Behavior of GeSbTeBi phase-change optical recording media under subnanosecond pulsed laser irradiation

We investigated the variations in reflectivity during the phase transition between amorphous and crystalline states of a Bi-doped GeTe-Sb2Te3 pseudobinary compound film with subnanosecond laser pulses, using a pump-and-probe technique. We also used a two-laser static tester to estimate the onset time of crystallization under 2.0-micros pulse excitation. Experimental results indicate that the formation of a melt-quenched amorphous mark is completed in approximately 1 ns, but that crystalline mark formation on an as-deposited amorphous region requires several hundred nanoseconds. Simple arguments based on heat diffusion are used to explain the time scale of amorphization and the threshold for creation of a burned-out hole in the phase-change film.     

Crystallization studies on phase-change optical recording media by use of a two-dimensional periodic mark array

We present the results of crystallization studies in thin-film samples of amorphous and crystalline Ge(x)Sb(y)Te(z). The experiments, conducted at moderately elevated temperatures, are based on measurements of the first-order diffraction efficiency from a two-dimensional periodic array of recorded marks. When the samples are slowly heated above room temperature, changes in the efficiencies of various diffracted orders give information about the on-going crystallization process within the sample. Two different compositions of the GeSbTe alloy are used in these experiments. Measurements on Ge(2)Sb(2.3)Te(5) films show crystallization dominated by nucleation. For the Sb-rich eutectic composition Ge-(SbTe), crystallization is found to be dominated by growth from crystalline boundaries. We also show that crystalline marks written by relatively high-power laser pulses are different in their optical properties from the regions crystallized by slow heating of the sample to moderate temperatures.     

Large area crystallization of amorphous Si with overlapping high repetition rate laser pulses

This paper presents a pulsed laser crystallization technique, enabling large area crystallization of amorphous Si to produce grains having well-defined size and orientation. The method is developed by first determining the parameters influencing crystallization induced by single laser pulses of circular cross-sectional profile. In a second step, crystallization by overlapping round spots is examined. The experiments reveal three zones characterized by distinctly different crystallized morphologies following the laser irradiation. One of these zones corresponds to the regime of lateral crystal growth, wherein grains are driven towards the center of the spot by the radial temperature gradient. These findings are then applied to processing via line beam profiles that facilitate large area crystallization upon rapid translation of the specimen. Crystallization of extended areas hinges on the determination of the crystal growth length for a single spot. The pitch between successive pulses is then set on the basis of this information. It is shown that the pulse energy has only a weak effect on the crystal growth length.     

Amorphization induced by subnanosecond laser pulses in phase-change optical recording media

We have investigated the dynamics of amorphization induced in phase-change optical recording media by focused laser pulses of subnanosecond duration. We initiated localized amorphism by using a focused laser beam to melt the phase-change material and completed the change by rapid cooling by means of thermal diffusion. These studies were conducted by use of real-time reflectivity measurements with a pump-and-probe technique in which both pump and probe pulses had a duration of approximately 510 ps. Our transient-reflectivity measurements indicate that the process that leads to amorphism has three distinct stages, namely, rapid melting, solidification, and slow relaxation.     

Crystallization and amorphization studies of a Ge(2)Sb(2.3)Te(5) thin-film sample under pulsed laser irradiation

We present the results of crystallization and amorphization studies on a thin-film sample of Ge(2)Sb(2.3)Te(5), encapsulated in a quadrilayer stack as in the media of phase-change optical disk data storage. The study was conducted on a two-laser static tester in which one laser, operating in pulsed mode, writes either amorphous marks on a crystalline film or crystalline marks on an amorphous film. The second laser, operating at low power in the cw mode, simultaneously monitors the progress of mark formation in terms of the variations of reflectivity both during the write pulse and in the subsequent cooling period. In addition to investigating some of the expected features associated with crystallization and amorphization, we noted certain curious phenomena during the mark-formation process. For example, at low-power pulsed illumination, which is insufficient to trigger the phase transition, there is a slight change in the reflectivity of the sample. This is believed to be caused by a reversible change in the complex refractive index of the Ge(2)Sb(2.3)Te(5) film in the course of heating above the ambient temperature. We also observed that the mark-formation process may continue for as long as 1 mus beyond the end of the write laser pulse. This effect is especially pronounced during amorphous mark formation under high-power, long-pulse illumination.     

Crystallization behavior of Ge-doped eutectic Sb70Te30 films in optical disks

We report laser-induced crystallization behavior of binary Sb-Te and ternary Ge-doped eutectic Sb70Te30 thin film samples in a typical quadrilayer stack as used in phase-change optical disk data storage. Several experiments have been conducted on a two-laser static tester in which one laser operating in pulse mode writes crystalline marks on amorphous film or amorphous marks on crystalline film, while the second laser operating at low-power cw mode simultaneously monitors the progress of the crystalline or amorphous mark formation in real time in terms of the reflectivity variation. The results of this study show that the crystallization kinetics of this class of film is strongly growth dominant, which is significantly different from the crystallization kinetics of stochiometric Ge-Sb-Te compositions. In Sb-Te and Ge-doped eutectic Sb70Te30 thin-film samples, the crystallization behavior of the two forms of amorphous states, namely, as-deposited amorphous state and melt-quenched amorphous state, remains approximately same. We have also presented experiments showing the effect of the variation of the Sb/Te ratio and Ge doping on the crystallization behavior of these films.     

Modification of the structure and hydrogen content of amorphous hydrogenated silicon films under conditions of femtosecond laser-induced crystallization

We have studied the Raman spectra of initially amorphous hydrogenated silicon (a-Si:H) films upon their exposure to femtosecond laser-radiation pulses with the fluence varied within 30–155 mJ/cm². The distribution of the volume fraction of a crystalline phase over the surface of processed films is determined for the first time and a correlation is established between changes in this value and the hydrogen content in a-Si:H films upon the crystallization induced by femtosecond laser radiation.     

The dynamics of annealing of ion-amorphized silicon by nanosecond pulses of excimer laser UV radiation

Phase transitions in ion-amorphized silicon annealed by nanosecond UV radiation pulses of an ArF excimer laser were studied by time-resolved reflectivity measurements at λ=633 nm. It was established that epitaxial crystallization of a melted layer of silicon takes place at a laser energy density of W < 0.8 J/cm². At 0.2 J/cm² < W < 0.7 J/cm², silicon exhibits amorphization in the course of solidification, the initial and final amorphous phases being different. This amorphization of solidifying silicon is accompanied by the nucleation of separate crystallization centers. The presence of such centers changes the kinetics of phase transformations in the course of repeated laser action, leading to the formation of a polycrystalline structure, and provides for the possibility of obtaining intermediate crystallization states of Si in a sequence of laser-induced phase transitions.     

LASER INDUCED CRYSTALLIZATION OF AMORPHOUS Se80Te20 ALLOY THIN FILMS

The present study is concerned with the laser induced crystallization of amorphous thin films of Se₈₀Te₂₀ alloy. The films were prepared on a glass substrate by vacuum evaporation from bulk Se₈₀Te₂₀ alloy. The as-grown films were amorphous. The crystallization induced by an argon ion laser irradiation was studied at different beam intensities ranging from 50 mW to 600 mW and different time durations. The 486 nm (blue green) line was chosen for irradiation. The crystallization and growth processes in the laser irradiated samples were studied in the electron microscope at low temperature (173 K). it was seen that the crystallization was quicker at higher laser beam intensities as expected. The conditions for the onset of nucleation and the progress of crystallization in these films are compared with those observed in the films irradiated by electron beam.     

Microstructural investigation of quartz submitted to ultra-short shock loading

A high-energy pulsed laser was used to induce very short (2 ns) pressure pulses in quartz single crystals. The microstructure of recovered specimens was characterized by optical microscopy, scanning electron microscopy and transmission electron microscopy. Whatever the peak pressures (20–90 GPa), the shocked materials showed no shock defects (amorphous lamellae, Brazil twins, etc.). The microstructure was dominated by fracturing. The present study thus suggests that for very short pulse durations, quartz can be loaded at pressures well above the Hugoniot elastic limit without undergoing solid-state amorphization. The behaviour of quartz is purely elastic-brittle.     

聚焦脉冲激光作用下Ge2Sb2Te5薄膜晶化过程及机理

采用聚焦脉冲激光研究了Ge2Sb2Te5薄膜在沉积和激光淬火两种非晶态下反射率与激光脉冲宽度变化的关系，发现沉积态的Ge2Sb2Te5薄膜在晶化触发阶段内的反射率随激光脉冲宽度增加而减小，经过激光淬火的非晶态Ge2Sb2Te5薄膜在晶化触发阶段内的反射率随激光脉冲宽度增加而变化平缓。本文借用气－液体系中过饱和度分析液滴形成的原理，从统计物理学角度详细研究了两种非晶态Ge2Sb2Te5薄膜在脉冲激光作用下的晶化过程及机理，结果表明，当Ge2Sb2Te5的非晶态程度处于未饱和或饱和状态时不形成晶核；当Ge2Sb2Te5的非晶态程度处于过饱和状态时，此时的Ge2Sb2Te5为亚稳态，可能形成大小不等的晶核，但只有半径大于临界晶核尺寸时才可能长大成晶粒，而应力降低晶化能垒，增加非晶态Ge2Sb2Te5的过饱和度是导致沉积态与激光淬火态的Ge2Sb2Te5薄膜在晶化触发阶段内反射率随激光脉冲宽度变化规律不一致的根本原因，并据此解释了Ge2Sb2Te5薄膜在这两种状态下的反射率随激光脉冲宽度的变化特点及规律。     

Formulation of tablets containing an 'in-process' amorphized active pharmaceutical ingredient

The aim of this work was a preliminary study of the "in-process" amorphization of clopidogrel hydrogensulfate (CLP) as model drug during the production of tablets as dosage form. A solvent method was used for amorphization and the crystalline phase of CLP was detected by differential scanning calorimetry; the physical parameters of fresh and stored tablets were investigated. For the amorphous form, Aerosil 200 was selected as crystallization inhibitor as the most suitable of eight auxiliary agents. The optimum composition of the product for amorphization in the scaling-up process (100-fold) was 7 parts of CLP to 3 parts of Aerosil 200. In this scaled-up product, the amorphous CLP was fixed on the surface of microcrystalline cellulose. The tablet form further stabilized the amorphous form. Finally, the steps of an "in-process" amorphization are given as a protocol, which can promote stabilization of an amorphized active pharmaceutical ingredient.     

Formulation of tablets containing an ‘in-process’ amorphized active pharmaceutical ingredient

The aim of this work was a preliminary study of the “in-process” amorphization of clopidogrel hydrogensulfate (CLP) as model drug during the production of tablets as dosage form. A solvent method was used for amorphization and the crystalline phase of CLP was detected by differential scanning calorimetry; the physical parameters of fresh and stored tablets were investigated. For the amorphous form, Aerosil 200 was selected as crystallization inhibitor as the most suitable of eight auxiliary agents. The optimum composition of the product for amorphization in the scaling-up process (100-fold) was 7 parts of CLP to 3 parts of Aerosil 200. In this scaled-up product, the amorphous CLP was fixed on the surface of microcrystalline cellulose. The tablet form further stabilized the amorphous form. Finally, the steps of an “in-process” amorphization are given as a protocol, which can promote stabilization of an amorphized active pharmaceutical ingredient.     

聚焦脉冲激光作用下Ge2Sb2Te5薄膜晶化过程及机理

采用聚焦脉冲激光研究了Ge₂Sb₂Te₅薄膜在沉积和激光淬火两种非晶态下反射率与激光脉冲宽度变化的关系,发现沉积态的Ge₂Sb₂Te₅薄膜在晶化触发阶段内的反射率随激光脉冲宽度增加而减小,经过激光淬火的非晶态Ge₂Sb₂Te₅薄膜在晶化触发阶段内的反射率随激光脉冲宽度增加而变化平缓.本文借用气-液体系中过饱和度分析液滴形成的原理,从统计物理学角度详细研究了两种非晶态Ge₂Sb₂Te₅薄膜在脉冲激光作用下的晶化过程及机理,结果表明,当Ge₂Sb₂Te₅的非晶态程度处于未饱和或饱和状态时不形成晶核;当Ge₂Sb₂Te₅的非晶态程度处于过饱和状态时,此时的Ge₂Sb₂Te₅为亚稳态,可能形成大小不等的晶核,但只有半径大于临界晶核尺寸时才可能长大成晶粒.而应力降低晶化能垒,增加非晶态Ge₂Sb₂Te₅的过饱和度是导致沉积态与激光淬火态的Ge₂Sb₂Te₅薄膜在晶化触发阶段内反射率随激光脉冲宽度变化规律不一致的根本原因,并据此解释了Ge₂Sb₂Te₅薄膜在这两种状态下的反射率随激光脉冲宽度的变化特点及规律.     

The nature of amorphization in crystalline systems

The conditions of the transition from the crystalline to amorphous state and the process of amorphization of crystalline systems under cold plastic deformation have been studied. Two concepts of crystalline system amorphization are considered. Fusion and amorphization in the solid state are analysed, particularly in terms of the thermodynamics of reversible processes of the transition from the crystalline to the amorphous state. The mechanism of amorphization of a crystalline alloy is considered when it undergoes deformation or low-temperature annealing. The emphasis is on the system of Fe-B alloys.     

LASER INDUCED MICROCRYSTALLIZATION OF BULK AMORPHOUS Ge15Se85-xTex

Bulk amorphous samples of Ge₁₅Se_85-xTe_x (x = 10,15,20,25) were prepared by a rapid quenching. X-ray diffraction analysis revealed that the as-grown samples were amorphous. In order to understand the laser induced changes, the samples were irradiated with Q-switched Nd: YAG laser pulses of various energy densities (2-50 mJ/cm²). These studies showed that low energy pulses (≤10 mJ/cm²) have no influence on the structure and the transport properties of the samples whereas energy pulses (≥ 10 mJ/cm²) resulted in microcrystallization of the samples. Electrical transport properties such as d.c. electrical conductivity and thermoelectric power were measured as a function of temperature (200 -350 K) and composition. Results were analysed in terms of Small polaron model and two carrier model respectively. The electrical conduction, interestingly, was observed as intrinsic in the entire temperature range of measurements for both as-grown and irradiated samples.     

Amorphization reaction during mechanical alloying: influence of the milling conditions

Amorphous Ni-Zr powders have been prepared by mechanical alloying of elemental crystalline powders. The glass-forming range has been determined in detail at different milling intensities. Depending on the milling conditions, at least partial crystallization of the formerly amorphous material can occur from 66 to 75 at% Ni, due to a temperature rise during milling at high intensity. In comparison with isothermal annealing experiments at various temperatures on completely amorphous powder, a relation between milling temperature and milling time is shown. This confirms the similarity of the amorphization process during mechanical alloying with the solid-state interdiffusion reaction in alternating crystalline multilayers.     

Stimulated structural changes of Se in nanolayered composite films

Amorphous selenium (a-Se) is the simplest model material for investigation of the well-known photoinduced structural and optical transformations in amorphous chalcogenides. Since a lot of parameters and characteristics of materials essentially change at nanoscale, we applied nanostructuring to a-Se in nanomultilayers, obtained by pulsed laser deposition. The enhancement of photo- and thermally-induced crystallization was observed in a-Se/aluminosilicate nanomultilayers due to the initially heterogeneous state of Se in such samples, in comparison with single a-Se layers.     

Polycarbonate surface cell's adhesion examination after Nd:YAG laser irradiation

Nd:YAG laser treatment was used in order to increase surface cell adhesion aspects of polycarbonate (PC) films prepared via melt process. The treatment was carried out under different wavelengths and beam diameters. ATR-FTIR and UV spectra obtained from different samples before and after laser treatment in air showed that laser irradiation has induced some chemical and physical changes in surface properties. The irradiated films were also characterized using scanning electron microscopy (SEM) and contact angle measurements. Effect of pulse numbers on the surface properties was also investigated. Cell culture test was used to evaluate cell adhesion property on the PC films before and after treatment. The results obtained from this test showed that after laser treatment, the cells were attached and proliferated extensively on the Nd:YAG laser treated films in comparison with the unmodified PC. Moreover, it was revealed that a decrease in the laser beam diameter and an increase in the irradiated pulse numbers increased surface wettability and caused a better cell attachment on the polymer surface.The obtained results also showed that a decrease in the laser beam diameter and an increase in the irradiated pulse numbers increased surface wettability and caused a better cell attachment on the polymer surface.     

Investigation of the phase formation wave in the model of solid state amorphization

Computation results of the model of solid state amorphization (SSA) based on a general approach to non-equilibrium phase transitions are reported. The model takes into account the mutual interaction of the structural elements of the amorphous phase via a deformation field. For the experimental parameters, corresponding to semiconductors undergoing amorphization by high-pressure treatment, a family of self-sustaining autowave solutions in the form of a traveling front, a traveling pulse and a series of pulses associated with the traveling front was obtained. The relation of these solutions with the expected morphology of amorphous samples produced by SSA is discussed.