碳热还原氮化法制备碳氮化钛粉末

以物质的量比为1∶2.5的TiO_2粉和活性炭粉为原料,于N2气氛下采用碳热还原氮化法在不同的合成温度(分别为1500℃、1600℃、1650℃、1700℃、1750℃,N2压力固定为0.1MPa)和N2压力(分别为0.05MPa、0.1MPa、0.15MPa、0.2MPa,温度1700℃)下保温3h合成了碳氮化钛粉末。研究结果表明提高合成温度和降低N2压力有利于合成碳含量高的碳氮化钛粉末;在N2压力为0.1MPa的条件下,于1700℃保温3h热处理后,可以获得平均粒径为2μm的碳氮化钛粉末。     

天然原料碳热还原氮化合成β''''-SiAlON的研究进展

本文介绍β'-SiAlON的结构、基本性能及应用领域,阐述了合成β'-SiAlON的原材料和各种合成方法,重点介绍了利用天然原料合成β'-SiAlON的还原剂外加法和还原剂内加法即有机插层法.详细阐述了各工艺条件(反应原料的组成、反应温度、反应时间、反应气氛、流速及反应物颗粒尺寸、添加剂等)对合成β'-SiAlON反应结果的影响.同时本文指出目前该研究可能存在的问题及解决的途径.     

天然原料碳热还原氮化合成β′-SiAlON的研究进展

本文介绍β′-SiAlON的结构、基本性能及应用领域,阐述了合成β′-SiAlON的原材料和各种合成方法,重点介绍了利用天然原料合成β′-SiAlON的还原剂外加法和还原剂内加法即有机插层法。详细阐述了各工艺条件(反应原料的组成、反应温度、反应时间、反应气氛、流速及反应物颗粒尺寸、添加剂等)对合成β′-SiAlON反应结果的影响。同时本文指出目前该研究可能存在的问题及解决的途径。     

碳热还原氮化法制备β''''-SiAlON的工艺条件研究

采用质量分数80%的粘土(广西高岭土或吉林球粘土)和20%的炭黑为原料,以白云石、CaO、TiO2为烧结助剂,经碳热还原氮化反应制备了β’-SiAlON材料。研究了烧成温度、保温时间、烧结助剂、成型压力和粘土种类等因素对制备β’-SiAlON材料的影响。结果表明,烧成温度以1450℃为宜,延长保温时间有利于β’-SiAlON相的形成;烧结助剂的催化效果以TiO2最好,白云石次之;随着成型压力的增大,合成试样中β’-SiAlON相减少;粘土原料的化学组成(m(SiO2)/m(Al2O3))对β’-SiAlON的Z值产生影响,m(SiO2)/m(Al2O3)减小时,Z值趋于增大。     

叶蜡石在碳热还原氮化过程中的相变

研究了叶蜡石在不同温度下碳热还原氮化合成SiAlON过程中的相变。SEM、XRD以及EDS分析结果表明 :130 0℃开始氮化形成O’ SiAlON ,14 0 0℃时O’ SiAlON的XRD峰已经很明显 ,14 5 0℃时O’ SiAlON大量生成并在 15 0 0℃时达到最大值 ;14 5 0℃时开始形成β SiAlON(z=2 )和少量SiC ;15 5 0℃时 ,β SiAlON成为主要的氮化产物 ,与少量的O’ SiAlON并存 ;莫来石和方石英直到 15 0 0℃仍然存在 ,15 5 0℃消失。     

高岭土在碳热还原氮化过程中的相变

系统研究了苏州高岭土碳热还原氮化合成SiAlON过程在不同温度下的相变。对试样的XRD、SEM以及EDXA分析结果表明 ,1 30 0℃之前 ,试样中没有氮化物生成 ,物相为莫来石、石英和方石英 ;1 30 0℃时 ,高岭土开始发生氮化反应 ,生成过渡型SiAlON和β SiAlON。此时 ,石英和方石英相基本消失 ;1 4 0 0℃时 ,过渡型SiAlON、β SiAlON和X SiAlON三相共存 ,β SiAlON有所增多并有少量刚玉相生成 ;从 1 4 50℃到 1 550℃ ,Z值为 3的β SiAlON成为惟一的氮化产物 ,与少量SiC和刚玉相并存。莫来石在 1 50 0℃时完全消失     

粉煤灰合成SiAlON粉体研究

以粉煤灰、石墨粉、氧化铝、二氧化硅等为主要原料,采用碳热还原氮化法合成了SiAlON粉体。研究了Fe2O3含量不同的粉煤灰,即未除铁粉煤灰(Fe2O3的质量分数为4.16%)、酸洗除铁后的粉煤灰(Fe2O3的质量分数几乎为0)和磁选除铁后的粉煤灰(Fe2O3的质量分数为3.46%),配料的m(SiO2)∶m(Al2O3)(分别为1.176、1.55和2.35),碳加入量(分别为理论加入量、过量10%、过量100%和过量150%)以及反应温度(分别为1350℃、1400℃、1420℃、1430℃和1460℃)对合成产物相组成的影响。研究表明:以经过磁选除铁后的粉煤灰(Fe2O3的质量分数为3.46%)为原料,当配料的m(SiO2)∶m(Al2O3)为1.4,碳粉加入量为理论值的2倍(即过量100%)时,于1420℃保温20h合成的产物的主要物相为βSiAlON。     

碳热还原氮化法合成氮化钒/氮化铬复合粉末

以纳米V_2O_5、纳米Cr_2O_3和纳米碳黑为原料,经过干燥、球磨混料后,在流动氮气中焙烧,得到了氮化钒/氮化铬(VN/CrN)复合粉末。利用XRD、TG-DSC、SEM、BET和TEM对合成产物进行了表征和测试,考察了反应温度和保温时间对VN/CrN复合粉末的微观结构和性能的影响。结果表明:在1 200℃、保温2 h条件下,可制备出平均晶粒直径为40 nm的VN/CrN复合粉末。该复合粉末主要由VN、CrN和VCrN_2组成,这3种物质均为面心立方结构,空间群均属于Fm3m。复合粉末的比表面积为21.09 m~2/g。将复合粉末作为添加剂加入到陶瓷磨具结合剂中进行性能测试,结果显示:当w(复合粉末)=0.2%时,陶瓷磨具结合剂抗折强度和流动性分别提高约20%和50%;当w(复合粉末)=1.0%时,其抗折强度和流动性均达到最大值115.6 MPa和207.2%。     

碳热还原氮化粉煤灰的研究

以粉煤灰加入炭黑为主要原料,在氮气气氛下对粉煤灰进行了碳热还原氮化研究.研究了碳加入量、合成反应温度、保温时间和Fe2O3含量等因素对生成物物相的影响.实验结果表明:选用理论加入碳含量的样品,在反应温度为1350℃、保温9h条件下,产物中含有较多β-Sialon相;而且经磁选除铁后的粉煤灰较未除铁粉煤灰在反应温度为1400℃、保温9h条件下,碳化还原氮化产物中15R相含量明显增多.     

碳热还原—氮化法合成—β′—sialon的研究

本文对β′－ｓｉａｌｏｎ的碳热还原———氮化合成进行了详细研究。结果表明：影响β′－ｓｉａｌｏｎ粉料合成的因素依次为合成温度、添加剂用量、氮气流量、保温时间。对合成的粉料进行含氮量和ＸＲＤ检测。给出了本实验条件下合成β′－ｓｉａｌｏｎ的最佳工艺参数：合成温度１４５０℃,添加剂（Ｓｉ３Ｎ４）用量５％,氮气流量为１．０Ｌ／ｍｉｎ,保温时间为６ｈ。同时探讨了反应过程和Ｚ值的测量与计算方法。     

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.     

Grain-Boundary Wetting-Dewetting in z= 1 SiAlON Ceramic

The grain-boundary structure of a model SiAlON polycrystal with nominal composition Si₅AlON₇ was characterized by transmission electron microscopy (TEM) both in an equilibrium (as-processed) state at room temperature and after quenching from elevated temperature. In addition, low-frequency (1–13 Hz) internal friction data were recorded as a function of temperature, showing a pronounced grain-boundary sliding peak positioned at 1030°C. High-resolution transmission electron microscopy (HRTEM) of the equilibrated low-temperature microstructure revealed residual glass only at multigrain junctions, but no amorphous intergranular films were observed. The detection of clean interfaces in the as-processed sample contradicts the internal friction data, which instead suggests the presence of a low-viscosity grain boundary phase, sliding at elevated temperatures. Therefore, a thin section of the as-sintered material was heated to 1380°C and rapidly quenched. HRTEM analysis of this sample showed, apart from residual glass pockets, wetted grain boundaries, which is in line with the internal friction experiment. This wetting-dewetting phenomenon observed in z = 1 SiAlON is expected to have a strong impact not only on high-temperature engineering ceramics but also on geological, temperature-activated processes such as volcanic eruptions.     

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。     

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.     

Spark plasma sintering of SiAlON ceramics

Investigated was the spark plasma sintering (SPS) of sialon ceramics from SHS-produced powders. Experimentally established were (a) sintering temperatures that ensure a required density, phase composition, and microstructure of sintered multicomponent sialon ceramics, (b) individual stages of the SPS process, and (c) the effect of starting powder composition on the phase composition and microstructure of sintered sialon ceramics.      

SiC/SiAlON对原位SiC结合刚玉材料抗侵蚀性的影响

采用矾土基高铝刚玉为骨料,以电熔刚玉细粉、Si粉、SiC粉或SiAlON粉为基质料,用酚醛树脂为结合剂,试样于1450℃埋炭烧成后,制备了烧结良好的原位SiC结合刚玉复合材料;采用静态坩埚法研究了加入SiC或SiAlON对这种复合材料抗渣性的影响.结果表明:原位SiC结合刚玉材料具有良好的抗侵蚀性能,加入适量SiC或SiAlON后复合材料的抗侵蚀性进一步提高;原位SiC结合刚玉基材料抗侵蚀行为和机理为:熔渣侵蚀材料的过程是SiC和SiAlON等非氧化物先被氧化,然后其氧化产物SiO2和Al2O3与熔渣中的CaO和Al2O3以及材料基质中的Al2O3反应生成钙长石,材料被侵蚀;原位生成的SiC难被熔渣润湿,且填充在气孔中,堵塞了熔渣渗透的主要通道;加入SiC和SiAlON,材料中非氧化物的量明显增多,因此抗侵蚀性明显提高.     

The effect of silicon nitride powder characteristics on SiAlON microstructures,densification and phase assemblage

The surface characteristics, particle size distribution and impurities of starting Si₃N₄ powders exert a very significant influence on the microstructure of sintered silicon nitride based ceramics. Even a change of the processing conditions such as milling liquid media (water or isopropyl alcohol) and milling time can have a substantial effect on particle surface groups, and hence on the microstructure of sintered samples. In this study, SEM, XRD, FTIR, BET, elemental analysis and laser diffraction techniques were used for the comprehensive characterization of Si₃N₄ powders which were produced by diimide, direct nitridation and combustion synthesis, in as received state, and after milling in different liquid media (aqueous or alcohol), for various milling durations. The correlation of the surface characteristics and properties of the Si₃N₄ powders with sintering behavior, and microstructural evolution, densification and phase assemblages of the resulting SiAlON ceramics were reported. The milling conditions affected the surface chemistry of Si₃N₄ powders and the subsequent microstructural evolution. The microstructures evolved from the coarser β-Si₃N₄ powders were coarser, but the fine β-Si₃N₄ powders yielded a bimodal microstructure. The critical particle diameter of the β-Si₃N₄ powder for the formation of needle like SiAlON grains was determined to be less than 0.5 µm.     

Thermodynamic Analysis for Carbothermal Reduction and Nitridation of TiO2

The diagrams of stability relations(namely,Predominance area phase diagram,PAPD)of nitride,carbide and oxides in Ti-C-N-O system were plotted by thermodynamic calculation.The optimum conditions and main influence factors for the synthesis of titanium nitride and titanium carbide by carbothermal reduction in nitrogen atmosphere were discussed.     

Formation Process of Calcium-α SiAlON Hollow Balls Composed of Nanosized Particles by Carbothermal Reduction–Nitridation

Carbothermal reduction–nitridation (CRN) of SiO₂–Al₂O₃–CaO powders was performed under various firing conditions to investigate the formation process of Ca-α sialon hollow balls composed of nanosized particles. Scanning electron microscopy and transmission electron microscopy observations of the samples obtained at different firing temperatures confirmed that solid spherical particles were formed at the early stage of the reaction, and nanosized particles were subsequently produced on the surface of these solid balls. From X-ray diffraction and energy-dispersive spectrometry analyses, it was found that the solid balls initially formed at 1450°C were mainly amorphous and contained Si, Al, Ca, O, and a small amount of N. Further nitridation at 1450°C gradually converted the solid balls into Ca-α sialon hollow balls over time. The results revealed that the formation of Ca-α sialon hollow balls depends on the formation of solid balls from the Si–Al–Ca–O liquid phase at the initial stage of the CRN process.