磁控反应溅射制备择优取向氮化铝薄膜

以氮气为反应气体，采用磁控反应溅射方法制备了择优取向的氮化铝薄膜．通过XRD测试发现．靶基距、溅射气压影响薄膜的择优取向：大的靶基距及高的溅射气压利于（100）面择优取向，小的靶基距和低的溅射气压利于（002）面择优取向．通过对沉积速率的分析发现．高的沉积速率利于（002）面择优取向，低的沉积速率利于（100）面择优取向．研究结果表明：沉积速率影响了核在衬底表面的生长方向，从而影响了各晶面的生长速度．最终决定薄膜的择优取向．     

Optical properties of aluminium nitride films obtained by pulsed laser deposition: an ellipsometric study

Aluminium nitride (AlN) films obtained by pulsed laser deposition (PLD) at different low ambient nitrogen pressure have been optically investigated by spectral ellipsometry within the 300–800 nm wavelength range, Sellmeier and Wemple–DiDomenico approximation approaches have been applied for the ellipsometric data analysis. Optical parameters such as refractive index and single oscillator energies of deposited films were estimated and their dependence on the N₂ pressure was studied. The obtained refractive index values of AlN films are around 2 in a wide wavelength region above 400 nm and suggest the growth of a polycrystalline structure. The relatively low (<3.4 eV) threshold energies indicate the formation of a defective and disordered structure, formed during the deposition process. PACS 78.20.-e; 78.20.Ci; 78.66.Fd     

GaN缓冲层对直流反应磁控溅射AlN薄膜的影响(英文)

通过直流磁控反应溅射制备了氮化铝(AlN)薄膜,研究了沉积条件与氮化镓(GaN)缓冲层对薄膜质量的影响。利用X-射线衍射仪(XRD)和扫描电镜(SEM)表征了AlN薄膜的晶体结构和表面形貌。XRD研究结果表明,低工作压强、短靶距和适当的氮气偏压有利于(002)择优取向的AlN薄膜沉积。随着沉积时间的增加,沉积在50 nm厚的GaN缓冲层上的AlN薄膜的(002)面的衍射峰的半高宽急剧减小,而沉积在1μm厚的GaN薄膜上的AlN薄膜的(002)面的衍射峰的半高宽几乎不变。SEM测试结果表明:在沉积的初期,沉积在1μm厚的GaN薄膜上的AlN薄膜的(002)面的晶粒大小分布比沉积在50 nm厚的GaN缓冲层上的AlN薄膜的均匀,而随着沉积时间的增加,它们的晶粒大小分布几乎趋向一致。     

Texturing effects in molybdenum and aluminum nitride films correlated to energetic bombardment during sputter deposition

Molybdenum films sputter-deposited at low pressure show a (110) to (211) texture turnover with increasing film thickness, which is accompanied by a transition from a fiber texture to a mosaic-like texture. The degree of (002) texturing of sputtered aluminum nitride (AlN) films strongly depends on nitrogen pressure in Ar/N₂ or in a pure N₂ atmosphere. For the understanding of these phenomena, the power density at the substrate during sputter deposition was measured by a calorimetric method and normalized to the flux of deposited atoms. For the deposition of Mo films and various other elemental films, the results of the calorimetric measurements are well described by a model. This model takes into account the contributions of plasma irradiation, the heat of condensation and the kinetic energy of sputtered atoms and reflected Ar neutrals. The latter two were calculated by TRIM.SP Monte Carlo simulations. An empirical rule is established showing that the total energy input during sputter deposition is proportional to the ratio of target atomic mass to sputtering yield. For the special case of a circular planar magnetron the radial dependence of the Mo and Ar fluxes and related momentum components at the substrate were calculated. It is concluded that mainly the lateral inhomogeneous radial momentum component of the Mo atoms is the cause of the in-plane texturing. For AlN films, maximum (002) texturing appears at about 250 eV per atom energy input. Received: 23 June 2000 / Accepted: 12 December 2000 / Published online: 3 April 2001     

Influence of substrate temperature and ion-beam energy on the syntheses of aluminium nitride thin films by nitrogen-ion-assisted pulsed-laser deposition

Aluminium nitride (AlN) thin films have been grown on Si(100), Si(111) and Sapphire Al₂O₃(001) substrates by pulsed KrF excimer laser (wavelength 248 nm, duration 30 ns) ablation of an AlN target with the assistance of nitrogen-ion-beam bombardment. The influence of process parameters such as substrate temperature and ion-beam energy has been investigated in order to obtain high-quality AlN films. The AlN films deposited by pulsed-laser deposition (PLD) have been characterized by X-ray diffraction (XRD) to determine the crystalline quality, grain size and growth orientation with respect to the substrate. The XRD spectra of AlN films on Si(100), Si(111) and Sapphire substrates yield full-width-half-maximum (FWHM) values of approximately 1.6. The bonding characteristics in the films have been evaluated by Raman spectroscopy. The chemical composition of the films has been characterized by X-ray photoelectron spectroscopy (XPS). The surface morphology of the films has been measured by atomic force microscopy (AFM). At a substrate temperature of at least 600 °C, polycrystalline AlN films with orientations of AlN(100) and AlN(101) have been synthesized. PACS 68.55.-a; 81.15.Fg; 77.84.Bw     

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.     

AlN thin films prepared by ArF plasma assisted PLD. Role of process conditions on electronic and chemical–morphological properties

Aluminium nitride thin films were deposited on n-Si <100> substrates by RF plasma activated reactive pulsed laser deposition (PLD). An ArF excimer pulsed laser, 10 Hz and 2.5 J/cm² energy fluence, has been used to ablate a pure Al target in a reactive atmosphere of N₂ plasma (generated by a RF source), at varying processing parameters (substrate temperature, time, and N₂ plasma configuration). We studied the dependence and correlation of structural and electronic properties with the experimental conditions. The chemical composition of deposited material has been determined by both Raman and X-ray photoelectron spectroscopy (XPS). Electrical resistivity has been evaluated by the sheet resistance method. Both spectroscopic characterizations (Raman and XPS) show a strong dependence in the formation of AlN on the deposition temperature. At low temperatures, there is little formation of nitride, with a prevalence of aluminium oxide, while at higher temperatures the N uptake increases, with AlN formation. Raman analysis also highlights the formation of nano-structures, for temperatures ≥400^°C. These material characteristics have a fundamental influence on the electronic properties. Indeed, electrical resistivity properties have been found to be strongly dependent on the film structure, nitrogen incorporation, and presence of mixed oxide compounds, closely related to deposition temperature.     

Growth and characteristics of reactive pulsed laser deposited molybdenum trioxide thin films

Molybdenum trioxide thin films were prepared by reactive pulsed laser deposition on Corning 7059 glass substrates. The influence of oxygen partial pressure and deposition temperature on the structure, surface morphology and optical properties of these films was studied to understand the growth mechanism of MoO₃ thin films. The films formed at 473 K in an oxygen partial pressure of 100 mTorr exhibited predominantly a (0k0) orientation, corresponding to an orthorhombic layered structure of α-MoO₃. The evaluated optical band gap of the films was 3.24 eV. The crystallite size increased with increase of deposition temperature. The films formed at an oxygen partial pressure of pO₂=100 mTorr and at a deposition temperature greater than 700 K exhibited both (0k0) and (0kl) orientations, representing α-β mixed phases of MoO₃. The films formed at an oxygen partial pressure less than 100 mTorr were found to be sub-stoichiometric with α-β mixed phases. The investigation revealed the growth of polycrystalline and single-phase orthorhombic-layered-structure α-MoO₃ thin films with composition nearly approaching the nominal stoichiometry at moderate substrate temperatures in an oxygen partial pressure of 100 mTorr. Received: 9 April 2001 / Accepted: 6 August 2001 / Published online: 17 October 2001     

Structural evolution and epitaxial stabilisation of pulsed laser deposited Sm0.55Nd0.45NiO3 solid solution nanostructured films on undoped Si (1 0 0) and NdGaO3 substrates

We report on the effects of substrate, ambient oxygen pressure and deposition time on the crystal structure, and morphology of Sm_0.55Nd_0.45NiO₃ solid solution nanostructured films synthesized by pulsed-laser deposition. In each film the structure was found to be consistent with a perovskite structure with preferential planes growth and reveals a strong orientation along the orthorhombic (2 1 0) plane of the perovskite subcell for the film deposited on NdGaO₃ where highly crystalline films were obtained within 15 min deposition time with a low surface roughness of 8.79 nm. Similar structure is observed on Si (1 0 0) substrate only at O₂ pressure of 0.4 mbar. The surface morphology of the different samples shows a net dense film structure with several droplets population. The nano-scaled droplets are in general spherical in shape; a detailed analysis indicates that the laser ablation of this nickelate family is governed to a certain extent by a heat transfer phenomenon.     

Crystallographic orientation dependence of the dielectric constant in polymorphic BaNb<Subscript>2</Subscript>O<Subscript>6</Subscript> thin films deposited by laser ablation

Well-crystallized barium metaniobate (BaNb₂O₆) thin films were fabricated on fused quartz substrates by pulsed laser deposition. The influence of substrate temperature and oxygen pressure on the crystal structure and preferred orientation were studied to understand the growth mechanism of BaNb₂O₆ thin films. The films formed at 600 °C at an oxygen pressure of 100 mTorr exhibited predominantly the orthorhombic (040) orientation, and turned to the orthorhombic (230) orientation at 800 °C. It was found that (220)-oriented hexagonal thin films were formed at 600 °C at an oxygen pressure less than 50 mTorr. The dielectric constant of the BaNb₂O₆ thin films was measured by scanning microwave microscopy (SMM). Preferentially (230)-oriented orthorhombic and (220)-oriented hexagonal BaNb₂O₆ thin films were shown to have significantly enhanced dielectric constants of 47.8 and 56.7, respectively. This could be attributed to the dependence of the dielectric constant on crystallographic orientation. PACS 77.55.+f; 77.84.Dy     

Influence of substrate crystallography on the room temperature synthesis of AlN thin films by reactive sputtering

A pulsed DC reactive ion beam sputtering system has been used to synthesize aluminium nitride (AlN) thin films at room temperature by reactive sputtering. After systematic study of the processing variables, high-quality polycrystalline films with preferred c-axis orientation have been grown successfully on silicon and Au/Si substrates with an Al target under a N₂/(N₂ + Ar) gas flow ratio of 55%, 2 mTorr processing pressure and keeping the temperature of the substrate holder at room temperature. The crystalline quality of the AlN layer as well as the influence of the substrate crystallography on the AlN orientation has been characterized by high-resolution X-ray diffraction (HR-XRD). Best ω-FWHM (Full Width at Half Maximum) values of the (0 0 0 2) reflection rocking curve in the 1 μm thick AlN layers are 1.3°. Atomic Force Microscopy (AFM) measurements have been used to study the surface morphology of the AlN layer and Transmission Electron Microscopy (TEM) measurements to investigate the AlN/substrate interaction. AlN grew off-axis from the Si substrate but on-axis to the surface normal. When the AlN thin film is deposited on top of an Au layer, it grows along the [0 0 0 1] direction but showing a two-domain structure with two in-plane orientations rotated 30° between them.     

Fabrication of piezoelectric AlN thin film for FBARs

This paper focuses on the fabrication of film bulk acoustic-wave resonator (FBAR) comprising an aluminum nitride (AlN) piezoelectric thin film sandwiched between two metal electrodes and located on a silicon substrate with a low-stress silicon nitride (Si₃N₄) support membrane for high frequency wireless applications, and analyzes the optimization of the thin AlN film deposition parameters on Mo electrodes using the reactive RF magnetron sputter system. Several critical parameters of the sputtering process such as RF power and Ar/N₂ flow rate ratio were studied to clarify their effects on different electrodes characteristics of the AlN films. The experiment indicated that the process for Mo electrode was easier compared with that of the Pt/Ti or Au/Cr bi-layer electrode as it entailed only one photo resist and metal deposition step. Besides, Pt/Ti or Au/Cr electrodes reduced the resonance frequency due to their high mass density and low bulk acoustic velocity. Compared with the case of the Al bottom electrode, there is no evident amorphous layer between the Mo bottom electrode and the deposited AlN film. The characteristics of the FBAR devices depend not only upon the thickness and quality of the AlN film, but also upon the thickness of the top electrode and the materials used. The results indicate that decreasing the thickness of either the AlN film or the top electrode increases the resonance frequency. This suggests the potential of tuning the performance of the FBAR device by carefully controlling AlN film thickness. Besides, increasing either the thickness of the AlN film or higher RF power has improved a stronger c-axis orientation and tended to promote a narrower rocking curve full-width at half-maximum (FWHM), but increased both the grain size and the surface roughness. An FBAR device fabricated under optimal AlN deposition parameters has demonstrated the effective electromechanical coupling coefficient (k _eff²) and the quality factor (Q _{f x} ) are about 1.5% and 332, respectively.     

Growth of b-axis oriented VO2 thin films on glass substrates using ZnO buffer layer

VO₂ thin films are grown on glass substrates by pulsed laser deposition using vanadium metal as a target. In this study, a ZnO thin film was used as a buffer layer for the growth of VO₂ thin films on glass substrates. X-ray diffraction studies showed that the VO₂ thin film had b-axis preferential orientation on a c-axis oriented ZnO buffer layer. The thickness of the ZnO buffer layer and the oxygen pressure during VO₂ deposition were optimized to grow highly b-axis oriented VO₂ thin films. The metal-insulator transition properties of the VO₂ film samples were investigated in terms of infrared reflectance and electrical resistance with varying temperatures.     

AlN:Cr thin films synthesized by pulsed laser deposition: Studies by X-ray diffraction and spectroscopic ellipsometry

The structure and optical properties of AlN thin films doped with Cr atoms were studied by X-ray diffractometry, Fourier transform infrared spectroscopy and spectroscopic ellipsometry analyses. The films were synthesized by pulsed laser deposition from an AlN:Cr (10% Cr) target onto Si(1 0 0) wafers in vacuum at residual pressure of 10⁻³ Pa or in nitrogen at a dynamic pressure of 0.1 Pa. The study of the XRD patterns revealed that both phases co-existed in the synthesized films and that the amorphous one was prevalent. Two different amorphous matrices, i.e. two types of chemical bond arrangements, were found in films deposited at 0.1 Pa N₂. By difference, deposition in vacuum resulted in the coexistence of hexagonal and cubic crystallites embedded into an amorphous matrix. The introduction of Cr atoms into the AlN lattice causes a broadening of the IR spectrum along with the shift toward higher wavenumbers of the characteristic Al-N bands at 2351 cm⁻¹ and 665 cm⁻¹, respectively. This was related to the generation of a compressive stress inside films. In comparison to the optical constants of pure AlN films, the synthesized AlN:Cr films exhibited a smaller refractive index and showed a weak absorption throughout the 300-800 nm spectral region, characteristic to amorphous AlN structure.     

Effect of oxygen pressure on structure and properties of Bi1.5Zn1.0Nb1.5O7 pyrochlore thin films prepared by pulsed laser deposition

The Bi₂O₃-ZnO-Nb₂O₅ (BZN) cubic pyrochlore thin films were prepared on Pt/TiO₂/SiO₂/Si(1 0 0) substrates by using pulsed laser deposition process. The oxygen pressure was varied in the range of 5-50 Pa to investigate its effect on the structure and dielectric properties of BZN thin films. It is found that oxygen pressure during deposition plays an important role on structure and other properties of BZN films. The BZN films deposited at temperature of 650 °C and at O₂ pressure of 5 Pa have an amorphous BZN and Nb₂O₅ phases but exhibits a cubic pyrochlore structure with a preferential (2 2 2) orientation when the oxygen pressure increases to 10 Pa. Dielectric constant and loss tangent of the films deposited at 10 Pa are 185 and 0.0008 at 10 kHz, respectively. The dielectric tunability is about 10% at a dc bias field of 0.9 MV/cm.     

Influence of oxygen on structural and optoelectronic properties of CdS thin film deposited by magnetron sputtering technique

In this study, CdS thin films with thicknesses of approximately 100 nm were deposited at a substrate temperature of 100 °C by a sputtering technique under two different ambient conditions—pure Ar ambient and Ar/O₂ (99:1) ambient—at deposition power densities of 1.0 and 2.0 W/cm², respectively The films were polycrystalline with a preferential orientation along the (002) crystal plane; however, the films deposited in the Ar/O₂ ambient exhibited reduced crystallinity. Furthermore, the crystallite sizes, micro-strains, and dislocation densities of the films were significantly affected by oxygen diffusion into the films’ crystal structures. The CdS films deposited in the Ar/O₂ ambient demonstrated higher optical transmittance and higher bandgaps. Morphologies observed from scanning electron microscopy images revealed that the grains of the films were also significantly affected by the oxygen present in the deposition ambient. Additionally, photoluminescence analysis revealed that the sulfur vacancies in the CdS films were partially filled by oxygen atoms, causing significant variations in the electrical properties of the films.     

Selective fabrication of n‐ and p‐type SnO films without doping

Undoped n‐ and p‐type tin monoxide (SnO) films have been selectively fabricated by pulsed laser deposition with a Sn target and careful control of oxygen partial pressure. The films are epitaxially grown in optimal growth conditions on yttria‐stabilized zirconia (YSZ) substrates with out‐of‐plane and in‐plane orientation relationships of (001)_SnO//(001)_YSZ and [110]_SnO//[100]_YSZ, respectively. Both Seebeck and Hall measurements show consistent results on the carrier types of the films. The electron Hall mobility is approximately 11 cm²/Vs at room temperature and the carrier activation energy is 0.14 eV for the n‐type film. The growth at increased oxygen partial pressure yields p‐type films, demonstrating the selective fabrication of both n‐ and p‐type SnO films without doping. (© 2015 WILEY‐VCH Verlag GmbH &Co. KGaA, Weinheim)     

Physical investigations on pulsed laser deposited nanocrystalline ZnO thin films

The nanocrystalline ZnO thin films were deposited by pulsed laser deposition on quartz and i-Si (100) substrates at different substrate temperatures (473 K–873 K) and at different mixed partial pressures (0.05, 0.01, and 0.5 mbar) of Ar+O₂. The structural studies from XRD spectra reveals that the films deposited at 0.05 mbar and at lower substrate temperatures were c-axis oriented with predominant (002) crystallographic orientation. At 873 K along with (002) orientation, additional crystallographic orientations were also observed in case of films deposited at 0.01 and 0.5 mbar pressures. The composition of Zinc and Oxygen in ZnO films from EDAX reveals that the films deposited at lower partial pressures were have high at.% of O₂ whereas higher partial pressures and substrate temperatures had high at.% Zn. The surface microstructure of the films show that the films deposited at lower partial pressures (0.05 mbar ) and at lower substrate temperatures (473 K) were found to have nanoparticles of size 15 nm where as films deposited at 873 K have nanorods. The length of these nanorods increases with increasing Ar+O₂ partial pressure to 0.5 mbar. The optical energy gap of the film deposited at lower partial pressure and substrate temperature was 3.3 eV and decrease with the increase of substrate temperatures. The films deposited at 0.5 mbar and at 873 K emitted an intense luminescence at a wavelength of 390 nm. The measured thickness of deposited films by spectroscopic ellipsometry is around 456 nm.     

离子束增强沉积制备p型氧化锌薄膜及其机理研究

采用离子束增强沉积方法在Si和SiO₂/Si衬底上制备In-N共掺杂ZnO薄膜(INZO)，溅射靶是用ZnO和2 atm% In₂O₃粉体均匀混合并压制而成，在氩离子溅射ZnO靶的同时，氮、氩混合离子束垂直注入沉积的薄膜.实验结果显示INZO薄膜具有(002)的择优取向，并且为p型导电，电阻率最低为0.9Ωcm.薄膜在氮气、氧气气氛下退火，对薄膜的结构和电学特性与成膜和退火条件的关系进行了分析. 关键词： 氧化锌薄膜 p型掺杂 离子束增强沉积     

Mechanical and physicochemical properties of AlN thin films obtained by pulsed laser deposition

AlN thin films have been deposited on Si(100) substrates by a pulsed laser deposition method. The deposition parameters (pressure, temperature, purity of target) play an important role in the mechanical and physicochemical properties. The films have been characterized using X-ray diffraction, atomic force microscopy, Brillouin light scattering, Fourier transform infrared spectroscopy and wettability testing. With a high purity target of AlN and a temperature deposition of 750 C, the measured Rayleigh wave velocity is close to the one previously determined for AlN films grown at high temperature by metal–organic chemical vapour deposition. Growth of nanocrystalline AlN at low temperature and of AlN film with good crystallinity for samples deposited at higher temperature is confirmed by infrared spectroscopy, as it was by atomic force microscopy, in agreement with X-ray diffraction results. A high hydrophobicity has been measured with zero polar contribution for the surface energy. These results confirm that films made by pulsed laser deposition of pure AlN at relatively low temperature have good prospects for microelectromechanical systems applications.