AlN Films Research Articles

Improved Crystallinity of Annealed 0002 AlN Films on Sapphire Substrate

AlN is a piezoelectric material used in telecommunication applications due to its high surface acoustic wave (SAW) velocity, stability, and mechanical strength. Its performance is linked to film quality, and one method to achieve high-quality films goes through the process of annealing. Consequently, c-orientated AlN film with a thickness of 1.1 μm deposited on sapphire was annealed at temperatures of 1100 °C and 1150 °C in a N2 controlled atmosphere. This was compared to annealing at 1100 °C, 1450 °C, and 1700 °C with N2 flow in an open atmosphere environment. Sample rotation studies revealed a significant impact on the ⍵-2θ X-ray rocking curve. A slight variation in the film crystallinity across the wafer was observed. After the annealing, it was found that the lattice parameter c was increased by up to 2%, whereas the screw dislocation density dropped from 3.31 × 1010 to 0.478 × 1010 cm-2, and the full width at half maximum (FWHM) of reflection (0002) was reduced from 1.16° to 0.41° at 1450 °C. It was shown that annealing in a N2-controlled atmosphere plays a major role in reducing the oxidation of the AlN film, which is important for acoustic wave devices where the electrodes are placed directly on the piezoelectric substrate. The face-to-face arrangement of the samples could further reduce this oxidation effect.

Low donor ionization energy in Si-implanted heteroepitaxial AlN

We obtained high n-type conductivity and low donor ionization energy for an AlN film grown on SiC by Si ion implantation. The room temperature conductivity reaches 0.26 Ω−1 cm−1, and the donor ionization energy is only 112 meV, which is the best result of Si-implanted heteroepitaxial AlN. The lattice damage caused by ion implantation can be almost completely repaired by annealing at 1330 °C for 2 h. X-ray photoelectron spectroscopy (XPS) results show few O impurity in the sample. The low donor ionization energy is attributed to avoiding the introduction of O impurities and the mitigation of self-compensating effect. These results show the great potential of Si-implanted heteroepitaxial AlN for device applications.

Single-crystalline AlN/sapphire and composite electrode based ultra-high temperature surface acoustic wave devices

Single crystalline AlN material is very attractive for the development of high temperature electronic devices owing to its high temperature resistance. However, at ultrahigh temperatures, AlN film still will be oxidized and metal electrodes used for the devices will aggregate and vaporize. The deterioration of the material and metal electrodes eventually fails the AlN-based devices. Here, we report a single crystalline AlN film-based ultrahigh temperature surface acoustic wave (SAW) device. By using a thin alumina (Al2O3) protection layer on surface, oxidation of the AlN piezoelectric film was effectively inhibited at high temperatures. A composite electrode based on multilayer structure of Pt-Rh and Al2O3 was designed and fabricated, with the Al2O3 layer as the diffusion barrier layers to suppressed inter-diffusion, agglomeration and vaporization of the metals. The results showed that the developed AlN SAW devices can withstand high temperatures, and work well at temperatures up to 1400 °C.

Characteristics of c-axis oriented GeAlN films and applications to higher-order mode BAW resonators

AlN film bulk acoustic wave (BAW) resonators and filters that operate at frequencies above 5 GHz are required for 5G and beyond 5G communication applications. However, the power-handling capability, Q factor, and electromechanical coupling in high-frequency AlN film BAW resonators will be degraded as a result of the significantly reduced thickness and volume of the devices. Higher-order mode BAW resonators with polarity inverted (PI) multilayered films can operate at high frequencies while maintaining the thickness and volume of the devices. In this study, we fabricated an eight-layered PI GeAlN/AlN film BAW resonator by alternately growing Al-polar AlN layers and N-polar GeAlN layers. The PI GeAlN/AlN film BAW resonator resonated in the 8th-order mode. The film thickness of the PI GeAlN/AlN film BAW resonator was approximately thirteen times larger than that of a single-layer AlN film BAW resonator operating in the same frequency range.

High-Quality AlN Grown on Si(111) Substrate by Epitaxial Lateral Overgrowth

We report on the epitaxial lateral overgrowth (ELO) of high-quality AlN on stripe-patterned Si(111) substrates with various trench widths. By narrowing down the trench and ridge widths of patterned Si substrates, crack-free, 6-micrometer-thick, high-quality AlN films on Si substrates were produced. The full-width-at-half-maximum values of the X-ray-diffraction rocking curves for the AlN (0002) and (101¯2) planes were as low as 260 and 374 arcsec, respectively, corresponding to a record low dislocation density of 1.3 × 109 cm−2. Through the combination of a micro-Raman study and the X-ray diffraction analysis, it was found that narrowing the stripe width from 5 μm to 3 μm can reduce the vertical growth thickness before coalescence, resulting in a large decrease in the internal tensile stress and tilt angle, and, therefore, better suppression in the cracks and dislocations of the ELO–AlN. This work paves the way for the fabrication of high-performance Al(Ga)N-based thin-film devices such as ultraviolet light-emitting diodes and AlN bulk acoustic resonators grown on Si.

Research on nano-scale AlN nucleation layer growth and GaN HEMT characteristics based on MOCVD technology

The AlN nucleation layers of different thicknesses were grown on a 100 mm 4H-SiC substrate in a low-pressure MOCVD. By using in-situ high-temperature etching of the substrate steps, the AlN nucleation layer could achieve layered growth as soon as possible, and finally achieve 11.6 nm. The complete AlN film was prepared, and the surface morphology and interface quality of AlN were analyzed with atomic force microscope and transmission electron microscope. A 1.8 μm thick GaN HEMT epitaxial material was prepared based on the ultra-thin AlN nucleation layer. The (002) and (102) plane rocking curves of GaN had a FWHM of 138arcsec and 231arcsec, and the electrons mobility of the heterojunction two-dimensional electron gas reached 2200 cm2/V·s. The AlN interface thermal resistance measured by the high-precision 3ω method was reduced to 5.53 × 10−9 m2K/W.

Research on AlN thin film microstructure processing technology based on ultra-thin cantilever beam structure

Aiming at the problem of poor solution selection ratio when the AlN film and porous silicon sacrificial layer are released in the ultra-thin cantilever structure and at the problem of large surface roughness after AlN graphing, the wet corrosion process parameters were optimized, and the influence of different corrosive fluids and corrosion times on the surface roughness of AlN and the influence on the etching rate of AlN were studied, and different process parameters were selected for experiments. According to the experimental results, a suitable microstructure processing method was selected to effectively reduce the surface roughness of AlN and improve the integrity of the AlN film and the reliability and yield of the cantilever structure when the sacrificial layer is released. The microstructure fabrication of AlN films in ultra-thin cantilever structures enables the fabrication of ultra-micro-force sensors, accelerometers, acoustic sensors, and other devices.

The Effect of Defect Charge and Parasitic Surface Conductance on Aluminum Nitride RF Filter Circuit Loss

When AlN thin films are deposited directly on the high-resistance silicon (HR-Si) substrate, a conductive layer will be formed on the HR-Si surface. This phenomenon is called the parasitic surface conduction (PSC) effect. The presence of the PSC effect will increase the power consumption of electronic components. Therefore, it is necessary to reduce the PSC effect. In prior technology, the polysilicon layer is usually used as the trap-rich layer to reduce the PSC effect. Experiments show that compared to AlN films deposited directly on HR-Si, the AlN substrates with polysilicon introduced on HR-Si have less radio frequency (RF) loss. To verify the effect of polysilicon on RF loss, polysilicon films of three different thicknesses and several different roughnesses were introduced. The results show that the thickness of the polysilicon will affect the RF loss, while the roughness has almost no effect on it. The polysilicon trap-rich layer can reduce the RF loss, which gradually becomes smaller as the polysilicon thickness increases.

Experimental evidence for spin–triplet states in Titanium implanted AlN film: An electron spin resonance study

Spin carrying defects in wide-bandgap semiconductors are promising candidates for the development of quantum information and quantum sensing technology. Here we report experimental evidence for the formation of paramagnetic defects in AlN films, subjected to high-energy hydrogen and titanium ion implantation. X-ray diffraction and Raman spectroscopy show that ion species and implantation process could alter the amount of local strain in AlN films. Electron spin resonance spectroscopy reveals resonance peaks with g-value higher than the one of a free electron (2.0023) for both H-implanted and Ti-implanted AlN films. The origin of these peaks is identified and attributed to different types of point defects. For the Ti-implanted film, in addition to the central peak, a half-field resonance peak has been detected and assigned to spin–triplet (S=1). These results provide new insight into the electronic spin state of point defects in AlN, which opens up interesting perspectives for applications to quantum devices.

Homoepitaxy Growth of High‐Quality AlN Film on MOCVD AlN Template by Hydride Vapor Phase Epitaxy

Herein, AlN film grown on metal‐organic chemical vapor deposition (MOCVD) AlN template by high‐temperature hydride vapor phase epitaxy (HVPE) is characterized. High‐resolution X‐ray diffraction results show that the crystal quality of the film is improved compared with that of the template. Atomic force microscopy shows that the root mean square roughness value also decreases. Cathodoluminescence spectra show that the main impurities in the epitaxial layer and template are oxygen atoms. Raman spectroscopy and geometric phase analysis show that HVPE AlN samples maintain a compressive stress internally, which is the key to inhibit film cracking. Transmission electron microscope characterization reveals that most of the dislocations at the interface inherit from MOCVD AlN template, incline in the subsequent growth, react with each other, and finally annihilate. The dislocation bending and reduction mechanism are demonstrated.

The Effect of Nitridation on Sputtering AlN on Composited Patterned Sapphire Substrate.

Here, we report on the epitaxial growth of GaN on patterned SiO2-covered cone-shaped patterned sapphire surfaces (PSS). Physical vapor deposition (PVD) AlN films were used as buffers deposited on the SiO2-PSS substrates. The gallium nitride (GaN) growth on these substrates at different alternating radio frequency (RF) power and nitridation times was monitored with sequences of scanning electron microscopy (SEM) and atomic force microscopy (AFM) imaging results. The SEM and AFM show the detail of the crystalline process from different angles. Our findings show that the growth mode varies according to the deposition condition of the AlN films. We demonstrate a particular case where a low critical alternating current (AC) power is just able to break SiO2 covalent bonds, enabling the growth of GaN on the sides of the patterns. Furthermore, we show that by using the appropriate nitridation condition, the photoluminescence (PL) integral and peak intensities of the blue light epi-layer were enhanced by more than 5% and 15%, respectively. It means the external quantum efficiency (EQE) of epitaxial structures is promoted. The screw dislocation density was reduced by 65% according to the X-ray diffraction (XRD) spectra.

The relationship between annealing and nitrogen flow ratios during magnetron sputtering of AlN films

The relationship between annealing and nitrogen flow ratios during magnetron sputtering of AlN films

AlN Thin Films Grown on Different Substrates by Metal Nitride Vapor Phase Epitaxy

AbstractIn this paper, AlN thin films are fabricated by green and efficient metal nitride vapor phase epitaxy (MNVPE). First, AlN films are grown on c‐plane sapphire substrates at different molar flow ratios (V/III ratios) of the source material, and the effects of V/III on the crystal quality and surface morphology of the films are investigated. The growth conditions are kept constant (growth temperature of 1550 °C, growth pressure of 10 kPa, V/III ratio of 4420), and the AlN thin films are prepared by heterogeneous epitaxial growth on c‐plane sapphire, silicon (111), and GaN substrates. The crystal quality, residual stress, and luminescence properties of epitaxial AlN thin films on the three substrates are investigated using X‐ray diffraction, scanning electron microscopy, Raman spectroscopy, photoluminescence, and UV spectrophotometer. Among them, the FWHM value of the sample AlN/GaN (002) plane can reach 338 arcsec. The residual stress in samples AlN/Sapphire, AlN/GaN and AlN/Si are 1027, −81, and −541 MPa, respectively, and the sample AlN/GaN has fewer point defects. At the same time, a 50‐nanometer‐thick void layer appears in the AlN thin film samples prepared on GaN substrates, which provides a new technical idea for realizing large‐scale and high‐quality self‐supporting AlN thin films.

Investigation of Mo Doping Effects on the Properties of AlN-Based Piezoelectric Films Using a Sputtering Technique

In this study, AlN-based films are deposited using a sputtering deposition method, and Mo dopants with different concentrations are added in the proposed system by controlling the sputtering power in order to improve the crystallinity and piezoelectric properties of AlN films. Through a detailed material analysis including energy-dispersive X-ray spectroscopy (EDS), X-ray diffraction (XRD), scanning electron microscopy (SEM), atomic force microscopy (AFM), piezoresponse force microscopy (PFM), and nano-indentation, the piezoelectric property optimization mechanism of proposed films was explored and the best process parameters were determined. The piezoelectric coefficient d33 of AlN:Mo (3.46%) films reached 7.33 pm V−1, which is 82.79% higher than that of undoped AlN. As compared with the reported data about the dopants in AlN system, our proposed films have the better d33 values with those dopants in AlN-based films except Sc dopants. However, Sc is known as an expensive metal, our proposed films could be applied to low-cost piezoelectric MEMS applications.

Heteroepitaxy Growth and Characterization of High-Quality AlN Films for Far-Ultraviolet Photodetection.

The ultra-wide bandgap (~6.2 eV), thermal stability and radiation tolerance of AlN make it an ideal choice for preparation of high-performance far-ultraviolet photodetectors (FUV PDs). However, the challenge of epitaxial crack-free AlN single-crystalline films (SCFs) on GaN templates with low defect density has limited its practical applications in vertical devices. Here, a novel preparation strategy of high-quality AlN films was proposed via the metal organic chemical vapor deposition (MOCVD) technique. Cross-sectional transmission electron microscopy (TEM) studies clearly indicate that sharp, crack-free AlN films in single-crystal configurations were achieved. We also constructed a p-graphene/i-AlN/n-GaN photovoltaic FUV PD with excellent spectral selectivity for the FUV/UV-C rejection ratio of >103, a sharp cutoff edge at 206 nm and a high responsivity of 25 mA/W. This work provides an important reference for device design of AlN materials for high-performance FUV PDs.

Influence of growth temperature and miscut angle of m-plane sapphire substrate on the semi-polar (11–22) AlN film grown by HVPE

The high-quality semi-polar (11-22) AlN thin films were grown on m-plane sapphire substrates by hydride vapor phase epitaxy (HVPE). The surface morphology and crystalline quality of the AlN film were greatly influenced by the growth temperature and the substrate miscut angle. As the temperature increased, the grain size on the surface increased and the grain density decreased. In addition, the higher growth temperature also resulted in smaller values of the full width at half maximum (FWHM) of X-ray rocking curves (XRC) when temperature was more than 1,460 °C. At high temperature of 1,530 °C, the introduction of 1° -off miscut angle to the substrate resulted in smooth surface, low density of stacking faults and low FWHM of XRC. The misfit dislocation density was calculated from the tilt angle of epilayer measured by X-ray reciprocal space mappings along [−1−123] AlN. The misfit dislocation density of the sample grown on 1° -off substrates was 6.7 × 105 cm−2. The improvement of crystal quality is believed to be due to the enhancement of adatom mobility at higher temperatures and also the appropriate miscut variation.

Demonstration of Thin Film Bulk Acoustic Resonator Based on AlN/AlScN Composite Film with a Feasible Keff2.

Film bulk acoustic resonators (FBARs) with a desired effective electromechanical coupling coefficient (Keff2) are essential for designing filter devices. Using AlN/AlScN composite film with the adjustable thickness ratio can be a feasible approach to obtain the required Keff2. In this work, we research the resonant characteristics of FBARs based on AlN/AlScN composite films with different thickness ratios by finite element method and fabricate FBAR devices in a micro-electromechanical systems process. Benefiting from the large piezoelectric constants, with a 1 μm-thick Al0.8Sc0.2N film, Keff2 can be twice compared with that of FBAR based on pure AlN films. For the composite films with different thickness ratios, Keff2 can be adjusted in a relatively wide range. In this case, a filter with the specific N77 sub-band is demonstrated using AlN/Al0.8Sc0.2N composite film, which verifies the enormous potential for AlN/AlScN composite film in design filters.

Thermodynamic Analysis of Group-III-Nitride Alloying with Yttrium by Hybrid Chemical Vapor Deposition.

Group-IIIb-transition-metal-alloyed wurtzite Group-IIIa-nitride (IIIb-IIIa-N) thin films have higher piezoelectric characteristics than binary IIIa-N for a broad range of applications in photonic, electronic, sensing, and energy harvesting systems. We perform theoretical thermodynamic analysis for the deposition and epitaxial growth of Y-alloyed GaN and AlN films by a newly introduced growth technique of hybrid chemical vapor deposition (HybCVD), which can overcome the limitations of the conventional techniques. We investigate the equilibrium vapor pressures in the source zones to determine the dominant precursors of cations for the input of the mixing zone. Then, we study the driving force for the vapor-solid phase reactions of cation precursors in the growth zone to calculate the relationship between the solid composition of YxGa1-xN and YxAl1-xN and the relative amount of input precursors (Y vs. GaCl and AlCl3) in different deposition conditions, such as temperature, V/III precursor input ratio, and H2/inert-gas mixture ratio in the carrier gas. The xY composition in YAlN changes nearly linearly with the input ratio of cation precursors regardless of the growth conditions. However, YGaN composition changes non-linearly and is also substantially affected by the conditions. The thermodynamic analysis provides insight into the chemistry involved in the epitaxial growth of IIIa-IIIb-N by the HybCVD, as well as the information for suitable growth conditions, which will guide the way for ongoing experimental efforts on the improvement of piezoelectricity of the lead-free piezoelectric materials.

The ultra-thin AlN epitaxy on monolayer WS2 by helicon sputtering at 400 °C

This work demonstrates the epitaxial growth of ultra-thin AlN films grown on monolayer WS2/Sapphire by helicon sputtering. In our work, WS2 acts as a template to facilitate the initial two-dimensional (2D) AlN growth via van der Waals epitaxy (VDWE), and this growth method provides a promising semiconductor manufacturing process with low thermal budget (<450 °C) than the required for the backend-of-the-line (BEOL). The ultrathin AlN epitaxy on WS2 is characterized by synchrotron-based grazing-incidence wide-angle x-ray scattering (GIWAXS). There are two stages in AlN epitaxy on the WS2; the first is the layered AlN growth aligned with the underlying WS2 lattice. The subsequent development of AlN transforms into 3D growth, which is similar to Stranski–Krastanov (SK) mode. The ultrathin AlN films achieve atomic level smoothness and significant piezoelectric properties as indicated by the technique of atomic- and piezo force microscopy (AFM/PFM). This research broadens the application of 2D materials in assisting AlN epitaxy and has a potential avenue for hetero-epitaxial integration in developing future electronic devices.

Moisture barrier coating of AlN and Al2O3 multilayer film prepared by low-temperature atomic layer deposition

AlN and Al2O3 multilayer films intended as moisture barriers were deposited on polyethylene naphthalate films by remote-type plasma-enhanced atomic layer deposition. The deposition temperatures for AlN and Al2O3 were 160 and 20 °C, respectively. It was assumed that the AlN and Al2O3 interface would suppress the formation of dislocations and pinholes that lead to moisture diffusion. The AlN top layer was expected to act as a water-resistant layer. The surface morphology and the crystallinity of the deposited film were investigated by atomic force microscopy (AFM) and x-ray diffraction, respectively. The gas barrier property of the multilayer film was determined by the water vapor transmission rate, which was measured as 1.3 × 10−3 g/m2/day at a temperature of 40 °C and a relative humidity (RH) of 90%. The AFM image showed that the AlN top layer remained unchanged during water vapor contact for 120 h at 40 °C and 90% RH. The applicability of the multilayer film as a moisture barrier coating for compound semiconductor devices is discussed.