Epitaxial Aluminum Nitride Research Articles

Effect of stress control by growth adjustment on the edge thread dislocation density of AlN grown on the sapphire

The relationship between stress and dislocation density in MOCVD epitaxial AlN was studied. It has been found that the aluminum nitride (AlN) epitaxial layer generates tensile stress when the crystal islands are merged. By controlling the size and density of crystal islands at the end of 3D growth, the tensile stress generated during epitaxy can be effectively reduced. Mechanical calculations show that there is a linear relationship between the edge thread dislocations density of AlN and the tensile stress during growth. By controlling the stress during AlN growth below 0.1 Gpa, a high-quality AlN sample with an edge thread dislocation density of 6.31 × 107 cm−2 was obtained.

Room temperature quantum emitters in aluminum nitride epilayers on silicon

Room temperature quantum emitters have been reported in aluminum nitride grown on sapphire, but until now they have not been observed in epilayers grown on silicon. We report that epitaxial aluminum nitride grown on silicon by either plasma vapor deposition or metal-organic vapor phase epitaxy contains point-like emitters in the red to near-infrared part of the spectrum. We study the photon statistics and polarization of emission at a wavelength of 700–750 nm, showing signatures of quantized electronic states under pulsed and CW optical excitation. The discovery of quantum emitters in a material deposited directly on silicon can drive integration using industry standard 300 mm wafers, established complementary metal-oxide-semiconductor control electronics, and low marginal-cost mass-manufacturing.

Strain accumulation and relaxation on crack formation in epitaxial AlN film on Si (111) substrate

The formation of cracks is often observed in the epitaxial growth of ultrawide-bandgap aluminum nitride (AlN) semiconductor films on economical and versatile silicon (Si) substrates due to the significant differences in in-plane lattice parameters and thermal expansion coefficients between the film and the substrate, which hampers the development of template, buffer layer, and device structure with a relatively thick AlN layer for devices. The present study aims to elucidate the conditions of crack formation through a simple but comprehensive estimation of strain energy accumulation and relaxation by lattice strain, misfit dislocation density, and crack formation. Strain energy in the epitaxial film from lattice and thermal mismatches is evaluated by an elastic strain equation tailored to the epitaxy of the hexagonal crystal structure. The effects of temperature, thickness, and dislocation density on the lattice and dislocation strain energies of the film are also considered. Finally, the comparison in the changes in the total strain energy and cleavage energy with decreasing temperature shows that cleavage energy is higher than strain energy if the film is thinner than 400 nm but becomes lower than the strain energy if the film is thicker than 400 nm during cooldown, suggesting the crack formation, which matches well with experimental observations.

Molecular beam homoepitaxy of N-polar AlN: Enabling role of aluminum-assisted surface cleaning

N-polar aluminum nitride (AlN) is an important building block for next-generation high-power radio frequency electronics. We report successful homoepitaxial growth of N-polar AlN by molecular beam epitaxy (MBE) on large-area, cost-effective N-polar AlN templates. Direct growth without any in situ surface cleaning leads to films with inverted Al polarity. It is found that Al-assisted cleaning before growth enables the epitaxial film to maintain N-polarity. The grown N-polar AlN epilayer with its smooth, pit-free surface duplicates the structural quality of the substrate, as evidenced by a clean and smooth growth interface with no noticeable extended defects generation. Near band-edge photoluminescence peaks are observed at room temperature on samples with MBE-grown layers but not on the bare AlN templates, implying the suppression of nonradiative recombination centers in the epitaxial N-polar AlN.

X-band epi-BAW resonators

Using epitaxial aluminum nitride (AlN) developed for ultraviolet photonics and high-speed electronics, we demonstrate suspended AlN thin-film bulk acoustic resonators (FBARs) at 9.2 GHz in the X-band (8–12 GHz) of the microwave spectrum. The resonators show a Qmax≈614 and a figure of merit f⋅Q≈5.6 THz. The material stack of these epi-AlN FBARs allows monolithic integration with AlN/GaN/AlN quantum well high-electron-mobility-transistors to a unique RF front end and also enable integration with epitaxial nitride superconductors for microwave filters for quantum computing.

Comparative Spectroscopic Study of Aluminum Nitride Grown by MOCVD in H2 and N2 Reaction Environment

We report a comparative spectroscopic study on the thin films of epitaxial aluminum nitride (AlN) on basal plane sapphire (Al2O3) substrates grown in hydrogen (H2) and nitrogen (N2) gas reaction environments. AlN films of similar thicknesses (~3.0 µm) were grown by metal-organic chemical vapor deposition (MOCVD) for comparison. The impact of the gas environment on the AlN epilayers was characterized using high-resolution X-ray diffraction (HR-XRD), X-ray photoelectron spectroscopy (XPS), Raman scattering (RS), secondary ion mass spectroscopy (SIMS), cathodoluminescence (CL), atomic force microscopy (AFM), and scanning electron microscopy (SEM). The study showed that AlN layers grown in a N2 environment have 50% less stress (~0.5 GPa) and similar total dislocation densities (~109/cm2) as compared to the films grown in a H2 environment. On the other hand, AlN films grown in a H2 gas environment have about 33% lesser carbon and 41% lesser oxygen impurities than films grown in a N2 growth environment. The possible mechanisms that influenced the structural quality and impurity incorporation for two different gas environments to grow AlN epilayers in the MOCVD system on sapphire substrates were discussed.

Structure and Optical Properties of AlN Crystals Grown by Metal Nitride Vapor Phase Epitaxy with Different V/III Ratios.

The epitaxial aluminum nitride (AlN) crystals were grown on c-plane sapphire using high-temperature metal nitride vapor phase epitaxy at the source materials’ different molar flow ratios (V/III ratios). The effects of various V/III ratios on the surface morphology, crystalline quality, material straining, and optical properties of heteroepitaxial AlN thin films were studied using X-ray diffraction, scanning electron microscopy, Raman spectroscopy, and photoluminescence (PL). With the increase in the V/III ratio from 1473 to 7367, the substrate surface underwent changes that vary from whiskers to three-dimensional island structures, two-dimensional layered stack structures, and stacked sheet structures. Additionally, due to the presence of nanoscale pits on the substrate surface, almost all samples were tensile stressers. The PL spectra demonstrated the defect luminescence of the epitaxial films, indicating that nitrogen vacancies and oxygen impurities were the samples’ main defects.

AlN quasi-vertical Schottky barrier diode on AlN bulk substrate using Al0.9Ga0.1N current spreading layer

An aluminum nitride (AlN) quasi-vertical Schottky barrier diode (SBD) was fabricated on an AlN bulk substrate. An undoped AlN layer, a Si-doped Al0.9Ga0.1N current spreading layer and an AlN buffer layer were grown by plasma-enhanced molecular beam epitaxy. The epitaxial AlN layer was etched down to the n-Al0.9Ga0.1N layer to form an Ohmic contact. Ni/Au and V/Al/Ni/Au were deposited on the top AlN layer as Schottky contacts and on the exposed n-Al0.9Ga0.1N layer as Ohmic contacts, respectively. The Ohmic characteristics on the n-Al0.9Ga0.1N layer, capacitance–voltage (C–V) and current–voltage (I–V) characteristics of the AlN SBD were investigated.

Low-Temperature Epitaxial Growth of AlN Thin Films on a Mo Electrode/Sapphire Substrate Using Reactive Sputtering

High-crystalline aluminum nitride (AlN) thin films are essential for device applications, and epitaxial growth is a promising approach to improve their crystalline quality. However, a high substrate temperature is usually required for the epitaxial growth, which is not compatible with the complementary metal-oxide-semiconductor (CMOS) process. Furthermore, it is very difficult to obtain epitaxial AlN thin films on the deposited metal layers that are sometimes necessary for the bottom electrodes. In this work, epitaxial AlN thin films were successfully prepared on a molybdenum (Mo) electrode/sapphire substrate using reactive sputtering at a low substrate temperature. The structural properties, including the out-of-plane and in-plane relationships between the AlN thin film and the substrate, were investigated using X-ray diffraction (XRD) 2θ-ω, rocking curve, and pole figure scans. Additional analyses using scanning electron microscopy (SEM), atomic force microscopy (AFM), and transmission electron microscopy (TEM) were also carried out. It was shown that highly c-axis-oriented AlN thin films were grown epitaxially on the Mo/sapphire substrate with an in-plane relationship of AlN [112¯0]//sapphire [101¯0]. This epitaxial growth was attributed to the highly ordered and oriented Mo electrode layer grown on the sapphire substrate. In contrast, the AlN deposition on the Mo/SiO2/Si substrate under the same conditions caused poorly oriented films with a polycrystalline structure. There coexisted two different low-crystalline phases of Mo (110) and Mo (211) in the Mo layer on the SiO2/Si substrate, which led to the high mosaicity and polycrystalline structure of the AlN thin films.

Vapor-Phase Epitaxy of AlN Layers on AlN/Si(111) Templates Synthesized by Reactive Magnetron Sputtering

Epitaxial aluminum nitride (AlN) layers on Si(111) substrates have been grown by sequential application of several techniques including reactive magnetron sputter deposition to a thickness of 20 nm, metalorganic vapor-phase epitaxy (MOVPE) to a total thickness of 450 nm, and hydride vapor-phase epitaxy (HVPE) to a final thickness of 2 μm. Synthesis of AlN layers by this combined method provides a significant decrease in the residual strain and suppresses the formation of cracks in the epilayer.

Specific Features of the Pyroelectric Effect in Epitaxial Aluminum Nitride Layers Obtained on Si Substrates

Specific Features of the Pyroelectric Effect in Epitaxial Aluminum Nitride Layers Obtained on Si Substrates

Optical characterization of sputtered aluminum nitride thin films – correlating refractive index with degree of c-axis orientation

Aluminum Nitride (AlN) is a well-known compound piezoelectric material with high Complementary Metal-Oxide Semiconductor process compatibility. Previous results show that the piezoelectric coefficient correlates with the c-axis orientation of AlN. In this work, the optical properties of reactively sputtered AlN thin-films have been investigated to find a relation with the structural properties of the film (i.e. c-axis orientation) using spectroscopic ellipsometry. The results show that for almost the same film thickness, highly c-axis orientated films have higher refractive indices compared to films with low c-axis orientation or amorphous layers. A relationship between (002) peak intensity measured with x-ray diffractometry and refractive index is shown. At 546 nm wavelength, the refractive index decreased from 2.15 for films with high (002) peak intensity, to 2.11 for films with about half the peak intensity, and further down to 1.90 for films without preferred orientation. Additionally, with the same sputtering conditions, the variation of the film thickness seems to have no significant effect on the refractive index. The results of AlN thin-film mass density obtained from x-ray reflectivity measurements are consistent with refractive index measurements. The mass density of AlN thin-films with high c-axis orientation that resulted in a higher refractive index is 2.99 g/cm−3, compared to 3.23 g/cm−3 for epitaxial grown AlN layers. This value decreased to 2.82 g/cm−3 for films with poor c-axis orientation.

Photo-Enhanced Acid Chemical Etching of High-Quality Aluminum Nitride Grown by Metal-Organic Chemical Vapor Deposition

Photo-enhanced chemical (PEC) etch of wurtzite aluminum nitride (AlN) was investigated to overcome its low etch rate. Epitaxial AlN grown on Al2O3 substrate by metal-organic chemical vapor deposition method was immersed in phosphoric acid at different temperatures under 185 nm deep-UV excitation. An inverted pyramid structure with {10-1-1} faces initially appeared, after chemical etching, evolving into hexagonal columns with {1-100} m-planes. The PEC etch rate of m-plane AlN was six-fold higher than that of non-PEC one because the reaction was enhanced by the electron-hole pairs photo-generated by 185 nm wavelength. The decrease of the activation energy from 68.5 kJ/mol (non-PEC etch) to 48.1 kJ/mol (PEC etch) was extracted, implying a reaction-limited etching process. The PEC etch mechanism of wurtzite AlN in phosphoric acid was proposed, including the initiation and growth of the etch pit and the agglomeration of the hexagonal columns. Our results propose a facile method to control the surface morphology of AlN-based electronic and optoelectronic devices.

17 000%/W second-harmonic conversion efficiency in single-crystalline aluminum nitride microresonators

High quality factor optical microcavities have been employed in a variety of material systems to enhance nonlinear optical interactions. While single-crystalline aluminum nitride microresonators have recently emerged as a low loss platform for integrated nonlinear optics such as four wave mixing and Raman lasing, few studies have investigated this material for second-harmonic generation. In this letter, we demonstrate an optimized fabrication of dually resonant phase-matched ring resonators from epitaxial aluminum nitride thin films. An unprecendented second-harmonic generation efficiency of 17 000%/W is obtained in the low power regime, and pump depletion is observed at a relatively low input power of 3.5 mW. This poses epitaxial aluminum nitride as the highest efficiency second-harmonic generator among current integrated platforms.

Broadband tunable microwave photonic phase shifter with low RF power variation in a high-Q AlN microring.

An all-optically tunable microwave photonic phase shifter is demonstrated based on an epitaxial aluminum nitride (AlN) microring with an intrinsic quality factor of 3.2×106. The microring adopts a pedestal structure, which allows overcoupling with 700 nm gap size and facilitates the fabrication process. A phase shift for broadband signals from 4 to 25 GHz is demonstrated by employing the thermo-optic effect and the separate carrier tuning technique. A phase tuning range of 0°-332° is recorded with a 3 dB radio frequency (RF) power variation and 48 mW optical power consumption. In addition, AlN exhibits intrinsic second-order optical nonlinearity. Thus, our work presents a novel platform with a low propagation loss and the capability of electro-optic modulation for applications in integrated microwave photonics.

High-quality AlN films grown on chemical vapor-deposited graphene films

We report the growth of high-quality AlN films on graphene. The graphene films were synthesized by CVD and then transferred onto silicon substrates. Epitaxial aluminum nitride films were deposited by DC magnetron sputtering on both graphene as an intermediate layer and silicon as a substrate. The structural characteristics of the AlN films and graphene were investigated. Highly c-axis-oriented AlN crystal structures are investigated based on the XRDpatterns observations.

SEM, Dielectric, Pyroelectric, and Piezoelectric Response of Thin Epitaxial AlN Films Grown on SiC/Si Substrate

Structural characterization of the epitaxial thin aluminum nitride (AlN) 1-μm-thick films grown on SiC/(111)Si substrate by molecular beam epitaxy method was done. The films are shown to be single crystals of (0002) orientation with parameter full width half maximum FWHMωθ = 0.5°. A comparative study of the film electrical properties with the films grown by chloride vapor-phase epitaxy has revealed the difference in polar axis orientation, pyroelectric response, and piezoelectric hystograms.

Influence of the V/III ratio in the gas phase on thin epitaxial AlN layers grown on (0001) sapphire by high temperature hydride vapor phase epitaxy

Thin (0001) epitaxial aluminum nitride (AlN) layers were grown on c-plane sapphire using high temperature hydride vapor phase epitaxy. The experimental set-up consists of a vertical cold-wall quartz reactor working at low pressure in which the reactions take place on a susceptor heated by induction. The reactants used are ammonia and aluminum chlorides in situ formed via hydrogen chloride reaction with high purity aluminum pellets. As-grown AlN layers have been characterized by scanning electron microscopy, atomic force microscopy, X-ray diffraction, transmission electron microscopy, photoluminescence and Raman spectroscopies. The influence of the V/III ratio in the gas phase, from 1.5 to 15, on growth rate, surface morphology, roughness and crystalline quality is investigated in order to increase the quality of thin epitaxial AlN layers grown at high temperature. Typical growth rates of around 0.45μm/h were obtained for such thin epitaxial AlN layers. The growth rate was unaffected by the V/III ratio. An optimum for roughness, crystalline quality and optical properties seems to exist at V/III=7.5. As a matter of fact, for a V/III ratio of 7.5, best root mean square roughness and crystalline quality — measured on 0002 symmetric reflection — as low as 6.9nm and 898arcsec were obtained, respectively.

Epitaxial growth and optical properties of Al- and N-polar AlN films by laser molecular beam epitaxy

Epitaxial aluminum nitride (AlN) films with c-axis orientation were grown on both (1 1 1) MgO and c-sapphire substrates by laser molecular beam epitaxy. The in-plane epitaxial relationships were determined to be [1 1 0]AlN‖[0 1]MgO and [1 0 0]AlN‖[1 1 0]sapphire, and the lattice mismatch was 4.2% and 13.2% for AlN films on MgO and sapphire, respectively. The AlN films were shown to be Al- and N-polar on MgO and sapphire, respectively. The former is assumed to be caused by the centre of inversion symmetry of (1 1 1) MgO substrate, while the latter is due to the O polarity of sapphire. The full-width at half-maximum of the ω-scanning spectrum for AlN film on (1 1 1) MgO substrate is smaller than that on the c-sapphire substrate. The optical band-gap energies for AlN films grown on MgO and sapphire were found to be 5.93 and 5.84 eV, close to the standard band gap of 6.2 eV, and the calculated Urbach energies were 0.27 eV and 0.53 eV, respectively. These results indicate a lower amorphous content and/or less defects/impurities in Al-polar than N-polar AlN.

Microstructure of epitaxial AlN layers on sapphire substrates deposited by physical vapor deposition

ABSTRACTAsymmetric (10L) XRD peaks have been employed as a measure of epitaxial quality for aluminum nitride (AlN) nucleation layers (NL) deposited on sapphire substrate. Epitaxial AlN films have been deposited on 2-6” sapphire substrate by reactive sputtering. FWHM of AlN (103) and (105) were found to be an excellent indicator of quality of AlN films for GaN growth. AlN films produced nucleation layers with highly reproducible microstructure and GaN film growth. NLs had in-plane and out-of-plane texture as evident by the pole-figure results and selected area diffraction pattern. Based on electron microscopy results, AlN film thickness for complete atomic ordering was estimated to be 6-7 nm and most of the edge dislocations were seen in the first 20 nm of the film. Excellent thickness and texture uniformity were seen on planar and patterned sapphire substrates. A compressive stress of 2.9±0.2 GPa was seen in our BKM films. The maximum screw and edge dislocation densities of films were found to be ∼3 x 108 cm−2 and ∼9 x 109 cm−2 respectively. The root mean square roughnesses of A-polar films were found to be < 0.3 nm.