Al2O3-C-N2系统反应热力学初步探讨

通过热力学计算 ,研究了高温下流动氮气床中碳热还原氧化铝反应过程 ,提出了其反应机理为气 固反应机制 ,很好地解释了在碳热还原法合成氮化铝过程中存在的现象。     

Al2O3—C—N2系统反应热力学初步探讨

通过热力学计算，研究了高温下流动氮气床中碳热还原氧化铝反应过程，提出了其反应机理为气－固反应机制，很好地解释了在碳热还原法合成氮化铝过程中存在的现象。     

高氮压法制备氮化铝粉

对在加压氮气中金属铝粉的直接氮化和氧化铝粉的碳热还原氮化法制备氮化铝粉末进行了研究。研究结果表明：铝粉在高温高氮压下快速氮化，生成氮化铝，其临界温度为７００℃，氮气的临界压力为１ＭＰａ；在高氮压下，氧化铝可通过碳热还原氮化法生成氮化铝，其含氮量与保温温度，氮气压力和保温时间有关；在高氮压下，碳热还原氮化法制备氮化铝，可使用铝粉为晶种，能获得高质量的氮化铝（Ｎ〉３３％，Ｏ〈１％，按质量计）粉末。     

Effect of Ca-compound on low temperature synthesis of AIN ultrafine powders by carbothermal reduction nitride route from sol-gel precursor

以硝酸铝、葡萄糖和硝酸钙为原料,通过溶胶-凝胶工艺获得了组分均匀的Al2 O3、C和CaO前驱体,进而利用碳热还原反应合成超细氮化铝粉体,探讨了钙助剂对氮化铝合成温度及粉体颗粒生长的影响规律.结果表明:钙助剂的添加,通过与前驱体中氧化铝在较低温度下发生反应,先后生成CaAl4 O7、Ca3 Al10O18、CaAl2 O4和Ca12Al14O33等铝酸钙相;上述铝酸钙相能在较低温度下形成液相,可有效促进氮化铝的合成和粉体颗粒的生长,从而在1400℃合成纯相氮化铝.当原料中钙铝摩尔比为0.0262时,在1350℃氮化得到了粒径60～80 nm的氮化铝粉体,仅有少量铝酸钙相存在;当氮化温度上升至1400℃时,铝酸钙相因挥发而消失,得到粒径100～180 nm的单相氮化铝粉体.     

机械力活化合成纳米晶氮化铝研究

通过氧化铝碳热还原反应,用机械力活化法合成了纳米结构的氮化铝,研究了球磨活化对氧化铝碳热还原反应的作用。发现氧化铝经球磨活化后,氮化铝在１０００℃开始生成,碳热还原反应加快,反应激活能由５２９ｋＪ／ｍｏｌ降低到４５７ｋＪ／ｍｏｌ。机械力活化合成的氮化铝晶粒尺寸为２９ｎｍ,粒平均为８μｍ,颗粒尺寸符合对数－正态分布。     

钙辅助溶胶-凝胶碳热还原法合成超细氮化铝粉体

以硝酸铝、葡萄糖和硝酸钙为原料,通过溶胶-凝胶工艺获得了组分均匀的Al2O3、C和CaO前驱体,进而利用碳热还原反应合成超细氮化铝粉体,探讨了钙助剂对氮化铝合成温度及粉体颗粒生长的影响规律。结果表明：钙助剂的添加,通过与前驱体中氧化铝在较低温度下发生反应,先后生成CaAl4O7、Ca3Al10O18、CaAl2O4和Ca12Al14O33等铝酸钙相;上述铝酸钙相能在较低温度下形成液相,可有效促进氮化铝的合成和粉体颗粒的生长,从而在1400 ℃合成纯相氮化铝。当原料中钙铝摩尔比为0.0262时,在1350 ℃氮化得到了粒径60-80 nm的氮化铝粉体,仅有少量铝酸钙相存在;当氮化温度上升至1400 ℃时,铝酸钙相因挥发而消失,得到粒径100-180 nm的单相氮化铝粉体。     

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。     

球磨对碳热还原氮化法制备氮化铝粉末的作用

研究了高能球磨对氧化铝碳热还原反应制备氮化铝的作用。结果表明：氧化铝及没料经高能球磨后,碳热还原反应开始温度降低,完全反应的温度降至1250℃。与未经球磨的反应相比,反应进行程度提高。球磨产生的机械化学作用,如细化晶粒、晶格畸变和大量缺陷及表面断健作用是球磨促进碳热还原反应的主要原因。     

碳热还原法制备氮化铝反应机制的研究进展

本文综述了碳热还原反应制备AlN的各种反应机制,并进行了评述,详述了气-固反应机制和固-固反应机制的特点、实验证据及存在的不足.认为Al2O3蒸发分解零级反应与固相扩散反应共存的机理能较好地解释目前的实验现象,但仍需进行完善.     

高温氮气下镁碳耐火材料的物相重构与微结构演变

以电熔镁砂、鳞片石墨和金属铝粉为原料,酚醛树脂为结合剂,在氮气气氛中,经1300～1600℃热处理后制备了镁碳耐火材料.分析了镁碳耐火材料的物相重构和微结构演变,揭示了化学气相沉积反应形成两种不同形貌氧化镁的机制.结果表明:在1300～1500℃时,试样的非氧化物组成为碳化铝(Al4C3)、氮化铝(AlN)和镁铝氮化物...     

碳热还原法合成AIN粉末的径向反应器设计

本文将传质原理与化学反应动力学相结合,导出了氮气流量与碳热还原法合成AIN反应速率之间的关系。基于动量守恒定律分析了径向反应器内部气体压力及其分布的规律,提出了气体在反应器内均匀分布的条件和反应器选型准则。根据这些条件和准则设计了合成AIN粉末的径向反应器。实验结果显示AIN的转化率及颗粒度在径向反应器内均匀分布,且产率高于平底状反应器。这一结果证明反应器设计合理,径向反应器比平底状反应器有更好的传质效果。     

Carbothermal Synthesis of Aluminum Nitride Using Sucrose

Several aluminum oxides (α-Al₂O₃, θ-Al₂O₃, and AIOOH) were examined to study the differences in reaction behavior and powder characteristics during carbothermal nitrida-tion to AIN using sucrose and carbon black. The reaction conditions investigated were carbon-to-alumina ratio, reaction temperature, and time. Carburized sucrose resulted in Full conversion to AIN and produced a uniform powder morphology using a near-istoichiometric ratio of C:Al₂O₃ while carbon black required higher C:Al₂O₃ ratios (i.e., >4:1) for full conversion and led to agglomeration of the AIN powder. The most favorable reaction temperature was 1600°C, with the reaction time to full conversion being dependent on the type of Al₂O₃. The particle and agglomerate size of the AIN powders did not change significantly with reaction time. However, the particle size and morphology were strongly dependent on that of the initial AI₂O₃ with sucrose, whereas agglomeration of the AIN occurs when using carbon black. A solid–solid reaction mechanism is proposed.     

Stabilization of Cubic Zirconia by Aluminum Nitride

Cubic ZrO₂ is stabilized at room temperature by the addition of AIN. The percentage of c-ZrO₂ in the mixture of c-ZrO₂ and m-ZrO₂ increases linearly with the addition of up to 20 mol% AIN and decreases thereafter. Stabilization becomes complete at 50 mol% AIN. The lattice spacing of the cubic phase gradually expands up to 20 mol% AIN. A displacement reaction ZrO₂+ AIN → ZrN+Al₂O₃ occurs above 20 mol% AIN and is completed at 50 mol% AIN.     

ZrO2-AlN复相材料的制备与性能研究

试样以部分稳定氧化锆（PSZ）和金属Al粉为原料。在N5气氛下经1600℃×4h烧结可制备出以AIN为结合相的ZrO2-AlN复相材料（ZAN）。试验研究了金属Al的氮化反应过程。以及金属Al的加入量对复相材料性能的影响。结果显示：Al粉反应生成AIN的全过程,主要由界面反应和内扩散反应交替完成．且整个反应过程应为扩散机制控制。随金属Al粉引入量的增加、ZAN试样的热膨胀系数减小,抗折强度增大,抗热震性及抗氧化性提高。ZAN-3试样的综合性能优良,其常温抗折强度为73．61MPa,热膨胀系数为6．06×10^-6/℃。室温～1100℃水冷残余抗折强度为4．64MPa。     

AlN-Re2O3液相烧结碳化硅

采用非氧化物AlN和Re2O3作为复合烧结助剂(Re2O3-La2O3与Y2O3)进行碳化硅液相烧结得到了致密的烧结体.烧结助剂占原料粉体总质量的20%,其中:AIN与(La0.5Y0.5)2O3的摩尔比为2:1,在30MPa压力下,1850℃保温0.5h热压烧结的碳化硅陶瓷,抗弯强度>800MPa,断裂韧性>8MPa·m1/2,明显高于同组分1 950℃无压烧结0.5h的碳化硅陶瓷的抗弯强度(433.7MPa)和断裂韧性(4.8MPam·m1/2.热压烧结的陶瓷晶粒呈单向生长,断裂模式为沿晶断裂.同组分无压烧结碳化硅陶瓷的显微结构可以观察到核壳结构.     

Kinetics of the Reduction of Carbon/Alumina Powder Mixture in a Flowing Nitrogen Stream

The reduction of carbon/alumina powder mixture in a flowing nitrogen stream was investigated by weight loss measurement and X-ray diffraction. Experimental results indicated that the reaction rate could be increased by increasing the nitrogen flow rate, weight ratio of C/Al₂O₃, or reaction temperature. The rate was also found to be increased by decreasing the sample size, the grain sizes of carbon or aluminum oxide, or initial bulk density. Empirical expressions of consumption rates of Al₂O₃ and C as well as production rate of AIN have been determined.     

Investigation of SiC-AlN: Part II, Mechanical Properties

SiC/AIN composites with controlled interfacial solid solution were employed in the present work for investigating the effects of interfacial bonding and A1N polytypes on the mechanical properties. Platelike A1N polytypes and interfacial bonding were found to have substantial effects on the flexural strength, hardness, and fracture toughness.     

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.     

Formation of β-SiAION as an Intermediate Oxidation Product of SiC–AIN Ceramics

The oxidation mechanisms in SiC-AlN solid solutions, exposed at 1370°C for 200 h in air, have been investigated by scanning electron microscopy (SEM), analytical and high-resolution electron microscopy (HREM), and X-ray diffraction techniques. Five hot-pressed compositions, including pure SiC and pure AIN, were examined. Assuming parabolic rate behavior, the values of the parabolic rate constants based on oxide layer thickness increased by over 2 orders of magnitude by increasing AIN contents from 0% to 62%. A continuous amorphous phase containing cristobalite and mullite crystallites was present at the oxide layer in 13% AIN and 27% AIN samples. Two reaction layers were found in the oxidized SiC–62% AIN solid solution. The inner layer consisted of a mixture of β-SiAION and graphite phases, while the outer layer consisted of mullite as a major phase and cristobalite as a minor phase. The oxidation proceeded in two stages: a partial oxidation of SiC–AIN to β-SiAION and carbon (graphite), and a final oxidation of β-SiAION to mullite + SiO₂.     

八氟戊醇硫酸盐的合成及性能研究

以八氟戊醇与氨基磺酸为原料,N,N-二甲基甲酰胺(DMF)为溶剂,经催化反应制备出一种新型的阴离子表面活性剂八氟戊醇硫酸铵。研究了催化剂种类、反应时间、反应温度、物料配比对转化率的影响。确定了最佳工艺条件为:以尿素为催化剂,n(八氟戊醇)∶n(氨基磺酸)=1∶1.20,反应温度120℃,反应时间3 h,转化率为97.83%。对产物进行了性能测定,其临界胶束浓度为3.24×10-3mol/L,表面张力为28.59 m N/m。