Nano-structured Fe thin film deposition using plasma focus device

This paper reports the deposition of nano-structured Fe thin films using 3.3 kJ Mather-type plasma focus. The conventional hollow copper anode was replaced by anode fitted with solid Fe top and the deposition was done using different numbers of deposition shots at two different angular positions. Scanning Electron Microscopy shows that the size of nano-phase agglomerate is smaller when the sample is deposited using either lesser number of deposition shots or at higher angular position with respect to anode axis. X-ray Diffraction shows that crystal structure characteristics change with increase in number of deposition shots. Measurements of magnetic properties using Vibrating Sample Magnetometer identify intermediate magnetization and coercivity in Fe thin films deposited at smaller angular position with respect to anode axis. It is concluded that the morphological, structural and magnetic characteristics of Fe thin films deposited using plasma focus device depend not only on the number of focus deposition shots but also on the angular position of the sample.     

Synthesis of nano-crystalline zirconium aluminium oxynitride (ZrAlON) composite films by dense plasma Focus device

Zirconium aluminium oxynitride multiphase composite film is deposited on zirconium substrate using energetic nitrogen ions delivered from dense plasma Focus device. X-ray diffractometer (XRD) results show that five Focus shots are sufficient to initiate the nucleation of ZrN and Al₂O₃ whereas 10 Focus shots are sufficient to initiate the nucleation of AlN. XRD results reveal that crystal growth of nitrides/oxides increases by increasing Focus shots (up to 30 Focus shots) and resputtering of the previously deposited film is taken place by further increase in Focus shots (40 Focus shots). Scanning electron microscopic (SEM) results indicate the uniform distribution of spherical grains (∼35 nm). A smoother surface is observed for 20 Focus shots at 0° angular position. SEM results also show a net-type microstructure (thread like features) of the sample treated for 30 Focus shots whereas rough surface morphology is observed for 40 Focus shots. Energy dispersive spectroscopic profiles show the distribution of different elements present in the deposited composite films. A typical microhardness value of the deposited composite films is 5255 ± 10 MPa for 10 grams imposed load which is 3.3 times than the microhardness values of unexposed sample. The microhardness values of the exposed samples increases with increasing Focus shots (up to 30 Focus shots) and decreases for 40 Focus shots treatment due to resputtering of the previously deposited composite film. The microhardness values of the composite films decreases by increasing the sample's angular position.     

Room-temperature epitaxial growth of CeO2(001) films on YSZ buffered Si(001) substrates

2 (001) epitaxial thin films deposited on Si(001) with yttria-stabilized zirconia buffers have been obtained for the first time at room temperature by pulsed-laser deposition. The influence of oxygen pressure on the crystal quality of CeO₂ was studied for the films deposited at 100 °C. The rocking curve full width at half maximum of the CeO₂(002) peak for films deposited at room temperature and 100 °C was between 1° and 2°, for oxygen pressures below 3×10^-2 mbar. The best crystal quality was obtained at around 3×10^-3 mbar. Epitaxial growth at room temperature was confirmed by cross-sectional transmission electron microscopy. Scanning electron microscopy and atomic force microscopy revealed very smooth surfaces for oxygen pressure below 3×10^-2 mbar, with rms roughness values around 0.3 nm over 5 μm×5 μm. Received: 25 September 1997/Accepted: 22 April 1998     

Diffusion and chemical composition of TiNxOy thin films studied by Rutherford Backscattering Spectroscopy

Thickness and chemical composition of the TiN_xO_y thin films deposited by reactive magnetron sputtering from Ti target at controllable oxygen flow rate were determined by Rutherford Backscattering Spectroscopy (RBS) using 2 MeV He⁺ ions. The films were deposited on carbon foils and amorphous silica (a-SiO₂) substrates at 25 °C and 250 °C. The estimated film thickness is of 75-100 nm. The O/Ti atomic ratio in the films increases up to 1.5 with increasing oxygen flow rate, while that of N/Ti decreases from about 1.1 for TiN to 0.4 at the highest oxygen flow rate. Substantial out-diffusion of carbon from the substrate is observed which is independent of the substrate temperature. Films grown onto a-SiO₂ substrates can be treated as homogeneous single layers without interdiffusion. It is more difficult to determine the nitrogen and oxygen content due to superposition of RBS signals arising from film and substrate. RBS analysis of the depth profile indicates that for the investigated films the carbon diffusion and oxidation not only at the topmost surface layers but over the bulk of the films were found. Comparison with XPS results indicates substantial oxygen adsorption at the surface of TiN_x thin films obtained at zero oxygen flow rate.     

Low energy repetitive miniature plasma focus device as high deposition rate facility for synthesis of DLC thin films

Diamond-like carbon (DLC) films were deposited on Si (1 0 0) substrate using a low energy (219 J) repetitive (1 Hz) miniature plasma focus device. DLC thin film samples were deposited using 10, 20, 50, 100 and 200 focus shots with hydrogen as filling gas at 0.25 mbar. The deposited samples were analyzed by XRD, Raman Spectroscopy, SEM and XPS. XRD results exhibited the diffraction peaks related to SiO₂, carbon and SiC. Raman studies verified the formation amorphous carbon with D and G peaks. Corresponding variation in the line width (FWHM) of the D and G positions along with change in intensity ratio (I_D/I_G) in DLC films was investigated as a function of number of deposition shots. XPS confirmed the formation sp² (graphite like) and sp³ (diamond like) carbon. The cross-sectional SEM images establish the 220 W repetitive miniature plasma focus device as the high deposition rate facility for DLC with average deposition rate of about 250 nm/min.     

The effect of TiN nanoparticles deposition with different number of shots on SS316L by plasma focus device

In this paper, we present the result of TiN nanocrystalline deposition on SS316L, using a 4 kJ plasma focus (PF) device for 10, 20, and 30 focus shots. The effect of different number of focus shots on micro-structural changes of thin film is characterized by field emission scanning electron microscope. Existence of grains in different size confirms the formation of TiN nanocrystals on the surface of SS316L substrate. X-ray diffraction (XRD) reveals the formation of a nanocrystalline titanium nitride coating on the surface of SS316L samples. The crystalline size of TiN obtained from XRD data is strongly dependent on the number of focus shots. Thickness of the elements found on the surface of the treated sample that obtain by Rutherford backscattering spectroscopy (RBS) analysis is in the range of 150×10¹⁵?200×10¹⁵ atoms/cm². All the existence elements in the coated samples are identified by Particle Induced X-ray Emission (PIXE) spectra. Investigation on the corrosion resistance of TiN coatings was performed using an electrochemical potentiodynamic polarization. Our results suggest that TiN nanocrystalline implantation with proper ion fluences using PF can significantly improve the corrosion resistance of SS316L.     

Structural and optical properties of a-Si1−xCx:H films synthesized by dc magnetron sputtering technique

Hydrogenated amorphous SiC films (a-Si_1−xC_x:H) were prepared by dc magnetron sputtering technique on p-type Si(1 0 0) and corning 9075 substrates at low temperature, by using 32 sprigs of silicon carbide (6H-SiC). The deposited a-Si_1−xC_x:H film was realized under a mixture of argon and hydrogen gases. The a-Si_1−xC_x:H films have been investigated by scanning electronic microscopy equipped with an EDS system (SEM-EDS), X-ray diffraction (XRD), secondary ions mass spectrometry (SIMS), Fourier transform infrared spectroscopy (FTIR), UV-vis-IR spectrophotometry, and photoluminescence (PL). XRD results showed that the deposited film was amorphous with a structure as a-Si_0.80C_0.20:H corresponding to 20 at.% carbon. The photoluminescence response of the samples was observed in the visible range at room temperature with two peaks centred at 463 nm (2.68 eV) and 542 nm (2.29 eV). In addition, the dependence of photoluminescence behaviour on film thickness for a certain carbon composition in hydrogenated amorphous SiC films (a-Si_1−xC_x:H) has been investigated.     

Structural evolution of nanocrystalline/amorphous Fe/Ni75B25 multilayers: temperature dependence of electrical resistivity

X-ray specular-reflectivity measurements have been carried out on nanocrystalline/amorphous Fe/Ni₇₅B₂₅ multilayer films which were sputter-deposited on Si substrates, to investigate the evolution of interface roughness and the correlation between structure and transport properties. A significant interface roughness correlation with increasing Fe/NiB layer repetition was observed. The investigated films indicated a temperature dependent high electrical resistivity—10⁴ μΩ-cm at 10 K and 10³ μΩ-cm at 300 K—with a semiconductor-metal transition like behavior. Selected area electron diffraction revealed the presence of crystalline bcc Fe phase and NiB in amorphous state. The structural and transport properties of the multilayers are discussed.     

Structural and luminescent characteristics of pulsed laser deposited Eu3+-doped Y2O3 thin films

Thin films of Eu-doped Y₂O₃ were deposited using the pulsed laser ablation technique on amorphous fused silica substrates. The effect of oxygen partial pressure (pO₂) and substrate temperature on the structural and optical characteristics of the deposited films were investigated. All the deposited films were crystalline, showing preferred orientation along the (111) plane, irrespective of oxygen partial pressure and substrate temperature. The film deposited at 0.005?mbar pO₂ exhibited better crystallinity with minimum FWHM at a substrate temperature of 600°C. All the films deposited at various substrate temperatures and different partial pressure (at 600°C) exhibited a red luminescence peak at 615?nm corresponding to the ⁵D₀–⁷F₁ transition in Eu³⁺. Photoluminescence excitation spectra exhibited two bands, one corresponding to band to band excitation (212?nm) of the host and the other to charge transfer band excitation (245?nm). A microstructure analysis revealed that surface roughness of the as-deposited films increases with increase in oxygen partial pressure.     

Elemental depth profiling of a-Si1−xGex:H films by elastic recoil detection analysis and secondary ion mass spectrometry

The hydrogen content in a-Si_1−xGe_x:H thin films is an important factor deciding the density and the optical band gap. We measured the elemental depth profiles of hydrogen together with Si and Ge by elastic recoil detection analysis (ERDA) combined with Rutherford backscattering (RBS) using MeV He²⁺ ions. In order to determine the hydrogen depth profiles precisely, the energy- and angle-dependent recoil cross-sections were measured in advance for the standard sample of a CH₃⁺-implanted Si substrate. The cross-sections obtained here are reproduced well by a simple expression based on the partial wave analysis assuming a square well potential (width: r₀ = 2.67 × 10⁻¹³ cm, depth: V₀ = −36.9 MeV) within 1%. For the a-Si_1−xGe_x:H films whose elemental compositions were determined by ERDA/RBS, we measured the secondary ions yields of HCs₂⁺, SiCs₂⁺, H⁻, Si⁻ and Ge⁻ as a function of Ge concentration x. As a result, it is found that the useful yield ratios of HCs₂⁺/SiCs₂⁺, H⁻/Si⁻ and Ge⁻/Si⁻ are almost constant and thus the elemental depth profiles of the a-Si_1−xGe_x:H films can be also determined by secondary ion mass spectrometry (SIMS) within 10% free from a matrix effect.     

Atomic layer deposition of HfO2 on graphene from HfCl4 and H2O

Atomic layer deposition of HfO₂ on unmodified graphene from HfCl₄ and H₂O was investigated. Surface RMS roughness down to 0.5 nm was obtained for amorphous, 30 nm thick hafnia film grown at 180°C. HfO₂ was also deposited in a two-step temperature process where the initial growth of about 1 nm at 170°C was continued up to 10–30 nm at 300°C. This process yielded uniform, monoclinic HfO₂ films with RMS roughness of 1.7 nm for 10–12 nm thick films and 2.5 nm for 30 nm thick films. Raman spectroscopy studies revealed that the deposition process caused compressive biaxial strain in graphene, whereas no extra defects were generated. An 11 nm thick HfO₂ film deposited onto bilayer graphene reduced the electron mobility by less than 10% at the Dirac point and by 30–40% far away from it.     

Reactively sputtered Ni, Ni(N) and Ni3N films: Structural, electrical and magnetic properties

Nickel thin films were deposited on glass substrates at different N₂ gas contents using a dc triode sputtering deposition system. Triode configuration was used to deposit nanostructured thin films with preferred orientation at lower gas pressure and at lower substrate temperature compared to the dc diode sputtering system. A gradual evolution in the composition of the films from Ni, Ni(N), to Ni₃N was found by X-ray diffraction analysis. The preferred growth orientation of the nanostructured Ni films changed from (1 1 1) to (1 0 0) for 9% N₂ at 100 °C. Ni₃N films were formed at 23% N₂ with a particle size of about 65 nm, while for 0% and 9% of nitrogen, the particles sizes were 60 nm, and 37 nm, respectively, as obtained by atomic force microscopy. Magnetic force microscopy imaging showed that the local magnetic structure changed from disordered stripe domains of about 200 nm for Ni and Ni(N) to a structure without a magnetic contrast, indicating the paramagnetic state of this material, which confirmed the structural transformation from Ni to Ni₃N.     

Composition, XRD and morphology study of laser prepared LiNbO3 films

LiNbO₃ films were deposited by PLD from LiNbO₃ crystalline or from three different stoichiometric or Li-enriched LiNbO₃ targets. Polycrystalline films were prepared on SiO₂/Si or sapphire substrates at temperatures T _S ～650–750 °C. Main attention was paid to the influence of targets preparation and the deposition conditions on films composition, morphology and crystallinity. The thin-film morphology was determined by SEM microscopy. The composition was measured by SIMS, RBS, PIXE and PIGE methods. Highly oriented, smooth and stoichiometric LiNbO₃ films were synthesized.     

Pulsed KrF laser deposited GaN/TiN/Si(111) heterostructures by sequential TiN and liquid Ga laser ablation

GaN/TiN heterostructures were deposited on 4° miscut Si(111) substrates by pulsed KrF laser ablation of TiN through vacuum, followed by reactive pulsed KrF laser ablation of liquid Ga through 70-75 mTorr of microwave-activated NH₃. Deposition temperatures of 950 °C and 1050 °C were employed for the TiN layer while 900 °C was employed for the GaN layer. The targets were positioned 5 cm from the substrate and ablated by using a reimaging beamline at a nominal energy density of 3-4 J/cm². X-ray diffraction (XRD) revealed a highly textured heterostructure with GaN(0001)//TiN(111)//Si(111) and with a rocking curve width for both GaN(0001) and TiN(111) equal to ~1.1°. The mosaic spread through the TiN(001) reflection was ~1.3°, whereas that of the GaN(101_1) was undetectable because of low S/N. Scanning electron microscopy revealed large oriented 10 7m-sized hexagonal crystallites decorating large depressions in the TiN film with many smaller pits also present. The effect of substrate processing and TiN film processing on pit formation was explored.     

用激光分子束外延在Si衬底上外延生长高质量的TiN薄膜

采用激光分子束外延技术,利用两步法,在Si单晶衬底上成功地外延生长出TiN薄膜材料.原子力显微镜分析结果显示, TiN薄膜材料表面光滑,在10 μm×10 μm范围内,均方根粗糙度为0842nm.霍耳效应测量结果显示,TiN薄膜在室温条件下的电阻率为36×10^-5Ω·cm,迁移率达到5830 cm²/V·S,表明TiN薄膜材料是一种优良的电极材料.X射线θ—2θ扫描结果和很高的迁移率均表明,高质量的TiN薄膜材料被外延在Si衬底 关键词： 激光分子束外延 TiN单晶薄膜 外延生长     

Characterization of ultrathin nickel layers on Si(111) using RHEED and RBS

Ultrathin nickel layers (0–40 Å) on Si(111) were characterized using reflection high energy electron diffraction (RHEED) in conjunction with high-resolution Rutherford backscattering spectrometry (RBS). RBS shows that Ni, when deposited on Si(111) at 300 K, reacts with the Si to form clusters with an average composition close to Ni₂Si, until the clusters coalesce into a continuous layer. RHEED measurements show that the microstructure of this layer also matches the Ni₂Si composition: the film consists mainly of very fine-grained Ni₂Si crystallites (∼ 15 Å grain size) which are randomly oriented. Additional Ni deposition results in the accumulation of an unreacted fine-grained Ni layer on top of the silicide film.     

The interplay between molecular orientation, film morphology and luminescence properties of tetracene thin films on epitaxial AlOx/Ni3Al(1 1 1)

We report a systematic study of the interplay between molecular orientation, film morphology and luminescence properties of tetracene thin films on epitaxial alumina films on Ni₃Al(1 1 1), employing high resolution electron energy loss spectroscopy (HREELS), X-ray photoelectron spectroscopy (XPS), low energy electron diffraction (LEED), and photoluminescence spectroscopy (PL). If deposited at low temperatures, tetracene forms laterally disordered and compact films in which at least the first monolayer is oriented parallel to the substrate. For thicknesses in the range of 10 Å or below, these as-deposited films show no luminescence, while thicker films exhibit weak luminescence from higher layers. On annealing to 210 K, tetracene films dewet the AlO_x/Ni₃Al(1 1 1) surface and transform into an island morphology. At the same time, molecules tend to re-orient into a more upright configuration. In this island configuration, even thin films show luminescence. We can thus conclude that in spite of the insulating nature of the surface, the interaction of flat-lying tetracene molecules with AlO_x/Ni₃Al(1 1 1) is strong enough to provide at least one efficient non-radiative decay channel.     

Deposition of tungsten nitride thin films by plasma focus device at different axial and angular positions

Tungsten nitride thin films were deposited on stainless steel-304 substrates by using a low energy (2 kJ) Mather type plasma focus device. X-ray diffraction (XRD), scanning electron microscopy (SEM), atomic force microscopy (AFM) and microhardness are used to study the surface of treated samples. The XRD analysis shows that the degree of crystallinity of deposited thin films strongly depends on axial and angular positions of samples. The SEM micrographs of the deposited films at different angular positions (0°, 10° and 30°) and axial position of 8 cm show that the content of WN sub-micro crystalline structures on the surface of deposited films decreased with increasing the angle with respect to anode axis. From AFM results we observe that for the sample deposited at 8 cm and 0° axial and angular positions, respectively, the most uniform surface and the most homogenous distribution of grains are obtained. Also the hardness results show that the highest mechanical hardness is obtained when the film is deposited at 8 cm and 0° axial and angular positions, respectively.     

Preparation and characterization of metallorganic chemical vapour deposited LixMoyOz using a single source solid precursor

Thin films of Li_xMo_yO_z have been deposited on glass substrate in a one step chemical vapour deposition using a single source solid precursor. The films were characterized using Rutherford Backscattering Spectroscopy (RBS), X-Ray Diffractometry, Scanning Electron Microscopy (SEM), Impedance Spectroscopy (IS), van der Pauw conductivity measurement and Ultraviolet-Visible Spectroscopy. Results of the characterization showed that the films are dendritic, polycrystalline and semiconducting with an optical transition energy of 3.0 eV. IS characterization gave a semicircle in the complex impedance plot. The conductivity vs. temperature plot showed a transition at 450 °C and also a hysteresis. Analysis showed the film to be mixture of phases.     

Pulsed laser deposition of magnetic films by ablation of Co- and Fe-based amorphous alloys

Magnetic films were prepared by pulsed laser ablation of amorphous magnetic ribbons (composition Co₆₇Cr₇Fe₄Si₈B₁₄, Fe_73.5Nb₃Cu₁Si_13.5B₉, and Fe₄₀Ni₄₀B₂₀) and permalloy foils (composition Fe_xNi_1-x with x=22,50). Depositions were performed in a vacuum of (2–4)×10^-5 Pa by KrF excimer laser pulses at fluences of between 2 and 7 Jcm². Films were deposited on oxidized silicon wafers, placed 60–80 mm apart from the target. Films were analyzed by SEM, XRD, RBS, and EDS. Ferromagnetic resonance (FMR) spectra were studied at GHz frequencies. From RBS and EDS measurements it follows that the stoichiometry of the targets is preserved in the films to a large extent. The films deposited from amorphous targets remain amorphous. From FMR studies it follows that Fe and Fe-Ni rich films exhibit properties close to those of bulk alloys, having very low magnetization motion damping parameter () of 7.0–7.8×10⁷ rad/s, which are appropriate for fast magnetic sensors. PACS 79.20.Ds; 75.50.Kj; 75.70.-i