Nb20 and MgO are amorphous in the as-deposited condition.     

Nanostructure and chemical characterisation of individual NiFe/Pt multilayer nanowires

NiFe/Pt multilayer nanowires have been successfully fabricated by pulse electrodeposition into the channels of porous anodic aluminum oxide (AAO) templates, and characterized at the nanoscale. Individual nanowires have uniform structure and regular periodicity. The NiFe and Pt layers are polycrystalline, with random orientation fcc lattice structure crystallites and grain sizes 3-10 nm, and the average layer growth rate is 30 nm/s for NiFe and 4 nm/s for Pt. Nanoscale chemical analysis of individual NiFe/Pt nanowires by EDX and EELS shows that they contain alternating NiFe and Pt layers, with a small approximately 1% inclusion of Pt in the NiFe layer due to electrochemical co-deposition.     

Growth kinetics of gold nanocrystals: a combined small-angle X-ray scattering and calorimetric study

The growth of gold nanocrystals prepared by the reduction of tetrachloroauric acid by tetrakis(hydroxymethyl)phosphonium chloride, which allows slow reduction, is investigated by small-angle X-ray scattering and isothermal titration calorimetry in combination with transmission electron microscopy. The growth of the nanocrystals does not follow the diffusion-limited Ostwald ripening but instead follows a sigmoidal rate curve. The activation energy obtained from the temperature-dependent growth study is very small. The heat change associated with the growth is determined for the first time as approximately 10 kcal mol(-1) per 1 nm increase in the nanocrystals' diameter.     

In-situ high temperature X-ray diffraction study of Ni/SiC interface reactions

In-situ experiments on the Ni/SiC interface reaction were carried out with a high temperature X-ray diffractometer capable of measuring the X-ray diffraction pattern in 1–2 s using an imaging plate. The kinetic formation processes of the interface reaction layer were measured in short-period exposure experiments with the apparatus. The time-temperature phase diagram of Ni/SiC in N2 was determined. -Ni2Si and -Ni2Si (high temperature phase of -Ni2Si) were formed at the Ni/SiC interface between 1072 K and 1418 K in N2. The formation of -Ni2Si obeyed the parabolic rate law. The value of the activation energy suggests that the diffusion of Ni through -Ni2Si controls the rate of formation. The results of thermal expansion coefficient measurements suggest that when a sample is cooled to room temperature, compression caused by -Ni2Si occurs on SiC.     

X-ray diffraction study of an amorphous Al60Ge30Ni10 alloy

The ordinary X-ray diffraction profile and anomalous X-ray scattering profiles at nickel and germanium K absorption edges of amorphous Al₆₀Ge₃₀Ni₁₀ alloy have been determined. The results indicate the characteristic feature of the coexistence of nickel-rich highly ordered crystal-like regions and germanium-rich amorphous regions. From the environmental radial distribution function around germanium atoms, the coordination number around a germanium atom is estimated at about 4. Thus, an amorphous germanium-like structure may be quite feasible in this region.     

A study of interdiffusion in multilayer Cu/Ni films by Auger electron depth profiling

The change in concentration profile due to interdiffusion was studied in multilayer Cu/Ni films using the Auger electron depth profiling technique. A sinusoidal distribution was obtained with an amplitude which depends on the annealing time and annealing temperature. The diffusion coefficient was calculated from the amplitude.     

GMR in Ni/Cu multilayers: an electronic structure study

Ab initio self-consistent semi-relativistic spin-polarized TB-LMTO energy band calculations have been carried out on Ni/Cu(100) multilayers, to study the in-plane as well as perpendicular to plane giant magnetoresistance (GMR) effects. The magnetic interaction energies, evaluated as a function of layer thickness, indicate that the antiferromagnetic ordering is a possible ground state for manifestation of GMR. Using the density of states at Fermi level and the Fermi velocity, GMR has been estimated as a function of the Cu spacer thickness.     

薄壳层核壳型Ni/Pt纳米粒子的制备及电催化性能

通过胶体-化学镀法制备不同厚度薄壳层核壳型Ni/Pt纳米粒子, 采用HRTEM、EDS、XPS和XRD手段对粒子的形貌、晶型和组成进行物理表征. 采用动电位、循环伏安法对其氧电还原和甲醇电氧化活性进行测试. 实验结果表明, 核壳结构Ni/Pt纳米颗粒基本为球形, 其中Ni₁-Pt_0.067平均直径为7 nm左右, 壳层厚度约1 nm. 与Pt/C相比, 核壳型Ni/Pt纳米粒子对氧电还原和甲醇电氧化的催化活性显著提高. 在所制备的不同壳层厚度催化剂中, Ni₁-Pt_0.067/C在0.5 mol/L H₂SO₄中氧电还原的最大峰电流密度可达到143.06 mA/mg, 是相同反应条件Pt/C峰电流密度的1.4倍; 而Ni₁-Pt_0.067/C在0.5 mol/L H₂SO₄+1.0 mol/L CH₃OH溶液中甲醇电氧化峰电流密度可达538.3 mA/mg, 是Pt/C峰电流密度的5.2倍. 若以1 mg贵金属Pt为基准, Ni₁-Pt_0.067/C的比质量活性相对Pt/C的提高了30倍.     

Wetting and reactivity in Ni–Si/C system: experiments versus model predictions

Wetting of vitreous carbon C_v by NiSi alloys is studied in high vacuum using the sessile drop and dispensed drop techniques. The role of reactions between NiSi and C_v (simple dissolution or SiC formation) on wetting, adhesion and mechanical behaviour of the interface is determined and discussed. The experimental results on reactive wetting are compared with the predictions of two different approaches proposed recently in order to explain the thermodynamics and kinetics of this type of wetting.