Influence of sputtering atmosphere on crystallinity and crystal orientation of AlN thin films deposited on polycrystalline MoSi2 substrates

Highly oriented AlN thin films have been deposited on polycrystalline MoSi2 substrates by r.f. magnetron sputtering. The total sputtering pressure and the nitrogen concentration in the sputtering gas had a significant influence on the crystallinity and crystal orientation of the films. The film deposited at a sputtering pressure of 0.6 Pa and a nitrogen concentration of 20% indicated high crystallinity, high c-axis orientation (=3.1°) and very low surface roughness (Ra=0.7 nm). The crystallinity, crystal orientation, composition and morphology of the films were investigated by X-ray diffraction, X-ray photoelectron spectroscopy, and atomic force microscopy. The nitrogen concentration hardly had an effect on the composition of the films; however, it had a great influence on the shape of the fine grains constituting the films. The shape of the grains drastically changed from triangular pyramids of various sizes to uniform fine grains with increasing nitrogen concentration. © 1998 Chapman & Hall     

Influence of growth rate on the structural and morphological properties of TiN, ZrN and TiN/ZrN multilayers

The effect of the deposition rate on the structural and morphological properties of TiN and ZrN single layers and TiN/ZrN multilayers deposited by radiofrequency reactive magnetron sputtering has been studied. The total pressure was kept constant and the growth rate variation was obtained by small difference of nitrogen concentration in the fed gas. The decreasing deposition rate results in a structural change in the thin films from (111) orientation to (100) one. As consequence the surface morphology becomes smoother. Films roughness is strongly related with texture and it decreases with an increase in the (100) X-ray diffraction line intensity. In order to achieve a clear interpretation of our experimental results, the ratio between the N⁺ ions of the plasma and the atoms number reaching the substrate was considered. At high deposition rate with respect to the N⁺ concentration, the chemical potential of transition metal on (100) growth surface is higher than (111) one favouring the (111) orientation of the films. On the contrary, when the growth rate is low with respect to the nitrogen concentration, the chemical potential of transition metal on (111) growth surface is higher than the (100) one leading to a preferential growth in the (100) direction.     

Effects of nitrogen partial pressure on microstructure,morphology and N/Ti ratio of TiN films deposited by reactive magnetron sputtering

Abstract

TiN films were deposited on Si(111) substrates at different nitrogen partial pressures with reactive magnetron sputtering. The crystal structure and preferred growth orientation of the films were determined using X-ray diffraction (XRD) analysis. Their morphology and composition were analysed using field emission scanning electron microscopy (FESEM) and energy dispersive spectroscopy (EDS). It is found that with the increase in nitrogen partial pressure, the growth of TiN films varies from the {111} preferred orientation to the {100} preferred orientation and the deposition rate of TiN films decreases. When the {111} preferred orientation is presented, TiN films reveal a kind of surface morphology of triangular pyramid with right angles; while the {100} orientation is dominant, TiN films characterise another kind of domelike surface morphology. Furthermore, the N/Ti ratio of the TiN films first increases, then decreases and increases again as nitrogen partial pressure enlarges.     

Electrical,morphological and structural properties of RF magnetron sputtered Mo thin films for application in thin film photovoltaic solar cells

Molybdenum (Mo) thin films were deposited using radio frequency magnetron sputtering, for application as a metal back contact material in “substrate configuration” thin film solar cells. The variations of the electrical, morphological, and structural properties of the deposited films with sputtering pressure, sputtering power and post-deposition annealing were determined. The electrical conductivity of the Mo films was found to increase with decreasing sputtering pressure and increasing sputtering power. X-ray diffraction data showed that all the films had a (110) preferred orientation that became less pronounced at higher sputtering power while being relatively insensitive to process pressure. The lattice stress within the films changed from tensile to compressive with increasing sputtering power and the tensile stress increased with increasing sputtering pressure. The surface morphology of the films changed from pyramids to cigar-shaped grains for a sputtering power between 100 and 200 W, remaining largely unchanged at higher power. These grains were also observed to decrease in size with increasing sputtering pressure. Annealing the films was found to affect the resistivity and stress of the films. The resistivity increased due to the presence of residual oxygen and the stress changed from tensile to compressive. The annealing step was not found to affect the crystallisation and grain growth of the Mo films.     

Influence of thickness on the crystallography and surface topography of TiN nano-films deposited by reactive DC and pulsed magnetron sputtering

TiN films of 50 nm and 500 nm thickness were deposited on M2 tool steel substrates by reactive closed field unbalanced magnetron sputtering operating in direct current (DC) and pulsed magnetron sputtering (PMS) modes. Parameters of the crystallographic structure and surface roughness and their evolution during the films growth were analyzed via X-ray diffraction and atomic force microscopy. The obtained results show that all the analyzed films have polycrystalline and mono-phase (TiN) structures. In the 50 nm films, the in plane crystallographic texture that formed was 100% {111}. During film growth a weakening of the preferred crystallographic orientation and a decrease of the concentration of lattice imperfections occurred. Both processes are more pronounced in the film deposited by PMS compared to that deposited by DC sputtering. Film growth is accompanied by increasing of surface smoothness. Pulsing the target power led to a decrease of the mean surface roughness of both the 50 nm and 500 nm films.     

Influence of target-substrate distance and composition on the preferential orientation of yttria-stabilized zirconia thin films

The use of yttria-stabilized zirconia (YSZ) thin films calls for a controlled deposition with full understanding on the influence of deposition parameters on the crystallographic properties of YSZ. YSZ thin films were deposited using magnetron sputtering from two sources, enabling to modify the sample composition in a flexible way. The influence of target-substrate (T-S) distance and the Y content on the crystallographic orientation were studied under different chamber pressures. Correlations were found under both conditions. This way, a two-dimensional map was obtained by showing the change in preferential orientation as a function of sample composition. This map shows the existence of two different trends depending on the pressure. At low pressure, the addition of Y and the decrease in T-S distance, change the orientation from [200] to a complete [111] out-of-plane orientation resulting in a competition between the fastest growth direction and the lowest surface energy. However, a different trend was observed at high pressure, where T-S distance and composition do not influence the preferential orientation of the film.     

反应磁控溅射制备氮化钽扩散阻挡层的研究

采用反应磁控溅射在硅衬底上制备了TaN薄膜,研究了氮分压、溅射功率及衬底温度对薄膜晶体结构、表面形貌和电学性能的影响。结果表明,晶体结构随工艺参数的改变发生变化,GIXRD图谱衍射峰强度随溅射功率和衬底温度的增加而增强,氮气分压的增加使择优取向向(111)晶面偏移;TaN薄膜的表面形貌与溅射功率和氮气分压密切相关,与衬底温度的关系不大,其粗糙度随溅射功率的增加而增大,随氮气分压的增加而减小;TaN薄膜的方块电阻随溅射功率的增加逐渐减小,随氮气分压的增加逐渐增大,温度对方块电阻的影响不大;对Cu/TaN/Si互联体系热处理后发现TaN薄膜具有优异的阻挡性能,在600℃时依然可有效阻止Cu向Si的扩散。     

溅射气氛对氟碳疏水薄膜表面结构及性能的影响

以聚四氟乙烯(PTFE)为靶材,用射频磁控溅射方法在玻璃衬底上制备了氟碳高分子薄膜,并对其结构和表面性能进行了研究.由XPS的结果可知,构成薄膜的大分子由-CF-、-CF2-和-CF3等组分组成.随着氩气压强的增加,缺氟基团-C-增加,而-CF2-、-CF3等富氟基团以及F/C均减少;随着氮气偏压的增加,-CF-、-CF2-和-CF3以及F/C和N/C增加.同时探讨了溅射气氛对薄膜表面形貌、疏水性能及表面能的影响.     

Effect of solution concentration on surface morphology and photocatalytic activity of ZnO thin films synthesized by hydrothermal methods

ZnO thin films were synthesized via hydrothermal method on silicon substrate at various solution concentrations. The thin films were characterized by X-ray diffraction, field-emission scanning electron microscope and UV–Vis spectrophotometer. The results show that the thin films are polycrystalline with wurtzite hexagonal structure. The T _c values of (101) surface of the thin film increase from 0.929 to 1.840 at first, and then decrease to 0.779 with increasing solution concentration. The preferential orientation along the (101) crystal surface can be controlled by changing the solution concentration. Solution concentration has a significant effect on surface morphology of the thin films. The optical band gap of the thin films decreases, when the solution concentration of zinc nitrate hexahydrate increases from 0.01 to 0.06 mol/L and then increases when the solution concentration of zinc nitrate hexahydrate further increases to 0.08 mol/L. Photocatalytic activity of the thin films on degradation of methyl orange under UV light irradiation was studied in detail. The ZnO thin film with many cracks prepared from 0.01 mol/L shows the higher photocatalytic activity but the tower-like ZnO thin film prepared from 0.08 mol/L reveals the lower photocatalytic activity. Therefore, the photocatalytic activity of the thin films are mainly relate to surface morphology and crystallographic orientation.     

Bias voltage dependence properties of cadmium oxide films deposited by d.c. reactive magnetron sputtering

Cadmium oxide films were grown on glass substrates using d.c. reactive magnetron sputtering technique by sputtering from a metallic cadmium target in an oxygen partial pressure of 1×10^–3 mbar under various substrate bias voltages. The substrate bias voltage significantly influences the crystallographic structure of the deposited films. The influence of substrate bias voltage on the electrical and optical properties of the films was systematically studied. The films formed at a substrate temperature of 473 K and bias voltage of –80 V showed an electrical resistivity of 1×10^–3 cm, optical transmittance of 86%, optical band gap of 2.47 eV and a figure of merit of 7×10^{–3 –1}.     

Nitrogen pulsing to modify the properties of titanium nitride thin films sputter deposited

TiN _x thin films were grown on (100) Si and glass substrates by dc reactive magnetron sputtering. A titanium target was sputtered in Ar + N₂ atmosphere using a pulsing flow rate of the nitrogen gas. A constant pulsing period was used for every deposition whereas the nitrogen injection time was changed. The systematic variation of the nitrogen injection time led to a gradual decrease of the deposition rate and to a controlled modulation of the chemical composition of the TiN _x films (x between 0 and 1.05). Analysis of the crystallographic structure by X-ray diffraction showed that both Ti and TiN phases coexisted and a change of the preferential orientation from (200) to (111) occurred. The electrical conductivity and colour measurements in the CIE-L*a*b* system of colourimetry were also performed and correlated with the evolution of the N/Ti ratio.     

Preparation of highly oriented AlN thin films on glass substrates by helicon plasma sputtering and design of experiments

Aluminum nitride (AlN) thin films were deposited by a helicon plasma sputtering system with a radical cell. We investigated the effects of eight sputtering control factors on the crystal orientation of the films by design of experiments and the analysis of variance (ANOVA) in order to prepare highly oriented AlN thin films on silica glass substrates. Consequently, it was proved statistically that the distance between a target and a substrate, the sputtering pressure and the substrate temperature are significant control factors for the crystal orientation of the films. Especially, the distance is the most important factor of the eight control factors, which has not been reported so far. On the other hand, the effects of the cathode r.f. coil power, the radical cell power, the nitrogen concentration, the sputtering time and the cathode power are not statistically significant. Moreover, a detailed investigation of the dependence of the orientation on the three important control factors was carried out to optimize the sputtering conditions. The full width at half-maximum (FWHM) of the X-ray rocking curve of the film deposited under the optimized sputtering conditions is 2.4° (σ=1.3°). This orientation is the highest in the AlN thin films deposited on amorphous substrates reported to our knowledge.     

Structures and electrical properties of zinc oxide films prepared by low pressure sputtering system

Polycrystalline zinc oxide films with and without admixed aluminum and copper were prepared on amorphous substrates by using a co-sputtering process. The crystallographic orientation and electrical properties varied with both sputtering gas pressure and contents of admixed aluminum or copper. In a high sputtering gas pressure a normal orientation with c-axis perpendicular to the film surface was predominant, whereas, in a low sputtering gas pressure a parallel orientation with c-axis parallel to the film surface was predominant. The admixed aluminum inhibited growth of the normal orientation, but the admixed copper enhanced a growth of the parallel one.     

Orientation control and electrical properties of sputtered Pb(Zr,Ti)O3 films

Relationship between the crystallographic orientation and the electrical properties of the Pb(Zr,Ti)O₃, (PZT) thin films prepared by rf magnetron sputtering was investigated. The PZT films were deposited at 150, 250 or 340°C and, followed by rapid thermal annealing (RTA). It was found that the crystallographic orientation of the PZT films could be controlled only by the deposition temperature and the ferroelectric properties were dependent upon the orientation of the films. It was suggested that the difference in the atomic mobility at the substrate surface during deposition was closely related to the film orientation. The films with (111) orientation showed relatively high capacitance and the remanant polarization values.     

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     

Nanoindentation and atomic force microscopy measurements on reactively sputtered TiN coatings

Titanium nitride (TiN) coatings were deposited by d.c. reactive magnetron sputtering process. The films were deposited on silicon (111) substrates at various process conditions, e.g. substrate bias voltage (V_B) and nitrogen partial pressure. Mechanical properties of the coatings were investigated by a nanoindentation technique. Force vs displacement curves generated during loading and unloading of a Berkovich diamond indenter were used to determine the hardness (H) and Young’s modulus (Y) of the films. Detailed investigations on the role of substrate bias and nitrogen partial pressure on the mechanical properties of the coatings are presented in this paper. Considerable improvement in the hardness was observed when negative bias voltage was increased from 100–250 V. Films deposited at |V _B| = 250 V exhibited hardness as high as 3300 kg/mm². This increase in hardness has been attributed to ion bombardment during the deposition. The ion bombardment considerably affects the microstructure of the coatings. Atomic force microscopy (AFM) of the coatings revealed fine-grained morphology for the films prepared at higher substrate bias voltage. The hardness of the coatings was found to increase with a decrease in nitrogen partial pressure.     

Influence of sputtering parameters and nitrogen on the microstructure of chromium nitride thin films deposited on steel substrate by direct-current reactive magnetron sputtering

Chromium nitride thin films were deposited on SA-304 stainless steel substrates by using direct-current reactive magnetron sputtering. The influence of process conditions such as nitrogen content in the fed gas, substrate temperature, and different sputtering gases on microstructural characteristics of the films was investigated. The films showed (200) preferred orientation at low nitrogen content (< 30%) in the fed gas. The formation of Cr₂N and CrN phases was observed when 30% and 40% N₂ were used, with a balance of Ar, respectively. Field emission scanning electron microscopy and atomic force microscopy were used to characterize the morphology and surface topography of the thin films, respectively. Microhardness tests showed a maximum hardness of 16.95 GPa for the 30% nitrogen content.     

Characterization of epitaxial Bi2Sr2CaCu2O8+δ thin films

We report a dc sputtering method for the fullin situ preparation of Bi₂Sr₂CaCu₂O₈₊ thin films on SrTiO₃ and LaAlO₃.T _c values of more than 90 K can be achieved by oxidizing annealing below the melting point, followed by a reducing anneal at 500°C. The structural properties of the films are revealed by X-ray diffraction in Bragg-Brentano geometry (strongc-axis orientation with FWHM (0 0 10)=0.3) and also by scans (epitaxy within the substrate plane). Rutherford backscattering and channeling confirmed the correct composition of the cations while the minimum yield, _min, is 23%. Depth profiles by SNMS show a very homogeneous distribution of the cations with no detectable loss of bismuth near the surface. The surface morphology of the films was studied by SEM and by STM. Patterning of the films in lateral geometry can be performed by photolithographic techniques without degradation ofT _c .     

The effects of incident angle on C-axis orientation in sputtered Co-Cr films

The effects of the incident angle of the sputtered atoms on the crystallographic orientation in the Co-Cr films have been investigated in detail. Specimen films 1000 - 2000 Å thick were prepared by the Facing Targets Sputtering (FTS) system. The specially designed mask was used for collecting only the sputtered particles with the quasi-coherent incidence to the substrate. When the films are prepared at relatively low argon gas pressures, the effect of incident angle is not so apparent and the well c-axis oriented films can be obtained for the incident angle below 45°. This result indicate that the surface diffusion may be dominant over the incident angle for attaining the desired crystallographic orientation in the films when they are prepared at low working gas pressures. Owing to the unique target/substrate layout, the plasma-free FTS system with low working gas pressures may have much larger flexibilities for preparing the well c-axis oriented Co-Cr films as compared with the conventional sputtering systems or the vacuum evaporation one.     

Deposition of low-resistivity gallium-doped zinc oxide films by low-temperature radio-frequency magnetron sputtering

The transparent and conductive gallium-doped zinc oxide (GZO) film was deposited on 1737F Corning glass using the radio-frequency (RF) magnetron sputtering system with a GZO ceramic target. (The Ga₂O₃ contents are approximately 5 wt. %). In this study, the effect of the sputtering pressure on the structural, optical and electrical properties of GZO films upon the glass or polyester film (PET) substrate was investigated and discussed in detail. The GZO film was grown under a steady RF power of 400 W and a lower substrate temperature from room temperature up to 200 °C. The crystal structure and orientation of GZO thin films were examined by X-ray diffraction. All of the GZO films under various sputtering pressures had strong c-axis (002)-preferred orientation. Optical transparency was high (> 80%) over a wide spectral range from 380 nm to 900 nm. According to the experimental data, the resistivity of a single-layered GZO film was optimized at  8.3 × 10^− 4 Ω cm and significantly influenced by the sputtering pressure. In further research, the sandwich structure of the GZO film/Au metal/GZO film was demonstrated to improve the electrical properties of the single-layered GZO film. The resistivity of the sandwich-structured GZO film was around 2.8 × 10^− 4 Ω cm.