Structural investigations of laser-deposited Fe/Al multilayers

Fe/Al multilayers are prepared by crossed-beam pulsed laser deposition and investigated by Rutherford backscattering, conversion electron M?ssbauer spectroscopy, and transmission electron microscopy. The results are compared to purely ballistic simulations of the deposition process using the TRIDYN4.0 code. It is found that the intermixing of adjacent layers must be described in terms of ballistic mixing followed by chemical mixing. The phase formation in the transition layer between adjacent layers follows the non-equilibrium behavior of Fe/Al in analogy to investigations on mechanically alloyed and ion-beam-mixed Fe/Al. In Fe-rich areas a bcc solid solution is formed. In Al-rich environment an amorphous phase is observed. Received: 13 January 1999 / Accepted: 14 January 1999 / Published online: 7 April 1999     

Effect of Si-substrate heating during laser-induced B-doping

Substrate temperature has been studied as an experimental parameter, which inflences the outcome of Gas-Immersion Excimer-Laser Doping (GILD). By means of SPR, SEM and DCD, the difference of the doped samples kept at different initial temperature are discussed. It is found that substrate heating can reduce the defects induced by laser doping and improve the electrical properties of devices.     

Ion beam mixing of Al/Fe binary systems

Ion beam mixing of Al layers on Fe and Fe layers on Al are studied by irradiation with 200 keV Xe⁺-ions at room temperature as a function of the thickness of the top layer and of the ion fluence from 5×10¹⁵ to 7.5×10¹⁶ions/cm². Deconvolution procedures are needed to separate the influence of the ion sputter profiling by AES from the ion beam induced mixing effects. Auger electron spectroscopy data reveal that the mixing induced diffusivity ought to be considered as a function of concentration. The diffusion coefficients are evaluated by the Boltzmann-Matano method. A strong dependence of the diffusion coefficients and also the mixing efficiencies from the ion dose, the depth of the interface and the nuclear energy deposition were observed. Results are discussed in terms of the diffusional and collisional mixing as well as chemical affinity of both Fe and Al.     

Effect of Al content on the properties of Cr1−xAlxC films prepared by RF reactive magnetron sputtering

Cr_1−xAl_xC films were deposited on high-speed steel by RF reactive magnetron sputtering. In this study, we aimed to identify the effect of the Al content on the properties of Cr_1−xAl_xC films. We found that Cr_1−xAl_xC films exhibited a fine columnar grain microstructure with some special characteristics, such as high hardness of Hv 1426, a low friction coefficient of 0.29, and a large contact angle of 90° for x = 0.18. Furthermore, an increase in Al content resulted in a decrease in film hardness and an increase in contact angle. Moreover, on annealing at 923 K, the mechanical properties of the films improved and a dense protective film of complex Cr₂O₃ and Al₂O₃ oxides was formed on the surface for better wear resistance, which will ultimately increase the lifetime of the high-speed steel substrate.     

Swift ion irradiations of Fe/Fe/Si trilayers

We report here on changes in magnetism and microstructure when implanting, at 92 or 300 K, up to 5 × 10¹⁵ Au²⁶⁺-ions cm⁻² of 350 MeV into ^natFe(45 nm)/⁵⁷Fe(20 nm)/Si trilayers. This choice of ions and energy allowed to test the irradiation effects in the regime of pure electronic stopping. The samples were analysed before and after irradiation by Rutherford back-scattering spectroscopy, X-ray diffraction, conversion electron Mössbauer spectroscopy, and magneto-optical Kerr effect. Up to 1 × 10¹⁵ ions cm⁻², there was interface broadening at a mixing rate of Δσ²/Φ = 55(5) nm⁴, followed by full Fe-Si inter-diffusion. The Mössbauer spectra revealed fractions of α-Fe and amorphous ferromagnetic and paramagnetic iron silicides, but no crystalline Fe-Si phase. The magnetic remanence in the as-deposited Fe-layer showed small components of uniaxial and four-fold magnetization. For increasing ion fluence, the component with four-fold symmetry grew at the expense of the uniaxial component. For the highest fluences, an isotropic magnetization was found.     

Stress corrosion cracking behavior of Nd:YAG laser-treated aluminum alloy 7075

Nd-YAG laser surface treatment was conducted on 7075-T651 aluminum alloy with the aim of improving the stress corrosion cracking resistance of the alloy. Laser surface treatment was performed under two different gas environments, air and nitrogen. After the laser treatment, coarse constituent particles were removed and fine cellular/dendritic structures had formed. In addition, for the N₂-treated specimen, an AlN phase was detected. The results of the stress corrosion test showed that after 30 days of immersion, the untreated specimen had been severely attacked by corrosion, with intergranular cracks having formed along the planar grain boundaries of the specimen. For the air-treated specimen, some relatively long stress corrosion cracks and a small number of relatively large corrosion pits were found. The cracks mainly followed the interdendritic boundaries; the fusion boundary was found to be acting as an arrestor to corrosion attacks. In contrast, only few short stress corrosion cracks appeared in the N₂-treated specimen, indicating an improvement in corrosion initiation resistance. The superior corrosion resistance was attributed to the formation of the AlN phase in the surface of the laser-melted layer, which is an electrical insulator. The electrochemical impedance measurements taken during the stress corrosion test showed that the film resistance of the laser-treated specimens was always higher than that of the untreated specimen, with the N₂-treated specimen showing the highest resistance.     

Thermal annealing of a-Si:H/a-SiNx:H multilayers

The crystallinity of Si/SiN_x multilayers annealed by a rapid thermal process and furnace annealing is investigated by a Raman-scattering technique and transmission electron microscopy. It is found that the crystallization temperature varies from 900 °C to 1000 °C when the thickness of a-Si:H decreases from 4.0 nm to 2.0 nm. Raman measurements imply that the high crystallization temperature for the a-Si:H sublayers originates from the confinement modulated by the interfaces between a-Si:H and a-SiN_x:H. In addition to the annealing temperature, the thermal process also plays an important role in crystallization of a-Si sublayers. The a-Si:H sublayers thinner than 4.0 nm can not be crystallized by furnace annealing for 30 min, even when the annealing temperature is as high as 1000 °C. In contrast, rapid thermal annealing is advantageous for nucleation and crystallization. The origin of process-dependent crystallization in constrained a-Si:H is briefly discussed. Received: 11 April 2001 / Accepted: 20 June 2001 / Published online: 30 August 2001     

Structural ripple formation in Ge/Sb multilayers induced by laser irradiation

Thin multilayer films (Ge/Sb/Ge/Sb/Si substrate) have been irradiated with single nanosecond laser pulses (=193 nm). Real-Time Reflectivity (RTR) measurements have been used to follow the transformation in situ and cross-sectional transmission electron microscope analysis was used to study both the microstructure and the composition profile before and after irradiation. Melting and mixing are both found to nucleate at preferential sites in the upper Ge/Sb interface. During this process the film surface topography changes in a way not previously seen, and rippling of the film is observed due to lateral mass flow induced in the Sb layer underneath the surface, most probably arising from volume changes upon melting. For the highest irradiation energy densities, melting of the whole multilayer configuration takes place, the ripples are no longer observed, and following cooling and solidification, a mixed amorphous GeSb film is formed.     

Structural evolution and metastable phase formation in Ni-W multilayers upon ion irradiation

A crystal-to-amorphous structural transition was induced in the Ni₂₅W₇₅ and Ni₃₅W₆₅ multilayers by ion irradiation at room temperature. More interestingly, prior to complete amorphization, a sequential disordering of first Ni and then W crystalline lattices was observed in the Ni₂₅W₇₅ sample with increasing ion dose. Such sequence in disordering is attributed to the difference in melting points between the two constituent metals. In another two multilayered samples with overall compositions of Ni₆₀W₄₀ and Ni₇₈Nb₂₂, ion irradiation under similar conditions resulted in the formation of two Ni-based fcc solid solutions, respectively. In comparison, the same Ni-based fcc solid solution was formed in the Ni₃₅W₆₅ multilayered sample upon solid-state reaction at 500 °C. Solid-state reaction at 550 °C resulted in the formation of a new W-rich metastable hcp phase in the Ni₂₅W₇₅ multilayered sample and the bcc–hcp transition was thought to be realized through a shearing mechanism. A Gibbs free-energy diagram, including the free-energy curves of the newly formed metastable crystalline phases, of the Ni-W system was calculated based on Miedema’s model and it can give a reasonable explanation of the observed sequential disordering. The calculated results also showed that the free-energy difference between the amorphous and metastable crystalline phases was quite small, leading to a situation that the phase selection, namely which phase was more favored to be formed eventually than its competitors, was influenced or even determined by the kinetics involved in the respective processes. Besides, the growth kinetics of the MX phases was also discussed. Received: 26 January 1999 / Accepted: 8 March 1999 / Published online: 14 June 1999     

Effective biaxial modulus and strain energy density of ideally (h k l)-fiber-textured cubic polycrystalline films

The effective biaxial modulus (M_eff) and strain energy density (W) of cubic polycrystalline films with ideally (h k l) fiber textures are estimated using Vook-Witt (VW) grain interaction model and the data are compared with those derived from Voigt, Reuss and Voigt-Reuss-Hill (VRH) models. Numerical results show that the VW average of M_eff for ideally (1 0 0)- or (1 1 1)-fiber-textured films is identical to the VRH average of M_eff. For (1 1 0) and (1 1 2) planes, however, the VW average of M_eff for (1 1 0)-fiber-textured film is larger than that of (1 1 2)-fiber-textured film when the Zener anisotropic factor (A_R) is not equal to 1. Furthermore, M_eff and W exhibit incremental tendencies with the increase of the orientation factor (Γ_h k l) for the [h k l] axis when A_R > 1, implying that M_eff and W have the minimums on the (1 0 0) plane. Reversely, M_eff and W decrease with the increasing Γ_h k l when A_R < 1. This means that M_eff and W on (1 1 1) plane have the minimums.     

Phase explosion induced by high-repetition rate pulsed laser

The characteristics and mechanisms of the damage to absorbing glass with high-repetition laser pulses (several kHz) are discussed. The results show that: (1) in the range of comparatively low-repetition rate, the damage is characterized by material melting and a small crater on the surface of substrate; (2) with the increase in repetition rate, a bigger and deeper crater is surrounded by re-deposition and crystalline granules originating from the cooling of vapor; and (3) the crater, surrounded by evaporation and an large number of solid particulates which is obviously the characters of phase explosion, becomes even bigger and deeper when the repetition rate is further increased. We modeled the temperature distribution in different repetition rate regime and found that heat accumulation plays a significant role in damage process. Because of the temperature dependence of damage mechanism, the temperature of the area irradiated by laser beam will ramp up with increasing the repetition rate, which triggers the melting and evaporation of dielectrics and phase explosion successively. Our results may benefit the understanding of laser-induced damage in optical materials.     

Thermally induced changes in magnetic, transport and electronic properties of Fe/Al multilayers

The effect of thermal annealing on the magnetic, transport and electronic properties of electron beam evaporated Fe/Al multilayer samples (MLS), with an overall atomic concentration ratio of Fe/Al 1:1, have been investigated. The grazing incidence X-ray diffraction, resistivity and valance band photoemission measurements indicates the formation of sub-stoichiometric B2 FeAl intermetallic phase at the interface for the MLS annealed at higher temperatures. The corresponding magnetization measurements show large increase in coercivity and drastic reduction in magnetization values. The observed magnetization behaviour in each case is interpreted in terms of their structural and electronic properties changes induced due to the annealing treatment.     

Probe-beam deflection diagnostics of shock waves generated during laser drilling

A probe-beam deflection technique was employed to investigate the evolution of shock waves generated during drilling processes of optical materials by a high repetition rate copper vapor laser. Experimental observations were analyzed by using a theoretical model of shock wave expansion which also furnished quantitative information on the main physical functions associated to laser-induced acoustic phenomena.     

Structural evolution of nanocrystalline/amorphous Fe/Ni75B25 multilayers: temperature dependence of electrical resistivity

X-ray specular-reflectivity measurements have been carried out on nanocrystalline/amorphous Fe/Ni₇₅B₂₅ multilayer films which were sputter-deposited on Si substrates, to investigate the evolution of interface roughness and the correlation between structure and transport properties. A significant interface roughness correlation with increasing Fe/NiB layer repetition was observed. The investigated films indicated a temperature dependent high electrical resistivity—10⁴ μΩ-cm at 10 K and 10³ μΩ-cm at 300 K—with a semiconductor-metal transition like behavior. Selected area electron diffraction revealed the presence of crystalline bcc Fe phase and NiB in amorphous state. The structural and transport properties of the multilayers are discussed.     

Structural and magnetic properties of La/Fe multilayers

The structural and magnetic properties of La/Fe multilayers were investigated by X-ray diffraction, RHEED, magnetometry and⁵⁷Fe Mössbauer spectroscopy. Comparison is made with previous results obtained for Ce/Fe multilayers. Remarkably sharp interfaces are found, with roughness between 2 and 2.5 Å. The magnetic interface in the Fe sublayers resulting from the distribution of magnetic hyperfine fields distinctly exceeds the extension of the structural interface and points to a magnetic proximity effect. This is discussed in relation to a strong 3d-5d hybridization recently found in measurements of magnetic circular X-ray dichroism. Both the structural and magnetic La/Fe interface is less extended than the interface in Ce/Fe multilayers. Below a thickness of about 25 Å, the individual Fe layers grow in an amorphous structure on the La layers. In this case, Curie temperatures are below 200 K and the Fe-layer saturation magnetization is reduced up to 50%, and there is evidence of a non-collinear spin structure. It is argued that this mainly reflects the properties of pure amorphous Fe.     

Atomic mixing of Ni2O3/SiO2, NiO/SiO2, and Ni/SiO2 interfaces induced by swift heavy ion irradiation

We have investigated the interface mixing of Ni₂O₃/SiO₂, NiO/SiO₂, and Ni/SiO₂ induced by the irradiation with Ar, Kr and Xe ions of energies ranging from 90 MeV to 260 MeV. Since these energies are in the electronic stopping regime, atomic transport processes will not be directly initiated by elastic ion–target collisions, but need to be excited by secondary processes like electron–phonon coupling or Coulomb explosion. Nevertheless, we have observed a strong mixing effect in the ceramic systems if the electronic energy loss exceeds a certain threshold value. Estimation of an effective diffusion constant indicates that diffusion takes place in the molten ion track. In contrast to the ceramics, the metallic Ni layer is still insensitive even for the highest electronic stopping power used (S_e=28 keV/nm) and does not exhibit mixing with its SiO₂ substrate. In addition, NiO/SiO₂ and Ni/SiO₂ were irradiated in the nuclear stopping regime with 600 keV Kr and 900 keV Xe–ions. Here the intermixing effect is in good agreement with the assumption of ballistic atomic transport. Received: 5 February 2002 / Accepted: 11 February 2002 / Published online: 3 May 2002 RID="*" ID="*"Corresponding author. Fax: +49-711/685-3866, E-mail: bolse@ifs.physik.uni-stuttgart.de     

Effect of Bi surfactant on the heteroepitaxial growth in Fe/Cr(100) multilayers

This study was to investigate the surfactant effect of Bi on the heteroepitaxial growth of Fe/Cr(100) multilayers by reflection high-energy electron diffraction (RHEED) measurements. With predeposition of submonolayer Bi on Fe(100) prior to evaporation of Fe/Cr multilayer, more long-lasting RHEED intensity oscillations were observed. This implies that the layer-by-layer growth of Fe/Cr multilayer is enhanced. The observations of grazing incidence X-ray reflectivity confirmed that the interface structures of Fe/Cr multilayer with Bi were sharper than that of multilayer without Bi. The study was also to investigate the magnetotransport properties between Bi surfactant-mediated multilayers and normal ones. The magnetoresistance (MR) ratio of the multilayers was enhanced by predeposition of Bi.     

Ion irradiation induced Al-Ti interaction in nano-scaled Al/Ti multilayers

Interactions induced in Al/Ti multilayers by implantation of Ar ions at room temperature were investgated. Initial structures consisted of (Al/Ti) × 5 multilayers deposited by d.c. ion sputtering on Si(1 0 0) wafers, to a total thickness of ∼250 nm. They were irradiated with 200 keV Ar⁺ ions, to the fluences from 5 × 10¹⁵ to 4 × 10¹⁶ ions/cm². It was found that ion irradiation induced a progressed intermixing of the multilayer constituents and Al-Ti nanoalloying for the highest applied fluence. The resulting nanocrystalline structure had a graded composition with non-reacted or interdiffused Al and Ti, and γ-AlTi and AlTi₃ intermetallic phases. Most intense reactivity was observed around mid depth of the multilayers, where most energy was deposited by the impact ions. It is presumed that Al-Ti chemical reaction is triggered by thermal spikes and further enhanced by chemical driving forces. The applied processing can be interesting for fabrication of tightly bond multilayered structures with gradual changes of their composition and properties.     

The formation of intermetallic phases by solid-phase reaction of Fe/Al multilayers

Thin film multilayers of Fe and Al with thicknesses ranging from 10 nm/2 nm to 10 nm/420 nm Fe/Al are used as starting structures to produce intermetallic phases by solid-phase reaction during high-vacuum thermal annealings. By measuring the relative concentrations of the reacting Fe and Al species nearby the growing interfaces and using the recently introduced concept of effective heat of mixing of binary thin-film metallic systems, a method is suggested to predict the phases to be obtained from different combinations of initial multilayer thickness and annealing temperature.     

Free energies of steps on (111) fcc surfaces

For a hexagonal two-dimensional lattice we derive, using a surprisingly simple route, exact expressions for the step free energies along the high symmetry directions, 〈1-10〉 and 〈11-2〉. If we consider only nearest-neighbor interactions, ε, and ignore step overhangs the step free energy vanishes at a temperature . In a more sophisticated model that incorporates step overhangs we find a reduction of T_R to about 0.87ε/k_b. The obtained step free energy expressions are also valid for the free energy of walls between two regions of opposite spins of the triangular 2D Ising system.