Sintering Behavior of Fine Aluminum Nitride Powder Synthesized from Aluminum Polynuclear Complexes

The sintering behavior of fine AIN powder synthesized from an aluminum polynuclear complex was investigated. The focus of this work was to investigate the densification behavior of the AIN powder with different particle sizes (specific surface area: 3.2–22.8 m²/g). The AIN powder was synthesized from basic aluminum chloride and glucose mixed in a water solution. This powder was divided into two groups: one with 2 wt% Y₂O₃ added as the sintering aid and the other without such an additive. The AIN powder investigated possessed favorable densification potential. The density of the AIN powder with a surface area of 16.6 m²/g and without additives attained theoretical density at 1700°C. Adding Y₂O₃ further decreased the sintering temperature required for full densification to 1600°C. It is speculated that low-temperature sintering of our fine AIN powder with Y₂O₃ proceeds in two steps: in the initial stage, sintering proceeds predominantly through interdiffusion between yttrium aluminates formed on the AIN powder surface; in the second stage, the densification may occur by the interdiffusion between solid phases formed by a reaction between the yttrium aluminates and AIN. To investigate the effect of oxygen on sintering, the content of oxygen in AIN powder was varied while the particle size was kept constant. In this study, the difference in surface oxygen content scarcely affected the sintering behavior of fine AIN powder.     

Reactivity of Aluminum Nitride Powder in Dilute Inorganic Acids

The reactivity of AlN powder in diluted inorganic acids was studied by measuring the pH and temperature during its hydrolysis. At very low starting pH (pH ∼1) no reaction was observed, regardless of the acid used. In contrast, in a less acidic environment, i.e., at higher pH values (pH ∼3), the reaction was fast enough to reveal the influence of different acids on the hydrolysis reaction. Monoprotonic acids which are completely dissociated (HCl, HF, HNO₃), and form water-soluble salts with aluminum, did not influence the hydrolysis reactions. In the presence of incompletely dissociated diprotonic H₂SO₄ and H₂CO₃ acids which form water-soluble salts with aluminum, the reaction was hindered but not prevented. In the presence of phosphoric acid the hydrolysis was prevented at room temperature, presumably because of the formation of insoluble phosphates on the powder surface. At elevated temperatures their solubility was substantial, and the reactivity of AlN powder in a diluted hot phosphoric acid was reestablished. In the presence of silicic acid the reaction was suppressed at both room and elevated temperatures, which was also ascribed to the formation of insoluble silicates. The adsorption of silicate anions onto the powder surface was confirmed by chemical analysis and zeta potential measurement. Using DRIFT measurements, however, the presence of Si–O bonds on the powder could not be unambiguously confirmed, since the characteristic wavelengths for these bonds are in the region of very strong Al–N stretching frequencies.     

Degradation of Aluminum Nitride Powder in an Aqueous Environmet

The degradation of A1N powder in excess H₂O at room temperature for up to 24 h was investigated. Samples were characterized by various techniques (IR; XRD; SEM; XPS; C, H, N analysis; surface area, particle size, and weight change measurements). The reaction rate was found to be significant, with 80% of the A1N being consumed in 24 h. The initial reaction product was found to be a porous, amorphous, hydrated alumina with stoichiometry near AlOOH. After ∽16 h a crystalline phase, bayerite Al(OH)₃, was detected which became the predominant phase after 24-h contact. The kinetics of the A1N consumption were found to be first order and the reaction rate linear. The kinetic data fitted an unreacted core model with a porous product layer where the surface chemical reaction controlled the overall kinetics.     

Novel Way to Synthesize Nanocrystalline Aluminum Nitride from Coarse Aluminum Powder

A new process has been developed for the synthesis of nanocrystalline AlN powder by the nitridation of coarse aluminum powder in flowing NH₃ gas, using NH₄Cl and KCl as additives. The resulting powders have been characterized using XRD, TEM, and XRF techniques. XRD-pure AlN nanoparticles with a diameter of 10–20 nm can be obtained by nitridation at 1273 K for 5 h. NH₃ is proved to eliminate the effect of water impurity. The effects of the additives on the conversion of aluminum are also discussed.     

Formation and Characterization of Amorphous Aluminum Nitride Powder and Transparent Aluminum Nitride Film by Chemical Vapor Deposition

Based on thermodynamic predictions that, in the gas-phase system AlCl₃/NH₃, AlN can be produced up to the theoretical yield, the performance of a chemical vapor deposition (CVD) reactor suitable for continuous powder production is investigated. Under the applied reaction conditions and reactor configuration, fine spherical AlN powders and transparent AlN films could be preferentially obtained. The generated amorphous CVD AlN powder is characterized by a BET surface area of 23.5 m²/g. The powder deposition rate was determined to be 3.5 g/h.     

Nanosize Powders of Aluminum Nitride Synthesized by Pulsed Wire Discharge

Nanosize particles of aluminum nitride have been successfully synthesized by a pulsed wire discharge (PWD). Intense pulsed current through an aluminum wire evaporated the wire to produce a high-density plasma. The plasma was then cooled by an ambient gas mixture of NH₃/N₂, resulting in nitridation. As a result, nanosize particles of aluminum nitride were formed. The average particle diameter was found to be ∼28 nm with a geometric standard deviation of 1.29. The maximum AlN content of 97% in the powders was achieved by optimizing various parameters: the gas pressure, the ratio of NH₃ and N₂, the wire diameter, the pulse width, and the input electrical energy. The ratio of the AlN powder production to the electrical energy consumption was evaluated as ∼40 g/(kW·h). Thus, PWD is a very efficient and promising method to synthesize nanosize powders of AlN.     

Al粉氮化制备超细AlN粉

以Al粉和C粉为原料,经球磨、干燥后在1400℃氮气气氛中氮化.氮化产物于650℃煅烧脱碳,制备出粒度为50nm左右的超细AlN粉.用SEM、TEM观察AlN粉的形貌.碳黑的高活性是形成无团聚纳米AlN粉的原因.     

Preparation of Nanostructured Hexagonal Boron Nitride Powder

In this communication, we describe an inexpensive and feasible method for the preparation of hexagonal boron nitride (h–BN) nanorods in the absence of metal catalyst. Tertiary calcium phosphate (Ca₃(PO₄)₂) and ammonium biborate hydrate (NH₄HB₄O₇·3H₂O) were selected as starting materials where calcium phosphate was used as a diluting agent to prevent the formation of bulk B₂O₃ during the thermolysis of ammonium biborate hydrate. The mixture was nitrided at 900°C in the flowing ammonia and was transformed into h–BN nanorods after subsequent crystallization. After crystallization at 1650°C for 2 h, the unique microstructure of h–BN nanorods was observed.     

Reactivity of Aluminum Nitride Powder in Aqueous Silicon Nitride and Silicon Carbide Slurries

The reactivity of AlN powder with water in supernatants obtained from centrifuged Si₃N₄ and SiC slurries was studied by monitoring the pH versus time. Various Si₃N₄ and SiC powders were used, which were fabricated by different production routes and had surfaces oxidized to different degrees. The reactivity of the AlN powder in the supernatants was found to depend strongly on the concentration of dissolved silica in these slurries relative to the surface area of the AlN powder in the slurry. The hydrolysis of AlN did not occur if the concentration of dissolved silica, with respect to the AlN powder surface, was high enough (1 mg SiO₂/(m² AlN powder)) to form a layer of aluminosilicates on the AlN powder surface. This assumption was verified by measuring the pH of more concentrated (31 vol%) Si₃N₄ and SiC suspensions also including 5 wt% of AlN powder (with respect to the solids).     

氧化铝/氮化铝陶瓷显微组织研究

氮化铝具有良好的热学、电学和机械等性能,是理想的电子封装材料和高性能陶瓷基板材料.本文研究了AlN加入量和烧结温度对Al2O3/AlN复相陶瓷相组成和显微组织的影响.结果表明该陶瓷在1400～ 1550℃烧结时,AlN被部分保留,少量氧原子进入AlN晶格,烧结生成4种铅锌矿结构新相,有利于提高复相陶瓷热导率;氮化铝含量和烧结温度的提高,有利于形成大尺寸晶粒.     

氮化铝陶瓷材料制备工艺与应用

概述了氮化铝材料的结构性质，粉末的合成方法，A1N陶恣的帛备方法及其应用。     

Aluminum Nitride Whisker Formation during Combustion Synthesis

In this study, the microstructural development of AlN during combustion synthesis (CS) in a nitrogen atmosphere was investigated. CS using an aluminum–50 wt% AlN–3 wt% MgCl₂ powder compact yielded a mixture of AlN whiskers and powder. The microstructural development during the combustion reaction was studied by heating the compact to various temperatures. Based on the experimental results, the formation mechanisms of the AlN with a whisker morphology were discussed.     

Synthesis of Nanosized Aluminum Nitride Powders by Pulsed Laser Ablation

The influence of the target material, fluence, laser wavelength, and nitrogen pressure on the synthesis of AlN nanosized powders via reactive laser ablation has been investigated. Using infrared laser radiation and fluences of ≥11 J/cm², pure AlN nanosized powders were produced at nitrogen pressures of ≥1.3 kPa via ablation of an AlN target and ≥13.3 kPa via ablation of an aluminum target. With ultraviolet laser radiation, AlN powders could be synthesized at a lower fluence (9 J/cm² at a pressure of 8 kPa). The mean powder size was 7.5−15 nm.     

氮化铝陶瓷的研制及应用

氮化铝 (AlN)因具有高热导率、低介电常数、与硅相匹配的热膨胀系数及其他优良的物理特性 ,在新材料领域越来越引起人们的关注。此文主要介绍并分析了AlN粉体合成、烧结、性能结构、AlN陶瓷的应用与前景     

硅粉直接氮化反应合成氮化硅研究

研究了硅粉直接氮化反应合成氮化硅粉末的工艺因素(包括硅粉粒度、氮化温度、成型压力、稀释剂含量等),借助XRD,SEM等测试手段测定和观察了氮化产物的物相组成和断口形貌.研究结果表明:硅粉在流动氮气氛下,高于1200℃氮化产物中氮含量明显增加;在氮化反应同时还伴随着硅粉的熔结过程,它阻碍硅粉的进一步氮化,其影响程度与氮化温度、氮化速度,素坯成型压力及硅粉粒度等工艺因素有关.在硅粉素坯中引入氮化硅作为稀释剂,提高了硅粉的氮化率,使产物中残留硅量降低;同样在实际生产中可以通过控制适当热处理制度(如分段保温、慢速升温),达到硅粉的完全氮化.在生产中批量合成了含氮量为32.5%,残留硅量为0.05%,主要为α相,含少量β相的针状、柱状的氮化硅.     

氮化铝陶瓷的制备及其在复合材料中的应用研究

氮化铝(AlN)陶瓷是一种性能优良的高技术陶瓷.本文概述了AlN陶瓷粉体的合成、成形、烧结的制备过程及其在复合材料中的应用研究,指出要更多地开展AlN复合材料及其在复合材料中应用的研究工作,以满足科技发展对材料提出的更高要求.     

Self-Propagating High-Temperature Synthesis of Aluminum Nitride under Lower Nitrogen Pressures

The synthesis of aluminum nitride (AlN) via self-propagating high-temperature synthesis (SHS) was attempted, using aluminum powder that was mixed with AlN powder as a diluent. The AlN content in the reactant was varied over a range of 30%–70%, and the nitrogen pressure was varied over a range of 0.1–1.0 MPa. The SHS reaction that was performed using a reactant that contained 50% AlN diluent, under a nitrogen-gas pressure of 0.8 MPa, yielded the highest conversion ratio of aluminum powder to AlN powder. A mechanism for the reaction of aluminum with nitrogen gas during the SHS process was discussed, based on observations of the microstructures of the reaction zone and products.     

Preparation of Dispersed Phase Ceramic Boron Nitride and Aluminum Nitride Composite Coatings by Chemical Vapor Deposition

Dispersed phase ceramic composite coatings containing BN and AIN were prepared by chemical vapor deposition. The BN + AIN coatings were deposited on Al₂O₃ from the BCI₃–AICI₃-NH₃ reagent system in the temperature range of 700° to 1200°C. Also, single-phase BN and AIN coatings were prepared for comparison purposes. The composite coatings consisted of very small BN and AIN regions which were either crystalline or amorphous, depending on deposition temperature and reagent concentrations. For example, a composite containing AlN whiskers of less than 100-nm diameter in a matrix of turbostratic BN of 2-nm grain size was deposited at 1100°C and 20 kPa.     

Composition and Microstructure of Chemically Vapor-Deposited Boron Nitride, Aluminum Nitride, and Boron Nitride + Aluminum Nitride Composites

The composition and microstructure of dispersed-phase ceramic composites containing BN and AIN as well as BN and AIN single-phase ceramics prepared by chemical vapor deposition have been characterized using X-ray diffraction, scanning electron microscopy, electron microprobe, and transmission electron microscopy techniques. Under certain processing conditions, the codeposited coating microstructure consists of small single-crystal AIN fibers (whiskers) surrounded by a turbostratic BN matrix. Other processing conditions resulted in single-phase films of AIN with a fibrous structure. The compositions of the codeposits range from 2 to 50 mol% BN, 50 to 80 mol% AIN with 7% to 25% oxygen impurity as determined by electron microprobe analysis.     

Aluminum Nitride Prepared by Nitridation of Aluminum Oxide Precursors

Aluminum nitride (AlN) powders were prepared from the oxide precursors aluminum nitrate, aluminum hydroxide, aluminum 2-ethyl-hexanoate, and aluminum isopropoxide (i.e., Al(NO₃)₃, Al(OH)₃, Al(OH)(O₂CCH(C₂H₅)(C₄H₉))₂, and Al(OCH(CH₃)₂)₃). Pyrolyses were performed in flowing dry NH₃ and N₂ at 1000°–1500°C. For comparison, the nitride precursors aluminum dimethylamide (Al(N(CH₃)₂)₃) and aluminum trimethylamino alane (AlH₃·N(CH₃)₃) were exposed to the same nitridation conditions. Products were investigated using XRD, TEM, EDX, SEM, and elemental analysis. The results showed that nitridation was primarily controlled by the water:ammonia ratio in the atmosphere. Single-phase AlN powders were obtained from all oxide precursors. Complete nitridation was not obtained using pure N₂, even for the non-oxide precursors.