Influence of aluminium nitride as a foaming agent on the preparation of foam glass-ceramics from high-titanium blast furnace slag

To effectively reuse high-titanium blast furnace slag （TS）, foam glass-ceramics were successfully prepared by powder sintering at 1000℃. TS and waste glass were used as the main raw materials, aluminium nitride （AIN） as the foaming agent, and borax as the fluxing agent. The influence of the amount of A1N added （lwt%-5wt%） on the crystalline phases, microstructure, and properties of the produced foam glass-ceramics was studied. The results showed that the main crystal phases were perovskite, diopside, and augite. With increasing A1N content, a transformation from diopside to augite occurred and the crystallinity of the pyroxene phases slightly decreased. Initially, the aver- age pore size and porosity of the foam glass-ceramics increased and subsequently decreased; similarly, their bulk density and compressive strength decreased and subsequently increased. The optimal properties were obtained when the foam glass-ceramics were prepared by adding 4wt% AIN.

SiC WHISKER-TOUGHENED ALUMINIUM NITRIDE CERAMICS

Aluminium nitride ceramics containing 15 -30 w/o of SiC whiskers can be sintered to full density (by hot pressing at 1800℃)using 2-3 w/o of Y2O3 additions. The whiskers increase the toughness and strength of the composite, KIC increasing from 2. & to about 5.0 and flexural strength increasing by 30-50%. However, the whiskers must be well dispersed and if the dispersion is not satisfactory, toughness may increase but the strength decreases. The hot-pressing temperature can be reduced by up to 100℃ if Y(NO3)3 . 5H2O is used as the sintering additive instead of Y2O3, but some oxidation of the AIN occurs during heating. Isopropan-2-01 is a better dispersing agent than cyclohexane, but again some oxidation of the AIN does occur.The best sample prepared during this work contained 20 w/o of SiC whiskers and 2 w/o Y2O3 added as Y(NO3)3. 5H2O and mixed in isopropanol. This exhibited a mean strength of 453MPa (maximum 522MPa, measured by disc flexure) and a fracture toughness of5. 5MPam1/2.

First principle study of nitrogen vacancy in aluminium nitride

In the framework of density functional theory, using the plane-wave pseudopotential method, the nitrogen vacancy （VN） in both wurtzite and zinc-blende AlN is studied by the supercell approach. The atom configuration, density of states, and formation energies of various charge states are calculated. Two defect states are introduced by the defect, which are a doubly occupied single state above the valance band maximum （VBM） and a singly occupied triple state below the conduction band minimum （CBM） for wurtzite AlN and above the CBM for zinc-blende AlN. So VN acts as a deep donor in wurtzite AlN and a shallow donor in zinc-blende AlN. A thermodynamic transition level E（3＋/＋） with very low formation energy appears at 0.7 and 0,6eV above the VBM in wurtzite and zinc-blende structure respectively, which may have a wide shift to the low energy side if atoms surrounding the defect are not fully relaxed. Several other transition levels appear in the upper part of the bandgap. The number of these levels decreases with the structure relaxation. However, these levels are unimportant to AlN properties because of their high formation energy.

Design and Analysis of MEMS Based Aluminum Nitride (AlN), Lithium Niobate (LiNbO₃) and Zinc Oxide (ZnO) Cantilever with Different Substrate Materials for Piezoelectric Vibration Energy Harvesters Using COMSOL Multiphysics Software

Interest in energy harvesters has grown rapidly over the last decade. The cantilever shaped piezoelectric energy harvesting beam is one of the most employed designs, due to its simplicity and flexibility for further performance enhancement. The research effort in the MEMS Piezoelectric vibration energy harvester designed using three types of cantilever materials, Lithium Niobate (LiNbO3), Aluminum Nitride (AlN) and Zinc Oxide (ZnO) with different substrate materials: aluminum, steel and silicon using COMSOL Multiphysics package were designed and analyzed. Voltage, mechanical power and electrical power versus frequency for different cantilever materials and substrates were modeled and simulated using Finite element method (FEM). The resonant frequencies of the LiNbO3/Al, AlN/Al and ZnO/Al systems were found to be 187.5 Hz, 279.5 Hz and 173.5 Hz, respectively. We found that ZnO/Al system yields optimum voltage and electrical power values of 8.2 V and 2.8 mW, respectively. For ZnO cantilever on aluminum, steel and silicon substrates, we found the resonant frequencies to be 173.5 Hz, 170 Hz and 175 Hz, respectively. Interestingly, ZnO/steel yields optimal voltage and electrical power values of 9.83 V and 4.02 mW, respectively. Furthermore, all systems were studied at different differentiate frequencies. We found that voltage and electrical power have increased as the acceleration has increased.

Effects of AlN hydrolysis on fractal geometry characteristics of residue from secondary aluminium dross using response surface methodology

The effects of aluminium nitride(AlN)hydrolysis on fractal geometry characteristics of residue from secondary aluminium dross were studied using response surface methodology.The results show that the fractal dimensions of the residue can be significantly influenced by the AlN hydrolysis from secondary aluminium dross.The hydrolysis of AlN in the dross was spontaneous under temperatures of303-373K.The actual fractal dimensions of residue were significantly affected by the liquid-solid ratio(p<0.05)and changed from1.16to1.80,which accurately aligned with those from the calculations.Moreover,the fractal dimensions of residue were significantly affected by the interactions between hydrolysis temperature and hydrolysis time,liquid-solid ratio and hydrolysis time,respectively(p<0.01).The minimum fractal dimensions of the residue reached1.15under the optimized conditions,which included a hydrolysis temperature of30℃,liquid-solid ratio of5mL/g and hydrolysis time of10min.The results suggest that response surface methodology can guide in optimizing the conditions of AlN hydrolysis in order to obtain the minimum fractal dimensions of residue for improving the reutilization of the dross.

连续网状结构Ti_(2)AlN/TiAl复合材料的制备及力学性能

采用高温气体渗氮法将氮引入TiAl预合金粉末中,然后采用放电等离子烧结法制备具有连续网络增强相结构的Ti_(2)AlN/TiAl复合材料。结果表明,复合材料的硬度明显高于TiAl合金的硬度,并随着氮化时间的增加而增加。该强化效果是粉末渗氮引起的固溶体强化、具有高硬度和弹性模量的连续网状Ti_(2)AlN相以及位错密度增加协同作用的结果。同时,与TiAl合金相比,Ti_(2)AlN/TiAl复合材料的抗压强度降低,这与氮化后直接形成的一部分Ti_(2)AlN颗粒和过多的增强相含量有关。

Fabrication and residual stresses of aluminum nitride ceramics sintered at high-pressure

High-density AlN ceramics were fabricated without sintering additives at high pressure(5.0 GPa) and temperature(1300～1800℃).The sintered bodies were characterized by XRD,SEM and micro-Raman spectroscopy(MRS).Controlling fracture mode was intragranular when the sintering temperature was as low as 1400℃under 5.0 GPa.The values of residual stresses due to the distortion of the AlN lattice were assessed using the Micro-Raman Spectroscopy(MRS).The residual compression stress of the AlN ceramics sintered at 5.0 GPaand 1700℃for 125 min is 2.0 GPa.The residual compression stress is increased according to the extension of the sintering time.

原位直接氮化法制备片状AlN粉体

片状AlN粉体作为热界面材料的填料应用前景广阔,但制备工艺难度大、成本高限制了其实际应用。本文以球磨处理后得到的片状Al粉为铝源,在氮气气氛中通过原位直接氮化法成功制备出由等轴状微米颗粒结合而成的片状AlN粉体,并研究了球磨处理、氮化温度和升温速率对产物物相组成及显微形貌的影响。结果表明,球磨处理可增强Al粉的反应活性、提升氮化速率。升高氮化温度可提升Al粉的氮化率,但过高的氮化温度则会导致产物无法保持片状形貌;提高升温速率会增大等轴状微米颗粒的粒径。当氮化温度为640℃、升温速率为5℃/min时,制备的片状AlN粉体表面最为致密、平整,有望作为热界面材料的填料使用。

ADC12铝合金表面氮化铝(AlN)涂层的制备及其耐磨性能研究

为了提高ADC12铝合金材料的耐磨性能,利用多功能离子渗氮炉在ADC12铝合金表面进行离子渗氮,制备氮化铝(AlN)涂层。通过X射线衍射仪、扫描电子显微镜对表面AlN涂层的相结构与微观形貌进行表征;利用WS-2005涂层附着力自动划痕仪、WTM-2E可控气氛微型摩擦磨损试验仪和3D光学显微镜研究AlN涂层与基体的膜基结合力、摩擦系数、比磨损率和摩擦磨损机理。结果显示:表面AlN涂层的相结构为面心立方,没有发现有Al_(2)O_(3)衍射峰存在。随着渗氮时间的延长和渗氮温度的升高,表面AlN涂层的厚度逐渐增大,膜基结合力先增大再减小,在510℃、4 h时膜基结合力最大,为56.60 N。相对于基体来说,AlN涂层样品在负载1 N、进行摩擦磨损试验10 min后,摩擦系数变小,比磨损率降低,表面AlN涂层厚度越厚,减缓磨损效果越明显。ADC12铝合金表面离子渗氮所得氮化铝(AlN)涂层具有优异的耐磨损性能。

HPMA modified aluminium nitride powder for aqueous tape casting of AlN ceramic substrates

Aluminum nitride(AlN)is considered one of the most desirable materials for integrated circuits and electronic packaging substrates.However,raw AlN powder reacts easily with water,forming Al(OH)3 or AlOOH on the surface and hindering the development of an aqueous tape-casting process for preparing AlN ceramic substrates.In this study,hydrolyzed polymaleic anhydride(HPMA)was used to modify AlN powder,which has good water solubility and dispersibility.The AlN powder was modified with 5 wt%HPMA remained stable in water for at least 90 h under magnetic stirring condition and 24 h under ball milling condition,indicating that HPMA-modified AlN powder has good resistance to hydrolysis.The action mechanism of HPMA is revealed.Firstly,–COOH of the HPMA polymer and the oxide layer on the surface of the AlN powder underwent a dehydration condensation reaction to form a compound.Secondly,long chains of the polymer further coated the surface of the AlN powder,forming an anti-hydration layer with a thickness of about 7.0 nm on the surface of the AlN particles.In addition,AlN green sheets were successfully prepared by aqueous tape casting using the HPMA-modified AlN powder without additional dispersants.Subsequently,AlN ceramic substrates were obtained by sintering at 1750℃for 4 h under an N2 atmosphere with a pressure of 0.2 MPa.The relative density and thermal conductivity were tested to be 97.3%and 122 W/(m·K),respectively.

Low-Temperature Synthesis of Nano-AlN Based on Solid Nitrogen Source by Plasma-Assisted Ball Milling

Plasma-assisted ball milling was carried out on the Al+C3H6N6 system and Al+C_(4)H_(4)N_(4) system,respectively.The phase structure,functional groups and synthesis mechanism were analyzed by XRD and FT-IR,and the differences in the synthesis process of nano-AlN with different solid nitrogen sources were discussed.The results show that C3H6N6 has a stable triazine ring structure,and its chemical bond is firm and difficult to break,so AlN cannot be synthesized directly by solid-solid reaction at room temperature.However,there are a large number of nitrile groups(-CN)and amino groups(-NH_(2))in C_(4)H_(4)N_(4) molecules.Under the combined action of plasma bombardment and mechanical energy activation,C_(4)H_(4)N_(4) molecules undergo polycondensation and deamination,so that the ball milling tank is filled with a large number of active nitrogen-containing groups such as N=,≡N,etc.These groups and ball milling activated Al can synthesize nano-AlN at room temperature,with a conversion rate of 92%.SEM,DSC/TG analysis showed that the powder obtained by ball milling was formed by soft agglomeration of many fine primary particles about 50–80 nm.The surface morphology of the powder was loose and porous,and it had strong activity.After annealing at 800℃,the conversion rate of the Al+C_(4)H_(4)N_(4) system reached 99%.

AlN陶瓷粉末制备方法特点和进展

本文就国内外AlN粉末合成的研究情况 ,综述了直接氮化法、Al2 O3 碳热还原法、自蔓延高温合成法、等离子体法、气溶胶法等主要的几种AlN粉末制备方法的特点和研究进展 。

AlN陶瓷的空心阴极等离子烧结工艺研究

将空心阴极效应运用于AIN陶瓷的烧结,选用自蔓延高温合成的AIN粉体为原料,用Y2O3-Li2O-CaO(YLC)作为烧结助剂,进行了烧结试验,并探讨了工艺参数的影响。结果表明,空心阴极烧结工艺可制备出致密度高,导热性能好的AIN陶瓷。添加质量分数为5.5%的YLC烧结助剂,在1 700℃、保温3h的烧结条件下,获得相对密度为98.9%、热导率为93.8W/(m.K)的AIN烧结体。烧结体断口的SEM照片显示,烧结试样的晶粒生长发育完善,晶粒轮廓清晰,呈尖锐的多面体形状,晶粒大小均匀,孔隙和晶界相少,断裂模式主要为穿晶解理断裂。TEM观测表明,晶界相少,且大部分都缩至三角晶界,AIN晶粒与晶粒接触紧密。

AlN-BN复合陶瓷的介电性能

以ＡｌＮＢＮ复合陶瓷为研究对象，着重探讨了ＡｌＮＢＮ复合陶瓷的极化机理，应用基本的电介质物理理论，结合ＡｌＮＢＮ复合陶瓷的组成和结构特点，研究了ＡｌＮＢＮ复合陶瓷介电性能（介电常数、介电损耗角正切值）随测量温度、测量频率变化而发生变化的温度特性和频率特性。

碳热还原氮化法制备AlN超细粉体新工艺

为降低碳热还原氮化法制备AlN粉体的反应温度,减小粉体粒径、缩短反应时间,以勃母石(-γAlOOH)为铝源、蔗糖为碳源,采用碳热还原氮化法在不同温度下制备了AlN超细粉体,用XRD、TEM等方法分析了所制备粉体的物相组成与形貌。结果表明:在1 480℃、流通氮气氛中保温1 h可制备出平均粒径为350 nm的AlN粉体,大幅度降低了反应温度,缩短了反应时间;在高温下,-γAlOOH分解成Al2O3,部分Al2O3被碳还原成气态铝和铝的低价氧化物(Al2O,AlO),它们与氮气直接反应生成AlN和中间相AlON,随后中间相AlON也发生反应生成AlN。

AlN陶瓷的介电性能

着重探讨了ＡｌＮ陶瓷的极化机理，应用基本的电介质物理理论，结合ＡｌＮ陶瓷的组成特点，研究了ＡｌＮ陶瓷介电性能（介电常数、介电损耗角正切值）随测量温度、测量频率变化而变化的温度特性和频率特性．结果表明：ＡｌＮ陶瓷的主要极化机理为空间电荷极化；经典的极化理论适用于ＡｌＮ陶瓷；ＡｌＮ陶瓷因介电性能较好，导热率较高而有望成为比Ａｌ２Ｏ３陶瓷性能更加优良的基板材料．

添加剂对自蔓延高温合成AlN的影响

着重研究了添加剂对自蔓延高温合成AlN中的含氧量增加的影响 ,讨论了AlN形态与含氧量之间的关系 .疏松剂NH4 Cl虽可使得产物疏松 ,易于破碎 ,但它增加了体系中水蒸汽量 ,促进AlN中含氧量的增加 .碳的存在可降低体系中的水蒸汽量 ,使NH4 Cl对产物中含氧量的促进作用受到抑制 .部分碳化的蔗糖在自蔓延过程中发生碳化 ,可获得较大的表面积 ,使得其较明显地抑制含氧量的增加 .在自蔓延高温合成过程中 ,AlN的含氧量与其形态关系密切 .含氧量高的AlN倾向于形成晶须 ,而含氧量低的AlN倾向于形成颗粒状 .AlN晶须以固 -液 -气 (VLS)机制生长 .VLS机制所需液相的生成与氧有关 .液相产生所需的氧应主要来自气体中的含氧杂质(氧气和水蒸汽 ) .

影响AlN陶瓷热导率的本征氧缺陷

对ＡｌＮ晶格中的铝空位、延展缺陷等进行了研究。研究表明，在固溶氧浓度较低（＜０．７５％，原子百分数）的高热导率ＡｌＮ试样中，铝空位的存在会造成ＡｌＮ晶胞局域收缩的现象，并观察到了铝空位的存在；固溶氧浓度较高（＞０．７５％）时，孤立的缺陷产生团聚，形成铝氧八面体；在氧浓度很高（＞＞０．７５％）的低热导率试样中观察到了反相区、多型体等延展缺陷。

反应自生成AlN传质过程的研究

根据反应自生成AIN的传质及生长特征，构造出传质模型，并建立了传质方程.分析表明：整个反应过程分AlN晶体生长并伴随Si元素富集及AlN、Sicry，晶体共生两个阶段进行;N原子的扩散传质速率是控制总反应速率的关键因素.

GaN缓冲层上低温生长AlN单晶薄膜

采用电子回旋共振等离子体增强金属有机物化学气相沉积(ECR PEMOCVD)技术,在α Al2O3(0001)(蓝宝石)衬底上,分别以高纯氮气(N2)和三甲基铝(TMAl)为氮源和铝源低温生长氮化铝(AlN)薄膜。利用反射高能电子衍射(RHEED)、原子力显微镜(AFM)和X射线衍射(XRD)等测量样品,研究了AlN缓冲层和氮化镓(GaN)对六方AlN外延层质量的影响,实验表明在GaN缓冲层上能够低温生长出C轴取向的AlN单晶薄膜。