反应原料对微波碳热还原法合成AlN粉末的影响

根据微波加热特点,选择合适的反应原料,合成出优质的AlN粉末.结果表明,采用合适的反应原料微波合成AlN,由于微波的"非热效应"以及微波环境下整个反应系统的均匀加热,降低了反应温度,缩短了反应时间,极大的减少了合成成本.     

溶胶-凝胶还原氮化合成β-sialon超细粉

以硝酸铝、正硅酸乙脂、无水乙醇、蔗糖等为起始原料,通过溶胶-凝胶、还原氮化工艺制备了β-sialon超细粉体。研究了β-sialon晶种、Si3N4晶种、AlN晶种、添加剂、氮化温度等工艺条件对合成β-sialon粉体的影响。结果证明：晶种的加入可以促进β-sialon的合成,降低其合成温度,其用量的多少对β-sialon的合成影响不明显;晶种种类对β-sialon合成影响较大,其中β-sialon晶种的促进效果最明显;1450～1500℃是比较合适的氮化温度。SEM的结果表明,合成的β-sialon的粒径在300nm左右。同时还研究了Sialon,Si3N4和AlN的水解性能。     

燃烧合成AlN粉体的放电等离子烧结及其导热性能

利用放电等离子烧结(spark plasma sintering,SPS)工艺研究了燃烧合成法制备的2种具有不同形貌的AlN粉以及1种碳热还原氮化法制备的市售亚微米级AlN粉的烧结性能、致密化机理以及导热性能。结果表明:燃烧合成法制备的AlN纳米晶须状粉末具有与亚微米级标准市售AlN粉末同样优异的烧结性能,都能够在无烧结助剂情况下在1600℃的较低温度下烧结致密。在烧结过程中,由于燃烧合成AlN粉自身的高化学活性和SPS产生的等离子体活化作用,使得AlN粉以自身的分解-再结晶-凝聚机制进行致密化,导致晶界强度很高,断裂时以穿晶断裂为主;而在市售AlN粉末烧结过程中以表面扩散机制致密化,在晶界处形成了AlON相,降低了晶界强度,因此以沿晶断裂为主。AlN原料的氧含量对热导率的影响很大。由于燃烧合成AlN粉体的氧含量较碳热还原法制备的市售AlN粉体略高,导致其烧结试样热导率略低。     

合成工艺对氮化硅铁物相和结构的影响

以硅铁合金(FeSi75)为原料,分别采用闪速燃烧合成工艺和自蔓延高温合成工艺制备氮化硅铁样品,利用X射线衍射仪和扫描电镜对样品进行了表征,探讨了合成工艺对氮化硅铁物相和显微结构的影响。采用闪速燃烧工艺合成的氮化硅铁相组成为β-Si3N4,α-Si3N4,Fe3Si和少量SiO2;而采用自蔓延高温合成的氮化硅铁由β-Si3N4,α-Si3N4,Fe3Si和Si2N2O组成。闪速燃烧合成的氮化硅铁样品中存在大量长径比较高的柱状氮化硅晶体,Fe3Si位于柱状结晶所包裹材料的内部;自蔓延高温合成的氮化硅铁显微结构为致密的氮化硅块体,在块体表面覆盖有氧氮化硅膜,块体的间隙存在晶形细小的氮化硅晶体,含铁组分镶嵌在致密的块体中。闪速燃烧合成的氮化硅铁结构疏松,活性较强;自蔓延高温合成的氮化硅铁结构致密,性质稳定。     

在NH3-C3H8混合气氛下通过还原-氮化γ-Al2O3合成制备AlN纳米粉

以NH3和C3H8作为反应气体,通过还原-氮化γ-Al2O3可合成制得AlN纳米粉。我们已经通过分析确认:通过NH3和C3H8的混合气流,在1100℃～1400℃保温120min的条件下通过气相还原-氮化γ-Al2O3制得的合成产物中确实存在AlN相,而且在1100℃保温120min后合成制得的产物中还包含未反应的γ-Al2O3。Al核磁共振的图谱显示:产物中的Al-N键随反应温度的提高而增强:[AlO4]四面体比[AlO6]八面体的谐振先削弱,这表明γ-Al2O3中的[AlO4]四面体比[AlO6]八面体更易氮化,基于这一点,可在低温条件下从γ-Al2O3中直接制得AlN纳米粒子。通过气相还原-氮化γ-Al2O3制得AlN纳米粒子的原因是:一方面因为反应温度足够低限制了晶粒生长;另一方面也因为γ-Al2O3只含有[AlO6]一种配位体,而γ-Al2O3则包含两种配位多面体结构即[AlO4]和[AlO6]。     

微波烧结AlN陶瓷的初步研究

采用微波高温烧结工艺,制备了致密的AlN陶瓷,并初步探讨了微波烧成环境对烧结体性能的影响.结果表明:利用微波烧结AlN陶瓷,虽然在节能省时方面效果显著,但是微波烧成环境对AlN陶瓷的烧成影响比较复杂,本文着重指出烧成环境中的碳热还原气氛能极大地加快AlN陶瓷的致密化速率,但容易在AlN陶瓷晶界相内部产生气孔,使AlN陶瓷的热导率降低.     

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.     

工艺条件对粘土碳热还原氮化合成β'-Sialon粉体的影响

利用失重和XRD分析研究了试样组成、合成温度、保温时间和N2分压等工艺条件对粘土碳热还原氮化合成β'-Sialon粉体的影响.结果表明加入超过化学计量10%的碳,适当提高合成温度和延长保温时间,适当减小氮气分压,都有利于β'-Sialon的形成.轻烧粘土对氮化反应影响不大;β'-Sialon形成过程的分析表明碳热还原氮化反应主要受中间产物CO和SiO的控制.     

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.     

硅铁闪速燃烧合成氮化硅铁

利用闪速燃烧合成新技术 ,以粒度≤ 0 .0 88mm的FeSi75硅铁细粉为原料 ,在 0 .2MPa的低氮气压力与 14 0 0℃的燃烧温度条件下 ,制备了细蜂窝状氮化硅铁。XRD和SEM分析结果表明 ,这种氮化硅铁主要由短柱状β Si3N4 相和Si3Fe相组成 ,其结构特征是以Si3Fe形成核心 ,并被Si3N4 包裹。同时 ,还用热力学原理探讨了由硅铁闪速燃烧合成氮化硅铁的工艺条件、形成产物的形式、反应的中间产物和残留金属的形态。热力学研究结论和实验检测结果相一致 ,从而在理论上阐明了闪速燃烧合成是制备氮化硅铁的一种理想工艺     

氮化铝粉末的制备方法与机理

论述了氮化铝陶瓷粉末的各种制备方法,评述了各种方法的优缺点,总结了氮化铝形成的主要机理以及影响氮化铝粉末质量的因素.提供了一些有用的工艺参数和有关氮化铝粉末质量的数据.     

Nanocrystalline Aluminum Nitride: I, Vapor-Phase Synthesis in a Forced-Flow Reactor

A forced-flow reactor has been designed for the synthesis of nanocrystalline AlN via in situ and ex situ nitridation of aluminum. Various reactor parameters, including evaporation temperature, microwave plasma generation, reactor pressure, gas flow rate, nitriding gas, carrier gas, and crucible purge, have been examined and optimized. Fully nitrided powders with crystallite sizes of 10–100 nm and surface areas of 45–370 m²/g were produced using these techniques. These ultrafine AlN particles were highly moisture-sensitive, but they could be processed and handled without exposure to air to achieve fully dense materials with low oxygen content.     

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.     

氮化铝粉末的制备及扩大实验研究

主要进行了碳热还原法制备氮化铝粉末扩大实验研究。研究了不同的铝源、碳源、氮化温度、保温时间、添加剂对合成氮化铝粉末的影响,并采用XRD、SEM、化学物理分析等手段对中试实验制备的氮化铝粉末进行分析。研究结果表明,采用经砂磨处理的铝源B（α-Al₂O₃）和3^#碳源（乙炔黑）为原料,有助于碳热还原反应;采用添加剂C可以降低反应活化能,提高氮化率;造粒工艺有助于扩大实验的碳热还原反应。     

铝源孔容和焙烧升温过程对碳热还原法制备氮化铝粉体的影响

碳热还原氮化法是大规模制备高纯度氮化铝（AlN）粉体的主要方法,通过微反应器制备不同孔容的铝源,系统探究了前体孔容和微观形貌对AlN粉体产物的影响,并通过动力学模拟验证了筛选出的前体的活性。同时对氮化反应升温过程的影响也做了探究,最终通过对前体和焙烧升温过程的优化,得到纯度99%以上的AlN粉体,其平均粒径约为150 nm,O元素含量为0.55%。     

合成和烧结工艺对微波介质陶瓷性能的影响

综述了微波介质陶瓷的性能与最新的研究进展,分析了合成方法对微波介质陶瓷介电性能的影响,总结了微波介质陶瓷的烧结工艺对其性能的影响,指出了微波介质陶瓷的问题及今后的发展方向。     

Effects of Additive on the Microwave Synthesis of AlN Powder

In this paper, a series of aluminum nitride powders were synthesized using a microwave synthesis method with various additives. The effects of additives on the nitridation of aluminum powder by microwave processing were studied. The results showed that the pure AlN powder with regular and fine grains could be obtained at a temperature of 1050°C for 30 min by the mixed additive under atmospheric pressure of nitrogen. The mixed additive composed by ammonium fluoride and zinc granules played a vital role in the microwave synthesis process.     

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.     

大型煤制甲醇的气化和合成工艺选择

阐述了大型煤制甲醇装置中煤气化和甲醇合成的工艺路线选择。对比了固定床、流化床和气流床三种气化工艺,得出:大型煤制甲醇的煤气化宜选气流床气化技术;对比了干粉煤气化和水煤浆气化两种流化床工艺,得出:前者优于后者。并以固定床的甲醇合成为例,介绍了串塔合成流程和双级合成流程以及几种大型甲醇合成塔的选用。     

Preparation of AlN powder of low oxygen content via carbothermal reduction and nitridation by active gas exchange technique

By generating a periodic impulse-like pressure (2.0–4.4 kPa, 84 s) to actively exchange the gas in synthesis furnace, pure AlN powder of low oxygen content was synthesized via additive free carbothermal reduction and nitridation (CRN) of Al₂O₃ powder. Compared with the conventional CRN method, the proposed extra gas exhaust process can more effectively remove the side-produced CO from the reaction sites to accelerate nitridation process and decrease the residual oxygen content in the obtained AlN powder. For example, with 39 wt% activated carbon loaded in the raw material at 1650 °C for 4 h, the prepared AlN powder by the proposed synthesis scheme has only 0.68 wt% residual oxygen. The effects of carbon content, synthesis temperature and holding time on the residual oxygen content in AlN powder by the proposed synthesis scheme were also studied. The ball-milled as-prepared AlN powder was pressureless sintered at 1880 °C for 2.5 h to obtain a translucent AlN ceramics (37.6% at ~5700 nm), which demonstrates the excellent sinterability of the as-prepared AlN powder.