Epitaxial growth of Al on Si(1 1 1) with Cu buffer layers

The structure of thin Al films grown on Si(1 1 1) with thin Cu buffer layers has been investigated using synchrotron radiation photoemission spectroscopy. A thin Cu(1 1 1) layer between the Si(1 1 1) substrate and an Al film may enhance quantum well effects in the Al film significantly. The strength of quantum well effects has been investigated qualitatively with respect to the thickness of the Cu buffer layer and to the Al film thickness. Deposition of Cu on Si(1 1 1)7 × 7 leads to formation of a disordered silicide layer in an initial regime before a well-ordered Cu(1 1 1) film is formed after deposition of the equivalent of 6 layers of Cu. In the regime below 6 layers of Cu the disorder is transferred to Al layers subsequently grown on top. The initial growth of up to 8 layers of Al on a well-ordered Si/Cu(1 1 1) layer leads to a disordered film due to the lattice mismatch between the two metals. When the Cu buffer layer and the Al over-layer are above 6 and 8 layers, respectively the Al film shows sharp low energy electron diffraction patterns and very sharp quantum well peaks in the valence band spectra signalling good epitaxial growth.     

Microstructure and tribological performance of self-lubricating diamond/tetrahedral amorphous carbon composite film

In order to smooth the rough surface and further improve the wear-resistance of coarse chemical vapor deposition diamond films, diamond/tetrahedral amorphous carbon composite films were synthesized by a two-step preparation technique including hot-filament chemical vapor deposition for polycrystalline diamond (PCD) and subsequent filtered cathodic vacuum arc growth for tetrahedral amorphous carbon (ta-C). The microstructure and tribological performance of the composite films were investigated by means of various characterization techniques. The results indicated that the composite films consisted of a thick well-grained diamond base layer with a thickness up to 150 μm and a thin covering ta-C layer with a thickness of about 0.3 μm, and sp³-C fraction up to 73.93%. Deposition of a smooth ta-C film on coarse polycrystalline diamond films was proved to be an effective tool to lower the surface roughness of the polycrystalline diamond film. The wear-resistance of the diamond film was also enhanced by the self-lubricating effect of the covering ta-C film due to graphitic phase transformation. Under dry pin-on-disk wear test against Si₃N₄ ball, the friction coefficients of the composite films were much lower than that of the single PCD film. An extremely low friction coefficient (∼0.05) was achieved for the PCD/ta-C composite film. Moreover, the addition of Ti interlayer between the ta-C and the PCD layers can further reduce the surface roughness of the composite film. The main wear mechanism of the composite films was abrasive wear.     

Deposition of thick and adherent Teflon-like coating on industrial scale stainless steel shell using pulsed dc and RF PECVD

A unique combination of pulsed dc and radio frequency (RF) discharge deposition was used to deposit thick (∼5 μm) and adherent (2-4 MPa) Teflon-like coatings on a stainless steel (SS) shell of 2 m diameter size, through plasma enhanced chemical vapor deposition (PECVD). The details of deposition on such a big industrial scale component are reported for the first time. In this method, highly adherent thin interface layers were grown on SS shell that was electrically grounded, using pulsed dc discharge, followed by RF discharge deposition to build up the required coating thickness. The fluorocarbon precursor molecules, required for the deposition of Teflon-like coating, are generated indigenously by pyrolyzing the Teflon powder. The deposited coating was studied for its chemical bond state, surface roughness (Ra), morphology, thickness, and adhesive strength. These studies were carried out by using XPS, AFM, SEM, etc. The adhesive strength of the coating was measured by pin-pull test as per ASTM D4541 standard test. The coatings deposited with pulsed dc discharge were observed to have higher adhesive strength when compared with those deposited with RF discharge.     

TEM and XPS studies on CdS/CIGS interfaces

Copper indium gallium selenide (CIGS) was deposited by metallic precursors sputtering and subsequently submitted to a selenization process. The upper CdS layers were deposited by chemical bath deposition (CBD) technique. The CdS/CIGS interfaces were investigated by Transmission Electron Microscopy (TEM) and X-ray Photoelectron Spectroscopy (XPS). As checked by XPS analysis, the CIGS surface exhibited a hydroxide-terminated CdSe layer when treated with Cd Partial Electrolyte solution (Cd PE). Its thickness was roughly estimated to several nanometers. A 100 nm thick CdS layer was deposited onto CIGS surface. The TEM images revealed a clear and sharp interface between CdS and CIGS. XPS analysis showed a CIGS surface covered by a pinhole free and homogeneous CdS layer. XPS depth profile measurement of the CdS/CIGS interface did not evidence elemental inter-diffusion between the CIGS and CdS layers, in very good agreement with TEM observations.     

In situ deposition behavior of silica-based layers and its effect on thermal degradation of IN713 turbine blades during operation of a micro-gas turbine

This study examined the in situ deposition behavior of silica-based layers on IN713 turbine blades during the operation of a 13 kgf-class gas turbine at a rotation speed of 20,000/min as well as its effect on the degradation of the metallic substrate. Tetraethylorthosilicate (TEOS) was mixed with the fuel (liquid petroleum gas, LPG) and burned to generate silica-based coating precursors for deposition from the flame. Two deposition conditions were adopted. For condition 1 (C1), the silicon-to-carbon ratio in the mixed fuel was set at 0.1 mol% for the first 5 min and at zero mol% for the final 95 min in a 100-min operation. For condition 2 (C2), the ratio was set at 0.005 mol% during the entire 100 min operation. The total TEOS feed was the same under both conditions. C1 resulted in a rather uniform and thicker (5-10 μm on the pressure side) porous silica-based coating on the blade than C2. The in situ deposited layer of C1 was well preserved on the blade and protected the underlying metallic substrate from oxidation during the entire 100 min operation. The layer on the C2 blades was ∼5 μm thick at the region near to root, but was too thin in the other areas on the blade to be protective. The early build-up of a porous layer to an effective thickness on the blades produced a thermal barrier toward the substrate as well as a diffusion barrier toward the oxidizing elements during operation.     

Effect of thickness and porous structure of SiC layers on the spectral response of the Pd/SiC-pSi Schottky photodiodes

In this work, we study the effect of the thickness and porous structure of silicon carbide (PSC) layers on the electrical properties of Schottky photodiodes by using a palladium (Pd) layer deposited on non-porous silicon carbide (SiC) and porous-SiC (PSC) layers. The non-porous and porous-SiC layers were realized on a p-type silicon (Si(1 0 0)) substrate by pulsed laser deposition using a KrF laser (248 nm) and thermal deposition of a thin Pd layer. The porous structure of the SiC layer deposited was developed by an electrochemical (anodization) method. The electrical measurements were made at room temperature (295 K) in an air ambience. The effect of the porous surface structure and the thickness of the SiC layer were investigated by evaluating electrical parameters such as the ideality factor (n) and barrier height (?_Bp). The thickness of the porous layer significantly affects the electrical properties of the Schottky photodiodes. Analysis of current-voltage (I-V) characteristics showed that the forward current might be described by a classical thermal emission theory. The ideality factor determined by the I-V characteristics was found to be dependent on the SiC thickness a value For a thin SiC layer (0.16 μm) n was around 1.325 with a barrier height 0.798 eV, while for a thick layer (1.6 μm), n and ?_Bp were 1.026 and 0.890 eV, respectively for Pd/SiC-pSi. These results indicate Schottky photodiodes with high performance are obtained for thicker SiC layer and for thin layer of PSC. This effect showed the uniformity of the SiC layer. In the same case the ideality factor (n) decreases for Pd/PSC-pSi(1 0 0) for low SiC thickness by report of Pd/PSC-pSi(1 0 0) Schottky photodiodes, but for Pd/PSC-pSi(1 0 0) n increase for large SiC thickness layer. We notice that the barrier height (?_Bp) was reversely depend by report of ideality factor. A spectral response value of (SR) of 34 mA/W at λ = 400 nm was measured for Pd/0.16 μm SiC-pSi Schottky photodiode with low SiC thickness. On the other hand, a value of SR = 0.14 mA/W at λ = 900 nm was obtained when we used PSC layer (Pd/PSC-pSi(1 0 0)). A reverse behaviour occurs for thicker SiC layer. Finally, it was found that the thickness and surface porous structure have strong effect on sensitivity.     

Enhanced diamond nucleation on copper substrates by graphite seeding and CO2 laser irradiation

Diamond nucleation on copper (Cu) substrates was investigated by graphite seeding and CO₂ laser irradiation at initial stages of the combustion-flame deposition. A graphite aerosol spray was used to generate a thin layer of graphite powders (less than 1 μm) on Cu substrates. The graphite-seeded Cu substrates were then heated by a continuous CO₂ laser to about 750 °C within 1 min. It was found that diamond nucleation density after this treatment was more than three times as much as that on the virgin Cu substrates. As a consequence, diamond films up to 4 μm were obtained in 5 min. The enhancement of diamond nucleation on the graphite-seeded Cu substrates was attributed to the formation of defects and edges during the etching of the seeding graphite layers by the OH radicals in the flame. The defects and edges served as nucleation sites for diamond formation. The function of the CO₂ laser was to rapidly heat the deposition areas to create a favorable temperature for diamond nucleation and growth.     

Diamond deposition on siliconized stainless steel

Silicon diffusion layers in AISI 304 and AISI 316 type stainless steels were investigated as an alternative to surface barrier coatings for diamond film growth. Uniform 2 μm thick silicon rich interlayers were obtained by coating the surface of the steels with silicon and performing diffusion treatments at 800 °C. Adherent diamond films with low sp² carbon content were deposited on the diffused silicon layers by a modified hot filament assisted chemical vapor deposition (HFCVD) method. Characterization of as-siliconized layers and diamond coatings was performed by energy dispersive X-ray analysis, scanning electron microscopy, X-ray diffraction and Raman spectroscopy.     

Structural, electrical and piezoelectric properties of LiNbO3 thin films for surface acoustic wave resonators applications

In this work, 0.30 μm thick LiNbO₃ layers have been deposited by sputtering on nanocrystalline diamond/Si and platinised Si substrates. The films were then analyzed in terms of their structural and optical properties. Crystalline orientations along the (0 1 2), (1 0 4) and (1 1 0) axes have been detected after thermal treatment at 500 °C in air. The films were near-stoichiometric and did not reveal strong losses or diffusion in lithium during deposition or after thermal annealing. Pronounced decrease of the roughness on top of the LiNbO₃ layer and at the interface between LiNbO₃ and diamond was also observed after annealing, compared to the bare nanocrystalline diamond on Si substrate. Furthermore, ellipsometry analysis showed a better density and a reduced thickness of the surface layer after post-deposition annealing. The dielectric constant and losses have been measured to 50 and less than 3.5%, respectively, for metal/insulator/metal structures with 0.30 μm thick LiNbO₃ layer. The piezoelectric coefficient d₃₃ was found to be 7.1 pm/V. Finally, we succeeded in switching local domain under various positive and negative voltages.     

Study on metal microparticle content of the material transferred with Absorbing Film Assisted Laser Induced Forward Transfer when using silver absorbing layer

Absorbing Film Assisted Laser Induced Forward Transfer (AFA-LIFT) is a modified LIFT method where a high absorption coefficient thin film coating of a transparent substrate is used to transform the laser energy into kinetic in order to transfer the “target” material spread on it. This method can be used for the transfer of biomaterials and living cells, which could be damaged by direct irradiation of the laser beam. In previous experiments, ∼50-100 nm thick metal films have been used as absorbing layer. The transferred material can also contain metal microparticles originating from the absorbing thin film and acting as non-desired impurities in some cases. The aim of our work was to study how the properties (number, size and covered area) of metal particles transferred during the AFA-LIFT process depend on film thickness and the applied fluence. Silver thin films with different thickness (50-400 nm) were used as absorbing layers and real experimental conditions were modeled by a 100 μm thick water layer. The particles transferred without the use of water layer were also studied. The threshold laser fluence for the complete removal of the absorber from the irradiated area was found to strongly increase with increasing film thickness. The deposited micrometer and submicrometer particles were observed with optical microscope and atomic force microscope. Their size ranged from 100 nm to 20 μm and depended on the laser fluence. The increase in fluence resulted in an increasing number of particles of smaller average size.     

Process and performance of hot dip zinc coatings containing ZnO and Ni-P under layers as barrier protection

A new coating system of under layer for hot dip zinc coating was explored as an effective coating for steel especially for application in relatively high aggressive environments. The influence of different barrier layers formed prior to hot dip galvanization was investigated to optimize high performance protective galvanic coatings. The deposition of ZnO and Ni-P inner layers and characteristics of hotdip zinc coatings were explored in this study. The coating morphology was characterized by scanning electron microscope (SEM) analysis. The hot dip zinc coatings containing under layer showed substantial improvement in their properties such as good adhesion, and high hardness. In addition, a decrease in the thickness of the coating layer and an enhancement of the corrosion resistance were found. Open circuit potential (OCP) of different galvanized layers in different corrosive media viz. 5% NaCl and 0.5 M H₂SO₄ solutions at 25 ± 1 °C was measured as a function of time. A nobler OCP was exhibited for samples treated with ZnO and Ni than sample of pure Zn; this indicates a dissolution process followed by passivation due to the surface oxide formation. The high negative OCP can be attributed to the better alloying reaction between Zn and Fe and to the sacrificial nature of the top pure zinc layer.     

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.     

The influence of compressive stress applied by hard coatings on the power loss of grain oriented electrical steel sheet

To reduce the core loss of electrical steel the vacuum arc ion plating technique has been used to deposit titanium nitride (TiN) layers on highly grain oriented electrical steel sheets. The layer thickness, the stresses of layers and coated sheets and the achieved reduction in core losses have been measured as functions of coating duration and applied bias voltage. Well adhered layers with high compressive stress up to 6.8 GPa have been produced. With increasing bias voltage the layer thickness decreases and the intrinsic stress of the layers increase. A further increase of bias voltage leads to a drop in stress due to thermal relaxation. In general, the tensile stress of the coated sheets rises with increasing layer thickness while the core loss of the coated material decreases with increasing tensile stress of the steel sheet and increasing bias voltage. The highest reduction of core loss has been found to be 28% (from P_1.7=0.86 W/kg for commercially coated HGO electrical steel sheet with glass film to 0.62 W/kg for TiN coated material) and is due to the reduction of excess loss only.     

Effect of mesh patterning with UV pulsed-laser on optical and electrical properties of ZnO/Ag-Ti thin films

In this study, the ZnO/Ag-Ti structure for transparence conducting oxide (TCO) is investigated by optimizing the thickness of the Ag-Ti alloy and ZnO layers. The Ag-Ti thin film is deposited by DC magnetron sputtering and its thicknesses is well controlled. The ZnO thin film is prepared by sol-gel method using zinc acetate as cation source, 2-methoxiethanol as solvent and monoethanolamine as solution stabilizer. The ZnO film deposition is performed by spin-coating technique and dried at 150 °C on Corning 1737 glass. Due to the conductivity of ZnO/Ag-Ti is dominated by Ag-Ti, the sheet resistance of ZnO/Ag-Ti decrease dramatically as the thickness of Ag-Ti layer increases. However, the transmittances of ZnO/Ag-Ti become unacceptable for TCO application after the thickness of Ag-Ti layer beyond 6 nm. The as-deposited ZnO/Ag-Ti structure has the optical transmittance of 83% @ 500 nm and the low resistivity of 1.2 × 10⁻⁵ Ω-cm. Furthermore, for improving the optical and electrical properties of ZnO/Ag-Ti, the thermal treatment using laser is adopted. Experimental results indicate that the transmittance of ZnO/Ag-Ti is improved from 83% to 89% @ 500 nm with resistivity of 1.02 × 10⁻⁵ Ω-cm after laser drilling. The optical spectrum, the resistance, and the morphology of the ZnO/Ag-Ti will be reported in the study.     

Ceramic membrane by tape casting and sol-gel coating for microfiltration and ultrafiltration application

Alumina membrane filters in the form of thin (0.3-0.8 mm) discs of 25-30 mm diameter suitable for microfiltration application have been fabricated by tape-casting technique. Further using this microfiltration membrane as substrate, boehmite sol coating was applied on it and ultrafiltration membrane with very small thickness was formed. The pore size of the microfiltration membrane could be varied in the range of 0.1-0.7 μm through optimisation of experimental parameter. In addition, each membrane shows a very narrow pore size distribution. The most important factor, which determines the pore size of the membrane, is the initial particle size and its distribution of the ceramic powder. The top thin ultrafiltration, boehmite layer was prepared by sol-gel method, with a thickness of 0.5 μm. Particle size of the sol was approximately 30-40 nm. The structure and formation of the layer was analysed through TEM. At 550 °C formation of the top layer was completed. The pore size of the ultrafiltration membrane measured from TEM micrograph was almost 10 nm. Results of microbial (Escherichia coli—smallest-sized water-borne bacteria) test confirm the possibility of separation through this membrane     

Electron scattering characteristics of polycrystalline metal transition films by in-situ electrical resistance measurements

In-situ electrical resistance measurements were performed to obtain the scattering characteristics of very thin polycrystalline metal transition magnetic alloys grown by ion beam deposition (IBD) on specific underlayers. The experimental curves show size effects at small film thicknesses and important differences between Co₈₅Fe₁₅ and Ni₈₁Fe₁₉ thin layers grown on identical underlayers of Ta70 Å/Ru13 Å. The largest difference was observed in Ni₈₁Fe₁₉ films grown on underlayers of amorphous Ta70 Å. The experimental curves of electrical resistivity/conductivity variation with layer thickness were well fit within the Mayadas and Shatzkes (M-S) model, assuming specific formulations for grain growth with layer thickness.     

Nitric acid method for fabrication of gate oxides in TFT

We have developed low temperature formation methods of SiO₂ layers which are applicable to gate oxide layers in thin film transistors (TFT) by use of nitric acid (HNO₃). Thick (>10 nm) SiO₂ layers with good thickness uniformity (i.e., ±4%) can be formed on 32 cm × 40 cm substrates by the two-step nitric acid oxidation method in which initial and subsequent oxidation is performed using 40 and 68 wt% (azeotropic mixture) HNO₃ aqueous solutions, respectively. The nitric acid oxidation of polycrystalline Si (poly-Si) thin films greatly decreases the height of ridge structure present on the poly-Si surfaces. When poly-Si thin films on 32 cm × 40 cm glass substrates are oxidized at azeotropic point (i.e., 68 wt% HNO₃ aqueous solutions at 121 °C), ultrathin (i.e., 1.1 nm) SiO₂ layers with a good thickness uniformity (±0.05 nm) are formed on the poly-Si surfaces. When SiO₂/Si structure fabricated using plasma-enhanced chemical vapor deposition is immersed in 68 wt% HNO₃, oxide fixed charge density is greatly decreased, and interface states are eliminated. The fixed charge density is further decreased by heat treatments at 200 °C, and consequently, capacitance-voltage characteristics which are as good as those of thermal SiO₂/Si structure are achieved.     

Study on the electrical and optical properties of Ag/Al-doped ZnO coatings deposited by electron beam evaporation

A layer of silver was deposited onto the surface of glass substrates, coated with AZO (Al-doped ZnO), to form Ag/AZO film structures, using e-beam evaporation techniques. The electrical and optical properties of AZO, Ag and Ag/AZO film structures were studied. The deposition of Ag layer on the surface of AZO films resulted in lowering the effective electrical resistivity with a slight reduction of their optical transmittance. Ag (11 nm)/AZO (25 nm) film structure, with an accuracy of ±0.5 nm for the thickness shows a sheet resistance as low as 5.6 ± 0.5 Ω/sq and a transmittance of about 66 ± 2%. A coating consisting of AZO (25 nm)/Ag (11 nm)/AZO (25 nm) trilayer structure, exhibits a resistance of 7.7 ± 0.5 Ω/sq and a high transmittance of 85 ± 2%. The coatings have satisfactory properties of low resistance, high transmittance and highest figure of merit for application in optoelectronics devices including flat displays, thin films transistors and solar cells as transparent conductive electrodes.     

Fabrication of MgO barrier for a magnetic tunnel junction in as-deposited state using amorphous RE–TM alloy

MgO (1 0 0) textured films on Fe buffer layer with (1 0 0) preferential orientation were prepared by a reactive facing targets sputtering system at a substrate temperature of 100 °C during MgO deposition. This process can allow fabrication of MgO (1 0 0) tunneling barrier layer without high-temperature annealing process after the sputter-deposition. In addition, FeCo (1 0 0) preferred orientation films prepared on GdFeCo layers were improved with GdFeCo thickness. MgO films deposited on Fe (or FeCo) buffer layers revealed apparent (1 0 0) preferred orientation at the early stage of the film growth. 3 nm-thick MgO films deposited on GdFeCo [100 nm]/Fe [3 nm] exhibited (1 0 0) texture. Magnetic characteristic of perpendicular-magnetic tunnel junction (P-MTJ) element with the structure of GdFeCo [100 nm]/Fe [3 nm]/MgO [3 nm]/Fe [3 nm]/TbFeCo [100 nm] exhibited high squareness ratio of 0.8 and coercivity of free layer as low as 117 Oe by anomalous Hall effect, and (1 0 0) preferred orientation of 3 nm-thick MgO layer was observed by an X-ray diffractometer.     

Empirical evaluation of metal deposition for the analysis of organic compounds with static secondary ion mass spectrometry (S-SIMS)

Metal-assisted (MetA) SIMS using the deposition of a thin Au or Ag layer on non-conducting samples prior to analysis has been advocated as a means to improve the secondary ion (S.I.) yields of organic analytes. This study focuses on the influence of time and temperature on the yield enhancement in MetA-SIMS using thick layers of poly(vinylbutyral-co-vinylalcohol-co-vinylacetate) (PVB) containing dihydroxybenzophenone (DHBPh) or a cationic carbocyanine dye (CBC) and spin-coated layers of the cationic dye on Si. Pristine samples as well as Au- and Ag-coated ones were kept between −8 °C and 80 °C and analysed with S-SIMS at intervals of a few days over a period of 1 month. The yield enhancement was found to depend strongly on the kind of evaporated metal, the storage temperature and time between coating and analysis.