Reactive species in RF plasma sputtering deposition of nanocrystalline calcium phosphate bio-active films

Optical emission of reactive plasma species during the synthesis of functionally graded calcium phosphate-based bioactive films has been investigated. The coatings have been deposited on Ti-6Al-4V orthopedic alloy by co-sputtering of hydroxyapatite (HA) and titanium targets in reactive plasmas of Ar + H2O gas mixtures. The species, responsible for the Ca-P-Ti film growth have been non-intrusively monitored in situ by a high-resolution optical emission spectroscopy (OES). It is revealed that the optical emission originating from CaO species dominates throughout the deposition process. The intensities of CaO, PO and CaPO species are strongly affected by variations of the operating pressure, applied RF power, and DC substrate bias. The optical emission intensity (OEI) of reaction species can efficiently be controlled by addition of H2O reactant.

Study of the processes occurring when sputtering YBa2Cu3O7-x in pure oxygen

The sputter deposition of YBa2Cu3O7-x in a de-diode was performed in pure oxygen medium and an optical spectroscopic study of the resultant discharge revealed strong emissions from both metal atoms and oxygen ions. Emission intensities were studied in pressure range from 0.5 to 3 mbar, with substrate temperatures from 150 to 850 degrees C. Raising the substrate temperature to 850 degrees C increased the number of positive ions and excited neutral atoms. Raising the pressure decreased the emission intensities of excited neutral and ionic species. The results have been compared with those obtained from Langmuir probe measurements. The rise in emission intensities of excited neutrals and ions with temperature suggested the possibility of chemically enhanced physical sputtering of YBa2Cu3O7-x. The effect of process conditions on film composition and quality is also discussed.

Effect of oxygen partial pressure on the structural and optical properties of dc reactive magnetron sputtered molybdenum oxide films

Molybdenum oxide films (MoO3) were deposited on glass and crystalline silicon substrates by sputtering of molybdenum target under various oxygen partial pressures in the range 8 × 10−5–8 × 10−4 mbar and at a fixed substrate temperature of 473 K employing dc magnetron sputtering technique. The influence of oxygen partial pressure on the composition stoichiometry, chemical binding configuration, crystallographic structure and electrical and optical properties was systematically studied. X-ray photoelectron spectra of the films formed at 8 × 10−5 mbar showed the presence of Mo6+ and Mo5+ oxidation states of MoO3 and MoO3−x. The films deposited at oxygen partial pressure of 2 × 10−4 mbar showed Mo6+ oxidation state indicating the films were nearly stoichiometric. It was also confirmed by the Fourier transform infrared spectroscopic studies. X-ray diffraction studies revealed that the films formed at oxygen partial pressure of 2 × 10−4 mbar showed the presence of (0 k 0) reflections indicated the layered structure of α-phase MoO3. The electrical conductivity of the films decreased from 3.6 × 10−5 to 1.6 × 10−6 Ω−1 cm−1, the optical band gap of the films increased from 2.93 to 3.26 eV and the refractive index increased from 2.02 to 2.13 with the increase of oxygen partial pressure from 8 × 10−5 to 8 × 10−4 mbar, respectively.

dc reactive magnetron sputtering of titanium‐structural and optical characterization of TiO2 films

This paper deals with the reactive sputtering of titanium in an argon and oxygen mixture. The variation in cathode potential as a function of oxygen partial pressure has been explained in terms of cathode poisoning effects. The titania films deposited during this process have been studied for their structural and optical characteristics. The effect of substrate temperature (from 25 to 400 °C) and annealing (from 250 to 700 °C) on the packing density, refractive index, extinction coefficient, and crystallinity has been investigated. The refractive index varied from 2.24 to 2.46 and extinction coefficient from 2.6 × 10-3 to 10.4× 10-3 at 500 nm as the substrate temperature increased from 25 to 400 °C. The refractive index increased from 2.19 to 2.35 and extinction coefficient changed from 3.2× 10-3 to 11.6 × 10-3 at 500 nm as the annealing temperature was increased from 250 to 700 °C. Anatase and rutile phases have been observed in the films deposited at 400 °C substrate temperature and annealed at 300 °C. The changes in the optical constants at higher substrate temperature have been attributed to an increase in packing density, oxygen content, and crystallinity of the films.

Diaphragm-type sputtered platinum thin film strain gauge pressure transducer

A diaphragm-type pressure transducer with a sputtered platinum film strain gauge (sensing film) has been designed and fabricated. The various steps followed to prepare thin film strain gauges on the diaphragm are described. M-bond 450 adhesive (Measurements Group, USA) has been employed as the insulating layer. A detailed procedure to cure this layer is given. A d.c. sputtering method is employed to prepare the platinum films. This paper also includes details of the strain gauge pattern and its location on the diaphragm. A description of the output characteristics and overall behaviour of the platinum thin film pressure transducer is reported.

Effect of Oxygen Pressure on Structural and Magnetic Properties of YIG Thin Films

The effect of oxygen pressure (P-O2) on the Yttrium Iron Garnet (YIG) thin films were grown on silicon substrate by rf sputtering method was studied. The as-deposited films at 300K were amorphous in nature. The crystallization of these films was achieved by annealing at a temperature of 800 degrees C/1hr in air. The structural, microstructural and magnetic properties were found to be dependent on P-O2.

A comparative study of room temperature ferromagnetism in MgO films deposited by rf/dc sputtering using high purity Mg and MgO targets

Thin films of nanocrystalline MgO were deposited on glass/Si substrates by rf/dc sputtering from metallic Mg, and ceramic MgO targets. The purpose of this study is to identify the differences in the properties, magnetic in particular, of MgO films obtained on sputter deposition from 99.99% pure metallic Mg target in a controlled Nitrogen + Oxygen partial pressure (O(2)pp)] atmosphere as against those deposited using an equally pure ceramic MgO target in argon + identical oxygen ambience conditions while maintaining the same total pressure in the chamber in both cases. Characterization of the films was carried out by X-ray diffraction, focussed ion beam cross sectioning, atomic force microscopy and SQUID-magnetometry. The `as-obtained' films from pure Mg target are found to be predominantly X-ray amorphous, while the ceramic MgO target gives crystalline films, (002) oriented with respect to the film plane. The films consisted of nano-crystalline grains of size in the range of about 0.4 to 4.15 nm with the films from metallic target being more homogeneous and consisting of mostly subnanometer grains. Both the types of films are found to be ferromagnetic to much above room temperature. We observe unusually high maximum saturation magnetization (MS) values of 13.75 emu/g and similar to 4.2 emu/g, respectively for the MgO films prepared from Mg, and MgO targets. The origin of magnetism in MgO films is attributed to Mg vacancy (V-Mg), and 2p holes localized on oxygen sites. The role of nitrogen in enhancing the magnetic moments is also discussed.

On the quality of hydrogenated amorphous silicon deposited by sputtering

Amorphous hydrogenated silicon (a-Si:H) is well-known material in the global semiconductor industry. The quality of the a-Si:H films is generally decided by silicon and hydrogen bonding configuration (Si-H-x, x=1,2) and hydrogen concentration (C-H). These quality aspects are correlated with the plasma parameters like ion density (N-i) and electron temperature (T-e) of DC, Pulsed DC (PDC) and RF plasmas during the sputter-deposition of a-Si:H thin films. It was found that the N-i and T-e play a major role in deciding Si-H-x bonding configuration and the C-H value in a-Si:H films. We observed a trend in the variation of Si-H and Si-H-2 bonding configurations, and C-H in the films deposited by DC, Pulsed DC and RF reactive sputtering techniques. Ion density and electron energy are higher in RF plasma followed by PDC and DC plasma. Electrons with two different energies were observed in all the plasmas. At a particular hydrogen partial pressure, RF deposited films have higher C-H followed by PDC and then DC deposited films. The maximum energy that can be acquired by the ions was found to be higher in RF plasma. Floating potential (V-f) is more negative in DC plasma, whereas, plasma potential (V-p) is found to be more positive in RF plasma. (C) 2014 Elsevier Ltd. All rights reserved.

Effect of sputtering parameters on the structure, microstructure and magnetic properties of Tb-Fe films

The effect of sputtering parameters such as gas pressure and power on the structure, microstructure and magnetic properties of sputtered Tb-Fe thin films was investigated. X-ray diffraction and transmission electron microscopy studies showed that all the films were amorphous in nature irrespective of the sputtering parameters. A fine island kind of morphology was observed at low sputtering power whereas large clusters were seen at higher sputtering power. While the composition of Tb-Fe films remained constant with increasing sputtering power, the magnetic behaviour was found to change from superparamagnetic to ferromagnetic. On the other hand, the increase in argon gas pressure was found to deplete the iron concentration in Tb-Fe thin films, which in turn reduced the anisotropy and Curie temperature. Annealing of the films at 773 K did not result in any crystallization and the magnetic properties were also found to remain unchanged. (C) 2015 Elsevier B.V. All rights reserved.

Chemical sputtering of ta-C: Implications for the deposition of carbon nitride

The majority of attempts to synthesize the theoretically predicted superhard phase β-C3N4 have been driven towards the use of techniques which maximize both the carbon sp3 levels and the amount of nitrogen incorporated within the film. However, as yet no attempt has been made to understand the mechanism behind the resultant chemical sputter process and its obvious effect upon film growth. In this work, however, the chemical sputtering process has been investigated through the use of an as-deposited tetrahedrally bonded amorphous carbon film with a high density nitrogen plasma produced using an rf-based electron cyclotron wave resonance source. The results obtained suggested the presence of two distinct ion energy dependent regimes. The first, below 100 eV, involves the chemical sputtering of carbon from the surface, whereas the second at ion energies in excess of 100 eV exhibits a drop in sputter rate associated with the subplantation of nitrogen within the carbon matrix. Furthermore, as the sample temperature is increased there is a concomitant decrease in sputter rate suggesting that the rate is controlled by the adsorption and desorption of additional precursor species rather than the thermal desorption of CN. A simple empirical model has been developed in order to elucidate some of the primary reactions involved in the sputter process. Through the incorporation of various previously determined experimental parameters including electron temperature, ion current density, and nitrogen partial pressure the results indicated that molecular nitrogen physisorbed at the ta-C surface was the dominant precursor involved in the chemical sputter process. However, as the physisorption enthalpy of molecular nitrogen is low this suggests that activation of this molecular species takes place only through ion impact at the surface. The obtained results therefore provide important information for the modeling and growth of high density carbon nitride. © 2001 American Institute of Physics.

The effects of oxygen partial pressure on the optical absorption edge and the UV emission energy of ZnO films

The optical absorption edge and ultraviolet (UV) emission energy of ZnO films deposited by direct current (DC) reactive magnetron sputtering at room temperature have been investigated. With the oxygen ratio increasing, the structure of films changes from zinc and zinc oxide coexisting phase to single-phase ZnO and finally to the highly (002) orientation. Both the grain size and the stress of ZnO film vary with the oxygen partial pressure. Upon increasing the oxygen partial pressure in the growing ambient, the visible emission in the room-temperature photoluminescence spectra was suppressed without sacrificing the band-edge emission intensity in the ultraviolet region. The peaks of photoluminescence spectra were located at 3.06---3.15 eV. From optical transmittance spectra of ZnO films, the optical band gap edge was observed to shift towards shorter wavelength with the increase of oxygen partial pressure.

Effect of growth conditions on the GaN thin film by sputtering deposition

The phase transition between thermodynamically stable hexagonal wurtzite (h-WZ) gallium nitride (GaN) and metastable cubic zinc-blende (c-ZB) GaN during growth by radio-frequency planar magnetron sputtering is studied. GaN films grown on substrates with lower mismatches tend to have a h-WZ structure, but when grown on substrates with higher mismatches, a c-ZB structure is preferred. GaN films grown under high nitrogen pressure also tend to have a h-WZ structure, whereas a c-ZB structure is preferred when grown under low nitrogen pressure. In addition, low target-power growth not only helps to improve hexagonal GaN (h-GaN) crystalline quality at high nitrogen pressure on low-mismatch substrates, but also enhances cubic GaN (c-GaN) quality at low nitrogen pressure on high-mismatch substrates. (c) 2007 Elsevier B.V. All rights reserved.

P-doped p-type ZnO films deposited on Si substrate by radio-frequency magnetron sputtering

P-doped ZnO films were deposited on n-Si substrate by radio-frequency magnetron sputtering. Hall measurements revealed that the films annealed in situ at 750 degrees C in an oxygen ambient at a pressure of 1.3x10(-3)-3.9x10(-3) Pa showed p-type behavior with a hole concentration of 2.7x10(16)-2.2x10(17) cm(-3), a mobility of 4-13 cm(2)/V s, and a resistivity of 10.4-19.3 Omega cm. Films annealed at 750 degrees C in a vacuum or in oxygen ambient at higher pressures (5.2x10(-3) and 6.5x10(-3) Pa) showed n-type behavior. Additionally, the p-ZnO/n-Si heterojunction showed a diodelike I-V characteristic. Our results indicate that P-doped p-type ZnO films can be obtained by annealing in oxygen ambient at very low pressures. (c) 2006 American Institute of Physics.

Properties of tantalum oxynitride thin films produced by magnetron sputtering: the influence of processing parameters

The main purpose of this work is to present and to interpret the change of structure and physical properties of tantalum oxynitride (TaNxOy) thin films, produced by dc reactive magnetron sputtering, by varying the processing parameters. A set of TaNxOy films was prepared by varying the reactive gases flow rate, using a N2/O2 gas mixture with a concentration ratio of 17:3. The different films, obtained by this process, exhibited significant differences. The obtained composition and the interpretation of X-ray diffraction results, shows that, depending on the partial pressure of the reactive gases, the films are: essentially dark grey metallic, when the atomic ratio (N + O)/Ta < 0.1, evidencing a tetragonal β-Ta structure; grey-brownish, when 0.1 < (N + O)/Ta < 1, exhibiting a face-centred cubic (fcc) TaN-like structure; and transparent oxide-type, when (N + O)/Ta > 1, evidencing the existence of Ta2O5, but with an amorphous structure. These transparent films exhibit refractive indexes, in the visible region, always higher than 2.0. The wear resistance of the films is relatively good. The best behaviour was obtained for the films with (N + O)/Ta ≈ 0.5 and (N + O)/Ta ≈ 1.3.

Construção de um aparato experimental para monitoramento in situ da deposição de filmes finos de titânio por magnetron sputtering

The technique of surface coating using magnetron sputtering is one of the most widely used in the surface engineering, for its versatility in obtaining different films as well as in the micro / nanometric thickness control. Among the various process parameters, those related to the active species of the plasma are of the most fundamental importance in the mechanism and kinetics of deposition. In order to identify the active species of the plasma, parameters such as gas flow, pressure and density of electric power were varied during titanium coating on glass substrate. By flowing argon gas of 10, 20, 30, 40 and 50 sccm (cubic centimeters per minute) for each gas flow a sequential scan of the electric current of 0.10, 0.20, 0.30, 0.40 , 0.50 A. The maximum value of 0.50 A was chosen based both on literature data and on limitations of the equipment. The monitoring of plasma species present during the deposition was carried out in situ by the technique of optical emission spectroscopy (OES) through the spectrometer Ocean Optics USB2000 Series. For this purpose, an apparatus was developed to adapt the OES inside the plasma reactor to stay positioned closest to the target. The radiations emitted by the species were detected by an optical fiber placed behind the glass substrate and their intensities as a function of wavelength were, displayed on a monitor screen. The acquisition time for each condition of the plain parameters was related to the minima of spectral lines intensities due to the film formed on the substrate. The intensities of different emission lines of argon and titanium were then analyzed as a function of time, to determine the active species and estimate the thickness of the deposited films. After the deposition, the coated glasses thin films were characterized by optical transmittance through an infrared laser. It was found that the thickness and deposition rate determined by in situ analysis were consistent with the results obtained by laser transmittance