Growth and characterization of β-SiC films obtained by fs laser ablation

We achieved the growth of cubic silicon carbide (SiC) films on (1 0 0)Si substrates by pulsed laser deposition (PLD) at moderate temperatures such as 750 °C, from a SiC target in vacuum. The as-deposited films are morphologically and structurally characterized by scanning electron microscopy (SEM), conventional and high-resolution transmission electron microscopy (TEM/HRTEM). The morphology of deposited films is dominated by columns nucleated from a thin nanostructured beta silicon carbide (β-SiC) interface layer. The combined effects of columnar growth, tilted facets of the emerging columns and the presence of particulates on the film surface, lead to a rather rough surface of the films.     

Study on crystalline to amorphous structure transition of Cr coatings by magnetron sputtering

The influence of deposition rate on crystalline to amorphous microstructure transition of Cr coatings was studied through preparation of Cr coatings deposited onto silicon wafers using magnetron sputtering technique. The microstructure and morphology of Cr coatings were characterized by scanning electron microscopy (SEM), X-ray diffraction (XRD) and transmission electron microscopy (TEM). Results show that Cr coating prepared at 400 W exhibits dense columnar crystalline structure and the crystallite size and crystallization rate are increased expressly in the initial 5 min. When the deposition rate achieved to the maximum, Cr coating shows a case of infinite periodic renucleation where new crystals are assumed to be nucleated periodically on the surfaces of growing crystals and strong persistence of the columnar growth morphology is apparent. However, Cr coating exhibits overall microstructure of amorphous phase mixed with a few nano-crystal grains as the deposition rate decreases to the minimum.     

Crystallization and surface morphology evolution of erbium fluoride films on different substrates

Erbium fluoride (ErF₃) films were thermally deposited on Ge(1 1 1), Si(0 0 1) and copper mesh grid with different substrate temperature. X-ray diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM) were used to characterize the structure and morphology of the films. The structure of ErF₃ films deposited on germanium and silicon changed from amorphous to crystalline with increasing the substrate temperature, while the crystallization temperature of the films on silicon is higher than that of on germanium. The infrared optical properties of the films change greatly with the evolution of crystal structure. It is also found that the morphology of ErF₃ film on Ge(1 1 1) at 200 °C is modulated by the stress between the substrate and film. The SEM and TEM results confirmed that the ErF₃ films on copper mesh grid were crystalline even at 100 °C. Interestingly, the ErF₃ films show flower-like surface morphology when deposited on copper mesh at 200 °C. The crystallization temperature (T_c) of ErF₃ films on the three substrates has the relation which is which is induced by the wetting angle of ErF₃ films on different substrates.     

Crystallization of hydrogenated amorphous silicon carbon films with laser and thermal annealing

The crystallization of silicon rich hydrogenated amorphous silicon carbon films prepared by Plasma Enhanced Chemical Vapor Deposition technique has been induced by excimer laser annealing as well as thermal annealing. The excimer laser energy density (E_d) and the annealing temperature were varied from 123 to 242 mJ/cm² and from 250 to 1200 °C respectively. The effects of the two crystallization processes on the structural properties and bonding configurations of the films have been studied. The main results are that for the laser annealed samples, cubic SiC crystallites are formed for E_d ≥ 188 mJ/cm², while for the thermal annealed samples, micro-crystallites SiC and polycrystalline hexagonal SiC are observed for the annealing temperature of 800 and 1200 °C respectively. The crystallinity degree has been found to improve with the increase in the laser energy density as well as with the increase in the annealing temperature.     

TEM studies on the formation of nano crystallites of Si by metal induced crystallization

In the present investigations, we have grown the nano-crystallites of Si by metal induced crystallization process. Layers of two different metals (Al and Au) were deposited on either side of Si using thermal evaporation technique to study metal induced crystallization. Annealing of such samples was carried out in the hot stage of TEM. We have found that the crystallization of amorphous silicon starts at 150 °C through the formation of metal silicides. Formation of metal silicides was observed through selected area diffraction. Nearly complete formation of nano crystallites of Si throughout the sample was observed at 200 °C. High-resolution TEM studies confirm the formation of nano-crystallites of Si all along the film.     

Electrodeposition of CoWP film: V. Structural and morphological characterisations

CoWP films were electrochemically deposited on copper-coated silicon wafers from citrate electrolytes containing cobalt sulphate, sodium tungstate and sodium hypophosphite under various deposition conditions and characterisations of the films were carried out using various instrumental techniques. Composition analyses using XPS showed that the surfaces of the films contained large amounts of oxides and hydroxide of tungsten and cobalt, respectively. An AES depth-profile, however, revealed that the bulk of the films predominantly consisted of cobalt, tungsten and phosphorus. Microstructural analyses using XRD showed that, depending on the composition and/or deposition conditions, CoWP films could be amorphous, polycrystalline and crystalline with a strong preferred orientation. Amorphous films were obtained when deposited at higher applied potential and current density or the films contained high amount of phosphorus and/or tungsten, while films deposited by very low applied potential and current density were crystalline with a preferred orientation of [0 0 2] of hexagonal cobalt. SEM images showed that the films deposited from neutral or acidic baths at room temperature had typical spherical nodular structures, while the films deposited from basic solution or at elevated temperature had needle-like crystallites. The crystalline films were much rougher than the amorphous films.     

Structural characterization of AlN films synthesized by pulsed laser deposition

We obtained AlN thin films by pulsed laser deposition (PLD) from a polycrystalline AlN target using a pulsed KrF* excimer laser source (248 nm, 25 ns, intensity of ∼4 × 10⁸ W/cm², repetition rate 3 Hz, 10 J/cm² laser fluence). The target-Si substrate distance was 5 cm. Films were grown either in vacuum (10⁻⁴ Pa residual pressure) or in nitrogen at a dynamic pressure of 0.1 and 10 Pa, using a total of 20,000 subsequent pulses. The films structure was characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM) and spectral ellipsometry (SE). Our TEM and XRD studies showed a strong dependence of the film structure on the nitrogen content in the ambient gas. The films deposited in vacuum exhibited a high quality polycrystalline structure with a hexagonal phase. The crystallite growth proceeds along the c-axis, perpendicular to the substrate surface, resulting in a columnar and strongly textured structure. The films grown at low nitrogen pressure (0.1 Pa) were amorphous as seen by TEM and XRD, but SE data analysis revealed ∼1.7 vol.% crystallites embedded in the amorphous AlN matrix. Increasing the nitrogen pressure to 10 Pa promotes the formation of cubic (≤10 nm) crystallites as seen by TEM but their density was still low to be detected by XRD. SE data analysis confirmed the results obtained from the TEM and XRD observations.     

Structural and optical properties of low temperature synthesized Nanostructured BiFeO3 thin films

Nanostructured bismuth ferrite (BiFeO₃) thin films were deposited on glass substrate by the sol-gel process. The as-fired film at 250 °C was found to be amorphous crystallizing to pure rhombohedral phase after annealing at 450 °C for 2 h in air. The XRD pattern shows that the sample is polycrystalline in nature. The average grain size of the film calculated from the XRD data was found to be 16 nm. The as-fired film show high transmittance that decreases after crystallization. The absorption edge of the films was found to be sharper and shifting towards the lower energy as the annealing temperature increases. The optical energy band gaps of the amorphous and crystalline films were found to be 2.63 and 2.31 eV, respectively. The refractive indices of the amorphous and crystalline films were 2.05 and 2.26, respectively.     

Study of the growth of fullerene-carbonized epitaxial SiC thin films by synchrotron radiation

 Thin SiC films have been deposited on silicon(0 0 1) substrates by fullerene-carbonization. Using synchrotron radiation X-ray diffraction pole figure measurements have been employed in order to study the texture of the layers. It is qualitatively shown that the films contain epitaxially aligned β-SiC crystallites with the same orientation as the underlying substrate and their twins of first and second order. The orientational spread of the epitaxial crystallites in terms of tilt against and rotation around the substrate normal is smaller than 3°. The formation of twins as a growth defect plays a major role which is even more pronounced at a higher substrate temperature. Furthermore, an additional preferred orientation has been identified which can only be explained by a non-cubic SiC phase. The portion of these crystallites in the film can be considerably reduced by an increase of the deposition temperature. Received: 18 April 1996/Accepted: 12 August 1996     

Structural modification of laser annealed a-Si1−xCx:H films

Hydrogenated amorphous silicon carbon films, with relatively low hydrogen content and carbon fraction x, C/(C + Si), ranging from 0.20 to 0.57 have been deposited by RF-plasma enhanced chemical vapor deposition (PECVD) for excimer laser annealing experiments. After the laser treatments all the films show structural modifications. It has been obtained that with increasing x the crystallinity degree of the Si phase decreases, while that of the SiC phase increases and becomes predominant for x = 0.39. In the overstoichiometric samples only the c-SiC phase has been observed. In all the treated samples 3C-SiC crystallites have been detected.     

Laser annealing study of PECVD deposited hydrogenated amorphous silicon carbon alloy films

The influence of carbon content on the crystallization process has been investigated for the excimer laser annealed hydrogenated amorphous silicon carbon alloy films deposited by Plasma Enhanced Chemical Vapour Deposition (PECVD) technique, using silane methane gas mixture diluted in helium, as well as for the hydrogenated microcrystalline silicon carbon alloy films prepared by PECVD from silane methane gas mixture highly diluted in hydrogen, for comparison. The study demonstrates clearly that the increase in the carbon content prevents the crystallization process in the hydrogen diluted samples while the crystallization process is enhanced in the laser annealing of amorphous samples because of the increase in the absorbed laser energy density that occurs for the amorphous films with the higher carbon content. This, in turn, facilitates the crystallization for the laser annealed samples with higher carbon content, resulting in the formation of SiC crystallites along with Si crystallites.     

Synthesis of crystalline SiC nanofiber through the pyrolysis of polycarbomethylsilane coated platelet carbon nanofiber

SiC nanofiber with high crystallinity was synthesized through the pyrolysis of polycarbomethylsilane (PS) coated platelet carbon nanofiber (PCNF) over 700 °C and burning PCNF under the oxidative atmosphere. The as-prepared β-SiC nanofiber exhibited a diameter less than 100 nm and a medium surface area of 50 m²/g. The crystallinity of silicon carbide (SiC) nanofiber increases with increasing heat-treatment temperature, showing the formation of high crystalline SiC nanofiber at 1400 °C. PCNF can be used as a unique template to govern the shape, crystallinity and morphology of SiC.     

Amorphous to crystalline phase transition in pulsed laser deposited silicon carbide

SiC thin films were grown on Si (1 0 0) substrates by excimer laser ablation of a SiC target in vacuum. The effect of deposition temperature (up to 950 °C), post-deposition annealing and laser energy on the nanostructure, bonding and crystalline properties of the films was studied, in order to elucidate their transition from an amorphous to a crystalline phase. Infra-red spectroscopy shows that growth at temperatures greater than 600 °C produces layers with increasingly uniform environment of the Si-C bonds, while the appearance of large crystallites is detected, by X-ray diffraction, at 800 °C. Electron paramagnetic resonance confirms the presence of clustered paramagnetic centers within the sp² carbon domains. Increasing deposition temperature leads to a decrease of the spin density and to a temperature-dependent component of the EPR linewidth induced by spin hopping. For films grown below 650 °C, post-deposition annealing at 1100 °C reduces the spin density as a result of a more uniform Si-C nanostructure, though large scale crystallization is not observed. For greater deposition temperatures, annealing leads to little changes in the bonding properties, but suppresses the temperature dependent component of the EPR linewidth. These findings are explained by a relaxation of the stress in the layers, through the annealing of the bond angle disorder that inhibits spin hopping processes.     

Crystallisation of magnetron sputtered amorphous Si1− x C x films (x = 1/3) studied by grazing incidence X-ray diffractometry

The crystallisation of amorphous Si_{1? x} C _x films (x = 1/3) produced via magnetron sputtering on silicon substrates was investigated. Grazing incidence X-ray diffractometry was used to analyse the crystalline precipitates obtained after annealing at temperatures between 1200°C and 1350°C. After annealing times of 15 h at 1200°C and 15 h at 1350°C, crystallisation of SiC is complete. The average crystallite size, d, was determined using the Scherrer equation. The rate constants for the initial growth of the crystallites were determined by straight line fits in the d ? t diagrams (t being the annealing time), which obey the Arrhenius law. The activation enthalpy of 4.0 ± 0.7 eV is, within error limits, the same as that found for the growth of silicon carbide crystallites in magnetron sputtered Si_{1? x} C _x films (x = 1/2).     

Substrate-dependent structure, microstructure, composition and properties of nanostructured TiN films

Titanium nitride films of a thickness of ∼1.5 μm were deposited on amorphous and crystalline substrates by DC reactive magnetron sputtering at ambient temperature with 100% nitrogen in the sputter gas. The growth of nanostructured, i.e. crystalline nano-grain sized, films at ambient temperature is demonstrated. The microstructure of the films grown on crystalline substrates reveals a larger grain size/crystallite size than that of the films deposited on amorphous substrates. Specular reflectance measurements on films deposited on different substrates indicate that the position of the Ti-N 2s band at 2.33 eV is substrate-dependent, indicating substrate-mediated stoichiometry. This clearly demonstrates that not only structure and microstructure, but also chemical composition of the films is substrate-influenced. The films deposited on amorphous substrates display lower hardness and modulus values than the films deposited on crystalline substrates, with the highest value of hardness being 19 GPa on a lanthanum aluminate substrate.     

碳化硅薄膜脉冲激光晶化特性研究

采用XeCl准分子激光对非晶碳化硅(a-SiC)薄膜的脉冲激光晶化特性进行了研究.通过原子力显微镜（AFM）和Raman光谱技术对退火前后薄膜样品的形貌、结构及物相特性进行了分析.结果表明，选用合适的激光能量采用激光退火技术能够实现a-SiC薄膜的纳米晶化.退火薄膜中的纳米颗粒大小随着激光能量密度的增加而增大；Raman谱分析结果显示了退火后的薄膜的晶态结构特性并给出了伴随退火过程存在的物相分凝现象.根据以上结果并结合激光退火特性，对a-SiC的脉冲激光晶化机理进行了讨论. 关键词： 激光退火 晶化 碳化硅     

Atomic layer deposition of HfO2: Effect of structure development on growth rate, morphology and optical properties of thin films

HfO₂ films were grown by atomic layer deposition from HfCl₄ and H₂O on Si(1 0 0), Si(1 1 1) and amorphous SiO₂ substrates at 180-750 °C and the effect of deposition temperature and film thickness on the growth rate and optical properties of the film material was studied. Crystallization, texture development and surface roughening were demonstrated to result in a noticeable growth rate increase with increasing film thickness. Highest surface roughness values were determined for the films deposited at 350-450 °C on all substrates used. The density of the film material increased with the concentration of crystalline phase but, within experimental uncertainty, was independent of orientation and sizes of crystallites in polycrystalline films. Refractive index increased with the material density. In addition, the refractive index values that were calculated from the transmission spectra depended on the surface roughness and crystallite sizes because the light scattering, which directly influenced the extinction coefficient, caused also a decrease of the refractive index determined in this way.     

The influence of using different substrates on the structural and optical characteristics of ZnO thin films

ZnO thin films with thikness d = 100 nm were deposited onto different substrates such as glass, kapton, and silicon by radio frequency magnetron sputtering. The structural analyses of the films indicate they are polycrystalline and have a wurtzite (hexagonal) structure.The ZnO layer deposited on kapton substrate shows a stronger orientation of the crystallites with (0 0 2) plane parallel to the substrate surface, as compared with the other two samples of ZnO deposited on glass and silicon, respectively.All three layers have nanometer-scale values for roughness, namely 1.7 nm for ZnO/glass, 2.4 nm for ZnO/silicon, and 6.8 nm for ZnO/kapton. The higher value for the ZnO layer deposited on kapton substrate makes this sample suitable for solar cells applications. Transmission spectra of these thin films are strongly influenced by deposition conditions. With our deposition conditions the transparent conducting ZnO layer has a good transmission (78-88%) in VIS and NIR domains. The values of the energy gap calculated from the absorption spectra are 3.23 eV for ZnO sample deposited onto glass substrate and 3.30 eV for the ZnO sample deposited onto kapton polymer foil substrate. The influence of deposition arrangement and oxidation conditions on the structural, morphological, and optical properties of the ZnO films is discussed in the present paper.     

Effect of substrate temperature on gold-catalyzed silicon nanostructures growth by hot-wire chemical vapor deposition (HWCVD)

The effect of substrate temperature on the structural property of the silicon nanostructures deposited on gold-coated crystal silicon substrate by hot-wire chemical vapor deposition (HWCVD) was studied. The uniformity and size of the as-grown silicon nanostructures is highly influenced by the substrate temperature. XRD, Raman and HRTEM measurements show the silicon nanostructures consist of small crystallites embedded within amorphous matrix. The crystallite size of the as-grown silicon nanostructures decreases with increases in substrate temperature. FTIR shows that these silicon nanostructures are highly disordered for sample prepared at substrate temperature above 250 °C. The correlation of crystallinity and structure disorder of the silicon nanostructures growth at different substrate temperature was discussed.     

Characteristics of electron beam evaporated nanocrystalline SnO2 thin films annealed in air

Tin oxide (SnO₂) thin films (about 200 nm thick) have been deposited by electron beam evaporation followed by annealing in air at 350-550 °C for two hours. Optical, electrical and structural properties were studied as a function of annealing temperature. The as-deposited film is amorphous, while all other annealed films are crystalline (having tetragonal structure). XRD suggest that the films are composed of nanoparticles of 5-10 nm. Raman analysis and optical measurements suggest quantum confinement effects that are enhanced with annealing temperature. For instance, Raman peaks of the as-deposited films are blue-shifted as compared to those for bulk SnO₂. Blue shift becomes more pronounced with annealing temperature. Optical band gap energy of amorphous SnO₂ film is 3.61 eV, which increases to about 4.22 eV after crystallization. Two orders of magnitude decrease in resistivity is observed after annealing at 350-400 °C due to structural ordering and crystallization. The resistivity, however, increases slightly with annealing temperature above 400 °C, possibly due to improvement in stoichiometry and associated decrease in charge carrier density.