Epitaxial aluminum nitride films on sapphire formed by pulsed laser deposition

Highly oriented aluminum nitride thin films were grown on sapphire (0001)-substrate by pulsed laser deposition technique. Characterization was done by X-ray-diffraction, elastic recoil detection analysis and Rutherford backscattering/channeling measurements. The epitaxial properties were studied as function of the substrate temperature and the deposition rate. An epitaxial relation to the sapphire substrate is found to be AlN [0001] || Al₂O₃ [0001] and AlN [11 0] || Al₂O₃ [10 0]. XRD-texture-analysis on films deposited at 850°C shows a full width half maximum Δω of 0.13° (rocking curve) and Δ of 1.1° (in-plane).     

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.     

Growth of aluminum nitride thin films prepared by plasma-enhanced atomic layer deposition

Aluminum nitride (AlN) thin films were deposited by atomic layer deposition from aluminum chloride (AlCl₃) and an ammonia/hydrogen plasma. The most important role of the ammonia/hydrogen plasma was to act as a reducing agent to extract Cl from AlCl₃, and to form AlN subsequently. The growth rate was saturated at ∼0.042 nm/cycle, and the thickness was proportional to the number of reaction cycles. Repeating this reaction cycle led to precisely controlled growth. The film properties were analyzed using Auger electron spectroscopy, X-ray photoelectron spectroscopy, Rutherford backscattering spectroscopy and time-of-flight elastic recoil detection analysis. The concentration of chlorine and hydrogen impurities was 0.23 and 2.01 at.%, respectively. AlN films showed good anti-oxidation properties when O₂ was annealed at 650 °C for 30 min.     

Nitridation of aluminum particles and formation process of aluminum nitride coatings by reactive RF plasma spraying

Nitridation of aluminum particles and formation process of aluminum nitride coatings by reactive RF plasma spraying was investigated by collecting splat and depositions and fabrication of the coating. Nitriding reaction of aluminum particles during flight in the plasma and after deposit on the substrate was confirmed by the observation of splats and the deposition morphologies, respectively. However, as nitriding reaction of aluminum particles easily forms brittle agglomerates on the substrate, the formation of sound coating was difficult. Though the coating was fabricated with the spraying condition of RF power of 5 kW, it was impossible to fabricate the coatings with RF power of 6 kW. In order to fabricate aluminum nitride coatings by reactive RF plasma spraying, it is necessary to control the plasma and the substrate temperature for the suitable conditions with changing RF power and nitrogen gas flow rate.     

Deposition and characterization of reactive magnetron sputtered aluminum nitride thin films for film bulk acoustic wave resonator

This work studies the relationship between the deposition process parameters and the properties of sputtered c-axis-oriented aluminum nitride (AlN) thin films. AlN films were deposited on a Pt electrode by reactive magnetron sputtering under various deposition conditions. The films were characterized by X-ray diffraction (XRD) and field-emission scanning electron microscopy (FESEM). A polycrystalline AlN film with highly c-axis-preferred orientation was achieved. The XRD rocking curve was 2.7°. The FESEM photographs also show that the AlN film has a dense hexagonal surface texture with uniform grain size and a highly ordered column structure.     

The characteristics and residual stress of aluminum nitride films grown by two-stage sputtering of mid-frequency power

The [0 0 2] oriented aluminum nitride has a high surface acoustic wave speed and high mechanic-electron couple coefficient. It is a potential material for manufacturing piezoelectric devices in high frequency application. The AlN films deposited onto silicon substrates were fabricated by two-stage sputtering process with mid-frequency generator. The results showed that the film did not have well [0 0 2] preferred orientation at 1.0 and 1.5 kW, and exhibited a [0 0 2] preferred orientation at 2.0 kW. The adhesion was poor when the film had a high preferred orientation because the substrate was damaged by high energetic atoms bombardment. A two-stage growth method was investigated in order to get high [0 0 2] preferred orientation and good adhesion. A good performance was obtained at the first stage power of 1.5 kW and the second stage power of 2.0 kW. The film showed a tensile stress state when the film was deposited at 1.0 kW. In contrast, the stress state was changed to compressive when the films were grown at 2.0 kW. The two-stage growth could succeed not only to get a high [0 0 2] preferred orientation but also to develop a reducing global stress film.     

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.     

Ab initio tensile testing simulation of aluminum and aluminum nitride ceramics based on density functional theory

The ideal strength and mechanical behavior of aluminum, aluminum nitride, and their composites at zero temperature are investigated using ab initio norm conserving pseudopotential methods based on local density approximation. The total energy and stress of supercells which contain these atomistic models are calculated under uniaxial tensile strain. Estimated various physical properties of aluminum and aluminum nitride at equilibrium state are in good agreement with the experiment. The tensile test of the composite model shows a failure of the composite in the aluminum matrix. The ideal strength of these models is also estimated.     

Preparation of triazinedithiol polymeric nanofilm by two-step potentiostatic polymerization technique on aluminum surface

The polymerization potential of triazinedithiol monosodium on an aluminum surface was studied by cyclic voltammetry. A polymeric nanofilm of triazinedithiol was prepared by a two-step potentiostatic polymerization technique on the aluminum surface. The polymeric nanofilm was characterized by means of FT-IR spectra, X-ray photoelectron spectroscopy (XPS) and atomic force microscopy (AFM). The results show that the triazinedithiol polymeric nanofilm can be obtained successfully by the two-step potentiostatic polymerization technique. The polymeric nanofilm on the aluminum surface obtained by this technique owes higher coverage compared with that prepared by the one-step technique. It is expected that this technique can meet application requirements of the triazinedithiol polymeric nanofilm in wider fields.     

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.     

Effect of Different Precursors on Synthesized AlN by Plasma-Assisted Ball Milling

A rapid and high efficient method for synthesized aluminum nitride (AlN) nano-powers by using plasma-assisted ball milling (p-milling) has been reported. P-Milling displayed an excellent synergistic effect as unique advantage, which is characterized by concurrent action of rapid heating from plasma and the impact stress from ball milling on the precursors, and it greatly reduced the synthesis temperature for precursors and effectively improved the synthesized efficiency of AlN. Additionally, the characterization of alumina (Al₂O₃) and mixture of alumina and carbon (Al₂O₃/C) precursors, as well as corresponding synthesized AlN, were investigated and compared, and the results showed that the synthesized AlN from Al₂O₃/C precursor has a much higher conversion rate at lower temperature even if the grain size was relatively greater than that from Al₂O₃ precursor. Moreover, the synthesized AlN powders from p-milling Al₂O₃/C have a better superiority on particle size, particle distribution, and crystal morphology.     

包覆成孔剂法制备高性能多孔氮化硅陶瓷工艺

为了制备高强度且分布均匀的氮化硅陶瓷,采用包覆成孔剂法改进普通添加成孔剂的方法,常压烧结氮化硅多孔陶瓷,采用阿基米德法、三点弯曲法分别测试材料的孔隙率及抗弯强度,用扫描电镜和光学放大镜对氮化硅多孔陶瓷显微结构和表观结构进行研究.结果表明,添加包覆过的成孔剂强度比添加未包覆的成孔剂强度高,孔隙率为50%时,强度增加近一倍.强度的提高归因于特殊的微观结构,即气孔的均匀分布和孔与孔之间相间隔分布.     

Preparation and properties of TiN and AlN films from alkoxide solution by thermal plasma CVD method

Single phase TiN and AlN films were prepared on a Si wafer from titanium tetra-etoxide and aluminum tri-butoxide solutions dissolved in ethanol and toluene, respectively, using an Ar/N₂/H₂ radio-frequency (r.f.) inductive thermal plasma chemical vapor deposition (CVD) method. The films were characterized by X-ray diffraction, X-ray photoelectron spectroscopy, scanning electron microscopy, measurement of electrical resistivity and Vickers microhardness. Factors affecting the formation of the films (lattice parameter, chemical composition, oxygen/carbon content, and deposition rate of the films) were examined in terms of the N₂ flow rate (2.5–4.5 slm), substrate temperature (300–700°C), feed rate of the solution (0.025–0.3 ml/min), and the mole ratio of the alkoxide solution (1:1–1:3). The optimum conditions for preparation of TiN films produced a film 0.2–3 μm thick with an oxygen content of 8 at.% and a free carbon content of 4 at.%, showing an electrical resistivity of 370 μΩ cm. The optimum conditions for AlN films produced a film 0.3 μm thick containing 14 at.% oxygen and 8 wt.% carbon. The deposition rate of the TiN film was determined to be 30–35 nm/min. The Vickers microhardness of the TiN and AlN films was found to be 10±1 and 13±3 GPa, respectively.     

Deposition and characterization of c-axis oriented aluminum nitride films by radio frequency magnetron sputtering without external substrate heating

Aluminum nitride (AlN) films were deposited on a variety of substrates (glass, Si, oxidized Si, Al-SiO₂-Si, Cr-SiO₂-Si, and Au-Cr-SiO₂-Si) by radio frequency (RF) magnetron sputtering using an AlN target. The films were deposited without external substrate heating. The effect of RF power, ambient gas (Ar and Ar-N₂) and sputtering pressure on deposition rate and crystallinity were investigated. The structure and morphology of the films were studied by X-ray diffraction, scanning electron microscopy and atomic force microscopy techniques. These investigations revealed that the AlN films prepared in mixed gas ambient (Ar-N₂) were highly c-axis oriented with moderate surface roughness on all the substrate. A strong IR absorption band was observed around 670 cm^− 1 which confirms the presence of Al-N bond in the film. The dc resistivity of the films was measured to be in the range of 10¹¹ to 10¹² Ω-cm at moderate electric fields. The application of these films in piezoelectric based micro-electro-mechanical systems is discussed.     

等离子体法制备超细粉体氮化铝的研究

以微米级铝粉为原料 ,用N2 热等离子体法制备了超细氮化铝粉体。在等离子体功率12kW ,运行N2 流量 2m3/h ,急冷NH3流量 0 6m3/h ,送粉N2 流量 0 8m3/h条件下 ,铝粉全部转化为纳米氮化铝。采用SEM技术和粒度分析仪对产品进行了分析 ,制得的氮化铝粉末平均粒径为10 0nm ,粒度分布为 4 0～ 14 0nm     

氮化铝的溶剂热合成及形貌研究

通过溶剂热方法合成出了氮化铝材料,并研究了溶剂种类、温度、表面活性剂等不同条件对合成氮化铝粉末的结晶度、纯度和形貌的影响。实验中通过控制条件得到了棒状、片状、球状和多孔形貌的氮化铝粉末。结果发现,用二甲苯为溶剂合成的氮化铝结晶度好,而生成的氮化铝纯度随着反应温度升高而增加,同时表面活性剂的加入对结晶度也存在一定的影响。     

Preparation of AlN thin films by nitridation of Al-coated Si substrate

AlN thin films have been grown on Al-coated Si(100) and Si(111) substrates by using nitridation in high-purity nitrogen ambient, where the Al layer was previously deposited on Si by ultra-high vacuum (UHV) electron beam evaporation. The temperature of nitridation was found to play an important role in the formation of AlN films. XRD results showed AlN films formed by nitridation at 1000°C for 30 min exhibited good crystallinity with the preferred orientation of (002) for both Si(111) and Si(100) cases. Other analysis techniques, like Fourier transform infrared spectroscopy and X-ray photoelectron spectroscopy have been used to evidence the formation and purity of the AlN films. Scanning electron microscope observations of the films revealed a closely-packed granular texture.     

潘宁放电溅射沉积纳米级AlN薄膜的性质

设计并制造了新的潘宁型等离子体源实验装置，分析了等离子体的发射光谱和产生AIN的动力学机理。在室温条件下，纯氮气的工作环境中用潘宁放电离子源溅射的方法，在Si（100）衬底上制备了纳米级的光滑平整AIN薄膜。本文用扫描电镜（SEM），原子力显微镜（ATM），红外吸收光谱（FTIR）和拉曼光谱（Raman shift）等测试分析技术用来研究了薄膜的微结构特征。