Preparation of single-crystal TiC (111) by radio frequency magnetron sputtering at low temperature

Single-crystal films of TiC (111) have been synthesized at room temperature on Al₂O₃ (0001) substrates by radio frequency magnetron sputtering using a compound Ti-C target. The substrate temperature and bias were varied to explore the influence of deposition parameters on the crystal structure. Both Al₂O₃ (0001) and Si (100) substrates were used for epitaxial growth of TiC films. A series of characterizations of TiC films were carried out, including Rutherford backscattering spectroscopy, X-ray diffraction, Raman and X-ray photoelectron spectroscopy. Single-crystal films of TiC (111) on the Al₂O₃ (0001) were demonstrated.     

Titanium oxide thin films synthesis by pulsed – DC magnetron sputtering

Titanium oxide thin films (1–4 μm) were deposited on the porous Hastelloy-X substrates using the pulsed – DC magnetron sputtering technique and characterized by X–ray diffraction (XRD) and scanning electron microscopy (SEM) methods. Firstly, the films were deposited at different distances between the magnetron and the substrate, as magnetron current and pressure in the deposition chamber were constant. The distance between the magnetron and the substrate was changed from 3 cm to 7 cm, and the deposition rate varied between 10.1 nm/min to 6.0 nm/min. Secondly, pressure influence for the deposition rate was investigated. The deposition rate decreased nearly 15% with the decrease of oxygen pressure from 1.3 to 6.0 Pa. Finally, the influence of the bias (applied to the substrate for the increase of deposition rate) on thin films phase and microstructure was investigated.The experimental results showed that formation of pure titanium oxide thin films was observed in all experimental cases. Only crystallite sizes and orientation were changed. The results showed that there is a possibility to change porosity and uniformity of the growing film by changing oxygen partial pressure during deposition or bias application to the substrate. The existence of columnar boundaries and nanocrystalline structure in the films was observed.     

Phase separated AlSi thin films prepared by filtered cathodic arc deposition

Phase separated AlSi films composed of Al cylinders embedded in an amorphous Si matrix were prepared on conducting Si substrates by filtered cathodic arc deposition. The compositional dependence of AlSi films on a negative substrate bias showed a different trend depending on the cathode composition because of the self-sputtering process during the deposition. The porous structure was obtained from the phase separated AlSi film after removal of Al cylinders by wet etching in an ammonia solution. Scanning electron microscope images of the etched AlSi films showed that the average diameter of pores was increased from 3 nm to 7 nm by applying a negative substrate bias voltage during the deposition. The honeycomb ordered arrangement of pores was observed at 0 V and − 25 V substrate bias. The substrate temperature during the depositions had almost the same effect on the film morphologies as the negative substrate bias.     

Physicochemical and structural characteristics of TiC and VC thin films deposited by DC reactive magnetron sputtering

Vanadium carbide and titanium carbide films were deposited on Si substrates by direct current reactive magnetron sputtering, varying the substrate temperature during deposition and the reactive gas (CH₄) pressure. The physicochemical and structural properties of the films were characterized for stoichiometric films (V/C = 1 and Ti/C = 1), which display good performance concerning wear, friction, and corrosion. The techniques used to characterize the films were Rutherford backscattering spectrometry in channeling geometry, ¹²C(α,α)¹²C nuclear resonant scattering, glancing angle X-ray diffraction, X-ray reflectometry, and X-ray photoelectron spectroscopy. The results revealed that the ideal conditions for deposition of these films are a CH₄ partial pressure of 0.5 × 10⁻³ mbar and a substrate temperature of 400 °C. In such conditions, the deposition rates are 7 nm s⁻¹ for TiC and 8.5 nm s⁻¹ for VC at a target power density of 5.5 W cm⁻². The density of the films, as determined here by X-ray reflectometry, are slightly higher than those for the bulk materials.     

Dependence of the electrical and optical properties on the bias voltage for ZnO:Al films deposited by r.f. magnetron sputtering

Aluminum-doped zinc oxide (ZnO:Al) thin films were deposited on glass, polycarbonate (PC), and polyethylene terephthalate (PET) substrates by r.f. magnetron sputtering. The substrate dc bias voltage varied from 0 V to 50 V. Structural, electrical and optical properties of the films were investigated. The deposition rate of ZnO:Al films on glass substrate initially increased with the bias voltage, and then decreased with further increasing bias voltage. It was found that the best films on glass substrate with a low as 6.2 × 10^− 4 Ω cm and an average transmittance over 80% at the wavelength range of 500-900 nm can be obtained by applying the bias voltage of 30 V. The properties of the films deposited on polymer substrate, such as PC and PET, have a similar tendency, with slightly inferior values to those on glass substrate.     

Influence of growth parameters on the microstructures of erbium films deposited on Si(111) substrates

Erbium films were grown on single crystal Si(111) substrates by electron beam vapor deposition. The microstructures of the erbium films were systematically investigated by X-ray diffraction, scanning electron microscopy, and energy dispersive spectroscopy. Results indicate that the surface morphologies and microstructures of the erbium films with Si as substrates are susceptible to the substrate temperatures when the deposition rates are fixed. The pure erbium films with columnar grains were obtained at temperatures below 200 °C, but in the films grown at temperatures higher than 350 °C, some pinholes that are composed of erbium silicides were found. The pinholes have triangular shapes which is in accordance with the geometry of the underlying Si(111) substrate. The films grown at a substrate temperature equal or greater than 450 °C have cracks which would be formed due to the different shrinkage degree of erbium and silicon when the substrate temperature was cooled down to room temperature. The films grown at 200 °C show the (002) preferred orientation, which is consistent to the prediction by the theory of surface energy minimization. The deposition rate and deposition time are considered as factors to affect the reaction of the erbium film and the silicon substrate.     

Morphological and structural characterisation of osseointegrable Mn2+ and CO32− doped hydroxylapatite thin films

We report a morphological and structural study of osseointegrable hydroxylapatite thin films doped with divalent manganese and carbonate ions. The films were grown by pulsed laser deposition on medical grade Ti substrates at low oxygen pressure (13 Pa). Deposition targets were prepared from powders obtained by precipitation. During deposition, the substrates were kept at constant temperature within the temperature range 350–450 °C and the obtained films were subsequently annealed in hot water vapours at the deposition temperature. The films were characterised by scanning electron microscopy (SEM), transmission electron microscopy (TEM), selected area electron diffraction (SAED), grazing incidence X-ray diffraction (GIXRD), energy dispersive X-ray spectrometry (EDS), and X-ray photoelectron spectroscopy (XPS). Film specimens for cross-section TEM were prepared by focused ion beam (FIB) machining. The inferred Ca/P atomic ratio in films varied between 1.6 and 1.8, depending on experimental conditions. XPS confirmed the presence of chemically bonded Mn²⁺. Cross-section TEM micrographs showed uniform thickness of the coatings, which consisted of amorphous and crystalline domains. Examination of the SEM micrographs revealed an increased smoothness of the surface with increase in substrate deposition temperature. XRD patterns of samples processed at temperatures over 400 °C showed well-crystallized hydroxylapatite, suggesting that deposition and annealing have to be performed at higher substrate temperature if highly crystalline coatings are required.     

Characterization of magnetron co-sputtered W-doped C-based films

In this paper, W-doped C-based coatings were deposited on steel and silicon substrates by RF magnetron sputtering, using W and C targets, varying the cathode power applied to the W target and the substrate bias. The chemical composition was varied by placing the substrates in a row facing the C and W targets. W content in the films increased from 1 to 2 at.% over the C target to ∼ 73 at.% over the W target. The coatings with W content lower than ∼ 12 at.% and ∼ 23 at.%, for biased and unbiased conditions, respectively, showed X-ray amorphous structures, although carbide nanocrystals must exist as shown by the detection of the WC_1−x phase in films with higher W content. C-rich films were very dense and developed a columnar morphology with increasing W content. An improvement in the hardness (from 10 GPa, up to 25 GPa) of the films was achieved either when negative substrate bias was used in the deposition, or when the WC_1−x phase was detected by X-ray diffraction. The adhesion of the coatings is very low with spontaneous spallation of those deposited with negative substrate bias higher than 45 V. Varieties in cathode power (90 W or 120 W) applied to the W target showed no observable influence on the characteristics of the films.     

Deposition and characterization of smooth ultra-nanocrystalline diamond film in CH4/H2/Ar by microwave plasma chemical vapor deposition

The smooth ultra-nanocrystalline diamond (UNCD) films were prepared by microwave plasma chemical vapor deposition (MWCVD) using argon-rich CH₄/H₂/Ar plasmas with varying argon concentration from 96% to 98% and negative bias voltage from 0 to −150 V. The influences of argon concentration and negative bias voltage on the microstructure, morphology and phase composition of the deposited UNCD films are investigated by using scanning electron microscopy (SEM), X-ray diffraction (XRD), atom force microscopy (AFM), and visible and UV Raman spectroscopy. It was found that the introduction of argon in the plasma caused the grain size and surface roughness decrease. The RMS surface roughness of 9.6 nm (10 micron square area) and grain size of about 5.7 nm of smooth UNCD films were achieved on Si(100) substrate. Detailed experimental results and mechanisms for UNCD film deposition in argon-based plasma are discussed. The deposited highly smooth UNCD film is also expected to be applicable in medical implants, surface acoustic wave (SAW) devices and micro-electromechanical systems (MEMS).     

Structural and biocompatible characterization of TiC/a:C nanocomposite thin films

In this work, sputtered TiC/amorphous C thin films have been developed in order to be applied as potential barrier coating for interfering of Ti ions from pure Ti or Ti alloy implants. Our experiments were based on magnetron sputtering method, because the vacuum deposition provides great flexibility for manipulating material chemistry and structure, leading to films and coatings with special properties. The films have been deposited on silicon (001) substrates with 300 nm thick oxidized silicon sublayer at 200 °C deposition temperature as model substrate. Transmission electron microscopy has been used for structural investigations. Thin films consisted of ~ 20 nm TiC columnar crystals embedded by 5 nm thin amorphous carbon matrix. MG63 osteoblast cells have been applied for in vitro study of TiC nanocomposites. The cell culture tests give strong evidence of thin films biocompatibility.     

Microcrystalline silicon films fabricated by bias-assisted hot-wire chemical vapor deposition

Microcrystalline silicon films (μc-Si:H) were deposited on stainless steel substrates by bias-assisted hot-wire chemical vapor deposition. The effect of substrate bias and substrate temperature on the crystallinity of μc-Si:H films was studied by Raman spectroscopy, X-ray diffraction and scanning electron microscopy. The results show that both the Raman peak position and the crystalline fraction of the μc-Si:H films deposited at 200 °C were obviously improved by introducing ?800 V substrate bias. The films deposited at 200 °C with ?800 V substrate bias show strongly sharpened Si (111) peak together with Si (220) and Si (311) peaks, which was different from a weak Si (111) peak for those deposited without substrate bias. By increasing the substrate temperature from 200 to 300 °C, while keeping the substrate bias at ?800 V, the crystallinity of the silicon films was further improved, and μc-Si:H films with crystalline fraction of 74 % was obtained.     

Titanium oxide thin films deposited by high-power impulse magnetron sputtering

Ionized physical vapor deposition processes are of great interest for surface modification because the flexibility of the thin film deposition process can be increased by ionizing the metallic vapor. Recently, high-power impulse magnetron discharges have been implemented to achieve high ionization rates.Thin films of titanium oxide have been deposited on glass and steel substrates using 450 × 150 mm rectangular titanium target in argon-oxygen atmosphere. The average power delivered to the plasma is ranging between 1.5 and 2 kW and peak current and voltage are respectively 200 A and 900 V.Films are characterized using Scanning Electron Microscopy, Grazing Incidence X-ray Diffraction and Optical Transmission Spectroscopy. One of the major findings is the presence of rutile deposited on steel substrate (even for 0 V bias grounded substrate) and the significant increase of the refractive index of the films deposited on glass compared to thin films deposited via conventional direct current bipolar pulsed magnetron sputtering. Films synthesized by high-power impulse magnetron sputtering are denser.     

The effect of substrate temperature on the oxidation behavior of erbium thick films

The effect of substrate temperature on the oxidation behavior of erbium thick films, fabricated by electron-beam vapor deposition (EBVD), was investigated by X-ray photoelectron spectroscopy (XPS), X-ray diffraction (XRD), and scanning electron microscopy (SEM). The erbium thick film is black when it is deposited at substrate temperature below 450 °C and turns gray at higher substrate temperature in a vacuum pressure of approximately 1.5 × 10⁻⁶ Torr, which indicates that the thickness of erbium oxide layer formed on the surface of erbium films increases with the decreasing substrate temperature. XPS depth profile results demonstrate that the thickness of the surface erbium oxide layer of erbium film deposited at substrate temperature of 550 and 350 °C are about 50 and 75 nm, respectively. The thicker oxide layer at lower substrate temperatures may be attributed to grain size and the dynamic vacuum condition around the substrates. Other possible factors involved in the oxidation behavior are also discussed.     

Substrate bias voltage influenced structural, electrical and optical properties of dc magnetron sputtered Ta2O5 films

Tantalum oxide (Ta₂O₅) films were formed on silicon (111) and quartz substrates by dc reactive magnetron sputtering of tantalum target in the presence of oxygen and argon gases mixture. The influence of substrate bias voltage on the chemical binding configuration, structural, electrical and optical properties was investigated. The unbiased films were amorphous in nature. As the substrate bias voltage increased to −50 V the films were transformed into polycrystalline. Further increase of substrate bias voltage to −200 V the crystallinity of the films increased. Electrical characteristics of Al/Ta₂O₅/Si structured films deposited at different substrate bias voltages in the range from 0 to −200 V were studied. The substrate bias voltage reduced the leakage current density and increased the dielectric constant. The optical transmittance of the films increased with the increase of substrate bias voltage. The unbiased films showed an optical band gap of 4.44 eV and the refractive index of 1.89. When the substrate bias voltage increased to −200 V the optical band gap and refractive index increased to 4.50 eV and 2.14, respectively due to the improvement in the crystallinity and packing density of the films. The crystallization due to the applied voltage was attributed to the interaction of the positive ions in plasma with the growing film.     

Structure and tribological properties of Ag films deposited at low temperature

The effects of substrate temperature on the structure and tribological properties of Ag films deposited at low temperatures (LT, 130-217 K) by arc ion plating (AIP) have been studied. The structure and morphology of the Ag films were analyzed by X-ray diffraction (XRD), transmission electron microscopy (TEM) and field emission scanning electron microscope (FESEM). The results showed that there exist (1 1 1) and (2 0 0) preferred orientation transitions for decreasing temperature at different bias voltages. The tribological properties were evaluated by a ball-on-disk tribometer and wear tracks were analyzed by means of scanning electron microscopy (SEM). The results show that substrate deposition temperature significantly affected the wear of LT Ag films. For each bias voltage studied, the film showing the highest wear rate was deposited at the lowest temperature and the film with the lowest wear rate, (significantly lower than room temperature (RT) deposited Ag films), was deposited at a temperature between the highest and the lowest temperatures examined. The wear mechanism was discussed in terms of lubrication effect of film material transferred to the counterpart and its dependence on the microstructure of the original deposited film.     

Influence of bias voltage on the optical and structural properties of nc-Si:H films grown by layer-by-layer (LBL) deposition technique

The effects of applying a positive bias of 25 to 100 V on the optical, structural and photoluminescence (PL) properties of hydrogenated nanocrystalline silicon (nc-Si:H) films produced by layer-by-layer (LBL) deposition technique has been studied. Optical characterization of the films has been obtained from UV-VIS-NIR spectroscopy measurements. Structural characterization has been performed using X-ray diffraction, micro-Raman spectroscopy and field emission scanning electron microscope (FESEM). PL spectroscopy technique has been used to investigate the PL properties of the films. In general, the films formed shows a mixed phase of silicon (Si) nanocrystallites embedded within an amorphous phase of the Si matrix. The crystalline volume fraction and grain size of the Si nanocrystallites have been shown to be strongly dependent on the applied bias voltage. High applied bias voltage enhances the growth rate of the films but reduces the refractive index and the optical energy gap of the films. Higher crystalline volume fraction of the films prepared at low bias voltages exhibits room temperature PL at around 1.8 eV (700 nm).     

Residual stress on nanocrystalline silicon thin films deposited under energetic ion bombardment by using internal ICP-CVD

Nano/microcrystalline silicon thin films were deposited using an internal-type, inductively coupled, plasma-chemical vapor deposition (ICP-CVD) at room temperature by varying the bias power to the substrate. The structural characteristics of the deposited thin film were investigated. The deposition rate was increased by the application of a small RF bias power of 30 W (12.56 MHz), but was then decreased as the bias power was increased above 30 W. In addition, the application of bias power generally increased the residual compressive stress, which was attributed to the increased defect formation in the thin film due to the formation of interstitial atoms. The crystalline volume fraction was also decreased with increasing bias power. However, in the low bias power range of 0-60 W, the compressive stress in the deposited thin film was in the range of − 34 to − 77 MPa, which was lower than the residual stress in the range of − 150 to − 1050 MPa that is observed for the nano/microcrystalline silicon thin films deposited by capacitively coupled plasma.     

Residual stresses in titanium nitride thin films deposited by direct current and pulsed direct current unbalanced magnetron sputtering

This work presents a study on the effect of deposition parameters on the residual stresses developed in titanium nitride (TiN) thin films deposited onto cemented carbide (WC-Co) substrates. Depositions were conducted by reactive unbalanced magnetron sputtering of a single titanium target. Six different conditions were selected, varying parameters such as bias (0, − 50 or − 100 V), power applied to the target (direct current or pulsed direct current) and, in the cases where substrate bias was zero, substrate condition (ground or floating). Pulsed power was applied at a frequency of 50 kHz and with a reverse pulse time of 1 μs. Residual stresses were evaluated through X-ray diffraction, using the sin²ψ method. Results confirmed the effect of substrate bias on the residual stresses of thin films. Additionally, it was possible to observe that by pulsing the power to the target, residual stress varies as a consequence of the increased ion energy.     

High-speed μc-Si films deposition and large-grain poly-Si films deposition by surface wave discharge

Microcrystalline silicon (μc-Si) and polycrystalline silicon (poly-Si) films are deposited by surface wave (SW) discharge at 2.45 GHz in H₂/SiH₄ gas. This high density SW plasma at relatively low pressures (4-60 Pa) enables strong dissociation of feedstock gas. The films deposited on substrate are investigated by X-ray diffraction (XRD), Raman spectroscopy and scanning electron microscopy (SEM). The SW discharge in 10% SiH₄ at total pressure of ∼ 30 Pa gives μc-Si films on a substrate at 250 °C, at a fairly high deposition rate of 4-20 nm/s, with a crystalline volume fraction of 0.5-0.8 and a grain size of 10-40 nm. Furthermore, poly-Si film with crystalline volume fraction of > 99% is deposited at higher substrate temperature (400 °C) in 2% SiH₄ discharge at lower pressure (4 Pa). X-ray diffraction and SEM results revealed that the grain size of poly-Si films is as large as 600 nm, which is almost 6 times larger than previously reported values.     

Deposition of TiB2 onto X40 CrMoV 5-1-1 steel substrates by DC magnetron sputtering

Titanium diboride (TiB₂) films are being investigated due to their promising uses not only in electronic devices but also for mechanical purposes. Its excellent corrosion resistance and chemical stability, as well as high hardness and wear resistance, makes TiB₂ particularly suitable for aluminium processing (e.g. extrusion, die-casting and machining). In the present work, TiB₂ coatings were produced by non-reactive DC magnetron sputtering from a TiB₂ target on a tool steel substrate (AISI H13 premium/EN X40 CrMoV 5-1-1). Substrates similar to those frequently found on the aluminium injection industry were produced by vacuum quenching and tempering. The deposition parameters, namely the target/substrate distance, discharge current and substrate bias, were varied in order to obtain crystalline and well-structured films, suiting the substrate composition and microstructure. The coatings were characterized by X-ray diffraction (XRD) and scanning electron microscopy/EDS.A deposition rate of 23 nm/min was obtained for 0.85 A cathode current intensity and 70 mm substrate–magnetron distance. For positively biased substrates, all films are dense, without a columnar structure and show a (0 0 1) texture. For negatively biased substrates, there are less surface heating effects due to a much lower electron current through the substrate, and an ordered structure appears only at −150 V.