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.     

Mo/Si软X射线多层膜的界面粗糙度研究

 用磁控溅射法分别制备了以Mo膜层和Si膜层为顶层的Mo/Si多层膜系列, 利用小角X射线衍射确定了各多层膜的周期厚度。以不同周期数的Mo/Si多层膜的新鲜表面近似等同于同一多层膜的内界面,通过原子力显微镜研究了多层膜界面粗糙度随膜层数的变化规律。并在国家同步辐射实验室测量了各多层膜的软X射线反射率。研究表明：随着膜层数的增加,Mo膜层和Si膜层的界面粗糙度先减小后增加然后再减小,多层膜的峰值反射率先增加后减小。     

正入射Mo/B_4C软X射线多层膜

采用Ｍｏ／Ｂ４Ｃ材料在短波长波段（λ＜１０．０ｎｍ）进行软Ｘ射线多层膜实验研究。在指定波长（８．０ｎｍ附近）处对多层膜进行结构设计，并制备出了周期结构准确的Ｍｏ／Ｂ４Ｃ多层膜样品。     

Amorphous Si/insulator multilayers grown by vacuum deposition and electron cyclotron resonance plasma treatment

a-Si/insulator multilayers have been deposited on (0 0 1) Si by electron gun Si evaporation and periodic electron cyclotron resonance plasma oxidation or nitridation. Exposure to an O or N plasma resulted in the formation of a thin SiO₂ and SiN_x layer whose thickness was self-limited and controlled by process parameters. For thin-layer (2 nm) Si/SiO₂ and Si/SiN_x multilayers no visible photoluminescence (PL) was observed in most samples, although all exhibited weak “blue” PL. For the nitride multilayers, annealing at 750°C or 850°C induced visible PL that varied in peak energy with Si layer thickness. Depth profiling of a-Si caps on thin insulating layers revealed no detectable contamination for the SiN_x layers, but substantial O contamination for the SiO₂ films.     

Investigation of phosphorus surface segregation by X-ray scattering measurements

The surface segregation of phosphorus in silicon at low temperatures is studied by using δ doping structures grown by molecular beam epitaxy. The samples are characterized by X-ray crystal truncation rod (CTR) scattering using synchrotron radiation as the light source. The 1/e decay length of P segregation and segregation barrier energy are obtained by fitting the CTR curves within kinematical approximation of X-ray diffraction theory. The surface segregation of P is strong at a growth temperature of 450 °C, with a 1/e decay length of 14 nm, while for growth temperatures below 350 °C, P segregation is negligible with a 1/e decay length not larger than 4 nm. The segregation barrier energy is determined to be 0.43 eV.     

New method to characterize mesoscopic range and very small strain with using multi-wave X-ray diffraction

A new technique to observe mesoscopic-range strain fields (up to several hundreds of nm) is proposed, using modulation of the crystal-truncation-rod (CTR) scattering caused by Bragg reflection. This technique is particularly sensitive to small, long-range strain fields near crystal surfaces and interfaces, which are usually difficult to be discriminated by using Bragg reflection. A simple interpretation can be made for the modulation profile: the technique is physically simple with a few parameters fitted to the data and, independently of any model, is able to determine the total displacement due to mesoscopic strain field for depths up to several hundreds of nanometers. We applied this method to a Si(0 0 1) wafer whose surface is covered with a thermal oxide layer 3 nm thick. On the basis of the expressions we obtained for the modulation profile a least-squares fitting was carried out to give a result that under the oxide layer there exists a total displacement of −0.16 Å. It was also revealed from the visibility of the modulation profile that the total displacement has a static fluctuation of at least ±0.13 Å in the lateral direction. The new method can be used for the correction of the errors of the X-ray standing wave (XSW) method produced by strained layers near crystal surfaces.     

Photoelectron spectroscopy measurements of the valence band structures of polymerized thin films of C60 and La0.1C60

The electronic valence band structures of polymerized thin films of C₆₀ and La_0.1C₆₀ have been studied by using ultra-violet photoelectron spectroscopy. Additionally, the films have been characterized by using Raman spectroscopy, X-ray photoelectron spectroscopy, and X-ray diffraction. The valence band of the C₆₀ film shows major peaks at binding energies of 2.6, 7.2, 10.3, and 12.6 eV. In the case of the doped film, we observe (i) an additional peak with a binding energy of 13.7 eV, (ii) evidence for redistribution of the density of electronic states due to hybridization between the 5d orbitals of La and the C₆₀ cage, and (iii) significantly higher density of the electronic states near the Fermi energy. The valence band spectra of the doped film are in good agreement with recent results of the density functional theory that support strong hybridization between the d-valence orbitals of La and the C₆₀ cage.     

In-situ study of the diffusion-reaction mechanism in Mo/Si multilayered films

We present a low temperature diffusion study on the formation of intermixing zones between periodic, nanometer thick films consisting of Mo and Si. An in-situ X-ray diffraction method at pm-accuracy was developed, including a model that explains the period change observed by diffusion limited interface growth. Experiments were carried out on Mo/Si multilayered films in the temperature range of 100-275 °C, resulting in the determination of diffusion coefficients. Temperature scaling showed Arrhenius-type behavior of the diffusion constant over the entire temperature range, with an activation energy of 0.5 eV.     

In situ X-ray analysis of solid/electrolyte interfaces: electrodeposition of Cu and Co on Si(1 1 1):H and GaAs(0 0 1) and corrosion of Cu3Au(1 1 1)

Electrochemical deposition of Cu and Co in monolayer amounts on hydrogen terminated Si(1 1 1) was studied ex situ and in situ by X-ray techniques. The X-ray beam was found to have a strong effect on the deposit causing desorption under the beam. Cu deposition on GaAs(0 0 1) from UHV is compared with electrodeposited Cu on the same surface, elucidating similarities and differences of electrochemical and UHV deposition. Roughening due to corrosion of Cu₃Au(1 1 1) is observed by crystal truncation scattering. The observed behaviour of passivation of this surface is explained by the formation of Au clusters, increasingly covering the surface at higher oxidation potential.     

Three-dimensional structure of the calcite-water interface by surface X-ray scattering

The three-dimensional structure of the calcite (104)-water interface has been determined with surface X-ray scattering. Nine crystal truncation rods (including specular and non-specular rods) were measured providing both vertical and lateral sensitivity to the interfacial structure. The results reveal that calcite is nearly ideally terminated with a single surface hydration layer that includes two inequivalent water molecules having distinct heights of 2.3 ± 0.1 and 3.5 ± 0.2 Å, each with a well-defined lateral registry with respect to the calcite surface. No additional layering of water is observed beyond this surface hydration layer. Small displacements in the outer two calcium carbonate layers were also observed. These results are compared with previous experimental and computational results.     

Interface roughness, surface roughness and soft X-ray reflectivity of Mo/Si multilayers with different layer number

A series of Mo/Si multilayers with the same periodic length and different periodic number were prepared by magnetron sputtering, whose top layers were respectively Mo layer and Si layer. Periodic length and interface roughness of Mo/Si multilayers were determined by small angle X-ray diffraction (SAXRD).Surface roughness change curve of Mo/Si multilayer with increasing layer number was studied by atomic force microscope (AFM). Soft X-ray reflectivity of Mo/Si multilayers was measured in National Synchrotron Radiation Laboratory (NSRL). Theoretical and experimental results show that the soft X-ray reflectivity of Mo/Si multilayer is mainly determined by periodic number and interface roughness, surface roughness has little effect on reflectivity.     

Nanoridge domains in α-phase W films

Two types of nanoridge domains oriented with each other with an angle ranging between 109° and 124° were measured by scanning tunneling microscopy on the α-W film sputter deposited on an oxidized Si surface. Each domain contains nanoridges with a period of 7.5 ± 1.0 nm. No such domains were observed on the β-W film surface. We argued that due to the anisotropy of the W(1 1 0) surface, the impinging W atoms diffuse faster along the 〈111〉 directions on the surface to form the nanoridge structure. There are two equivalent 〈111〉 directions, which give rise to two orientational domains with an angle of ∼110°. An isotropic β-W(1 0 0) phase has no preferred diffusion direction for the impinging W atoms and therefore, no nanoridge domain structure was observed.     

A surface X-ray diffraction study of TiO2(1 1 0)(3 × 1)-S

Surface X-ray diffraction has been used to investigate the structure of TiO₂(1 1 0)(3 × 1)-S. In concert with existing STM and photoemission data it is shown that on formation of a (3 × 1)-S overlayer, sulphur adsorbs in a position bridging 6-fold titanium atoms, and all bridging oxygens are lost. Sulphur adsorption gives rise to significant restructuring of the substrate, detected as deep as the fourth layer of the selvedge. The replacement of a bridging oxygen atom with sulphur gives rise to a significant motion of 6-fold co-ordinated titanium atoms away from the adsorbate, along with a concomitant rumpling of the second substrate layer.     

RHEED observation of BaTiO3 thin films grown by MBE

Ferroelectric BaTiO₃ thin films with a thickness of 10 monolayers (ML) were epitaxially grown on SrTiO₃(0 0 1) substrates by very slow deposition using molecular beam epitaxy (MBE). The investigations were carried out by two growth methods: (i) codeposition and (ii) alternate deposition of the metal elements in an oxygen atmosphere. In situ observation of reflection high-energy electron diffraction confirmed that an epitaxial cube-on-cube structure was prepared. After the deposition, X-ray diffraction measurements were carried out. The 10-ML-thick BaTiO₃ films were highly c-axis oriented single crystals with good film quality.     

Investigation in the interface roughness of DC-sputtered Mo/B4C multilayer mirrors with variable layer pairs for 7-nm soft X-ray polarizers

The surface and interface roughness of Mo/B₄C multilayer mirrors for 7-nm soft X-ray polarizer with variable layer pairs (N = 50, 70, 90 and 110), fabricated by DC sputtering technique is investigated by atomic force microscopy and X-ray scattering and reflecting. The experimental results present that the surface and interface roughness of Mo/B₄C multilayer mirrors increase layer by layer from its substrate as its Mo layer thickness greater than 2 nm, and the roughness grown tendency could be characterized by a quadratic function.     

Overpotential deposition of Ag monolayer and bilayer on Au(1 1 1) mediated by Pb adlayer underpotential deposition/stripping cycles

Ultra-thin Ag films on the Au(1 1 1) surface were prepared via overpotential deposition (OPD) in the presence of Pb²⁺ ions. By carrying out repetitive Pb adlayer underpotential deposition (UPD) and stripping cycles during Ag bulk deposition, the two-dimensional growth of Ag films was significantly enhanced in high OPD. The Ag monolayer sample was made by comparing the voltammetry curves, in which the signatures for Pb adlayer UPD on Au(1 1 1) changed to that on Ag(1 1 1). As demonstrated by the X-ray specular reflectivity measurements, nearly complete monolayer and bilayer films can be made with optimized deposition procedures. On subatomic scale, however, we found that these films have significant higher root-mean-square displacement amplitudes than those underpotentially deposited Ag monolayer and bilayer on either Au(1 1 1) or Pt(1 1 1).     

The ZnO non-polar (10 0) surface: an X-ray structural investigation

We performed a structural analysis of the non-polar ZnO (10 0) surface by means of grazing incidence X-ray diffraction. The analysis was conducted on ten rods, smooth surface domains, though of small coherent width, having been obtained after several Ar⁺ sputtering–annealing cycles. The surface derived from the bulk structure exposes one ZnO dimer per unit cell, parallel to the [001] axis. All the existing models, derived from ab initio calculations or low-energy electron diffraction (LEED) analyses, consist in a surface dimer whose O and Zn atoms are shifted inwards, with the O pointing outwards with respect to Zn. Whereas the LEED studies conclude on a dimer distance greater than in the bulk, the theoretical studies agree on a dimer contracted by amounts ranging from 5.5 to 7.5%. This contraction is interpreted as a result of the strong ionicity of ZnO, and is associated with a moderate dimer rotation. The latter, however, is found between 2.3 and 11.4°. Despite the discrepancies between the models, the Zn atom is always found shifted downwards by more than 0.25 Å. This is unambiguously rejected by our data, which show that the Zn atom keeps very close to its bulk position. It is displaced downwards by ΔZ_Zn=−0.06±0.02 Å, and it moves along [001] towards O by ΔX_Zn=0.05±0.02 Å. We denote a trend for the O atom to be displaced downwards too, with a concomitant displacement towards Zn. The faint X-ray scattering of O prevents us from assessing its position with accuracy. Depending on the choice of position for Zn in the error bar range, the buckling is evaluated as between −6.5 and 3°, or between −4 and 0.5°. The dimer distance is evaluated equal to 1.90 Å, with a deviation equal either to 0.06 or 0.11 Å.     

Massive transfer of vertically aligned Si nanowire array onto alien substrates and their characteristics

Si nanowires (NWs) are promising materials for future electronic, photovoltaic, and sensor applications. So far the Si NWs are mainly formed on particular substrates or at high temperatures, greatly limiting their application flexibility. Here we report a low temperature process for forming and massively transferring vertically aligned Si NWs on alien substrates with a large density of about (3-5) × 10⁷ NWs/mm². The X-ray diffraction spectrum reveals that the transferred NWs exhibit almost the same crystal property as the bulk Si. Our investigation further shows that the transferred NWs have exceptional optical characteristics. The transferred Si NWs of 12.14 μm exhibit the transmittance as low as 0.3% in the near infrared region and 0.07% in the visible region. The extracted absorption coefficient of Si NWs in the near infrared region is about 3 × 10³ cm⁻¹, over 30 times larger than that of the bulk Si. Because of the low temperature process, it enables a large variety of alien substrates such as glass and plastics to be used. In addition, the exceptional properties of the transferred NWs offer potential applications for photovoltaic, photo-detectors, sensors, and flexible electronics.