Preparation of CVD diamond coatings on gamma titanium aluminide using MPECVD with various interlayers

CVD diamond coatings were deposited on to γ-TiAl surfaces using a microwave plasma enhanced CVD to improve wear properties and the performance of γ-TiAl. Diamond coatings were directly deposited on to γ-TiAl substrates and deposited on to TiC, Ti₅Si₃, Al₂O₃ + TiO₂, and Si interlayers prepared on γ-TiAl substrates. The diamond coatings deposited directly on γ-TiAl suffered severe delamination and cracked. Those deposited on TiC and Ti₅Si₃ interlayers partially delaminated, whereas those deposited on Al₂O₃ + TiO₂ and Si interlayers adhered well to the underlying surfaces. The diamond films obtained were characterized using scanning electron microscopy, Raman spectroscopy, and X-ray diffraction. Raman spectra showed that polycrystalline and nanocrystalline diamond films grew on γ-TiAl. Residual internal stresses of the diamond coatings deposited on interlayered-γ-TiAl were estimated experimentally from Raman spectra. The coatings prepared on Al₂O₃ + TiO₂/γ-TiAl and Si/γ-TiAl showed lower residual stresses.     

Ag and O ion irradiation induced improvement in dielectric properties of the Ba(Co1/3Nb2/3)O3 thin films

We present the preliminary results of temperature and frequency dependent dielectric measurements on Ba(Co_1/3Nb_2/3)O₃ (BCN) thin films. These films were prepared on indium tin oxide (ITO) coated glass substrates by the pulse laser deposition (PLD) technique. It exhibits single-phase hexagonal symmetry. These films were irradiated with Ag¹⁵⁺ (200 MeV) and O⁷⁺ (100 MeV) beams at the fluence 1 × 10¹¹, 1 × 10¹², and 1 × 10¹³ ions/cm². On irradiating these films, its dielectric constant (?′) and dielectric loss (tan δ) parameters improve compared to un-irradiated film. Compared to O⁷⁺ irradiation induced point/cluster defects Ag¹⁵⁺ induced columnar defects are more effective in reducing/pinning trapped charges within grains. The present paper highlights the role of swift heavy ion irradiation in engineering the dielectric properties of conductive samples to enable them to be useful for microwave device applications.     

Influence of high temperature processing of sol-gel derived barium titanate thin films deposited on platinum and strontium ruthenate coated silicon wafers

Thin films of barium titanate (BTO) of 200 nm thickness, derived from an alkoxide-carboxylate sol-gel process, were deposited on Pt/Ti and SrRuO₃/ZrO₂-8%Y₂O₃ coated Si wafers. Films with a dense columnar microstructure were obtained by repeated deposition of thin amorphous layers from low-concentrated sols, and crystallization at 800 °C. This method added 10 nm thickness to the crystalline BTO film in each deposition step. The harsh processing conditions had a negative impact on the platinized silicon wafers, where Pt-Si silicides were formed. This led to diffusion of Si into BTO and interfacial silicate formation. The interfacial silicate layer was the cause of deteriorated dielectric and ferroelectric properties of the BTO layer. Use of SrRuO₃/ZrO₂-8%Y₂O₃/Si substrates solved the problem. No diffusion of Si was observed, and BTO films with good dielectric and ferroelectric properties were obtained.     

Structure and microwave dielectric properties of Bi1.5Zn1.0Nb1.5O7 thin films deposited on alumina substrates by pulsed laser deposition

Bi_1.5Zn_1.0Nb_1.5O₇ (BZN) thin films were deposited on polycrystalline alumina substrates by pulsed laser deposition at different substrate temperatures. The phase structure and surface morphology were characterized using X-ray diffractometer (XRD) and atomic force microscopy. Microwave dielectric properties were performed using split-post dielectric resonator method at spot frequencies of 10, 15 and 19 GHz, respectively. The XRD results indicate that the as-deposited Bi_1.5Zn_1.0Nb_1.5O₇ thin films deposited at 650 °C are amorphous in nature. The dielectric permittivity and loss tangent of the amorphous BZN thin films are 75.5 and 0.013 at 10 GHz, respectively. As the measure frequency increased to 19 GHz, the dielectric permittivity slightly decreases and loss tangent slightly increases. BZN thin films were crystallized after the post-annealing by a rapid thermal annealing in air for 30 min. The crystallized BZN thin films exhibit the excellent dielectric properties and frequency responses. The dielectric permittivity and loss tangent of the crystallized BZN thin films are 154 and 0.038 at 10 GHz, respectively.     

Effect of processing temperature on characteristics of metal-ferroelectric (BiFeO3)-insulator (HfLaO)-silicon capacitors

The effect of temperature in rapid thermal annealing (RTA) process on the physical and electrical properties of bismuth ferrite ceramic thin films on HfLaO/p-Si substrates has been investigated. In metal-ferroelectric-insulator-silicon (MFIS) capacitors, the high-k HfLaO dielectric layer was prepared as the insulator layer. On HfLaO/Si substrates the bismuth ferrite thin film was fabricated via sputtering process with a BiFeO₃ (BFO) target at room temperature followed by RTA. The RTA temperature ranged from 500 to 700 °C. It is found that the root mean square roughness of ceramic films increases for high-temperature process. The maximum ferroelectric memory window is 1.6 V obtained from a sweep voltage of ± 4 V at the lowest RTA temperature of 500 °C. This good ferroelectric memory performance can be attributed to the low leakage current as a result of smooth surface of nanocrystalline ferroelectric BFO and Bi₂Fe₄O₉ thin films.     

Synthesis of nanocrystalline iron oxide ultrathin films by thermal decomposition of iron nitropruside: Structural and optical properties

Ultrathin films of nanocrystalline α-Fe₂O₃ have been deposited on glass substrates from an inorganic precursor, iron nitropruside. This is a novel route of synthesis for iron oxide thin films on glass substrates, by annealing the precursor thin film in air at 650 °C for 15 min. The films were characterized using TG-DTA analysis, X-ray diffraction, UV-visible, FESEM, AFM and Raman measurements. X-ray diffraction and Raman analyses revealed that the deposited films contain α-phase of Fe₂O₃ (hematite). The synthetic route described here provides a very simple and cost-effective method to deposit α-Fe₂O₃ thin films on glass substrates with band gap energy of about 2.75 eV. The deposited films were found to show catalytic effect for the photo-degradation of phenol.     

Nanograins dependent dielectric constant, tunability, phase transition, impedance spectroscopy and leakage current of (Pb1 − xSrx)TiO3 thin films

Nanostructured (Pb_1 − xSr_x)TiO₃ (PST) (x = 0.1, 0.2 and 0.3) thin films have been prepared by chemical solution deposition process using spin coating technique. The solution as such was deposited on Pt/Ti/SiO₂/Si substrates and annealed at 650 °C/3h. Nanograins dependent dielectric properties of PST films show dielectric constant up to the higher frequency region, low losses, large tunability and phase transition at small temperature. The impedance data has been fitted by Cole-Cole model to study the effect of grain boundaries on the dielectric properties. The current-voltage characteristics have been measured to study leakage current in PST films and described by Poole-Frenkel emission model. It is suggested that the key carrier transport process in PST films is emission of electrons from a trap state near the metal-film interface into a continuum of states associated with each conductive dislocation. The activation energy value for carrier transport in PST films is obtained from temperature-dependent current-voltage characteristics.     

Titanium and zirconium hard coatings on glass substrates prepared by the sol-gel method

In this work innovative antiscratch sol-gel coating films deposited on a soda-lime glass substrate are examined. Sol-gel coatings of different composition (TiO₂, TiO₂/B₂O₃, ZrO₂ and ZrO₂/B₂O₃) were prepared starting from Titanium, Zirconium and Boron alkoxides and from boron oxide. Coatings were obtained at room temperature and at atmospheric pressure by dip-coating using common soda lime silicate glass slides as substrates. Densification was carried out at 550 °C for 2 h in air. The morphology of the coatings has been studied by Atomic Force Microscopy, Scanning Electron Microscopy, and with a profilometer. Roughness grows with thickness and with boron addition. The mechanical properties of the films were evaluated by micro scratch at fixed and variable load. The scratch hardness numbers of ZrO₂ and ZrO₂/B₂O₃ coatings reach 6 GPa (glass value = 1.9 GPa), whereas the best value for the critical load is 16.7 N (glass value = 9 N).     

Crystal orientation dependence of the out-of-plane dielectric properties for barium stannate titanate thin films

The orientation-dependent out-of-plane dielectric properties of barium stannate titanate (Ba(Sn_0.15Ti_0.85)O₃ (BTS)) thin films prepared by sol–gel method were investigated. Films with (1 0 0), (1 1 0), and (1 1 1) orientation were grown on LaNiO₃-buffered (1 0 0), (1 1 0), and (1 1 1) LaAlO₃ (LAO) single-crystal substrates, respectively. The different temperature of the dielectric constant maximum (T_m) of the BTS thin films with different orientation was believed to be attributing to stress inside the films. Films with the (1 1 1) orientation had higher relative dielectric constant and tunability than (1 0 0)- and (1 1 0)-oriented films. This difference in dielectric properties in these three kinds of oriented BTS films may be attributed to change in the direction and magnitude of electric polarization in orientation engineered BTS films and stress in the films.     

Magnetodielectric and dielectric properties of orthorhombic HoMnO3 thin films

Sandwich-structural multilayer films Au/HoMnO₃/YBa₂Cu₃O_7 − δ were prepared epitaxially on SrTiO₃ (001) single crystal substrates by using pulsed laser deposition technique. The HoMnO₃ films crystallized in a metastable orthorhombic structure and the Au and YBa₂Cu₃O_7 − δ were used as electrodes to investigate the dielectric and magnetodielectric properties of HoMnO₃ films. The impedance and electric modulus spectroscopic plots were used to discern the intrinsic characteristics of HoMnO₃ films or unwanted interface effects. The low-temperature (~ 2 K) dependence of the dielectric constant of HoMnO₃ films as function of frequency shows anomalies around 43 K and 22 K, which is corresponding to the Néel temperature and lock-in transition of Mn³⁺ moments, respectively. The magnetodielectric effects of HoMnO₃ films were investigated at 100 kHz under a 2T applied magnetic field, and the dielectric constant was tuned resulting in a decrease of 3%. The results indicate the strong coupling between the dielectric properties and magnetic orders in orthorhombic HoMnO₃ films.     

Reduction of microwave dielectric losses in KTa1 − xNbxO3 thin films by MgO-doping

KTa_1 − xNb_xO₃ (KTN) thin films were grown by pulsed laser deposition on sapphire and MgO substrates. Their structural and high frequency dielectric characteristics evidenced the strong influence of the substrate and suggested possible KTN/MgO interdiffusion that could be responsible for the lower dielectric losses obtained on this substrate. Both undoped and 6% MgO-doped KTN thin films were then grown on sapphire. Dielectric measurements performed at 12.5 GHz by a resonant cavity perturbation method evidenced reduction of losses by MgO-doping. Loss tangent (tan δ) was reduced by a factor of 3 in comparison with undoped films grown on sapphire.     

Electrical properties of Pb0.97La0.02(Zr0.95Ti0.05)O3 antiferroelectric thin films on TiO2 buffer layer

Pb_0.97La_0.02(Zr_0.95Ti_0.05)O₃ antiferroelectric thin films with thickness of 500 nm were successfully deposited on TiO₂ buffered Pt(1 1 1)/Ti/SiO₂/Si(1 0 0) and Pt(1 1 1)/Ti/SiO₂/Si(1 0 0) substrates via sol-gel process. Microstructure of Pb_0.97La_0.02(Zr_0.95Ti_0.05)O₃ thin films was studied by X-ray diffraction analyses. The antiferroelectric nature of the Pb_0.97La_0.02(Zr_0.95Ti_0.05)O₃ thin films was confirmed by the double hysteresis behaviors of polarization and double buffer fly response of dielectric constant versus applied voltage at room temperature. The capacitance-voltage behaviors of the Pb_0.97La_0.02(Zr_0.95Ti_0.05)O₃ films with and without TiO₂ buffer layer were studied, as a function of temperature. The temperature dependence of dielectric constant displayed a similar behavior and the Curie temperature (T_c) was 193 °C for films on both substrates. The current caused by the polarization and depolarization of polar in the Pb_0.97La_0.02(Zr_0.95Ti_0.05)O₃ films was detected by current density-electric field measurement.     

Dielectric properties of sol-gel derived Ta2O5 thin films

The dielectric constant and the dielectric loss of tantalum pentoxide (Ta₂O₅) thin films, produced by sol-gel spin-coated process on Corning glass substrates, have been investigated in the frequency range of 20-10⁵ Hz and the temperature range of 183-403 K, using ohmic Al electrodes. The frequency and temperature dependence of relaxation time has also been determined. The capacitance and loss factor were found to decrease with increasing frequency and increase with increasing temperature. The activation energy values were evaluated and a good agreement between the activation energy values obtained from capacitance and dielectric loss factor measurements were observed.     

Electrical and optical investigations on Pb1 − 3x/2LaxZr0.2Ti0.8O3 thin films obtained by radiofrequency assisted pulsed laser deposition

Thin films of ferroelectric relaxor Pb_1 − 3x/2La_xZr_0.2Ti_0.8O₃, x = 0.22 have been integrated in an oxidic heterostructure for electro-optical investigations. The quadratic electro-optic behavior and optical properties have been studied by means of variable angle spectroscopic ellipsometry method in reflection mode. Birefringence values up to δΔ = 0.17° have been obtained for quadratic compositions at λ = 540 nm and 65° angle of incidence. Structural, chemical and morphologic properties of Pb_1-3x/2La_xZr_0.2Ti_0.8O₃ (x = 0.22) thin films have been investigated by x-ray diffraction and atomic force microscopy techniques. The dielectric and ferroelectric behavior has been investigated using dielectric spectroscopy and a ferroelectric test system.     

Dielectric properties of DC reactive magnetron sputtered Al2O3 thin films

Alumina (Al₂O₃) thin films were sputter deposited over well-cleaned glass and Si < 100 > substrates by DC reactive magnetron sputtering under various oxygen gas pressures and sputtering powers. The composition of the films was analyzed by X-ray photoelectron spectroscopy and an optimal O/Al atomic ratio of 1.59 was obtained at a reactive gas pressure of 0.03 Pa and sputtering power of 70 W. X-ray diffraction results revealed that the films were amorphous until 550 °C. The surface morphology of the films was studied using scanning electron microscopy and the as-deposited films were found to be smooth. The topography of the as-deposited and annealed films was analyzed by atomic force microscopy and a progressive increase in the rms roughness of the films from 3.2 nm to 4.53 nm was also observed with increase in the annealing temperature. Al-Al₂O₃-Al thin film capacitors were then fabricated on glass substrates to study the effect of temperature and frequency on the dielectric property of the films. Temperature coefficient of capacitance, AC conductivity and activation energy were determined and the results are discussed.     

BaxSr1 − xTi1.02O3 metal-insulator-metal capacitors on planarized alumina substrates

Nanocrystalline barium strontium titanate (Ba_xSr_1 − xTi_1.02O₃) thin films with a barium content of x = 0.8, 0.9 and 1 have been fabricated in a metal-insulator-metal configuration on glass-planarized alumina substrates. Cost-effective processing measures have been utilized by using poly-crystalline alumina substrates, wet-chemical processing of the dielectric, and by a small physical area of the ferroelectric capacitors (as low as 50 µm² for radio frequencies measurements). Glass-planarization on alumina ceramic substrates enables barium strontium titanate films with high quality and homogeneity. We mainly focus on fine-tuning the electrical performance in the low gigahertz range (< 10 GHz). Extensive micro-structural and electrical characterization has been performed. Micro-structural information is obtained by: Transmission Electron Microscopy, Scanning Electron Microscopy and X-ray diffraction. The dielectric response is investigated as a function of temperature, frequency and electric field for each sample. We measured a relatively constant permittivity for typical operating temperatures of applications. The quality factor Q is between 21 and 27 at 1 GHz at zero DC bias and the tuning ratio η between 1.8 and 2.2 at |E| = 0.4 MV/cm.     

Synthesis of (Na2O,PbO)-Nb2O5, (Na2O,BaO)-Nb2O5, and (K2O,SrO)-Nb2O5 thin films using sol-gel method

Homogeneous pore-free Ba₂NaNb₅O₁₅, KSr₂Nb₅O₁₅, and 2·Na₂O-PbO-6·Nb₂O₅ thin films were fabricated on sapphire substrates using the sol-gel technique. By controlling the gelation and coating process, thickness of thin films fabricated was controllable from ~ 40 nm to ~ 10 μm. Synthesized thin films possessed highly preferred orientated microstructure. Another advantage of this method is the subsequent heat treatment temperature dramatically decreased compared with other methods. This increases stoichiometry control and makes the large scale fabrication more feasible and efficient.     

Layer-by-layer deposition of zirconia thin films from aqueous solutions

Thin films of ZrO₂ and Y₂O₃-doped ZrO₂ were deposited using a novel yet simple layer-by-layer technique by means of electrostatic assembling and surface precipitation via dipping substrates alternately in cationic and anionic precursor solutions. Uniform films have been made. A constant growth rate of 5.4 ± 0.3 nm per deposition cycle for the dehydrated nanocrystalline films was achieved. This generic technique can be adapted to make other oxide films and novel multilayers or functionally-graded coatings.     

Ferroelectric and dielectric multilayer heterostructures based on KTa0.65Nb0.35O3 and Bi1.5-xZn0.92-yNb1.5O6.92-1.5x-y grown by pulsed laser deposition and chemical solution deposition for high frequency tunable devices

Epitaxial growth of Bi_1.5-xZn_0.92-yNb_1.5O_6.92-1.5x-y (BZN) thin films was achieved on (100)_pc LaAlO₃ substrate by pulsed laser deposition (PLD) and by chemical solution deposition based on Pechini process. Effect of bismuth and zinc deficiency on the BZN thin films obtained by PLD was discussed, in relation with the starting target composition. Dielectric permittivity and bandgap values were determined from electrical and spectroscopic ellipsometry measurements performed on randomly oriented films grown on Pt/Si substrate. BZN thin films obtained by PLD exhibit, at 100 kHz, a dielectric constant of ε_r = 203 and quite low dielectric losses of tanδ = 5 × 10^− 2. Epitaxial ferroelectric − dielectric KTa_0.65Nb_0.35O₃ (KTN) − Bi_1.5-xZn_0.92-yNb_1.5O_6.92-1.5x-y (KTN on BZN and BZN on KTN) bilayers were obtained by PLD on (100)_pc LaAlO₃ with the insertion of a suitable buffer layer of KNbO₃ in the case of KTN on BZN. Such multilayer heterostructures with an epitaxial growth control of each layer are promising candidates for potential integration in microwave devices.     

Preparation and characterization of Ba1 − xSrxTiO3 thin films deposited on Pt/SiO2/Si by sol-gel method

BST thin films have been investigated as potential candidates for use in frequency agile microwave circuit devices. Stoichiometric (Ba_1 − xSr_x)TiO₃ (BST) thin films have been prepared on Pt/SiO₂/Si substrates using sol-gel method. The BST films were characterized by X-ray fluorescence (XRF) spectroscopy analysis, X-ray diffraction (XRD), scanning electron microscope (SEM) and electrical measurements. The relationships of processing parameters, microstructures, and dielectric properties are discussed. The results show that the films exhibit pure perovskite phase through rapid thermal anneal at 700 °C and their grain sizes are about 20-40 nm. The dielectric constants of BST5, BST10, BST15 and BST20 are 323, 355, 382 and 405, respectively, at 80 kHz.