复合稀土掺杂对β-Sialon陶瓷组织与力学性能影响

分别以Y2O3+Ce2O3,Y2O3+La2O3和Y2O3+Nd2O3复合稀土作为烧结助剂,采用无压烧结工艺制备β-Sialon陶瓷.通过对三组陶瓷试样的抗弯强度和断裂韧的测试,并结合扫描电镜(SEM)和XRD进行了分析,结果表明:烧结温度1 750℃、0.1MPa N2、保温1h的条件下,其中质量分数为52.64%α-Si3N4+9.4%AlN+31.96%Al2O3+3%Y2O3+3%La2O3的β-Sialon陶瓷,其抗弯强度、断裂韧性和相对密度最高分别为483.2MPa、5.3MPa·m1/2和94.12%,且其显微结构较均匀晶粒发育较完全.     

烧结助剂MgO和烧结温度对β-Sialon陶瓷的力学性能影响

以α-Si3N4粉、α-Al2O3粉和Al N粉及烧结助剂MgO为原料,采用热压烧结的工艺制备了β-Sialon陶瓷材料,研究了烧结助剂MgO和烧结温度对sialon陶瓷力学性能和组织形貌的影响.结果表明,加入烧结助剂MgO提高了β-sialon陶瓷的致密度且降低了烧结温度,随着烧结温度的升高,β-sialon陶瓷抗弯强度、断裂韧性呈先增加后降低的变化规律,当烧结温度为1600℃时制备的β-sialon陶瓷材料结合紧密,抗弯强度以及断裂韧性达到最大,值分别为423 MPa、2.73 MPa·m1/2,材料的断裂方式主要是沿晶断裂.     

Sialon陶瓷的常压烧结

在Si3N4,Al2O3,AIN和Y2O3混合料常压烧结过程中,由于过程反应生成SiO,CO,N2等气相物质和由于Si3N4原料在高温常压下分解压高,从而常压烧结致密化过程始终伴随着一个失重的塑致密化过程。为了解决这一问题,作者研究了填料成分、烧结温度、烧结时间等工艺条件对Sialon陶瓷常压烧结密度的影响,分析了烧结过程的物理化学机制和致密化机制。4种填料分别为Si3N4,Si3N4 SiO2,Si3N4 Al2O3 AIN和Si3N4 Al2O3 AIN BN。被烧料典型配方为：Si3N465%-70%,Al2O320%-25%,AIN10%,另加6％Y2O3。当填料成分为70％Si3N4 24%Al2O3 3%AIN 3%BN时,制得了相对密度达99％,抗弯强度达612．2MPa的常压烧结Sialon陶瓷。研究结果表明：对于通式为Si6-zAlzOzN8-z的Sialon陶瓷,当Z＝2时,其最佳烧结温度为1750℃,烧结时间为40min;Sialon的烧结过程是1个多因素控制的瞬时液相烧结过程。     

SiCN/Sialon复合材料的制备及微波介电性能研究

以AlN、Al2O3和Y2O3为添加剂，用无压烧结法制备了SiCN／Sialon复合材料。研究表明，在相同烧结条件下，随着纳米SiCN含量的增加，材料的烧结致密度下降。XRD结果表明，SiCN／Sialon复合材料由主晶相β—Sialon（Si3Al3O3N5）和极少量的SiO3、β—SiC组成。SEM研究表明，随着纳米SiCN含量的增加，材料中棒状的β—Sialon（Si3Al3O3N5）含量明显减少。抗弯强度研究表明，β—Sialon（Si3Al3O3N5）复合材料的抗弯强度随着纳米SiCN含量的升高而降低，从纯Sialon陶瓷的530MPa下降到含22．26％SiCN时的196MPa，其原因是由于随着纳米SiCN含量的增加，材料的致密度降低，β—Sialon（Si3Al3O3N5）含量减少所致。SiCN／Sialon复合材料复介电常数的实部和虚部均随纳米SiCN含量的升高而增大，但是低于预期值，其原因是由于长时间高温烧结时，纳米SiCN结构发生变化，其复介电常数的实部和虚部大幅度下降造成。     

SiC(N)/Si3N4吸波材料的制备与性能

通过掺杂纳米SiC(N)吸收剂，采用无压烧结工艺，制备了SiC(N)／Si3N4复合型吸波材料。对材料进行了XRD、SEM及强度分析，结果表明：随着纳米吸收剂SiC(N)加入量的增加，材料的烧结性能趋于下降，表现为α-Si3N4的含量增多，柱状β-Si3N4的尺寸变小，材料气孔增大，强度降低。     

Si3N4-SiC太阳能热发电吸热陶瓷的制备及性能

以SiC和Si3N4为主要原料,采用陶瓷制备工艺无压烧结制备了Si3N4-SiC吸热陶瓷材料。采用现代测试技术,测试和分析了烧结样品的烧结收缩率、抗折强度、吸水率、气孔率、体积密度、耐火度、氧化增重率、物相组成以及显微结构。结果表明,最佳配方是1 360℃烧结的D2样品,其Si3N4添加量为20%,抗折强度为79.60 MPa、气孔率为22.23%、吸水率为10.32%、体积密度为2.15g/cm3、耐火度为1 650℃、1 300℃氧化5h后的样品氧化增重率为1.333mg/cm2。XRD和SEM分析表明烧结样品由α-SiC、Si3N4、莫来石和石英组成,Si3N4在样品中呈短棱柱体分布,添加纳米SiC对Si3N4可以起到钉扎作用,阻止Si3N4晶粒长大,从而提高样品的抗折强度和抗热震性能。Si3N4-SiC吸热陶瓷具有高的强度以及良好的微观组织结构,是一种适合塔式太阳能热发电吸热器用吸热材料。     

Sialon陶瓷的无压烧结

以Si_3N_4、Al_2O_3和AlN为原料,Y_2O_3为烧结助剂,采用无压烧结制备Sialon陶瓷．对试样的体积收缩率、抗弯强度、洛氏硬度等力学性能进行测试,扫描电镜(SEM)观察表明,在无压烧结条件下,采用埋粉烧结并充N_2保护,烧结温度为1700℃,保温90min可得到Sialon陶瓷,其中成分为54%α-Si_3N_4 32%Al_2O_3 8%AlN 6%Y_2O_3的Sialon陶瓷,其抗弯强度为390．08MPa,硬度为92．5HRA,显微结构为明显的柱状晶．     

纳米SiC粉中的氧含量对Al2O3陶瓷无压煤结的影响

讨论了纳米SiC中的氧含量对Al2O3/SiC纳米复相陶瓷性能的影响,发现当氧含量偏高时,烧结体难以致密化,同时在组织中出现大尺寸气孔,实验证明,氧含量较低的纳米β-SiC可以使烧结体密度和强度得到极大提高;而氧含量偏高的Si/C/N非晶复合粉,提高性能的作用甚微,其根本原因就是,粉体中的氧与硅形成蒸气,从而使烧结体中出现气孔。     

含有定向排列颗粒的氮化硅陶瓷各向异性研究

通过添加α—Si3N4晶须,利用流延成型和热压烧结技术制备舍有定向排列颗粒、各向异性的Si3N4陶瓷。研究α-Si3N4相在流延膜及烧结块体中的分布状态,并通过XRD、SEM和力学性能对流延膜和烧结块体的各向异性进行表征。结果表明,1550℃下烧结制备的块体T（与流延方向平行的平面）、N（与流延方向垂直的平面）、P（侧面）三个面的I（210）／I（102）值与等轴状α-Si3N4粉体的相应值比较,其中T面的值较大,N面和P面的值较小;在T面的显微结构中存在平行于流延方向排列的大颗粒;试样不同面的力学性能（断裂韧性和抗弯强度）中,T面最好,P面次之,N面最差;I（210）／I（102）值、显微结构、力学性能测试结果表明所制备的氮化硅陶瓷存在各向异性。     

Si3N4/TiC纳米复合陶瓷材料显微结构

利用日立H-800透射电境、日立S-570型扫描电境及RAX-10A型X射线衍射仪对Si3N4/TiC纳米复合陶瓷材料的微观组织、结构和成分进行了研究.结果表明,TiC纳米颗粒弥散分布在基体β-Si3N4晶内和晶界,所制备的材料为晶内/晶间混合型纳米复合陶瓷.通过对Si3N4/TiC纳米复合陶瓷材料断裂方式的观察表明,材料断裂为沿晶断裂和穿晶断裂复合型,纳米粒子对裂纹扩展起到偏转和钉扎作用.纳米Si3N4颗粒的加入促进了基体长柱状β-Si3N4晶粒多峰分布的形成,类晶须晶粒在裂纹扩展过程中产生桥接和拔出.     

Preparation of Sialon powder from coal gasification slag

X-ray fluorescence spectrometry(XRF),X-ray powder diffractometry(XRD) and scanning electron microscopy(SEM) were used to characterize the chemical composition,phase constituent and microstructure of the coal gasification slag.Sialon powders were synthesized by carbothermal reduction and nitridation using the coal gasification slag as raw materials.The experimental results showed that glass and amorphous carbon were the main phases,quartz and calcite as minor crystalline phases were also presented in porous coal gasification slag.Main constituents of coal gasification slag were SiO2,Al2O3,CaO and residual carbon.Sialon powder with Ca-α-Sialon as main crystalline phase can be synthesized when coal gasification slag powders were reduced and nitrided at 1500 ℃ for 9 h using nitrogen flow of 500 ml/min.The coal gasification slag is a valuable and economic starting material for preparing Sialon powders.     

Comparative study of β-Si3N4 powders prepared by SHS sintered by spark plasma sintering and hot pressing

β-Si3N4 powders prepared by self-propagating high-temperature synthesis (SHS) with additions of Y2O3 and Al2O3 were sintered by spark plasma sintering (SPS). The densification, microstructure, and mechanical properties of Si3N4 ceramics prepared using this method were compared with those obtained by hot pressing process. Well densified Si3N4 ceramics with finer and homogeneous microstructure and better mechanical properties were obtained in the case of the SPS technique at 200℃ lower than that of hot pressing. The microhardness is 15.72 GPa, the bending strength is 716.46 MPa, and the fracture toughness is 7.03 MPa.m1/2.     

Si_3N_4-doped Zr_(50)Al_(15)Ni_(10)Cu_(25) glassy alloy by mechanical alloying and sintering process

Zr50Al15Ni10Cu25 amorphous powder was synthesized by mechanical alloying.The effect of Si3N4 addition on the crystallization behavior of the alloy during sintering process was studied.Thermal stability of the powders was performed by differential scanning calorimetry(DSC).The phase and microstructure of the powders and bulk specimens sintered were determined by X-ray diffractometry(XRD) and scanning electron microscopy(SEM).The results show that,introducing 0.05%(mass fraction) Si3N4 can enhance the crystallization activation energy of the Zr50Al15Ni10Cu25 amorphous powders,which indicates that Si3N4 addition has hindrance effect on forming crystals from Zr50Al15Ni10Cu25 amorphous powder.However,0.10% Si3N4 results in the decrease of the crystallization activation energy,which makes its crystallization process easy to occur.     

In-situ Synthesis and Oxidation Resistance of Sialon/SiC Composite Ceramics Applied as Solar Absorber

Sialon/SiC composites were synthesized in situ from SiC,α-Si₃N₄,AlN,calcined bauxite,quartz and Y₂O₃ via layered buried sintering at different temperatures (1 540-1 640 ℃).The results showed that the O’-sialon/SiC sample with 60 wt% silicon carbide sintered at 1 600 ℃ exhibited excellent mechanical properties,with apparent porosity of 16.01%,bulk density of 2.06 g·cm^-3,bending strength of 52.63 MPa,and thermal expansion coefficient of 5.83×10-6 ℃^-1.The oxide film formed on the surface was linked closely to O’-sialon,so the oxide film was not easily broken.After 100 h oxidization,the sample surface was smoother and denser,with oxidation weight gain rate 23.6 mg/cm² and oxidation rate constant 2.0 mg²·cm^-4·h^-1.Therefore,the sample had the excellent high-temperature oxidation resistance.It was confirmed that the in-situ sialon/SiC composites could be a promising candidate for solar absorber owing to its high-temperature oxidation resistance.     

Al2O3-SiC-SiAlON复合材料的制备和性能

以电熔白刚玉、α-Al2O3微粉、Si粉和矾土基β-SiAlON粉为原料,以树脂为结合剂,制备了复合材料试样.研究了1 500℃烧后试样的物相组成、显微结构以及常温物理性能、高温抗折强度和抗热震性.结果表明:(1)在刚玉中引入适量Si粉高温埋碳条件下可合成Al2O3-SiC-SiAlON复合材料,引入适量β-SiAlON可促进Si反应,且复合材料1 500℃烧结良好;(2)复合材料的高温抗折强度和抗热震性随Si粉加入量增加而提高,加入β-SiAlON后材料的高温机械性能进一步提高;(3)材料高温机械性能提高的原因在于Si粉在高温下与C、CO和N2反应生成晶须状或纤维状SiC和絮状O’-SiAlON填充气孔,形成交叉连锁的网络结构,对材料起增强和增韧作用.     

室温非晶硅薄膜热电阻温度系数研究

用离子束增强沉积（IBED）方法,在SiO2/Si衬底上沉积了非晶硅薄膜和注氢的非晶硅薄膜。研究薄膜的电阻温度系数（TCR）随制备工艺的变化,分析非晶硅薄膜电阻的稳定性对电阻温度系数的影响。本征非晶硅电阻太大,虽然经过适当地退火后,TCR能够达到6.39%K-1,但是电阻值还是过高,不适合制作器件。经过硼掺杂的非晶硅薄膜,电阻显著下降,相应的TCR可以达到6.80%K-1。制作的氢化非晶硅薄膜的电阻温度系数（TCR）高达8.72%K-1,且制作工艺简单,与常规集成电路工艺兼容性好。用离子束增强沉积的非晶硅薄膜可以用于制备红外探测仪。但实验还存在着重复性不好等问题,需要作深入的实验研究。     

纳米级 TIO_2 超细粉的水热合成及结构相变的研究

利用水热合成法以水、四氯化钛和浓硫酸为原料制备了纳米级锐钛矿型二氧化钛超细粉，并对其结构相变进行了研究。结果显示，其相变温度比传统的二氧化钛材料的要低得多     

中温烧结Mg_4Nb_2O_9-CaTiO_3陶瓷相结构的研究

采用传统固态反应方法制备了(1-x)Mg4Nb2O9+xCaTiO3[(1-x)MN-xCT]复合陶瓷。探讨了烧结温度、组分x对Mg4Nb2O9/CaTiO3复合材料相结构的影响。通过XRD和EDS进行物相分析。实验结果表明:V2O5添加能够有效降低Mg4Nb2O9/CaTiO3陶瓷的烧结温度;(1-x)MN-xCT复相的形成主要取决于烧结温度和x的含量。1150℃烧结、0.5≤x≤0.7范围内,形成了Mg4Nb2O9/CaTiO3复相,无新相生成,但元素在不同相之间发生了扩散。     

Sol-gel法制备CaSiO3基LTCC陶瓷

采用溶胶凝胶法(Sol-gel)制备了CaSiO3基低温共烧陶瓷,在800℃、825℃、850℃、875℃下烧结,并对烧结样品进行了热重-差热分析、X射线扫描分析、扫描电子显微镜形貌分析.测试了在烧结温度为800℃、825℃、850℃、875℃下各样品的烧结密度和介电性能.结果表明Sol-gel 法制备的CaSiO3基...