Study on structural properties of epitaxial silicon films on annealed double layer porous silicon

In this paper, epitaxial silicon films were grown on annealed double layer porous silicon by LPCVD. The evolvement of the double layer porous silicon before and after thermal annealing was investigated by scanning electron microscope. X-ray diffraction and Raman spectroscopy were used to investigate the structural properties of the epitaxial silicon thin films grown at different temperature and different pressure. The results show that the surface of the low-porosity layer becomes smooth and there are just few silicon-bridges connecting the porous layer and the substrate wafer. The qualities of the epitaxial silicon thin films become better along with increasing deposition temperature. All of the Raman peaks of silicon films with different deposition pressure are situated at 521 cm⁻¹ under the deposition temperature of 1100 °C, and the Raman intensity of the silicon film deposited at 100 Pa is much closer to that of the monocrystalline silicon wafer. The epitaxial silicon films are all (4 0 0)-oriented and (4 0 0) peak of silicon film deposited at 100 Pa is more symmetric.     

Macroporous fluoropolymeric films templated by silica colloidal assembly: A possible route to super-hydrophobic surfaces

A super-hydrophobic surface was obtained on a three-dimensional (3D) polyvinylidene fluoride (PVDF) macroporous film. The porous films were fabricated through self-assembled silica colloidal templates. The apparent water contact angle of the surface can be tuned from 106° to 153° through altering the sintering temperature and the diameter of the colloidal templates. A composite structure of micro-cavities and nanoholes on the PVDF surface was responsible for the super-hydrophobicity. The wettability of the porous surfaces was described by the use of the Cassie-Baxter model and Wenzel's equation.     

Effect of temperature on residual stress and mechanical properties of Ti films prepared by both ion implantation and ion beam assisted deposition

Ti films with a thickness of 1.6 μm (group A) and 4.6 μm (group B) were prepared on surface of silicon crystal by metal vapor vacuum arc (MEVVA) ion implantation combined with ion beam assisted deposition (IBAD). Different anneal temperatures ranging from 100 to 500 °C were used to investigate effect of temperature on residual stress and mechanical properties of the Ti films. X-ray diffraction (XRD) was used to measure residual stress of the Ti films. The morphology, depth profile, roughness, nanohardness, and modulus of the Ti films were measured by scanning electron microscopy (SEM), scanning Auger nanoprobe (SAN), atomic force microscopy (AFM), and nanoindentation, respectively. The experimental results suggest that residual stress was sensitive to film thickness and anneal temperature. The critical temperatures of the sample groups A and B that residual stress changed from compressive to tensile were 404 and 428 °C, respectively. The mean surface roughness and grain size of the annealed Ti films increased with increasing anneal temperature. The values of nanohardness and modulus of the Ti films reached their maximum values near the surface, then, reached corresponding values with increasing depth of the indentation. The mechanism of stress relaxation of the Ti films is discussed in terms of re-crystallization and difference of coefficient of thermal expansion between Ti film and Si substrate.     

Preparation and electroactive properties of a PVDF/nano-TiO2 composite film

In the present study, poly(vinylidene fluoride) (PVDF)/nano-TiO₂ electroactive film was prepared by coating a substrate with an acetone/DMF solution, which was evaporated at a high temperature (110 °C). The crystallisation behaviour, dynamic mechanical properties and electroactive properties of this PVDF/nano-TiO₂ electroactive film were investigated. The cross-section and surface of the film were observed with a scanning electron microscope (SEM). X-ray diffraction (XRD) results showed that the film containing the PVDF β phase, the desired ferroelectric phase, was obtained by crystallising the mixed solution of nano-TiO₂ and PVDF at 110 °C, while the film containing the α phase was obtained from the crystallisation of the pure PVDF solution at the same temperature. It was found that the storage modulus, the room-temperature dielectric constant and the electric breakdown strength of the composite films were much higher than those of a pure PVDF film. TiO₂ improved the mechanical properties and electroactive properties of the film. The results indicate that PVDF/nano-TiO₂ composite films can be applied to the fabrication of self-sensing actuator devices.     

Structural and mechanical characteristics of (1 0 3) AlN thin films prepared by radio frequency magnetron sputtering

The (1 0 3)-oriented aluminum nitride (AlN) thin film is an attractive piezoelectric material for the applications in surface acoustic wave and film bulk acoustic wave resonator devices. In this work, we repot structural and mechanical characteristics of (1 0 3) AlN thin films deposited onto (1 0 0) Si substrates with radio frequency magnetron sputtering at different sputtering powers at 150, 250, and 350 W. Comparisons were made on their crystalline structures with X-ray diffraction, surface morphologies with atomic force microscopy, mechanical properties with nanoindentation, and tribological responses with nanoscratch. Results indicate that for the sputtering power of 350 W, a high-quality (1 0 3) AlN thin film, whose hardness is 18.91 ± 1.03 GPa and Young's modulus is 242.26 ± 8.92 GPa, was obtained with the most compact surface condition.     

Synthesis of silicon carbide films by combined implantation with sputtering techniques

Silicon carbide (SiC) films were synthesized by combined metal vapor vacuum arc (MEVVA) ion implantation with ion beam assisted deposition (IBAD) techniques. Carbon ions with 40 keV energy were implanted into Si(1 0 0) substrates at ion fluence of 5 × 10¹⁶ ions/cm². Then silicon and carbon atoms were co-sputtered on the Si(1 0 0) substrate surface, at the same time the samples underwent assistant Ar-ion irradiation at 20 keV energy. A group of samples with substrate temperatures ranging from 400 to 600 °C were used to analyze the effect of temperature on formation of the SiC film. Influence of the assistant Ar-ion irradiation was also investigated. The structure, morphology and mechanical properties of the deposited films were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM) and nanoindentation, respectively. The bond configurations were obtained from IR absorption and Raman spectroscopy. The experimental results indicate that microcrystalline SiC films were synthesized at 600 °C. The substrate temperature and assistant Ar-ion irradiation played a key role in the process. The assistant Ar-ion irradiation also helps increasing the nanohardness and bulk modulus of the SiC films. The best values of nanohardness and bulk modulus were 24.1 and 282.6 GPa, respectively.     

Dielectric properties of anodic films on sputter-deposited Ti-Si porous columnar films

For electrolytic capacitor application of the single-phase Ti alloys containing supersaturated silicon, which form anodic oxide films with superior dielectric properties, porous Ti-7 at% Si columnar films, as well as Ti columnar films, have been prepared by oblique angle magnetron sputtering on to aluminum substrate with a concave cell structure to enhance the surface area and hence capacitance. The deposited films of both Ti and Ti-7 at% Si have isolated columnar morphology with each column revealing nanogranular texture. The distances between columns are ∼500 nm, corresponding to the cell size of the textured substrate and the gaps between columns are 100-200 nm. When the porous Ti-7 at% Si film is anodized at a constant current density in ammonium pentaborate electrolyte, the growth of a uniform amorphous oxide film continues to ∼35 V, while it is limited to less than 6 V on the porous Ti film. The maximum voltage of the growth of uniform amorphous oxide films on the Ti-7 at% Si films is similar for both the flat and porous columnar films, suggesting little influence of surface roughness on the amorphous-to-crystalline transition of growing anodic oxide under the high electric field. Due to the suppression of crystallization to sufficiently high voltages, the anodic oxide films formed on the porous Ti-7 at% Si film shows markedly improved dielectric properties, in comparison with those on the porous Ti film.     

Enhanced cell affinity of poly(l-lactide) film by immobilizing phosphonized chitosan

Graft polymerization of acrylic acid (AA) onto poly(l-lactide) (PLLA) film by UV irradiation was carried out to develop surfaces for N-methylene phosphonic chitosan (NMPC) immobilization. The properties of modified films were discussed by colorimetric method, attenuated total reflection-Fourier transform infrared spectroscopy (ATR-FTIR), contact angles, atomic force microscopy (AFM) and osteoblast incubation. The results showed that AA solution concentration and irradiation time had effect on the graft carboxyl densities. Comparing the ATR-FTIR images, two new peaks at 1561 cm⁻¹ and 1632 cm⁻¹ proved that NMPC was immobilized on the film surface successfully. The water contact-angles were decreased from 90 ± 5° to 37 ± 5° after modification. The AFM images indicated that the surface of the combined film was rougher than that of untreated film. The grafted film provided an excellent substrate for the growth of osteoblast.     

Influence of annealing temperature on the structural, optical and mechanical properties of ALD-derived ZnO thin films

ZnO thin films grown on Si(1 1 1) substrates by using atomic layer deposition (ALD) were annealed at the temperatures ranging from 300 to 500 °C. The X-ray diffraction (XRD) results show that the annealed ZnO thin films are highly (0 0 2)-oriented, indicating a well ordered microstructure. The film surface examined by the atomic force microscopy (AFM), however, indicated that the roughness increases with increasing annealing temperature. The photoluminescence (PL) spectrum showed that the intensity of UV emission was strongest for films annealed at 500 °C. The mechanical properties of the resultant ZnO thin films investigated by nanoindentation reveal that the hardness decreases from 9.2 GPa to 7.2 GPa for films annealed at 300 °C and 500 °C, respectively. On the other hand, the Young's modulus for the former is 168.6 GPa as compared to a value of 139.5 GPa for the latter. Moreover, the relationship between the hardness and film grain size appear to follow closely with the Hall-Petch equation.     

Mechanical properties of sol-gel derived lead zirconate titanate thin films by nanoindentation

Lead zirconate titanate (PZT) thin films are deposited on platinized silicon substrate by sol-gel process. The crystal structure and surface morphology of PZT thin films are characterized by X-ray diffraction and atomic force microscopy. Depth-sensing nanoindentation system is used to measure mechanical characteristics of PZT thin films. X-ray diffraction analyses confirm the single-phase perovskite structures of all PZT thin films. Nanoindentation measurements reveal that the indentation modulus and hardness of PZT thin films are related with the grain size and crystalline orientation. The increases of the indentation modulus and hardness with grain size are observed, indicating the reverse Hall-Petch effect. Furthermore, the indentation modulus of (1 1 1)-oriented PZT thin film is higher than those of (1 0 0)- and random-oriented films. The consistency between experimental data and numerical results of the effective indentation moduli for fiber-textured PZT thin films using Voigt-Reuss-Hill model is obtained.     

Modeling the influence of the porosity of laser-ablated silicon films on their photoluminescence properties

Nanostructured porous Si-based films produced by pulsed laser ablation (PLA) from a silicon target in residual helium gas can exhibit both size-dependent (1.6-3.2 eV) and fixed photoluminescent (PL) bands (1.6 and 2.2 eV) with their relative contributions depending on the film porosity. We study the influence of prolonged oxidation in ambient air on properties of the fixed PL bands, associated with oxidation phenomena, and their correlation with structural properties of the films. In addition, we propose a model describing the appearance of surface radiation states for oxidized films of various porosities. Our experiments and numerical simulations led to a conclusion that the 1.6 eV PL is due to a mechanism involving a recombination through the interfacial layer between Si core and an upper oxide of nanocrystals. This mechanism gives the optimal porosity of 73% for the most efficient production of 1.6 eV PL centers that is in excellent agreement with our experimental results.     

The structure and optical properties of evaporated Samarium fluoride films

Samarium fluoride (SmF₃) films have been deposited on quartz, silicon and germanium substrates by vacuum evaporation method. The crystal structure of the films deposited on silicon substrate is examined by X-ray diffraction (XRD). The films deposited at 100 °C, 150 °C and 250 °C have the (1 1 1) preferred growth orientation, but the film deposited at 200 °C has (3 6 0) growth orientation. The surface morphology evolution of the films with different thickness is investigated with optical microscopy. It is shown that the microcrack density and orientation of thin film is different from that of thick film. The transmission spectrum of SmF₃ films is measured from 200 nm to 20 μm. It is found that this material has good transparency from deep violet to far infrared. The optical constants of SmF₃ films from 200 nm to 12 μm are calculated by fitting the transmission spectrum of the films using Lorentz oscillator model.     

Field emission measured from nanostructured germanium and silicon thin films

We have prepared nanostructured thin films of germanium and silicon. The films were grown by an ion beam sputtering technique followed by a rapid annealing step using an electron beam annealer. The annealing temperature is a comparatively low 500 °C, resulting in well defined nano-islands on the film surface. Electron field emission has been measured from the surfaces under high vacuum. The threshold electric field value for significant current flow was measured as 2.5 V μm⁻¹ for a silicon thin film which is comparable to other silicon technologies. A value of 0.5 V μm⁻¹ for a germanium thin film represents an order of magnitude improvement for related germanium nanostructured systems.     

Fabrication of textured SnO2:F thin films by spray pyrolysis

Transparent conductive SnO₂:F thin films with textured surfaces were fabricated on soda-lime-silica glass substrates by spray pyrolysis. Structure, morphology, optical and electrical properties of the films were investigated. Results show that the film structure, morphology, haze, transmittance and sheet resistance are dependent on the substrate temperature and film thickness. An optimal 810 nm-thick SnO₂:F film with textured surface deposited at 520 °C exhibits polycrystalline rutile tetragonal structure with a (2 0 0) orientation. The sheet resistance, average transmittance in visible region, and haze of this film were 8 Ω/□, 80.04% and 11.07%, respectively, which are suitable for the electrode used in the hydrogenated amorphous silicon solar cells.     

The key factors in fabrication of high-quality ordered macroporous copper film

The template-directed fabrication of highly-ordered porous film is of significant importance in implementation of the photonic band gap structure. The paper reports a simple and effective method to improve the electrodeposition of metal porous film by utilizing highly-ordered polystyrene spheres (PSs) template. By surface-modification method, the hydrophobic property of the PSs template surfaces was changed into hydrophilic one. It was demonstrated that the surface modification process enhanced the permeability of the electrolyte solution in the nanometer-sized voids of the colloidal template. The homogeneously deposited copper film with the highly-ordered voids in size of less than 500 nm was successfully obtained. In addition, it was found that large defects, such as microcracks in the template, strongly influenced the macroporous films quality. An obvious preferential growth in the cracked area was observed.     

Berkovich nanoindentation and deformation mechanisms in GaN thin films

The deformation mechanisms of GaN thin films obtained by metal-organic chemical vapor deposition (MOCVD) method were studied using nanoindentation with a Berkovich diamond indenter, micro-Raman spectroscopy and the cross-sectional transmission electron microscopy (XTEM) techniques. Due to the sharpness of the tip of Berkovich indenter, the nanoindentation-induced deformation behaviors can be investigated at relatively lower load and, hence, may cover wider range of deformation-related phenomena over the same loading range. The load-displacement curves show the multiple “pop-ins” during nanoindentation loading. No evidence of nanoindentation-induced phase transformation and cracking patterns were found up to the maximum load of 300 mN, as revealed from the micro-Raman spectra and the scanning electron microscopy (SEM) observations within the mechanically deformed regions. In addition, XTEM observation performed near the cross-section of the indented area revealed that the primary deformation mechanism in GaN thin film is via propagation of dislocations on both basal and pyramidal planes. The continuous stiffness measurement (CSM) technique was used to determine the hardness and Young's modulus of GaN thin films. In addition, analysis of the load-displacement data reveals that the values of hardness and Young's modulus of GaN thin films are 19 ± 1 and 286 ± 25 GPa, respectively.     

Synthesis, structure, microstructure and mechanical characteristics of MOCVD deposited zirconia films

Zirconia (ZrO₂) thin films were deposited by metal organic chemical vapor deposition (MOCVD) on (1 0 0) Si over temperature and pressure ranges from 700 to 900 °C and 100 to 2000 Pa, respectively. The oxide films were characterized by field emission microscopy and X-ray diffraction so that microstructure and ratios of monoclinic and tetragonal phases could be estimated according to the process conditions. The mechanical behaviour of the substrate-film systems was investigated using Vickers micro-indentation and Berkovitch nano-indentation tests. The characteristics of silicon are not modified by the presence of a thin film of silicon oxide (10 nm), formed in the reactor during heating. Young's modulus and the hardness of tetragonal zirconia phase, 220 and 15 GPa, respectively, are greater than values obtained for monoclinic phase, 160 and 7 GPa, respectively. The zirconia films are well adherent and the toughness of tetragonal zirconia phase is greater than that of monoclinic phase.     

Nanocrystalline nickel films with lotus leaf texture for superhydrophobic and low friction surfaces

Nanostructured Ni films with high hardness, high hydrophobicity and low coefficient of friction (COF) were fabricated. The surface texture of lotus leaf was replicated using a cellulose acetate film, on which a nanocrystalline (NC) Ni coating with a grain size of 30 ± 4 nm was electrodeposited to obtain a self-sustaining film with a hardness of 4.42 GPa. The surface texture of the NC Ni obtained in this way featured a high density (4 × 10³ mm⁻²) of conical protuberances with an average height of 10.0 ± 2.0 μm and a tip radius of 2.5 ± 0.5 μm. This structure increased the water repellency and reduced the COF, compared to smooth NC Ni surfaces. The application of a short-duration (120 s) electrodeposition process that deposited “Ni crowns” with a larger radius of 6.0 ± 0.5 μm on the protuberances, followed by a perfluoropolyether (PFPE) solution treatment succeeded in producing a surface texture consisting of nanotextured protuberances that resulted in a very high water contact angle of 156°, comparable to that of the superhydrophobic lotus leaf. Additionally, the microscale protuberances eliminated the initial high COF peaks observed when smooth NC Ni films were tested, and the PFPE treatment resulted in a 60% reduction in the steady-state COFs.     

Synthesis of PS colloidal crystal templates and ordered ZnO porous thin films by dip-drawing method

Polystyrene spheres (PS) were synthesized by an emulsifier-free emulsion polymerization technique and the PS colloidal crystal templates were assembled orderly on clean glass substrates by dip-drawing method from emulsion of PS. Porous ZnO thin films were prepared by filling the ZnO sol into the spaces among the close-packed PS templates and then annealing to remove the PS templates. The effects of ZnO precursor sol concentration and dipping time in sol on the porous structure of the thin films were studied. The results showed an ordered ZnO porous thin film with designed pore size that depended on the sol concentration and PS size could be obtained. And the shrinkage of pore diameter was about 30-43%. X-ray diffraction (XRD) spectra indicated the thin film was wurtzite structure. The transmittance spectrum showed that optical transmittance decreased with the decrease of wavelength, but kept above 80% optical transmittances beyond the wavelength of 550 nm. Optical band gap of the porous ZnO thin film (fired at 500 °C) was 3.22 eV.     

Annealing effect on microstructure and mechanical properties of amorphous Al-C-N films

Al-C-N thin films with different Al contents were deposited on Si (1 0 0) substrates by closed-field unbalanced reactive magnetron sputtering in the mixture of argon and nitrogen gases. These films were subsequently vacuum-annealed at 700 °C and 1000 °C, respectively. The microstructures of as-deposited and annealed films were characterized by X-ray diffraction (XRD) and high-resolution transmission electron microscopy (HRTEM); while the hardness and elastic modulus values were measured by nano-indention method. The results indicated that the microstructure of both as-deposited and annealed Al-C-N films strongly depended on Al content. For thin films at low Al content, film delamination rather than crystallization occurred after the sample was annealed at 1000 °C. For thin films at high Al content, annealing led to the formation of AlN nanocrystallites, which produced nanocomposites of AlN embedded into amorphous matrices. Both the density and size of AlN nanocrystallites were found to decrease with increasing depth from the film surface. With increasing of annealing temperature, both hardness and elastic modulus values were decreased; this trend was decreased at high Al content. Annealing did not change elastic recovery property of Al-C-N thin films.