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.     

Deposition of c-axis orientation aluminum nitride films on flexible polymer substrates by reactive direct-current magnetron sputtering

Aluminum nitride (AlN) piezoelectric thin films with c-axis crystal orientation on polymer substrates can potentially be used for development of flexible electronics and lab-on-chip systems. In this study, we investigated the effects of deposition parameters on the crystal structure of AlN thin films on polymer substrates deposited by reactive direct-current magnetron sputtering. The results show that low sputtering pressure as well as optimized N₂/Ar flow ratio and sputtering power is beneficial for AlN (002) orientation and can produce a highly (002) oriented columnar structure on polymer substrates. High sputtering power and low N₂/Ar flow ratio increase the deposition rate. In addition, the thickness of Al underlayer also has a strong influence on the film crystallography. The optimal deposition parameters in our experiments are: deposition pressure 0.38 Pa, N₂/Ar flow ratio 2:3, sputtering power 414 W, and thickness of Al underlayer less than 100 nm.     

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.     

射频磁控溅射法制备碲化铅薄膜的X射线衍射分析

采用射频磁控溅射法,在单面抛光的Si(111)衬底上制备了PbTe薄膜,利用X射线衍射法分析了溅射工艺参数如溅射功率、溅射时间、衬底温度以及退火温度对PbTe薄膜的结晶质量的影响。结果表明:在溅射功率为30W,溅射时间为10 min,衬底未加热时制备的薄膜具有最好的〈100〉方向的择优取向性;退火处理可以改善薄膜的结晶质量,并且退火温度越高,薄膜的结晶质量越好。     

Optimizing hardness of CNxthin films by dc magnetron sputtering and a statistical approach

We have investigated the effects of seven sputtering control factors on the hardness of carbon nitride (CN _x ) thin films by design of experiments and the analysis of variance (ANOVA) to synthesize hard CN _x thin films. It was determined statistically that the substrate temperature, the sputtering pressure and the target to substrate distance are significant control factors for the hardness of the CN _x thin films within the experimental range of this study. Especially, the distance is the most important control factor of the seven factors; the hardest films are obtained at the distance of 4.5 cm. On the other hand, the effects of the substrate treatment, the dc power, the nitrogen concentration and the sputtering time are not statistically significant. It is suggested that these statistical methods are effective to compare the importance of many sputtering control factors. The CN _x thin films deposited under the optimized sputtering conditions exhibit a relatively high hardness value of 55 ± 11 GPa, Young's modulus of 228 ± 21 GPa and an elastic recovery (%R) of 98%. The compressive stress in the films is a low value of 0.3 GPa.     

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     

溅射功率对ZnO：Si透明导电薄膜性能的影响

采用直流磁控溅射法在室温玻璃基片上制备出了掺硅氧化锌（ZnO：Si）透明导电薄膜,研究了溅射功率对ZnO：Si薄膜结构、形貌、光学及电学性能的影响,实验结果表明,溅射功率对ZnO：Si薄膜的生长速率、结晶质量及电学性能有很大影响,而对其光学性能影响不大。实验制备的ZnO：LSi薄膜为六方纤锌矿结构的多晶薄膜,且具有垂直于基片方向的c轴择优取向。当溅射功率从45W增加到105W时,薄膜的晶化程度提高、晶粒尺寸增大,薄膜的电阻率减小;当溅射功率为105W时,薄膜的电阻率达到最小值3．83~104n·cm,其可见光透过率为94．41％。实验制备的ZnO：Si薄膜可以用作薄膜太阳能电池和液晶显示器的透明电极。     

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     

Characterization of crystalline structure and morphology of NiO thin films

We investigated the relation of sputtering powers with structural and morphological properties of nickel oxide (NiO) thin films. NiO thin films were fabricated by using an rf-reactive sputtering method on Si(100) substrates with a Ni target in a partial pressure of oxygen and argon. The films were deposited by various rf-sputtering powers from 100 to 200 W at room temperature. The phases and crystalline structures of the deposited films were investigated by using grazing incident X-ray diffraction (XRD). The thickness and surface morphology of the films were investigated by using a field emission-scanning electron microscopy (FE-SEM). The different sputtering conditions drastically affected the crystallinity and the surface morphology of NiO thin films. A combined analysis of the data obtained from X-ray diffraction and SEM images demonstrates that the preferred orientation of NiO films tends to grow from (111) to (200) direction as increasing the sputtering power, which can be explained by in terms of the surface energy along the indexing plane in an fcc structure. As increasing the rf power, lattice constants decreased from 4.26 to 4.20 angstroms and samples became high-quality crystals. Under our experimental condition, NiO films prepared at 150 W with 20% partial pressure of oxygen and 7 cm distance from the sample to the target show the best quality of the crystal.     

Preparation of highly oriented aluminum nitride thin films on molybdenum bottom electrodes using metal interlayers

We have investigated the influence of metal interlayers on the crystallinity and crystal orientation of aluminum nitride (AlN) thin films prepared on molybdenum (Mo) bottom electrodes. The interlayres were prepared between the Mo bottom electrodes and silicon substrates. Although the sputtering conditions of AlN films and Mo electrodes were the same, the Au/Ti interlayer drastically increased the XRD intensity of the (0002) AlN and (110) Mo planes, and decreased the full width at half maximum (FWHM) of the rocking curves of the (0002) AlN peaks from 9.22 to 3.02. The Au/Ti interlayers were effective for the improvement in the crystallinity and crystal orientation of AlN films deposited on Mo bottom electrodes. Furthermore, we clarified that the crystallinity and orientation of AlN films and Mo electrodes strongly depend on those of the Au interlayers, and the Au interlayers influence the morphologies of the Mo electrodes.     

Growth of GaN and AlN thin films by laser induced molecular beam epitaxy

Hexagonal GaN and AlN thin films were grown by laser induced molecular beam epitaxy using Al or Ga metal as target material and N₂as nitrogen source. The films were deposited on sapphire (0001) and SiC (0001) substrates. Epitaxial growth of GaN has been achieved at 730°C and 10⁻³ mbar N₂ pressure. The AlN films were polycrystalline with predominant (0001) orientation.     

Effect of particle bombardment on the orientation and the residual stress of sputtered AlN films for SAW devices

We present a study of the effect of particle bombardment on the preferred orientation and the residual stress of polycrystalline aluminum nitride (AlN) thin films for surface acoustic wave (SAW) applications. Films were deposited on silicon (100) substrates by radio frequency (RF) sputtering of an aluminum target in an argon and nitrogen gas mixture. The main deposition parameters were changed as follows: the total pressure from 4 mTorr to 11 mTorr, the N2 content in the gas mixture from 20% to 80%, and the substrate self-bias voltage from -10 V to -30 V. If a sufficiently high negative substrate self-bias voltage is induced, (00.2)-oriented films are obtained over the full ranges of pressure and N2 content. Such films have values of residual stress ranging from -3 GPa to +1 GPa, depending on the deposition conditions. Our results suggest that the energy of the Ar ions colliding with the substrate controls the preferred orientation of the films, whereas the directionality of the ions (for the same energy) is the main factor determining the residual stress. To demonstrate the suitability of our material for the intended application, SAW filters with good electroacoustic response have been fabricated using AlN thin films with optimized (00.2) orientation and controlled residual stress.     

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.     

Characterization of reactively sputtered c-axis orientation (Al, B)N films on diamond

In this research, we demonstrated the viability of oriented AlN layer that incorporated BN to enhance the texturing. Wurtzite (Al, B)N films were deposited on a diamond wafer (diamond film on Si wafer) by a co-sputtering technique. The preferred orientation structure is sensitive to sputtering control factors. The relationship between the microstructures and process conditions were examined with XRD, TEM and AFM analysis. The cross-section TEM images showed that amorphous and randomly aligned structures were produced in the initial sputtering period, but the higher c-axis orientation structure formed as the sputtering time increased. The thickness of the amorphous and randomly aligned layer decreased with increasing sputtering power, nitrogen concentration, substrate temperature and bias voltage. As the thickness of the amorphous and the randomly aligned layer decreased, an (Al,B)N film with higher film quality than AlN was observed.     

溅射工艺对BST薄膜取向行为的影响

采用射频磁控溅射法在Si(100)衬底上沉积了Ba0.65Sr0.35TiO3薄膜.借助XRD、AFM和SEM研究了衬底温度、退火温度、溅射气压等不同的溅射参数对Ba0.65Sr0.35TiO3薄膜的晶化行为和显微结构的影响.在室温下沉积并未经退火处理的Ba0.65Sr0.35TiO3 薄膜是无定形态,在较高温度下沉积的薄膜晶化相对较好;随着在氧气气氛中退火温度的升高,X射线衍射峰的半峰宽变窄,衍射峰强度增强;在0.37～1.2Pa气压下沉积的Ba0.65Sr0.35TiO3薄膜有(110)和(200)主衍射峰,且其强度随溅射气压的增加而增强;当溅射气压继续升到3.9Pa,(110)和(200)衍射峰明显增强,说明Ba0.65Sr0.35TiO3 薄膜具有(110) (200)择优取向.AFM和SEM结果显示薄膜晶粒细小均匀、结构致密、表面平整,且无裂纹、无孔洞.分析结果显示优化工艺参数制备的Ba0.65Sr0.35TiO3 薄膜是用以制备非致冷红外探测器的优质材料.     

射频磁控反应溅射制备Al2O3薄膜的工艺研究

采用射频磁控反应溅射法,以高纯Al为靶材,高纯O2为反应气体,在不锈钢和单晶Si基片上成功地制备了氧化铝(Al2O3)薄膜,并对氧化铝薄膜的沉积速率、结构和表面形貌进行了研究.结果表明,沉积速率随着射频功率的增大先几乎呈线性增大而后缓慢增大;随着溅射气压的增加,沉积速率先增大,在一定气压时达到峰值后继续随气压增大而减小,同时随着靶基距的增大而减小;随着氧气流量的不断增加,靶面溅射的物质从金属态过渡到氧化物态,沉积速率也随之不断降低.X射线衍射图谱表明薄膜结构为非晶态;用原子力显微镜对薄膜表面形貌观察,薄膜微结构为柱状.     

Deposition of Al-doped ZnO films on polyethylene naphthalate substrate with radio frequency magnetron sputtering

100 nm Al-doped ZnO (AZO) thin films were deposited on polyethylene naphthalate (PEN) substrates with radio frequency magnetron sputtering using 2 wt.% Al-doped ZnO target at various deposition conditions including sputtering power, target to substrate distance, working pressure and substrate temperature. When the sputtering power, target to substrate distance and working pressure were decreased, the resistivity was decreased due to the improvement of crystallinity with larger grain size. As the substrate temperature was increased from 25 to 120 °C, AZO films showed lower electrical resistivity and better optical transmittance due to the significant improvement of the crystallinity. 2 wt.% Al-doped ZnO films deposited on glass and PEN substrates at sputtering power of 25 W, target to substrate distance of 6.8 cm, working pressure of 0.4 Pa and substrate temperature of 120 °C showed the lowest resistivity (5.12 × 10^− 3 Ω cm on PEN substrate, 3.85 × 10^− 3 Ω cm on glass substrate) and high average transmittance (> 90% in both substrates). AZO films deposited on PEN substrate showed similar electrical and optical properties like AZO films deposited on glass substrates.     

Influence of aluminum nitride interlayers on crystal orientation and piezoelectric property of aluminum nitride thin films prepared on titanium electrodes

Highly c-axis-oriented aluminum nitride (AlN) thin films have been prepared on titanium (Ti) bottom electrodes by using AlN interlayers. The AlN interlayers were deposited between Ti electrodes and silicon (Si) substrates, such as AlN/Ti/AlN/Si. The crystallinity and crystal orientation of the AlN films and Ti electrodes strongly depended on the thickness of the AlN interlayers. Although the sputtering conditions were the same, the X-ray diffraction intensity of AlN (0002) and Ti (0002) planes drastically increased, and the full-width at half-maximum (FWHM) of the X-ray rocking curves decreased from 5.1° to 2.6° and from 3.3° to 2.0°, respectively. Furthermore, the piezoelectric constant d₃₃ of the AlN films was significantly improved from − 0.2 to − 4.5 pC/N.     

Structural and electrical properties of RuO2 thin films prepared by rf-magnetron sputtering and annealing at different temperatures

Conductive ruthenium oxide (RuO₂) thin films have been deposited at different substrate temperatures on various substrates by radio-frequency (rf) magnetron sputtering and were later annealed at different temperatures. The thickness of the films ranges from 50 to 700 nm. Films deposited at higher temperatures show larger grain size (about 140 nm) with (200) preferred orientation. Films deposited at lower substrate temperature have smaller grains (about 55 nm) with (110) preferred orientation. The electrical resistivity decreases slightly with increasing film thickness but is more influenced by the deposition and annealing temperature. Maximum resistivity is 861 μΩ cm, observed for films deposited at room temperature on glass substrates. Minimum resistivity is 40 μΩ cm observed for a thin film (50 nm) deposited at 540°C on a quartz substrate. Micro-Raman investigations indicate that strain-free well-crystallized thin films are deposited on oxidized Si substrates.     

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.