Structure and properties of Ta/TaOx barrier films deposited by direct current magnetron sputtering

Double-layer Ta/TaO_x films were deposited on glass substrates by direct current magnetron sputtering. The impact of the underlying TaO_x on the structure and properties was also investigated using X-ray diffraction analysis, Auger electron microscopy, scanning electron microscopy and atomic force microscopy. This study finds that the structure and properties of Ta/TaO_x films depends on the O₂ flow during the under-layer TaO_x deposition. As the O₂ gas flow ratio increases from 3 to 7%, more and more oxidized amorphous TaO_x films in the under-layer were formed, which caused the preferred growth orientation of upper Ta films to change from (200) to (221) systematically. Increasing the oxygen flow ratio of under-layer TaO_x films also makes the average grain size of upper Ta films decrease from 10.7 to 2.2 nm.     

Synthesis and characterization of hard ternary AlMgB composite films prepared by sputter deposition

Hard and superlight thin films laminated with boron carbide have been proposed as candidates for strategic use such as armor materials in military and space applications. Aluminum magnesium boride (AlMgB) films are excellent candidates for these purposes. We prepared AlMgB films by sputter deposition using multiple unbalanced planar magnetrons equipped with two boron and one AlMg targets. The film morphology changed and the film's root mean square (rms) roughness varied from 1.0 to 18 nm as the power density of the AlMg target increased from 0.2 to 1.0 W/cm² while the power density of each boron target was maintained at 2 W/cm². Chemical analyses show dominating Al, Mg, B and trace elements of oxygen, carbon and argon. The film composition also varies with altering the power density supplied to the AlMg target. The film with an atomic ratio of Al:Mg:B = 1.38:0.64:1 exhibits the highest hardness (~ 30 GPa). This value surpasses the hardness of hydrogenated diamond-like carbon films (24-28 GPa) prepared by plasma enhanced chemical vapor deposition.     

Low resistivity transparent conducting CdO thin films deposited by DC reactive magnetron sputtering at room temperature

Transparent conducting cadmium oxide (CdO) films were deposited on PET (polyethylene terephthalate) substrate by DC reactive magnetron sputtering at room temperature. All the films deposited at room temperature were polycrystalline in rock-salt structure. Dependences of the physical properties of the CdO films on the oxygen partial pressure were systematically studied. The films deposited at low oxygen flow rate were (200) oriented, while the films deposited at an oxygen flow rate greater than 20 sccm were (111) oriented. The average grain size of the CdO films decreased as the oxygen flow rate increases as determined by XRD and SEM. The Hall effect measurement showed that CdO films have high concentration, low resistivity, and high mobility. Both the mobility and the concentration of the carrier decreased with the increase of the oxygen flow rate. A minimum sheet resistance of 36.1 Ω/□, or a lowest resistivity of 5.44 × 10^− 4 Ω cm (6.21 × 10²⁰/cm³, μ = 19.2 cm²/Vs) was obtained for films deposited at an oxygen flow rate of 10 sccm.     

Structural characterization of ZnO thin films deposited by dc magnetron sputtering

In this work we present recent results on ZnO thin films grown by dc magnetron sputtering technique at room temperature (RT), focusing on structural and surface characterization using conventional cross-section transmission electron microscopy (XTEM) and high resolution cross section transmission electron microscopy (HRXTEM) in an attempt to understand the thickness influence on film, mechanical and optical properties as well as photoreduction/oxidation conductivity changes. Films were found to be polycrystalline with a columnar mode of growth. For films with thickness over 100 nm, XTEM and HRTEM analysis evidenced the presence of a small grains transition layer near interface with the substrate, feature which plays an important role in ZnO thin films for gas sensing application. The control of such structural parameters is proved to be critical for the improvement of their gas sensing performance.     

Thickness dependent properties of nickel oxide thin films deposited by dc reactive magnetron sputtering

Nickel oxide thin films of various thicknesses were grown on glass substrates by dc reactive magnetron sputtering technique in a pure oxygen atmosphere with sputtering power of 150 W and substrate temperature of 523 K. Crystalline properties of NiO films as a function of film thickness were investigated using X-ray diffraction. XRD analysis revealed that (200) is the preferred orientation and the orientation of the films changed from (200) to (220) at film thickness of 350 nm. The maximum optical transmittance of 60% and band gap of 3.82 eV was observed at the film thickness of 350 nm. The lowest electrical resistivity of 5.1 Ω cm was observed at a film thickness of 350 nm, thereafter resistivity increases with film thickness.     

Effect of sputtering pressure and post-annealing on hydrophilicity of TiO2 thin films deposited by reactive magnetron sputtering

A series of TiO₂ thin films was deposited onto glass substrates without intentional heating or biasing by magnetron sputtering of a titanium target using Ar/O₂ reactive mixtures over a broad range of total sputtering pressures from 0.12 Pa to 2.24 Pa. Each of the film types was deposited by the threshold poisoned mode at a specific given oxygen flow rate monitored in-situ by optical emission spectroscopy. Both the sputtering pressure and thermal annealing are the key factors for the TiO₂ films to yield fast-response superhydrophilicity with a water contact angle of 5°. The mechanism of superhydrophilicity for the TiO₂ films deposited by high-pressure sputtering will be discussed based on empirical studies of X-ray diffractometry, high-resolution scanning microscopy and atomic force spectroscopy.     

Infrared transmission properties of germanium carbon thin films deposited by reactive RF magnetron sputtering

Germanium carbon (GeC) thin films were prepared on ZnS substrates by reactive RF magnetron sputtering in Ar and CH₄ mixtures with a Ge disc as the target. H content in the films was studied as a function of the deposition parameters and low H content GeC film was obtained. RF power had a little effect on IR absorptions, hence had a little effect on H content. IR absorption of the GeC film increased a little with the increase in partial pressure of CH₄ as well as total pressure of gas mixture. Increase in substrate temperature decomposed CH₄ and CH_x in the GeC film into C and H and H was desorbed from the film, lowering the IR absorption. However, high substrate temperature prevented CH₄ or CH_x from adsorbing onto the substrate, which decreased C content in the GeC film and increased the film's refractive index. Higher annealing temperature of the GeC film reduced H content, but high annealing temperature (500 °C) caused the graphitization of the GeC film and destroyed its continuity.     

Electrical properties of AlNxOy thin films prepared by reactive magnetron sputtering

Direct current magnetron sputtering was used to produce AlN_xO_y thin films, using an aluminum target, argon and a mixture of N₂ + O₂ (17:3) as reactive gases. The partial pressure of the reactive gas mixture was increased, maintaining the discharge current constant. Within the two identified regimes of the target (metallic and compound), four different tendencies for the deposition rate were found and a morphological evolution from columnar towards cauliflower-type, ending up as dense and featureless-type films. The structure was found to be Al-type (face centered cubic) and the structural characterization carried out by X-ray diffraction and transmission electron microscopy suggested the formation of an aluminum-based polycrystalline phase dispersed in an amorphous aluminum oxide/nitride (or oxynitride) matrix. This type of structure, composition, morphology and grain size, were found to be strongly correlated with the electrical response of the films, which showed a gradual transition between metallic-like responses towards semiconducting and even insulating-type behaviors. A group of films with high aluminum content revealed a sharp decrease of the temperature coefficient of resistance (TCR) as the concentration ratio of non-metallic/aluminum atomic ratio increased. Another group of samples, where the non-metallic content became more important, revealed a smooth transition between positive and negative values of TCR. In order to test whether the oxynitride films have a unique behavior or simply a transition between the typical responses of aluminum and of those of the correspondent nitride and oxide, the electrical properties of the ternary oxynitride system were compared with AlN_x and AlO_y systems, prepared in similar conditions.     

Investigation of BST thin films deposited by RF magnetron sputtering in pure Argon

Ba_0.5Sr_0.5TiO₃ (BST) thin films were deposited by rf magnetron sputtering using a Ba_0.5Sr_0.5TiO₃ target in pure Argon on two electrodes (Pt and RuO₂) at room temperature. The interface formation between BST and bottom electrode (Pt or RuO₂) was investigated by XPS for thicknesses in the 1 to 50 nm range. The chemical composition of the BST layers can be modified by the electrode nature over the first five nanometers. A 1 h ex-situ annealing, under flowing oxygen at 600 °C, was necessary to obtain crystallized 150 nm thick BST films, as evidenced by XRD and TEM analysis.     

Varistor performance of nanocrystalline Zn-Bi-O thin films prepared by reactive RF magnetron sputtering at room temperature

The Zn-Bi-O films were deposited by reactive radio frequency magnetron sputtering in oxygen atmosphere from ZnBi alloy target (wt% ratio Zn:Bi=9:1) on glass substrate at room temperature. The XRD patterns show that the films deposited on tin-doped indium oxide/glass substrates were nanocrystalline. The microstructure of Bi-doped ZnO films was studied by scanning electron microscopy in combination with energy dispersive X-ray spectroscopy. All the obtained layers had varistor-type non-linear current-voltage (I-V) characteristics with low breakdown voltage varying from few tenths of a volt to few volts.     

Low-temperature deposited Titanium-doped zinc oxide thin films on the flexible PET substrate by DC magnetron sputtering

Transparent conducting Titanium-doped zinc oxide thin films (TZO) with high transparency and relatively low resistivity were firstly deposited on water-cooled polyethylene terephthalate (PET) substrates at room temperature by DC magnetron sputtering. The microstructure, optical and electrical properties of the deposited films were investigated and discussed. The XRD patterns show that all the deposited films are polycrystalline with a hexagonal structure and have a preferred orientation along the c-axis perpendicular to the substrate. The electrical resistivity decreases when the sputtering power increases from 45 W to 60 W. However, as the puttering power continue increases from 60 W to 90 W, the electrical resistivity increases rapidly. When the puttering power is 60 W, the films deposited on PET substrate have the lowest resistivity of 4.72 × 10⁻⁴ Ω cm and a relatively high transmittance of above 92% in the visible range.     

Scaling behavior and structure transition of ZrO2 films deposited by RF magnetron sputtering

ZrO₂ thin films were deposited onto Si wafers and glass slides by reactive rf magnetron sputtering with varying conditions of substrate temperature (T_s). Structural analysis was carried out using high-resolution transmission electron microscopy (HRTEM) and atomic force microscopy (AFM). The scaling behavior of the AFM topographical profiles was analyzed using one-dimensional power spectral density method (1DPSD). Morphological and structural evolution of ZrO₂ films have been studied in relation to T_s. With substrate temperatures ranging from RT to 550 °C, the structural transition of the films is a-ZrO₂ (below 250 °C) → m-ZrO₂ with a little a-ZrO₂ (450 °C) → m-ZrO₂ with a little t-ZrO₂ (550 °C). The roughness exponent α is 1.53 ± 0.02, 1.04 ± 0.01, 1.06 ± 0.05, 1.20 ± 0.03 for ZrO₂ thin films deposited at RT, 250 °C, 450 °C, and 550 °C, respectively. Quantitative surface characterization by spatially resolved 1DPSD analyses identified three different growth mechanisms of surface morphology for ZrO₂ thin films deposited at RT, 250∼450 °C and 550 °C. The evolution and interactions of surface roughness and microstructure are discussed in terms of surface diffusion, grain growth, and flux shadowing mechanisms.     

Tribological properties of Ti2N-Wx% coatings deposited by magnetron sputtering

Ti₂N-W_x% coatings with different tungsten contents were deposited using unbalanced magnetron sputtering technology. The microstructures and mechanical properties of Ti₂N-W_x% coatings have been characterized by SEM, X-ray diffraction (XRD), nanoindentation and adhesion techniques. The tribological performance of the coatings was investigated using an oscillating friction and wear tester under dry conditions. Indexable inserts with Ti₂N-W_x% coatings were applied to turning AISI 1045 steel material by a lathe. Micron-drills with Ti₂N-W_x% coatings were adopted in the ultra-high speed (10⁵ rpm) Printed Circuit Board (PCB) through-hole drilling test. Experimental results indicate that the coating microstructure, mechanical properties and wear resistance vary according to the tungsten content. Ti₂N-W_14% coated inserts showed the best wear resistance in 1045 steel turning and PCB through-hole drilling tests. The service life of a Ti₂N-W_14% coated tool is five times greater than that of an uncoated tool in PCB through-hole drilling test.     

Switching properties of vanadium doped TiO2 thin films prepared by magnetron sputtering

In the present work thin films of Ti-Me (where Me: V, Nb, Ta) were deposited onto glass substrates by magnetron sputtering of mosaic target in reactive oxygen plasma. The properties of the prepared thin films were studied by X-ray diffraction (XRD), electron dispersive spectroscopy, temperature-dependent electrical and optical transmission spectroscopy measurements. The structural investigations indicate that thin films were XRD-amorphous. Reversible thermoresistance effect, recorded at 52 ± 1 °C was found from electrical measurements. The prepared coatings were well transparent in the visible part of the light spectrum from ca. 350 nm.     

Cu2O thin films deposited by reactive direct current magnetron sputtering

The Cu₂O thin films were prepared on quartz substrate by reactive direct current magnetron sputtering. The influences of oxygen partial pressure and gas flow rate on the structures and properties of deposited films were investigated. Varying oxygen partial pressure leads to the synthesis of Cu₂O, Cu₄O₃ and CuO with different microstructures. At a constant oxygen partial pressure of 6.6 × 10^− 2 Pa, the single Cu₂O films can be obtained when the gas flow rate is below 80 sccm. The as-deposited Cu₂O thin films have a very high absorption in the visible region resulting in the visible-light induced photocatalytic activity.     

Mechanical and deformation behaviour of titanium diboride thin films deposited by magnetron sputtering

Nanoindentation studies have been carried out for TiB₂ films deposited on Si, glass and steel by sputtering for studying the influence of the substrates. It was observed that the modulus of the film was influenced by the substrates from 30 nm onwards. Plastic energy analysis has shown that as load increases more energy is absorbed by the substrate. Quantitative indentation depth limits for obtaining film only hardness, using a combination of log-log plot of load vs displacement and load vs (displacement)² functions, have shown the dependence on the threshold load for crack formation. Comparison of the hardness data with composite hardness models has been performed. Fracture toughness of the coatings was also evaluated using two methods which resulted in comparable results.     

Microstructure and mechanical properties of TiAlN/SiO2 nanomultilayers synthesized by reactive magnetron sputtering

TiAlN/SiO₂ nanomultilayers with different SiO₂ layer thickness were synthesized by reactive magnetron sputtering. The microstructure and mechanical properties were investigated by X-ray diffraction (XRD), high-resolution transmission electron microscopy (HRTEM) and nano-indentation. The results indicated that, under the template effect of B1-NaCl structural TiAlN layers, amorphous SiO₂ was forced to crystallize and grew epitaxially with TiAlN layers when SiO₂ layer thickness was below 0.6 nm, resulting in the enhancement of hardness and elastic modulus. The maximum hardness and elastic modulus could respectively reach 37 GPa and 393 GPa when SiO₂ layer thickness was 0.6 nm. As SiO₂ layer thickness further increased, SiO₂ transformed back into amorphous state and broken the coherent growth of nanomultilayers, leading to the decrease of hardness and elastic modulus.     

Influence of process parameters on structure and optical properties of GeC thin films deposited by RF magnetron sputtering

Germanium carbide (Ge_1 − xC_x) films on silicon and quartz substrates have been prepared by the radio frequency (RF) reactive sputtering of a pure Ge target in a CH₄/Ar discharge. Their structural and optical properties have been investigated as functions of the substrate temperature (T_S) and the CH₄ percentage to the gas mixture. The optical band gap of the films lies within the range 0.96-1.65 eV, varying proportionally with the carbon content and in inverse proportionality with T_S.     

Influence of N2 partial pressure on mechanical properties of (Ti,Al)N films deposited by reactive magnetron sputtering

The influence of the nitrogen partial pressure on the mechanical properties of (Ti,Al)N films deposited by DC reactive magnetron sputtering using a Ti-Al mosaic target at a substrate bias of −100 V is investigated. Nanoindentation tests reveal that with increasing N₂ partial pressure, the film hardness and elastic modulus increase initially and then decrease afterwards. The maximum hardness and elastic modulus are 43.4 GPa and 430.8 GPa, respectively. The trend is believed to stem from the variations in the grain size and preferential orientation of the crystals in the (Ti,Al)N films fabricated at varying N₂ partial pressure. The phenomenon is confirmed by results acquired using glancing angle X-ray diffraction (XRD) and energy dispersive X-ray spectroscopy (EDS).     

Fabrication and characterization of Fe3O4 thin films deposited by reactive magnetron sputtering

Fe-O thin films with different atomic ratio of iron to oxygen were deposited on glass and thermally oxidized silicon substrates at temperatures of 300, 473 and 593 K, by reactive magnetron sputtering in Ar+O₂ atmosphere. The composition and structure of the thin films were characterized by scanning electron microscopy (SEM), X-ray diffraction (XRD), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS) and electrical resistivity. It was found from XRD that with increasing the oxygen partial pressure in the working gas, the crystalline structure of the Fe-O films deposited at the substrate temperature of 473 K gradually changed from α-Fe, amorphous Fe-O, Fe₃O₄, γ-Fe₂O₃ to Fe_21.34O₃₂. The structure and chemical valence of the Fe₃O₄ films were analyzed by electron microscopy and XPS, respectively.