Femtosecond laser pulse irradiation of Sb-rich AgInSbTe films: Scanning electron microscopy and atomic force microscopy investigations

The single-layer and multilayer Sb-rich AgInSbTe films were irradiated by a single femtosecond laser pulse with the duration of 120 fs. The morphological feature resulting from the laser irradiation have been investigated by scanning electron microscopy and atom force microscopy. For the single-layer film, the center of the irradiated spot is a dark depression and the border is a bright protrusion; however, for the multilayer film, the center morphology changes from a depression to a protrusion as the energy increases. The crystallization threshold fluence of the single-layer and the multilayer films is 46.36 mJ/cm², 63.74 mJ/cm², respectively. PACS 79.20.Ds; 78.55.Qr; 78.66.Jg; 68.37.Ef; 68.37.Ps     

Analyses of surface coloration on TiO2 film irradiated with excimer laser

TiO₂ film of around 850 nm in thickness was deposited on a soda-lime glass by PVD sputtering and irradiated using one pulse of krypton-fluorine (KrF) excimer laser (wavelength of 248 nm and pulse duration of 25 ns) with varying fluence. The color of the irradiated area became darker with increasing laser fluence. Irradiated surfaces were characterized using optical microscopy, scanning electron microscopy, Raman spectroscopy and atomic force microscopy. Surface undergoes thermal annealing at low laser fluence of 400 and 590 mJ/cm². Microcracks at medium laser fluence of 1000 mJ/cm² are attributed to surface melting and solidification. Hydrodynamic ablation is proposed to explain the formation of micropores and networks at higher laser fluence of 1100 and 1200 mJ/cm². The darkening effect is explained in terms of trapping of light in the surface defects formed rather than anatase to rutile phase transformation as reported by others. Controlled darkening of TiO₂ film might be used for adjustable filters.     

Transmission electron microscopy studies of HfO2 thin films grown by chloride-based atomic layer deposition

Detailed transmission electron microscopy characterization of HfO₂ films deposited on Si(1 0 0) using atomic layer deposition has been carried out. The influence of deposition temperature has been investigated. At 226 °C, a predominantly quasi-amorphous film containing large grains of cubic HfO₂ (a₀ = 5.08 Å) was formed. Grain morphology enabled the nucleation sites to be determined. Hot stage microscopy showed that both the cubic phase and the quasi-amorphous phase were very resistant to thermal modification up to 500 °C. These observations suggest that nucleation sites for the growth of the crystalline cubic phase form at the growing surface of the film, rather homogeneously within the film. The films grown at higher temperatures (300-750 °C) are crystalline and monoclinic. The principal effects of deposition temperature were on: grain size, which coarsens at the highest temperature; roughness with increases at the higher temperatures due to the prismatic faceting, and texture, with texturing being strongest at intermediate temperatures. Detailed interfacial characterization shows that interfacial layers of SiO₂ form at low and high temperatures. However, at intermediate temperatures, interfaces devoid of SiO₂ were formed.     

The effects of substrate temperature on the structure, morphology and photoluminescence properties of pulsed laser deposited SrAl2O4:Eu,Dy thin films

In this study, SrAl₂O₄:Eu²⁺,Dy³⁺ thin film phosphors were deposited on Si (1 0 0) substrates using the pulsed laser deposition (PLD) technique. The films were deposited at different substrate temperatures in the range of 40-700 °C. The structure, morphology and topography of the films were determined by using X-ray diffraction (XRD), atomic force microscopy (AFM), scanning electron microscopy (SEM) and high resolution transmission electron microscopy (HRTEM). Photoluminescence (PL) data was collected in air at room temperature using a 325 nm He-Cd laser as an excitation source. The PL spectra of all the films were characterized by green phosphorescent photoluminescence at ∼530 nm. This emission was attributed to 4f⁶5d¹→4f⁷ transition of Eu²⁺. The highest PL intensity was observed from the films deposited at a substrate temperature of 400 °C. The effects of varying substrate temperature on the PL intensity were discussed.     

Effects of annealing on laser-induced damage threshold of TiO2/SiO2 high reflectors

The mechanism of improving 1064 nm, 12 ns laser-induced damage threshold (LIDT) of TiO₂/SiO₂ high reflectors (HR) prepared by electronic beam evaporation from 5.1 to 13.1 J/cm² by thermal annealing is discussed. Through optical properties, structure and chemical composition analysis, it is found that the reduced atomic non-stoichiometric defects are the main reason of absorption decrease and LIDT rise after annealing. A remarkable increase of LIDT is found at 300 °C annealing. The refractive index and film inhomogeneity rise, physical thickness decrease, and film stress changes from compress stress to tensile stress due to the structure change during annealing.     

Thickness-dependent surface morphology of La0.9Sr0.1MnO3 ultrathin films

La_0.9Sr_0.1MnO₃ (LSMO) ultrathin films with various thickness (in the range of 5-50 unit cells) are grown on (0 0 1) substrates of the single-crystal SrTi_0.99Nb_0.01O₃ by laser molecular-beam epitaxy (laser-MBE), and the surface morphology of these films were measured by scanning tunneling microscopy (STM). STM images of LSMO ultrathin film surface reveal that surface morphology becomes more flat with increasing film thickness. This study highlights the important effect of strain caused by the lattice mismatch between substrates and ultrathin films. And the results should be useful to the investigations on growing manganite perovskite materials.     

Ge/Sb2Te3 nanocomposite multilayer films for high data retention phase-change random access memory application

The amorphous-to-crystalline transition of Ge/Sb₂Te₃ nanocomposite multilayer films with various thickness ratios of Ge to Sb₂Te₃ were investigated by utilizing in situ temperature-dependent film resistance measurements. The crystallization temperature and activation energy for the crystallization of the multilayer films increased with the increase in thickness ratio of Ge to Sb₂Te₃. The difference in sheet resistance between amorphous and crystalline states could reach as high as 10⁴ Ω/□. The crystallization temperature and activation energy for the crystallization of Ge/Sb₂Te₃ nanocomposite multilayer films was proved to be larger than that of conventional Ge₂Sb₂Te₅ film, which ensures a better data retention for phase-change random access memory (PCRAM) use. A data retention temperature for 10 years of the amorphous state [Ge (2 nm)/Sb₂Te₃ (3 nm)]₄₀ film was estimated to be 165 °C. Transmission electron microscopy (TEM) images revealed that Ge/Sb₂Te₃ nanocomposite multilayer films had layered structures with clear interfaces.     

Au-assisted electroless etching of silicon in aqueous HF/H2O2 solution

The Au-assisted electroless etching of p-type silicon substrate in HF/H₂O₂ solution at 50 °C was investigated. The dependence of the crystallographic orientation, the concentration of etching solution and the silicon resistivity on morphology of etched layer was studied. The layers formed on silicon were investigated by scanning electron microscopy (SEM). It was demonstrated that although the deposited Au on silicon is a continuous film, it can produce a layer of silicon nanowires or macropores depending on the used solution concentration.     

Influence of substrate temperature on properties of MgF2 coatings

Thermal boat evaporation was employed to prepare MgF₂ single-layer coatings upon both JGS1 and UBK7 substrates at different substrate temperatures. Microstructure, transmittance and residual stress of these coatings were measured by X-ray diffraction, spectrophotometer, and optical interferometer, respectively. Measurement of laser induced damage threshold (LIDT) of the samples was performed at 355 nm, 8 ns pulses. The results showed that high substrate temperature was beneficial to crystallization of the film. Above 244 °C, the refractive index increased gradually with the substrate temperature rising. Whereas, it was exceptional at 210 °C that the refractive index was higher than those deposited at 244 and 277 °C. The tensile residual stresses were exhibited in all MgF₂ films, but not well correlated with the substrate temperature. In addition, the stresses were comparatively smaller upon JGS1 substrates. A tendency could be seen that the LIDTs reached the highest values at about 244 °C, and the films upon JGS1 had higher LIDTs than those upon UBK7 substrates at the same temperature. Meanwhile, the damage morphologies showed that the laser damage of the coating resulted from an absorbing center at the film-substrate interface. The features of the damages were displayed by an absorbing center dominated model. Furthermore, the reason of the difference in LIDT values was discussed in detail.     

Characterization of CdTe films with in situ CdCl2 treatment grown by a simple vapor phase deposition technique

A unique vapor phase deposition (VPD) technique was designed and built to achieve in situ CdCl₂ treatment of CdTe film. The substrate temperature was 400 °C, and the temperature of CdTe mixture with CdCl₂ source was 500 °C. The structural and morphological properties of CdTe have been studied as a function of wt.% CdCl₂ concentration by using X-ray diffraction (XRD), energy dispersive spectroscopy (EDS), scanning electron microscopy (SEM) and atomic force microscopy (AFM). XRD measurements show that the presence of CdCl₂ vapor induces (1 1 1)-oriented growth in the CdTe film. SEM measurements have shown enhance growth of grains, in the presence of CdCl₂. From AFM the roughness of the films showed a heavy dependence on CdCl₂ concentration. In the presence of 4% CdCl₂ concentration, the CdTe films roughness has a root mean square (rms) value of about 275 Å. This value is about 831 Å for the non-treated CdTe films.     

Characterization and luminescent properties of SiO2:ZnS:Mn and ZnS:Mn nanophosphors synthesized by a sol-gel method

ZnS and SiO₂-ZnS nanophosphors, with or without different concentration of Mn²⁺ activator ions, were synthesized by using a sol-gel method. Dried gels were annealed at 600 °C for 2 h. Structure, morphology and particle sizes of the samples were determined by using X-ray diffraction (XRD), highresolution transmission electron microscopy (HRTEM) and field emission scanning electron microscopy (FESEM). The diffraction peaks associated with the zincblende and the wurtzite structures of ZnS were detected from as prepared ZnS powders and additional diffraction peaks associated with ZnO were detected from the annealed powders. The particle sizes of the ZnS powders were shown to increase from 3 to 50 nm when the powders were annealed at 600 °C. An UV-Vis spectrophotometer and a 325 nm He-Cd laser were used to investigate luminescent properties of the samples in air at room temperature. The bandgap of ZnS nanoparticles estimated from the UV-Vis data was 4.1 eV. Enhanced orange photoluminescence (PL) associated with ⁴T₁→⁶A₁ transitions of Mn²⁺ was observed from as prepared ZnS:Mn²⁺and SiO₂-ZnS:Mn²⁺ powders at 600 nm when the concentration of Mn²⁺ was varied from 2-20 mol%. This emission was suppressed when the powders were annealed at 600 °C resulting in two emission peaks at 450 and 560 nm, which can be ascribed to defects emission in SiO₂ and ZnO respectively. The mechanism of light emission from Mn²⁺, the effect of varying the concentration on the PL intensity, and the effect of annealing are discussed.     

Formation of aligned silicon-nanowire on silicon in aqueous HF/(AgNO3 + Na2S2O8) solution

Highly oriented silicon nanowire (SiNW) layer was fabricated by etching Si substrate in HF/(AgNO₃ + Na₂S₂O₈) solution at 50 °C. The morphology and the photoluminescence (PL) of the etched layer as a function of Na₂S₂O₈ concentration were studied. The SiNW layers formed on silicon were investigated by scanning electron microscopy (SEM) and energy-dispersive X-ray (EDX). It was demonstrated that the morphology of the etched layers depends on the Na₂S₂O₈ concentration. Room-temperature photoluminescence (PL) from etched layer was observed. It was found that the utilisation of Na₂S₂O₈ decreases PL peak intensity. Finally, a discussion on the formation process of the silicon nanowires is presented.     

Pulsed plasma ion source to create Si nanocrystals in SiO2 substrates

A pulsed KrF excimer laser of irradiance of about 10⁸ W/cm² was utilized to synthesize Si nanocrystals on SiO₂/Si substrates. The results were compared with that ones obtained by applying low bias voltage to Si(1 0 0) target in order to control the kinetic energy of plasma ions. Glancing incidence X-ray diffraction spectra indicate the presence of silicon crystalline phases, i.e. (1 1 1) and (2 2 0), on SiO₂/Si substrates. The average Si nanocrystal size was estimated to be about 45 nm by using the Debye-Scherrer formula. Scanning electron microscopy and atomic force microscopy images showed the presence of nanoparticles of different size and shape. Their distribution exhibits a maximum concentration at 49 nm and a fraction of 14% at 15 nm.     

Multilayer Bi1.5Zn1.0Nb1.5O7/Ba0.6Sr0.4TiO3/Bi1.5Zn1.0Nb1.5O7 thin films for tunable microwave applications

Bi_1.5Zn_1.0Nb_1.5O₇/Ba_0.6Sr_0.4TiO₃/Bi_1.5Zn_1.0Nb_1.5O₇ tunable multilayer thin film has been fabricated by pulsed laser ablation and characterized. Phase composition and microstructure of multilayer films were characterized by X-ray diffraction, scanning electron microscopy (SEM) and atomic force microscopy (AFM). The film has very smooth surface with RMS roughness of 1.5-2 nm and grain size of 100-150 nm. Total film thickness has been measure to be 375 nm. The BZN thin films at 300 K, on Pt(1 1 1)/SiO₂/Si substrate showed zero-field dielectric constant of 105 and dielectric loss tangent of 0.002 at frequency of 0.1 MHz. Thin films annealed at 700 °C shows the dielectric tunability of 18% with biasing field 500 kV/cm at 0.1 MHz. The multilayer thin film shows nonferroelectric behavior at room temperature. The good physical and electrical properties of multilayer thin films make them promising candidate for tunable microwave device applications.     

In situ transmission electron microscopy study of the nucleation and grain growth of Ge2Sb2Te5 thin films

The nucleation and grain growth of the Ge₂Sb₂Te₅ (GST) thin films were studied using high voltage electron microscope operated at 1250 kV. As a result, we have found that 2 nm-sized nucleus forms as a cluster which atoms are arranged regularly at the stage of nucleation prior to the formation of grains having crystal structure. The high-resolution transmission electron microscopy study and fast-Fourier transformations revealed that coexistence of face-centered-cubic (FCC) and hexagonal structure occurs, and formation of twin defect is found in the hexagonal structure during the grain growth as the annealing temperature is increased. GST grain having the hexagonal structure grow from the surface, and the growth proceeded perpendicular to the [0 0 0 1], namely the path parallel to the (0 0 0 1) plane. Consequently, grain growth to a large-scale result in a lengthened shape.     

Disorder-order phase transition induced by size effect in bulk La2/3Sr1/3MnO3

Bulk La_2/3Sr_1/3MnO₃ ceramic samples prepared by thermal decomposition are investigated using transmission electron microscopy (TEM) and high-resolution transmission electron microscopy (HRTEM). An abnormal phenomenon, where three kinds of La_2/3Sr_1/3MnO₃ phases with different structures and the same composition coexist in the same grain, has been observed. Besides the stable rhombohedral majority phase, the two other phases are a simple cubic structure with a=0.389 nm and a new hexagonal structure with a=0.544 nm, c=0.668 nm. The simple cubic phase is a residual phase of high-temperature due to the size effect and bondage of twin boundary. Image simulations have suggested that the new hexagonal phase is the La-Sr ordered structure with space group , which is converted from the disordered simple cubic phase. The formation mechanism of the ordered phase is explained from volume energy and interface energy considerations.     

Enhanced emission of Er from alternately Er doped Si-rich Al2O3 multilayer film with Si nanocrystals as broadband sensitizers

Alternately Er doped Si-rich Al₂O₃ (Er:SRA) multilayer film, consisting of alternate Er-Si-codoped Al₂O₃ (Er:Si:Al₂O₃) and Si-doped Al₂O₃ (Si:Al₂O₃) sublayers, has been synthesized by co-sputtering from separated Er, Si, and Al₂O₃ targets. The dependence of Er³⁺ related photoluminescence (PL) properties on annealing temperatures over 700-1100 °C was studied. The maximum intensity of Er³⁺ PL, about 10 times higher than that of the monolayer film, was obtained from the multilayer film annealed at 950 °C. The enhancement of Er³⁺ PL intensity is attributed to the energy transfer from the silicon nanocrystals in the Si:Al₂O₃ sublayers to the neighboring Er³⁺ ions in the Er:Si:Al₂O₃ sublayers. The PL intensity exhibits a nonmonotonic temperature dependence: with increasing temperature, the integrated intensity almost remains constant from 14 to 50 K, then reaches maximum at 225 K, and slightly increases again at higher temperatures. Meanwhile, the PL integrated intensity at room temperature is about 30% higher than that at 14 K.     

Laser-induced forward transfer technique for maskless patterning of amorphous V2O5 thin film

A laser-induced forward transfer technique has been applied for the maskless patterning of amorphous V₂O₅ thin films. A sheet beam of a frequency doubled (SHG) Q-switched Nd:YAG laser was irradiated on a transparent glass substrate (donor), the rear surface of which was pre-coated with a vacuum-deposited V₂O₅ 180 nm thick film was either in direct contact with a second glass substrate (receiver) or a 0.14 mm air-gap was maintained between the donor film and the receiving substrate. Clear, regular stripe pattern of the laser-induced transferred film was obtained on the receiver. The pattern was characterized using X-ray diffraction (XRD), optical absorption spectroscopy, scanning electron microscopy (SEM), energy dispersive analysis of X-ray (EDAX), atomic force microscopy (AFM), etc.     

Morphological and structural characterizations of CrSi2 nanometric films deposited by laser ablation

The structure and morphology of chromium disilicide (CrSi₂) nanometric films grown on 〈1 0 0〉 silicon substrates both at room temperature (RT) and at 740 K by pulsed laser ablation are reported. A pure CrSi₂ crystal target was ablated with a KrF excimer laser in vacuum (∼3 × 10⁻⁵ Pa). Morphological and structural properties of the deposited films were investigated using Rutherford backscattering spectrometry (RBS), grazing incidence X-ray diffraction (GID), X-ray reflectivity (XRR), scanning (SEM) and transmission electron microscopy (TEM). From RBS analysis, the films’ thickness resulted of ∼40 nm. This value is in agreement with the value obtained from XRR and TEM analysis (∼42 and ∼38 nm, respectively). The films’ composition, as inferred from Rutherford Universal Manipulation Program simulation of experimental spectra, is close to stoichiometric CrSi₂. GID analysis showed that the film deposited at 740 K is composed only by the CrSi₂ phase. The RT deposited sample is amorphous, while GID and TEM analyses evidenced that the film deposited at 740 K is poorly crystallised. The RT deposited film exhibited a metallic behaviour, while that one deposited at 740 K showed a semiconductor behaviour down to 227 K.     

A comparative study of the physical properties of Sb2S3 thin films treated with N2 AC plasma and thermal annealing in N2

As-deposited antimony sulfide thin films prepared by chemical bath deposition were treated with nitrogen AC plasma and thermal annealing in nitrogen atmosphere. The as-deposited, plasma treated, and thermally annealed antimony sulfide thin films have been characterized by X-ray diffraction (XRD), energy dispersive X-ray spectroscopy, scanning electron microscopy, atomic force microscopy, UV-vis spectroscopy, and electrical measurements. The results have shown that post-deposition treatments modify the crystalline structure, the morphology, and the optoelectronic properties of Sb₂S₃ thin films. X-ray diffraction studies showed that the crystallinity of the films was improved in both cases. Atomic force microscopy studies showed that the change in the film morphology depends on the post-deposition treatment used. Optical emission spectroscopy (OES) analysis revealed the plasma etching on the surface of the film, this fact was corroborated by the energy dispersive X-ray spectroscopy analysis. The optical band gap of the films (E_g) decreased after post-deposition treatments (from 2.36 to 1.75 eV) due to the improvement in the grain sizes. The electrical resistivity of the Sb₂S₃ thin films decreased from 10⁸ to 10⁶ Ω-cm after plasma treatments.