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     

Structure, electrical and chemical properties of zirconium nitride films deposited by dc reactive magnetron sputtering

2 and Ar ambient. X-ray diffraction indicated that growth of ZrN with a preferred (111) orientation over Si(100) was achieved. The resistivity of the films varies from 200 μΩcm to 15 μΩcm depending on the N₂ content in the working gas. The square resistance of the films deposited on 96% Al₂O₃ ceramic wafers is stable below 300 °C. Received: 17 June 1996/Accepted: 9 December 1996     

The dispersion properties of surface acoustic wave devices on AlN/LiNbO3 film/substrate structure

Highly c-axis oriented aluminum nitride (AlN) films were deposited on z-cut LiNbO₃ substrates by reactive rf magnetron sputtering. The crystalline properties investigated by X-ray diffraction (XRD) revealed that AlN film with (0 0 2) preferred orientation was improved by an increase of the deposition time within the experimental range. However, the surface morphology of AlN film measured by scanning probe microscopy (SPM) showed that the roughness was getting worse with increase of deposition time. Surface acoustic wave (SAW) properties, measured by a network analyzer in the structure consisting of highly c-axis AlN films on z-cut LiNbO₃ substrates, were investigated. The phase velocity (V_P) was significantly increased by the increase of h/λ, where h is the thickness of AlN film and λ is the wavelength. However, the insertion loss (IL) of SAW filters was also increased by the increase of h/λ. Experimental results on the temperature characteristics of SAW devices are also presented.     

c轴定向氮化铝薄膜的制备

利用电子回旋共振 (ECR)微波增强化学气相沉积法 (PECVD)并使用氮气 (N2 ) ,氩气 (Ar)和AlCl3蒸气作为气源在直径为 6 .35cm的 (10 0 )单晶硅片表面制备了c轴定向氮化铝 (AlN)薄膜 ,并使用X射线衍射仪及其X射线特征能谱和扫描电镜 (SEM)分析了薄膜特征 ,研究了微波功率、基板温度和N2 流量对薄膜c轴定向的影响 ,得到了c轴偏差角小于 5°的高质量大面积AlN薄膜。     

分子束外延生长的ZnO压电薄膜及其声表面波器件特性

用RF-MBE在蓝宝石(0001)衬底上引入MgO和低温ZnO双缓冲层生长了ZnO薄膜,并制备了声表面波器件。在ZnO薄膜中,仅观测到(0002)面的XRD,且衍射峰增强,半高宽减小,表明ZnO薄膜c轴取向性更好,晶体结构更优。室温下自由激子吸收峰更尖锐和吸收边更陡峭以及仅观测到自由激子发光,且发光线宽变窄、发光强度变大,表明ZnO薄膜缺陷密度减小,薄膜质量提高。测得该ZnO压电薄膜的电阻率高达4×10⁷ Ω·cm,其声表面波的速度高达5 010 m/s。     

The effect of geometry and post-annealing on surface acoustic wave characteristics of AlN thin films prepared by magnetron sputtering

This paper describes experimental relationship between surface acoustic wave (SAW) properties of two-port SAW resonators based on polycrystalline aluminum nitride (AlN) thin films grown on Si substrates by using a pulsed reactive magnetron sputtering system and their geometry's parameters. Moreover, the influence of post-deposition heat treatment on SAW properties of AlN thin films was investigated at different annealing temperature (600 °C and 900 °C). The measurement results show the number of the inter-digital transducers (IDT) finger pairs (N), the number of reflectors grating pairs (R) and the IDT center-to-center distance (L) related to insertion loss of SAW resonators. The best result of insertion loss was 15.6 dB for SAW resonators with R = 160 pair, N = 5 pair and L = 750 μm. At the same geometry parameters, the SAW velocity and insertion loss were improved slightly after annealing at 600 °C and were worse for the films annealed at 900 °C by changes in the surface morphology and stress on the film.     

Effects of Mn‐doping on surface acoustic wave properties of ZnO films

Surface acoustic wave (SAW) filters based on Mn‐doped ZnO films have been fabricated and effects of Mn‐doping on SAW properties are investigated. It is found that the electromechanical coupling coefficient (K²) of Zn_0.913Mn_0.087O films is 0.73 ± 0.02%, which is 73.8% larger than that of undoped ZnO films (0.42 ± 0.02%). Zn_0.913Mn_0.087O film filters also exhibit a lower absolute value of insertion loss (|IL|) of 16.1 dB and larger bandwidth (BW) of 5.9 MHz compared with that of undoped ZnO film filter. However, Zn_0.952Mn_0.048O film filters exhibit a smaller K² of 0.34 ± 0.02%, larger |IL| of 26.9 dB and smaller BW of 3.5 MHz. It is suggested that the SAW properties can be improved by appropriate Mn‐doping and Mn–ZnO/Si multilayer structure with large d₃₃ is promising for wide‐band and low‐loss SAW applications. (© 2012 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Smooth and oriented AlN thin films deposited by laser ablation and their application for SAW devices

Aluminum nitride films of up to 1.2 7m thickness were deposited by excimer laser ablation onto c-, r-, m-, and a-cut sapphire substrates. The films were found to be of (00.1), (11.0), (10.0) and (00.1) orientation on c-, r-, m- and a-cut sapphire substrates, respectively. XRD pole figure measurements showed good in-plane alignment of all three sample sets. AFM measurements reveal that all films were atomically smooth in the initial stages of growth. Furthermore, for AlN(11.0) on r-cut sapphire the film surface remained smooth, with an r.m.s. roughness of about 1 nm up to a film thickness of 1.2 7m. AlN films with the polar c-axis parallel to the film surface are particularly favourable for SAW device applications, since the c-axis direction yields the strongest coupling coefficient. A smooth surface, as for AlN(11.0), is essential to prevent scattering of propagating surface acoustic waves. A SAW r.f. filter was fabricated with interdigital transducers of 5.6 7m wavelength on top of a 1.2 7m AlN(11.0) film on r-cut sapphire. The resonance frequency of 1.068 GHz corresponds well to theoretical expectations for the SAW velocity in this propagation geometry.     

Structural and interfacial stabilities of epitaxial (11-20)-oriented wurtzite AlN films grown on lattice-matched MnS buffered Si(100)

Epitaxial growth of non-polar wurtzite (11-20) AlN thin films was achieved on a Si(100) substrate by inserting an MnS buffer layer. The a-plane AlN film and MnS buffer layer were fabricated by pulsed KrF excimer laser deposition, and their micro- and interfacial atomic structures were investigated by transmission electron microscopy. The epitaxial relationship between films and substrate was found to be AlN(11-20)MnS(100)Si(100) with in-plane alignment of AlN[1-101]MnS[011]Si[011]. AlN[11-20] grown on Si is perpendicular to AlN[0001] and parallel to MnS[100]. The MnS/Si interface is abrupt enough to inherit the orientation of the Si(100) surface. A sharp interface was also observed for AlN/MnS without any intermediate layer. PACS 81.05.Ea; 81.05.Zx; 81.15.Fg; 68.37.Lp     

Structural and electrical properties of tantalum nitride thin films fabricated by using reactive radio-frequency magnetron sputtering

TaN thin film is an attractive interlayer as well as a diffusion barrier layer in [FeN/TaN]_n multilayers for the application as potential write-head materials in high-density magnetic recording. We synthesized two series of TaN films on glass and Si substrates by using reactive radio-frequency sputtering under 5-mtorr Ar/N₂ processing pressure with varied N₂ partial pressure, and carried out systematic characterization analyses of the films. We observed clear changes of phases in the films from metallic bcc Ta to a mixture of bcc Ta(N) and hexagonal Ta₂N, then sequentially to fcc TaN and a mixture of TaN with N-rich phases when the N₂ partial pressure increased from 0.0% to 30%. The changes were associated with changes in the grain shapes as well as in the preferred crystalline orientation of the films from bcc Ta [100] to [110], then to random and finally to fcc TaN [111], correspondingly. They were also associated with a change in film resistivity from metallic to semiconductor-like behavior in the range of 77–295 K. The films showed a typical polycrystalline textured structure with small, crystallized domains and irregular grain shapes. Clear preferred (111) stacks parallel to the substrate surface with embedded amorphous regions were observed in the film. TaN film with [111]-preferred orientation and a resistivity of 6.0 mΩ cm was obtained at 25% N₂ partial pressure, which may be suitable for the interlayer in [FeN/TaN]_n multilayers. Received: 6 December 1999 / Accepted: 24 July 2000 / Published online: 9 November 2000     

On the effectiveness of lateral excitation of shear modes in AlN layered resonators

We describe the fabrication and frequency characterization of different structures intended for the lateral excitation of shear modes in AlN c-axis-oriented films. AlN films are deposited on moderately doped silicon substrates covered either with partially metallic or fully insulating Bragg mirrors, and on insulating glass plates covered with insulating acoustic reflectors. TiO_x seed layers are used to promote the growth of highly c-axis oriented AlN films, which is confirmed by XRD and SAW measurements. The excitation of the resonant modes is achieved through coplanar Mo electrodes of different geometries defined on top of the AlN films. All the structures analyzed display a clear longitudinal mode travelling at 11,000 m/s, whose excitation is attributed to the direction of the electric field (parallel to the c-axis) below the electrodes; this is enhanced when a conductive plane (metallic layer or Si substrate) is present under the piezoelectric layer. Conversely, only a weak shear resonance (6,350 m/s) is stimulated through the effect of coplanar electrodes, which is explained by the weakness of the electric field strength parallel to the surface between the electrodes. A significantly more effective excitation of shear modes can be achieved by normal excitation of AlN films with tilted c-axis.     

SrTiO3(110) thin films grown directly on different oriented silicon substrates

We have grown (110)-oriented SrTiO₃ (STO) thin films on silicon without any buffer layer, by means of pulsed laser deposition technique. The crystal structures of the grown films were examined by X-ray diffraction analysis including θ–2θ scan and rocking curve as well as Laue diffraction methods. STO films with single (110) out-of-plane orientation were formed on all (100), (110) and (111)-oriented Si substrates. The in-plane alignments for the epitaxial STO films grown directly on Si (100) were found as STO[001]//Si[001] and STO[11̄0]//Si[010]. The results should be of interest for better understanding of the growth of perovskite oxide thin films on silicon wafers. PACS 77.55.+f; 68.55.JK; 81.15Fg     

常压化学气相沉积法在Ag/Si(111)模板上生长ZnO薄膜及其性能研究

在Si衬底上利用磁控溅射的方法沉积1.5 nm厚度的Ag膜用以阻挡Si衬底被氧化。采用常压金属有机化学气相沉积法(MOVCD),在Ag/Si(111)衬底上成功地生长出马赛克结构的ZnO薄膜。用光学显微镜观察表面形貌,结果显示有带晶向特征的微裂纹,裂纹密度为100 cm-1。依据X射线晶体衍射的结果,薄膜结晶质量良好,呈C轴高度择优取向。用双晶X射线衍射得到(002)面的ω扫描半峰宽为1.37°。温度10 K时光致发光谱(PL)观察到自由激子、束缚激子发射及它们的声子伴线。结果表明,金属有机化学气相沉积法方法在Si(111)衬底上制备ZnO薄膜时,Ag是一种有效的缓冲层。     

Morphological properties of AlN and GaN grown by MOVPE on porous Si(111) and Si(111) substrates

Metal Organic Vapour Phase Epitaxy (MOVPE) of AlN and GaN layers at a temperature of 1080 C were performed on porous Si(111) and Si(111) substrates. The thermal stability of porous silicon (PS) is studied versus growth time under AlN and GaN growth conditions. The surface morphology evolution of the annealed PS is revealed by scanning electron microscopy (SEM). Porous Si(111) with low porosity (40%) is more thermally stable than porous Si(100) with relatively high porosity (60%).AlN layers with various thicknesses were grown under the same conditions on the two substrates. Morphological properties of AlN were studied by atomic force microscopy (AFM) and compared taking into account the two different surfaces of the substrates. The two growth kinetics of AlN were found to be different due to the initial surface roughness of the PS substrate. The effect of AlN buffer morphology on the qualities of subsequent GaN layers is discussed. Morphological qualities of GaN layers grown on PS are improved compared to those obtained on porous Si(100) but are still less than those grown on Si substrate.     

Filtering performance improvement in V-doped ZnO/diamond surface acoustic wave filters

High-frequency surface acoustic wave (SAW) filters using undoped and V-doped ZnO films were fabricated on diamond. Compared with their counterparts, the SAW filters using V-doped ZnO films have higher electromechanical coupling coefficient of ∼2.9% and lower insertion loss. The filtering performance improvement is considered to be due to the ferroelectricity in V-doped ZnO films and the resultant high piezoresponse (∼110 pm/V), which is one order of magnitude larger than that of undoped ZnO films. In addition, more perfect (0 0 2) preferred orientation, better uniform grains and smoother surface of V-doped ZnO films also contribute to the filtering performance improvement.     

MOCVD法生长SAWF用ZnO/Diamond/Si多层结构

使用等离子体辅助MOCVD系统在金刚石,硅衬底上成功地制备了氧化锌多层薄膜材料,通过两步生长法对薄膜质量进行了优化。XRD测试显示优化后的样品具有c轴的择优取向生长,PL谱测试表明样品经优化后不仅深能级发射峰消失,同时紫外发射峰增强。对优化后的样品的表面测试显示出较低的表面粗糙度。比较氧化锌多层薄膜结构的声表面波频散曲线,ZnO薄膜声表面滤波器受膜厚和衬底材料的影响较大。当ZnO薄膜较薄时,在它上面的传播速度将与衬底上的传播速度接近,与其他衬底上生长的薄膜相比,以金刚石这种快声速材料为衬底的ZnO多层薄膜结构,声表面波滤波器的中心频率将提高1倍左右。     

Effects of substrate on surface morphology, crystallinity, and photoluminescence properties of sputtered ZnO nano films

Effects of substrate on crystallinity, surface morphology, and luminescence properties of radio frequency sputtered zinc oxide (ZnO) thin films were investigated. A variety of materials such as Si (100), Si (111), Al₂O₃, quartz, and silicon carbide (SiC) wafers were examined as substrates for deposition of ZnO thin films. The results showed smooth and uniform growth of c-axis orientation films. The thickness of the layers was about 50 nm. The average grain sizes of films were about 10, 13, and 12 nm for Si (111), quartz, and SiC samples, respectively. The deposited film on Al₂O₃ showed the largest grain size, about 500 nm. Grazing incidence x-ray diffraction patterns of the samples revealed that sputtered layers on Al₂O₃ and quartz had better crystallinity with higher peak at (002) orientation compared to Si and SiC substrates. Moreover, the Al₂O₃ sample exhibited a weak peak at position of (100) planes of ZnO too. The photoluminescence spectra of the samples showed a typical luminescence behavior with a broad UV band, including a main peak at around 388 nm and a weak shoulder peak at around 381 nm, corresponding with bound excitonic recombination and free excitonic recombination, respectively. The luminescence peak revealed that the intensity of UV emission is not necessarily dependent on the grain sizes and the micro-structural quality of ZnO films.     

Growth of preferentially-oriented AlN films on amorphous substrate by pulsed laser deposition

Preferentially-oriented aluminum nitride (AlN) films are grown directly on natively-oxidized Si (100) substrate by pulsed laser deposition (PLD) in nitrogen (N₂) environment. The AlN preferential orientation changes from (002) to (100) with increasing N₂ pressure. Such different behaviors are discussed in terms of deposition-rate-dependent preferential orientation, kinetic energy of depositing species and confinement of laser plume. Finally, sample deposited at 0.9 Pa is proved to have the highest (002) peak intensity, the lowest FWHM value, the highest deposition rate and a relatively low RMS roughness (1.138 nm), showing the optimal growth condition for c-axis-oriented AlN growth at this N₂ pressure.     

ZnO／AlN／Si（111）薄膜的外延生长和性能研究

用常压金属化学气相沉积法(MOCVD)在Si(111)衬底上制备了马赛克结构ZnO单晶薄膜。引入低温Al N缓冲层以阻止衬底氧化、缓解热失配和晶格失配。薄膜双晶X射线衍射2θ/ω联动扫描只出现了Si(111)、ZnO(000l)及Al N(000l)的衍射峰。ZnO/Al N/Si(111)薄膜C方向晶格常量为0.5195nm,表明在面方向处于张应力状态;其对称(0002)面和斜对称(1012)面的双晶X射线衍ω摇摆曲线半峰全宽分别为460″和1105″;干涉显微镜观察其表面有微裂纹,裂纹密度为20cm-1;3μm×3μm范围的原子力显微镜均方根粗糙度为1.5nm;激光实时监测曲线表明薄膜为准二维生长,生长速率4.3μm/h。低温10K光致发光光谱观察到了薄膜的自由激子、束缚激子发射及它们的声子伴线。所有结果表明,采用金属化学气相沉积法并引入Al N为缓冲层能有效提高Si(111)衬底上ZnO薄膜的质量。     

The effect of silicon-substrate orientation on the local piezoelectric characteristics of LiNbO<Subscript>3</Subscript> films

The domain structure of lithium-niobate thin films grown on Si(111) and Si(100) substrates coated with a native oxide layer with a thickness of no less than 2 nm is investigated by X-ray diffraction, scanning electron microscopy and piezoresponse force microscopy. The films are synthesized by the rf magnetron sputtering of a single-crystal lithium-niobate target. A high degree of grain orientation in the polycrystalline films is demonstrated. The piezoelectric coefficients d _zz of the lithium-niobate films on Si(111) and Si(100) substrates are calculated from the measured dependences of the amplitude of the piezoresponse signal on the ac voltage applied between the cantilever tip and the substrate. Piezoelectric hysteresis loops are obtained in the remanent piezoelectric response regime