Synthesis of aluminum nitride in a coke – calcium reduction bed using nitrogen in air

An experimental study on the heating of a mixture of aluminum and lithium hydroxide （LiOH） powders in a reductive bed under air atmosphere is reported. The formation of aluminum nitride （A1N） during this process was the focus of this study. The formation of A1N was achieved using LiOH as an additive and heating the sample in a resistance furnace in a specially designed double crucible within a bed of a mixture of coke and filamentous calcium. The temperature range of the reaction was between 700℃ and 1100℃. The optimum temperature of 1100℃ and the optimum LiOH amount （Swt%） required to achieve maximum yield were determined by powder X-ray diffraction （XRD） analysis. Scanning electron microscopy （SEM） micrographs clearly indicated the transformation of grain structures from rods （700℃） to cauliflower shapes （1100℃）.

Morphology control of aluminum nitride(AlN)for a novel high-temperature hydrogen sensor

Hydrogen is a promising renewable energy source for fossil-free transportation and electrical energy generation.However,leaking hydrogen in high-temperature production processes can cause an explosion,which endangers production workers and surrounding areas.To detect leaks early,we used a sensor material based on a wide bandgap aluminum nitride(AlN)that can withstand a high-temperature environment.Three unique AlN morphologies(rod-like,nest-like,and hexagonal plate-like)were synthesized by a direct nitridation method at 1400℃usingγ-AlOOH as a precursor.The gas-sensing performance shows that a hexagonal plate-like morphology exhibited p-type sensing behavior and showed good repeatability as well as the highest response(S=58.7)toward a 750 ppm leak of H2 gas at high temperature(500°C)compared with the rod-like and nest-like morphologies.Furthermore,the hexagonal plate-like morphology showed fast response and recovery times of 40 and 82 s,respectively.The surface facet of the hexagonal morphology of AlN might be energetically favorable for gas adsorption–desorption for enhanced hydrogen detection.

Recent Progress on Fabrication of Thermal Conductive Aluminum Nitride Fibers

Among nitride fibers,aluminum nitride(AlN)fibers have been developed for various advanced applications due to their mechanical flexibility,high thermal conductivity,and excellent electrical insulation and chemical stability.This article presents an overview on the recent progress of AlN fibers.The properties of AlN,particularly the thermal conductivity of AlN in polymer matrix composites are introduced.Afterward,two major approaches,carbothermal reduction and nitriding polycrystalline alumina fiber,for the preparation of AlN fibers are discussed.The carbothermal reduction includes electrospinning,solution blow spinning,and chemical vapor deposition.Furthermore,some perspectives on the future directions for the preparation and application of fibrous AlN are highlighted.This review is expected to provide readers with valuable guidance on the preparation of AlN fibers and inspire researchers to explore more potential applications.

In situ fabrication and properties of Al N dispersion strengthened 2024 aluminum alloy

Nanoscaled aluminum nitride （AlN） dispersion strengthened 2024 aluminum alloy was fabricated using a novel approach in which Al-Mg-Cu compacts were partially nitrided in flowing nitrogen gas. The compacts were subsequently consolidated by sintering and hot extrusion. The microstructure and mechanical properties of the material were preliminarily investigated. Transmission electron microscopy and X-ray diffraction results revealed that AlN particles were generated by the nitridation of Al-Mg-Cu compacts. The material exhibited excellent mechanical properties after hot extrusion and heat treatment. The ultimate tensile and yield strengths of the extruded samples containing 8.92vol% AlN with the T6 heat treatment were 675 and 573 MPa, respectively.

Chloride Assisted Growth of Aluminum Nitride Nanobelts and Their Enhanced Dielectric Responses

Aluminum nitride （AlN） nanobelts were successfully synthesized in high yield through a chloride assisted vapor-solid process. X-ray diffraction, transmission electron microscopy, and selected area electronic diffraction demonstrate that the as-prepared nanobelts are pure, structurally uniform and single crystalline, and can be indexed to hexagonal wurtzite structure. The micro observations show that there exist no defects in the obtained nanobelts. The growth direction of the nanobelts is along [0001]. The frequency spectra of the relative dielectric constant and of the dielectric loss were measured in the frequency range of 50 Hz to 5 MHz. Analysis of these spectra indicates that the interface in samples has great influence on the dielectric behavior of samples. As compared with AlN micropowders, AlN nanobelts have much higher relative dielectric constant, especially at low frequencies at room temperature.

Preparation of Nanometric Particles of Aluminum Nitride by Pyrolysis of Diethylaluminun Azide

Thermal stabilities of diethylaluminum azide were studied by means of theoretical analysis and expriments.The results have shown that diethylaluminum and azid be heated to vigorous refluxing under vacuum(400 Pa) at temperature as high as 420℃ without incident of explosion and decomposes smoothly during 460 ～580℃ to form nanometric particles of aluminum nitride in the aerosol synthesis reactor. A new way of preparing nanometric parties of aluminum nitrideis found.

Preparation of Ultra-fine Aluminum Nitride in Thermal Plasma

Ultra-fine aluminum nitride has been synthesized by the evaporation of aluminum powder at atmospheric-pressure nitrogen plasma in a hot-wall reactor. The average size of aluminum nitride particle is 0.11 μm measured by scanning electric mirror (SEM), and the purity is at least over 90% evaluated by X-Ray diffraction (XRD). The conversion of Al powder to aluminum nitride is strongly depended on the injection of NH3. Typical experimental parameters such as the feed rate of raw material, the flow rate of ammonia and the position of injecting aluminum powder into the reactor are given.

Aluminum Reduction and Nitridation of Bauxite

The application of bauxite with low Al2O3 content has been studied in this paper and β-SiAlON has been obtained from two kinds of bauxites （Al2O3 content 68.08 mass% and 46.30 mass% respectively） by aluminum reduction and nitridation method. The sequence of reactions has been studied using thermal analysis （TG-DTA）, X-ray diffraction （XRD） analysis and scanning electron microscopy （SEM） with EDS. Compared with carbon thermal reduction and nitridation of aluminosilicates employed presently, the reaction in the system of bauxite-Al-N2 occurs at lower temperature. β-SiAlON appears as one of the main products from 1573K and exists stably in the range of the present experimental temperature. The microstructure of β-SiAlON obtained at 1773 K is short column with 5-10μm observed by SEM.

Synthesis of aluminum nitride nano-powder by decomposed diethylaluminum azide in aerosols

An aerosol process for making aluminum nitride nano-powder by decompositionof single compound diethylalumimm az-ide was described. X-ray diffraction (XRD) and transmissionelectron microscopy (TEM) were used to study characters of the A1N powder. It is shown that theprocess can produce spherical A1N powder with mean particle diameters ranging from 10 to 50 nm at500-800°C. The generated amorphous A1N powder is characterized by a BET (Brunauer-Emmett-Teller)surface area of 103 m2/g and is very reactive to moisture.

Characteristics of inclusions in high-Al steel during electroslag remelting process

The characteristics of inclusions in high-A1 steel refmed by electroslag remelting （ESR） were investigated by image analysis, scanning electron microscopy （SEM）, and energy-dispersive spectrometry （EDS）. The results show that the size of almost all the inclusions observed in ESR ingots is less than 5 μm. Inclusions smaller than 3 μm take nearly 75% of the total inclusions observed in each ingot. Inclu- sions observed in ESR ingots are pure AIN as dominating precipitates and some fine spherical Al2O3 inclusions with a size of 1 μm or less. It is also found that protective gas operation and slag deoxidation treatment during ESR process have significant effects on the number of inclusions smaller than 2μm but little effects on that of inclusions larger than 2 μm. Thermodynamic calculations show that AIN inclusions are unable to precipitate in the liquid metal pool under the present experimental conditions, while the precipitation of AlN inclusions could take place at the solidifying front due to the microsegregation orAl and N in liquid steel during solidification.

Thermal conductivity behavior of SPS consolidated AlN/Al composites for thermal management applications

A1N/A1 composites are a potentially new kind of thermal management material for electronic packaging and heat sink applications. The spark plasma sintering （SPS） technique was used for the first time to prepare the A1N/A1 composites, and attention was focused on the effects of sintefing parameters on the relative density, microstructure and, in particular, thermal conductivity behavior of the composites. The results showed that the relative density and thermal conductivity of the composites increased with increasing sintering temperature and pressure. The composites sintered at 1550℃ for 5 min under 70 MPa showed the maximum relative density and thermal conductivity, corresponding to 99% and 97.5 W.m-1.K-1, respectively. However, the thermal conductivity of present A1N/A1 composites is still far below the theoretical value. Possible reasons for this deviation were discussed.

Dielectric properties of spark plasma sintered AlN/SiC composite ceramics

In this study, we have investigated how the dielectric loss tangent and permittivity of AlN ceramics are affected by factors such as powder mixing methods, milling time, sintering temperature, and the addition of a second conductive phase. All ceramic samples were pre-pared by spark plasma sintering （SPS） under a pressure of 30 MPa. AlN composite ceramics sintered with 30wt%-40wt%SiC at 1600℃ for 5 min exhibited the best dielectric loss tangent, which is greater than 0.3. In addition to AlN and β-SiC, the samples also contained 2H-SiC and Fe5Si3, as detected by X-ray difraction （XRD）. The relative densities of the sintered ceramics were higher than 93%. Experimental results indicate that nano-SiC has a strong capability of absorbing electromagnetic waves. The dielectric constant and dielectric loss of AlN-SiC ce-ramics with the same content of SiC decreased as the frequency of electromagnetic waves increased from 1 kHz to 1 MHz.

High Potential Columnar Nanocrystalline AlN Films Deposited by RF Reactive Magnetron Sputtering

Columnar nanocrystalline aluminum nitride(cnc-AlN) thin films with(002) orientation and uniform texture have been deposited successfully on large silicon wafers by RF reactive magnetron sputtering.At the optimum sputtering parameters, the deposited cnc-AlN thin films show a c-axis preferred orientation with a crystallite size of about 28 nm and surface roughness(RMS) of about 1.29 nm. The cnc-AlN thin films were well transparent with an optical band gap about 4.8 e V, and the residual compressive stress and the defect density in the film have been revealed by Ramon spectroscopy. Moreover, piezoelectric performances of the cnc-AlN thin films executed effectively in a film bulk acoustic resonator structure.

Fabrication of AlN-TiC/Al composites by gas injection processing

The fabrication of AlN-TiC/Al composites by carbon- and nitrogen-containing gas injection into Al-Mg-Ti melts was studied. It was shown that AlN and TiC particles could be formed by the in situ reaction of mixture gas （N2 ＋ C2H2 ＋ NH3） with Al-Mg-Ti melts. The condition for the formation of AlN was that the treatment temperature must be higher than 1373 K, and the amounts of AlN and TiC increased with the increase of the treatment temperature and the gas injection time It was considered that AlN was formed by the direct reaction of Al with nitrogen-containing gas at the interface of the gas bubble and the melt. However, the mechanism of TiC formation is a combination mechanism of solution-precipitation and solid-liquid reaction.

Synthesis of Nano-Size AlN Powders by Carbothermal Reduction from Plasma-Assisted Ball Milling Precursor

Nano-size aluminum nitride （A1N） powders have been successfully synthesized with a high efficiency method through annealing from milling assisted by discharge plasma （p-milling） alumina （Al2O3） precursors. The characterization of the p-milling Al2O3 powders and the synthesized AlN are investigated. Compared to conventional ball milling （c-milling）, it can be found that the precursors by p-milling have a finer grain size with a higher specific surface area, which lead to a faster reaction efficiency and higher conversion to A1N at lower temperatures. The activation energy of p-milling Al2O3 is found to be 371.5 kJ/mol, a value that is much less than the reported value of the unmilled and the conventional milled Al2O3. Meanwhile, the synthesized AlN powders have unique features, such as an irregular lamp-like morphology with uniform particle distribution and fine average particle size. The results are attributed to the unique synergistic effect of p-milling, which is the effect of deformation, fracture, and cold welding of Al2O3 powders resulting from ball milling, that will be enhanced due to the introduction of discharge plasma.

Resonance-mode effect on piezoelectric microcantilever performance in air,with a focus on the torsional modes

A high quality factor is preferred for a microresonator sensor to improve the sensitivity and resolution. In this paper we systematically investigate the performance of the microcantilever in different resonance modes, which are the first three flexural modes, the first lateral mode, and the first and the second torsional modes. An aluminum nitride-based piezoelectric cantilever is fabricated and tested under controlled pressure from an ultra-high vacuum to a normal atmosphere, using a custom-built vacuum chamber. From the experiment results, it can be seen that the torsional modes exhibit better quality factors than those of the flexural and lateral ones. Finally, an analytical model for the air damping characteristics of the torsional mode cantilever is derived and verified by comparing with experimental results.

Influence comparison of N2 and NH3 nitrogen sources on AlN films grown by halide vapor phase epitaxy

A comparison of the nitrogen sources(N2 and NH3)influence on AlN films grown by high-temperature halide vapor phase epitaxy(HVPE)is reported.The x-ray rocking curves(XRCs)indicate that the full width at half maximum(FWHM)of(0002)plane for AlN films using N2 as nitrogen source is generally smaller than that using NH3.Optical microscope and atomic force microscope(AFM)results show that it is presently still more difficult to control the crack and surface morphology of AlN films with thicknesses of 5-10µm using N2 as the nitrogen source compared to that using NH3.Compared with one-step growth,two-step growth strategy has been proved more effective in stress control and reducing the density of threading dislocations for AlN epilayers using N2 as the nitrogen source.These investigations reveal that using N2 as nitrogen source in HVPE growth of AlN is immature at present,but exhibits great potential.

Morphology-Controlled Growth of A1N One-Dimensional Nanostructures

Aluminum nitride （AIN） nanowires, serrated nanoribbons, and nanoribbons were selectively obtained through a simple chloride assisted chemical vapor deposition process. The morphologies of the products could be controlled by adjusting the deposition position and the flux of the reactant gas. The morphologies and structures of the AIN products were investigated in detail. The formation mechanism of the as-prepared different morphologies of AIN one-dimensional （ID） nanostructures was discussed on the basis of the experimental results.

The fabrication of AlN by hydride vapor phase epitaxy

Aluminum nitride(AlN)is the promising substrates material for the epitaxial growth ofⅢ-nitrides devices,such as high-power,high-frequency electronic,deep ultraviolet optoelectronics and acoustic devices.However,it is rather difficult to obtain the high quality and crack-free thick AlN wafers because of the low surface migration of Al adatoms and the large thermal and lattice mismatches between the foreign substrates and AlN.In this work,the fabrication of AlN material by hydride vapor phase epitaxy(HVPE)was summarized and discussed.At last,the outlook of the production of AlN by HVPE was prospected.

Mechanism and kinetics analysis of AlN combustion synthesis

Mechanism of AlN combustion synthesis was studied by DSC analysis and “quenching” experiment of combustion wave. In preheating region, Al powder melted at 660 ℃ and became spherical because of surface tension. In reaction region, Al volatilized rapidly at 1 000 ℃ and Al vapor reacted with N2 to form AlN, which nucleated and grew on the surface of AlN formed precedently as a diluent. Based on the experiment analysis, kinetics equations and modeling were established. Analysis showed the dramatic effect of temperature, aluminum particle size and nitrogen pressure on the reaction speed.