Synthesis and surface acoustic wave properties of AlN films deposited on LiNbO3 substrates

The c-axis-oriented aluminum nitride (AlN) films were deposited on z-cut lithium niobate (LiNbO₃) substrates by reactive RF magnetron sputtering. The crystalline orientation of the AlN film determined by x-ray diffraction (XRD) was found to be dependent on the deposition conditions such as substrate temperature, N₂ concentration, and sputtering pressure. Highly c-axis-oriented AlN films to fabricate the AlN/LiNbO₃-based surface acoustic wave (SAW) devices were obtained under a sputtering pressure of 3.5 mTorr, N₂ concentration of 60%, RF power of 165 W, and substrate temperature of 400°C. A dense pebble-like surface texture of c-axis-oriented AlN film was obtained by scanning electron microscopy (SEM). The phase velocity and the electromechanical coupling coefficient (K²) of SAW were measured to be about 4200 m/s and 1.5%, respectively. The temperature coefficient of frequency (TCF) of SAW was calculated to be about -66 ppm/°C     

Effect of beam voltage on the properties of aluminium nitride prepared by ion beam assisted deposition

The effects of nitrogen-beam voltage on the structure, stress, energy band gap and hardness of AIN thin films deposited on Si (111), Si (100) and sapphire (0001) by ion beam assisted deposition (IBAD) are reported. As the nitrogen-beam voltage was increased from 50 to 200 V, the stress and disorder in the AIN films increased as determined by X-ray diffraction, FTIR and Raman spectroscopy. The preferred orientation of the film's c-axis changed from completely normal to the film at 100 V, to a mixture of normal and in the plane of the film at 200 V. For AIN films deposited under the same conditions, the films were more highly oriented on sapphire (0001) than in Si (111). The hardness of the films increased from 18.2 to 23.7 GPa with the nitrogen-beam voltage, and possible reasons for this change in hardness are considered.     

Effect of substrate temperature and bias voltage on the crystallite orientation in RF magnetron sputtered AlN thin films

The crystal orientation and residual stress of AlN thin films were investigated using X-ray diffraction and substrate curvature method. The AlN films were deposited on Si(100) by RF magnetron sputtering in a mixed plasma of argon and nitrogen under various substrate negative bias V_s (up to − 100 V) and deposition temperature T_s up to 800 °C. The results show that lower temperature and moderate bias favor the formation of (002) plane parallel to the substrate surface. On the contrary, strong biasing beyond − 75 V and deposition temperature higher than 400 °C lead to the growth of (100) plane. At the same time nanoindentation hardness and compressive stress measured by substrate curvature method showed significant enhancement with substrate bias and temperature. The biased samples develop compressive stress while unbiased samples exhibit tensile or compressive stress depending on plasma power and temperature. The relationships between deposition conditions and crystallographic orientation of the films are discussed in terms of surface energy minimization and ion bombardment effects.     

Influence of the ion-atom flux ratio on the mechanical properties of chromium nitride thin films

In this paper we report the mechanical properties of chromium nitride (CrN) thin films deposited at different levels of ion bombardment and their relationship with the microstructural parameters, such as grain size, preferred orientation and residual stress. The samples were deposited by unbalanced magnetron sputtering changing the substrate-target distance and the substrate bias, keeping other deposition condition fixed. The mechanical properties were obtained by nanoindentation performed on 1.8 μm thick samples. Under the different deposition conditions all of the CrN films were approximately stoichiometric, but clear variations in the microstructure were seen. The hardness was nearly constant at 24-27 GPa even when the grain size, residual stress and crystalline orientation changed. However, the elastic modulus showed a steady increase from 300 to 350 GPa, proportional to the variations in grain size and the residual stress level.     

Deposition of AlN films by reactive sputtering: Effect of radiofrequency substrate bias

Piezoelectric AlN thin films were deposited on Silicon substrates by triode reactive sputtering. The variation of residual stress versus bias voltage on the substrate was investigated. A compressive stress was always observed with a maximum value for a negative substrate bias of 50 V. For higher negative bias voltage values, the compressive stress decreases. X-ray diffraction measurements showed two kinds of growth orientation. First, without bias voltage, films are well crystallized and (002) oriented. Second, with bias voltage, the (002) orientation disappears and a small peak appears (situated in the 2θ = 32°-33° range) which can be attributed to (100) orientation. Finally, the influence of compressive stress and ion bombardment on the change of orientation is discussed.     

Influence of the aluminum incorporation on the structure of sputtered ZrNx films deposited at low temperatures

We have studied the influence of the Al incorporation in the crystalline structure of ZrN thin films deposited by dc magnetron sputtering processes at low temperature. The incorporation of the aluminum in the films depends directly on the Ar/N₂ ratio in the gas mixture and the power applied to the aluminum cathode during the deposition. The chemical composition and the crystalline structure of the films were analyzed by Energy Dispersive X-ray (EDX) spectroscopy and X-ray Diffraction (XRD), respectively. When Al atoms are incorporated into the ZrN coatings, the strong ZrN (200) preferred orientation is modified to a combination of phases related to (111) ZrN with a contribution of cubic (111) AlN and possibly (211) Zr₃N_4, which are detected by XRD for high aluminum concentrations. Fourier Transform Infrared (FTIR)spectroscopy allowed us to complete the identification of the nitrides and oxides incorporated into the deposited films. The effect of a bias voltage applied to the substrate has also been investigated and related to the changes in the microstructure and in the nanohardness values of the ZrAlN films.     

Preferential growth of ZnO thin films by the atomic layer deposition technique

Preferred orientation of ZnO thin films deposited by the atomic layer deposition (ALD) technique could be manipulated by deposition temperature. In this work, diethyl zinc (DEZn) and deionized water (H(2)O) were used as a zinc source and oxygen source, respectively. The results demonstrated that (10.0) dominant ZnO thin films were grown in the temperature range of 155-220?°C. The c-axis crystal growth of these films was greatly suppressed. Adhesion of anions (such as fragments of an ethyl group) on the (00.2) polar surface of the ZnO thin film was believed to be responsible for this suppression. In contrast, (00.2) dominant ZnO thin films were obtained between 220 and 300?°C. The preferred orientations of (10.0) and (00.2) of the ZnO thin films were examined by XRD texture analysis. The texture analysis results agreed well with the alignments of ZnO nanowires (NWs) which were grown from these ZnO thin films. In this case, the nanosized crystals of ZnO thin films acted as seeds for the growth of ZnO nanowires (NWs) by chemical vapor deposition (CVD) process. The highly (00.2) textured ZnO thin films deposited at high temperatures, such as 280?°C, contained polycrystals with the c?axis perpendicular to the substrate surface and provided a good template for the growth of vertically aligned ZnO NWs.     

The characterization of sputtered polycrystalline aluminum nitrideon silicon by surface acoustic wave measurements

Polycrystalline aluminum nitride films were deposited on Si₃ N₄ coated (100) silicon substrates by the reactive sputtering method. We have carried out experiments to evaluate the effect of AlN material parameters on the SAW characteristics. The SAW transducers were fabricated by forming interdigitated Al electrodes on top of the AlN films and transmission measurements made over the frequency range from 50 MHz to 1.5 GHz. The SAW characteristics were correlated with material parameters of crystallite orientation, grain size, surface morphology and oxygen concentration. A key material parameter affecting the SAW characteristics was found to be the preferred degree of crystallite orientation with the c-axis normal to the plane of the substrate. The better oriented the AlN grains, the stronger the SAW response, the higher the SAW phase velocity, and the lower the insertion and propagation losses over the entire frequency range of measurement. Above 500 MHz the propagation losses of the well oriented films followed a frequency squared dependence only slightly higher than the reported values for the best epitaxial films. The coupling factors deduced from the transducer characteristics are in the upper range of values reported by Tsubouchi for epitaxial AlN films deposited on the basal plane of sapphire. There was a strong correlation between the X-ray diffraction intensity from the (002) planes and the oxygen content in the films     

Synthesis of c-axis oriented AlN thin films on different substrates: A review

Highly c-axis oriented AlN thin films have been deposited by reactive sputtering on different substrates. The crystallographic properties of layered film structures consisting of a piezoelectric layer, aluminum nitride (AlN), synthesized on a variety of substrates, have been examined. Aluminum nitride thin films have been deposited by reactive pulsed-DC magnetron sputtering using an aluminum target in an Ar/N₂ gas mixture. The influence of the most critical deposition parameters on the AlN thin film crystallography has been investigated by means of X-ray diffraction (XRD) analysis of the rocking curve Full-Width at Half Maximum (FWHM) of the AlN-(0 0 0 2) peak. The relationship between the substrate, the synthesis parameters and the crystallographic orientation of the AlN thin films is discussed. A guide is provided showing how to optimize these conditions to obtain highly c-axis oriented AlN thin films on substrates of different nature.     

Synthesis of aluminum nitride thin films by filtered arc ion plating deposition

Thin films of aluminum nitride (AlN) were deposited on stainless steel and glass substrates by a modified deposition technique, filtered arc ion plating, at an enhanced deposition rate. X-ray diffraction spectra confirmed the exclusive presence of AlN hexagonal wurtzite phase. Under a mixed gas (Ar + N₂) pressure of 0.90 Pa and a bias voltage of − 400 V, the deposited films exhibited a fairly low surface roughness of 2.23 nm. The thin films were proved higher than 75% transparent in the visible spectral region. The bonding strength between the film and substrate was verified higher than 20 N. Thus high performance of such AlN thin films can be expected in applications.     

等离子体辅助反应式脉冲激光熔蚀制备AlN薄膜的低温生长

使用等离子体辅助反应式脉冲激光溅射沉积薄膜的方法在Ｓｉ（１１１）和Ｓｉ（１００）基片上已经成功地低温制备出ＡｌＮ多晶膜。实验表明,当脉冲能量密度ＤＥ＝１．０Ｊ·ｃｍ－２,脉冲频率ｆ＝５Ｈｚ,氮气气压ＰＮ２＝１．３３×１０４Ｐａ,基底温度ｔｓｕｂ＝２００℃,放电电压Ｖ＝６５０Ｖ,基靶距离ｄＳ－Ｔ＝４ｃｍ时薄膜的生长速度等于６ｎｍ／ｍｉｎ。ＡｌＮ薄膜的折射率为２．０５,和基底的取向关系分别为：ＡｌＮ（１１０）∥Ｓｉ（１１１）和ＡｌＮ（１００）∥Ｓｉ（１００）。     

The influence of deposition rate on the stress and microstructure of AlN films deposited from a filtered cathodic vacuum arc

Aluminium nitride (AlN) thin films have been reactively deposited using a filtered cathodic vacuum arc system. A pulsed substrate bias was applied in order to increase the average energy of the depositing species. The stress and microstructure of the films were determined as a function of the deposition rate and pulse bias amplitude/frequency. The stress generated in films grown with high voltage pulsed bias depended on the deposition rate and a transition from tensile stress to compressive stress occurred as the deposition rate increased. This trend was accompanied by progressive changes in the microstructure. In order of increasing deposition rate, the films exhibited: a porous structure with tensile stress; a dense AlN film with compressive stress; and a dense AlN film showing evidence of a thermally induced reduction in stress.     

Growth of highly c-axis oriented aluminum nitride thin films on β-tantalum bottom electrodes

We have investigated the influence of tantalum (Ta) bottom electrodes on the crystallinity and crystal orientation of aluminum nitride (AlN) thin films. AlN thin films and Ta electrodes were prepared by using rf magnetron sputtering method. The crystal structure of the Ta electrodes was tetragonal (β-Ta, a metastable phase) at room temperature. The crystallinity and orientation of the AlN thin films and Ta electrodes strongly depended on sputtering conditions. Especially, the crystallinity and crystal orientation of the Ta electrodes were influenced by their film thickness and the substrate temperature. When the thickness of the Ta bottom electrodes was 200 nm and the substrate temperature was 100 °C, the AlN thin films indicated high c-axis orientation (the full width at half maximum of rocking curve of 3.9°). The crystal orientation of the AlN film was comparable to that of AlN thin films deposited on face centered cubic (fcc) lattice structure metal, such as Au, Pt and Al, bottom electrodes.     

Growth of columnar aluminum nitride layers on Si(111) by molecular beam epitaxy

Single crystalline aluminum nitride (AlN) thin films are deposited by molecular beam epitaxy (MBE) using thermally evaporated aluminum and RF-plasma excited nitrogen gas. In this paper we report on films grown on Si(111) at substrate temperatures of 800° with growth rates between 65 and 350 nm h⁻¹. All layers consist of hexagonal and exactly c-axis oriented AlN crystals with column-like structure. For the smoothest layers surface roughness (rms) around 1 nm is obtained. In the XRD-spectra (ω-scan) we have achieved a minimum FWHM of 0.4° (=25′) for the AlN(00.2) reflex. At maximum growth rates (350 nm h⁻¹) for AlN a transition zone of about 200 nm is formed with high defect density compared to the subsequent growth. For lower growth rates (65 nm h⁻¹) no transition zone exists. Application of a substrate nitridation leads to a partial loss of epitaxial relation between AlN layer and Si(111)-substrate.     

Synthesis and characterization of 4H-SiC on C-plane sapphire by C60 and Si molecular beam epitaxy

4H-SiC (silicon carbide) films were grown on (0001) sapphire substrate at rather low temperatures(1000-1100 °C) with relative high deposition rate by using fullerene (C₆₀) and silicon solid sources molecular beam epitaxy with substrate nitridation and aluminum nitride (AlN) buffer layer deposition prior to the SiC deposition. The effects of substrate nitridation and AlN buffer layer to the adhesion of the SiC thin films on sapphire have been studied. X-Ray diffraction, pole figure, atomic force microscope, Fourier transform infrared spectroscopy and photoluminescence were employed for the analysis of composition, orientation of the film and surface morphology. Relative high deposition rate at ∼ 165 nm/h was achieved.     

Optimization of the annealing process and nanoscale piezoelectric properties of (002) AlN thin films

In this paper, the effects of different annealing processes on the texture, surface morphology, and piezoelectric properties of aluminum nitride (AlN) thin films and the performance of AlN-based surface acoustic wave (SAW) devices were systematically investigated. Based on the crystallinity and the morphology results, it is evident that in-situ annealing method is superior to ex-situ annealing. For the AlN thin films, the crystallization and piezoelectricity were both enhanced and then receded as the annealing temperature increased from 300 to 600?°C. We demonstrated that good (002) orientation, excellent grain distribution and high relative piezoelectric coefficient of the AlN thin films were achieved via in-situ annealing at 500?°C. Meanwhile, the AlN thin films exhibited excellent polarization properties and polarization maintaining characteristics. Additionally, the uniform interdigital transducer (IDT) with 8 μm period (finger width?=?2 μm) were designed and the IDT/AlN/SiO₂/Si SAW devices with the center frequency f ₀ of 495 MHz and insert loss of ?24.1 dB were fabricated.     

超高真空电子束蒸发合成晶态AlN薄膜的研究

用超高真空蒸发Ａｌ膜，结合氮化合处理工艺在Ｓｉ（１００）衬底上制备了ＡｌＮ晶态薄膜，用Ｘ射线衍射，傅立叶变换红外光谱和Ｘ射线光电子能谱等测试分析技术研究了薄膜的微结构特征。结果表明：经过１０００℃分钟氮化处理后，能形成具有（００２）择优取向的ＡｌＮ薄膜。     

Effect of heating on the residual stresses in TiN films investigated using synchrotron radiation

The structure and residual stresses of TiN films deposited by arc ion plating (AIP) on a steel substrate were investigated using a synchrotron radiation system that emits ultra-intense X-rays. In a previous study, the crystal structures of TiN films deposited by AIP were found to be strongly influenced by the bias voltage. When high bias voltages were used, TiN films that were approximately 200 nm thickness had a preferred orientation of {110}, whereas TiN films that were approximately 600 nm thickness has a multilayer film orientation of {111}/{110}. In this present study, the two-tilt method was used to evaluate the residual stresses in TiN films by measuring lattice strains in two directions determined by the crystal orientation. Residual stresses in 600-nm-thick as-deposited TiN films were found to be −10.0 GPa and −8.0 GPa for {111}- and {110}-textured layers, respectively, while they were −8.0 GPa for {110}-textured layers in 200-nm-thick as-deposited TiN films. Residual stresses of both films relaxed to thermal stress levels upon annealing.     

The preparation and characterization of preferred (110) orientation aluminum nitride thin films on Si (100) substrates by pulsed laser deposition

The preferred (110) oriented aluminum nitride (AlN) thin films have been prepared by pulsed laser deposition on p-Si (100) substrates. The films were characterized with X-ray diffraction, Raman spectroscopy, Fourier transform infrared spectroscopy, X-ray photoelectron spectroscopy and atomic force microscope (AFM). The results indicate that the AlN thin films are well-crystallized when laser energy is higher than 300 mJ/puls. The AFM images show that the surface roughness of the deposited AlN thin films gradually increases with increasing laser energy, but the surface morphologies are still very smooth. The crystallinity and morphology of the thin films are found to be strongly dependent on the laser energy.     

SAW COM-parameter extraction in AlN/diamond layered structures

Highly c-axis oriented aluminum nitride (AlN) thin piezoelectric films have been grown on polycrystalline diamond substrates by pulsed direct current (DC) magnetron reactive sputter-deposition. The films were deposited at a substrate temperature below 50/spl deg/C (room temperature) and had a typical full width half maximum (FWHM) value of the rocking curve of the AlN-002-peak of 2.1 degrees. A variety of one-port surface acoustic wave (SAW) resonators have been designed and fabricated on top of the AlN films. The measurements indicate that various SAW modes are excited. The SAW phase velocities of up to 11.800 m/s have been measured. These results are in agreement with calculated dispersion curves of the AlN/diamond structure. Finally, the coupling of modes parameters have been extracted from S/sub 11/ measurements using curve fitting for the first SAW mode, which indicate an effective coupling K/sup 2/ of 0.91% and a Q factor of about 600 at a frequency of 1050 MHz.