Slip-casting properties of Si3N4 with Y2O3 and Al2O3 as sintering additives

The effects of particle charging and powder–liquid suspension stability on the slip-casting properties of Si3N4 powder were examined. Y2O3 and Al2O3, used as sintering additives, were seen to affect the dispersion stability of the base material (Si3N4). The zeta potentials of the three powders and the rheological behaviour of the 55 wt% solids-loaded slips, involving known concentrations of a polymeric deflocculant (Dolapix PC33), showed that the multicomponent system can be dispersed stably within the pH range 9–11. Green compacts, obtained by casting these slips into plaster moulds, were found to give densities in the range 50–61% of the theoretical value. © 1998 Chapman & Hall     

Preparation and Properties of Sintering Additives Coated Si3N4 from Heterogeneous Nucleation Processing

The sintering additives such as Al2O3 and /or Y2O3 were coated on the surfaces of Si3N4 particles via heterogeneous nucleation processing using a buffered pH solution as the precipitation reagent .They nucleated and grew only on the surfaces of Si3N4 and did not form sol particles in solution by TEM observation .The isoelectric point(IEP) of coated Si3N4 was different from that of as-received Si3N4.The IEP of Al(OH)3-coated Si3N4 occurred at pH8.4, which is close to that of alumina .When Al(OH)3-coated Si3N4 particles were coated with Y(OH)3,the IEP of coated Si3N4 powder shifted from pH8.4 to pH9.2 ,similar to that of yttria.In addition ,the rheological data showed that Al2O3 and /or Y2O3 coated Si3N4 suspension is nearly Newtonian and that added Si3N4 suspension shows a shear rate thinning behavior.     

ZrO2 (Y2O3) 增韧的氮化硅烧结体的性能及相关系

在高温(1400℃) 超高压(4. 2GPa) 下制备Y₂O₃ 部分稳定的ZrO₂ 增韧的氮化硅烧结体, 通过XRD 及机械性能测试等方法分析ZrO₂ 的相结构, 研究氮化硅烧结体的增韧机理。结果表明, 烧结体中加入少量的铝粉, 可提高t2ZrO₂ 的相变能力, 达到利用部分稳定的ZrO₂ 增韧氮化硅烧结体的目的。稳定剂Y₂O₃ 在ZrO₂ 中含量小于2. 5mol% 时, t→m 相变量及断裂韧性随Y₂O₃ 含量增加而逐渐提高, 韧性提高来源于相变增韧和微裂纹增韧; Y₂O₃含量大于2. 5mol% 时, t 相接近100% , 韧性主要来源于相变增韧, 增韧效果随Y₂O₃ 含量增加而逐渐减弱。Y₂O₃ 作为良好的烧结助剂, 促进氮化硅烧结体在超高压下致密化, 烧结体的硬度随Y₂O₃ 含量增加逐渐提高。      

Influence of TiC additions on the oxidation behaviour of Si3N4-based ceramics

The oxidation behaviour in air of Si3N4 ceramics containing Y2O3 and Al2O3 as sintering aids, with and without a dispersion of TiC particles, has been studied between 1200 and 1400 °C. The influence of TiC additions on the oxidation kinetics is discussed in comparison with the results obtained for the Si3N4–Y2O3–Al2O3 reference material. However, in all cases and within the experimental temperature range, the oxidation kinetics were observed to be of a parabolic type. The microstructure of the oxide scales formed, which has been characterized by scanning and transmission electron microscopy, was observed to depend on the oxidation temperature and the initial composition of the material. © 1998 Chapman & Hall     

Si3N4/TiC纳米复合陶瓷材料R曲线行为

在微米Si3N4基体中加入亚微米Si3N4及纳米TiC颗粒,热压烧结制备出力学性能良好的Si3N4/TiC纳米复合陶瓷材料。采用压痕-弯曲强度法测定了复合材料的裂纹扩展阻力曲线(R曲线)。结果表明:材料呈现出上升的阻力曲线特性,显示出增强的抗裂纹扩展能力。其中,加入质量分数为10%亚微米Si3N4颗粒和15%纳米TiC颗粒的复合材料显示出较为优越的抗裂纹扩展能力,其阻力曲线上升最陡,上升幅度最大。分析表明:弥散的TiC粒子同基体之间弹性模量和热膨胀失配以及Si3N4类晶须拔出与桥联补强协同增韧,有助于纳米复合材料抑制主裂纹失稳扩展,导致复合材料的阻力曲线行为。     

共沉淀法制备Nd3+:Y2O3透明陶瓷

以Y2O3为基质材料,掺杂不同含量的Nd3+添加PEG和(NH4)2SO4为分散剂,采用共沉淀法制备出性能良好的Nd3+:Y2O3纳米粉.对前驱体和不同温度下煅烧后的粉体进行差热热重、X射线衍射、比表面积和透射电镜等分析.结果表明,前驱体产物为Y2(OH)5(NO3)·nH2O时,Nd3+完全固溶于Y2O3的立方晶格中,Nd3+:Y2O3粉体大小均匀,近似球形.随着煅烧温度的升高,颗粒逐渐长大,900℃煅烧2h后颗粒尺寸约为40～60nm;粉体在1700℃和真空度为1×10-3Pa条件下烧结6h得到的Nd3+:Y2O3透明陶瓷的透光率接近78%.     

Effect of Y2O3– MgO Addition on Heterogeneous Precipitation-Thermal Reduction Synthesis and Sintering ofFe – Mo/Si3N4Powders

Effect of Y2O3-MgO addition on heterogeneous precipitation-thermal reduction synthesis and the sintering of Fe-Mo/Si3N4 powders has been investigated. It was found that the whiskers-like β-Si3N4, good wettability phases on Si3N4 surface, and high toughness Fe phase appeared in Fe-Mo/Si3N4 cermets with Y2O3-MgO additives. The results show that Y2O3-MgO additives can effectively optimize the microstructures of Fe-Mo/ Si3N4 cermets, and improve the material mechanical properties. Therefore, it indicated that Y2O3-MgO additives can be used for strengthening of eintered cermets, and the dual function of whiskers self-toughening and different metal-composition toughening can be achieved in Fe-Mo/Si3N4 cermets with Y2O3-MgO additives.     

Mechanical Properties and Microstructure of Si3N4-TiC Nanocomposites

1. IntroductionSilicon nitride is one of the promising structural ma-terials for high-temperature applications because of itshigh resistance to thermal shock, as well as high strength,high fracture toughness, and high resistance to chemicalattack[1~3]. However, wider application has been lim-ited mainly due to its inherent brittleness. Many effortshave been made to improve its properties by control-ling the microstructure or by fabricating various typesof composites[4~7].The silicon nitride wi…     

Neutron and X-ray powder diffraction studies of the oxynitrides SrW(O,N)3, Ba3W2(O,N)8 and Ba3Mo2(O,N)8

Oxynitrides of composition SrW(O,N)₃, Ba₃W₂(O,N)₈ and Ba₃Mo₂(O,N)₈ have been prepared by the ammonolysis of stoichiometric mixtures of oxides and carbonates. Combined Rietveld refinements of powder neutron and powder X-ray diffraction data have allowed the structure of each to be determined. SrW(O,N)₃ was found to have a cubic Perovskite structure whereas Ba₃W₂(O,N)₈ and Ba₃Mo₂(O,N)₈ have a layered hexagonal structure. In the hexagonal structures the oxygen and nitrogen atoms are distributed almost randomly over two sites in the unit cell producing 4-fold co-ordination to tungsten and molybdenum, a distorted octahedral co-ordination to one barium site and a 10-fold co-ordination to the other.     

Extended X-ray absorption fine structure (EXAFS) study of secondary phases in Yb2O3-doped Si3N4 ceramics

Liquid-phase sintered Si3N4 doped with Yb2O3 as a sintering aid was characterized by both transmission electron microscopy and extended X-ray absorption fine structure (EXAFS) measurements. Structural information about the secondary phases was obtained with an emphasis being placed on the evaluation of EXAFS data. Two Si3N4 samples were processed which contained either 5 vol% or 10 vol% Yb2O3 as sintering additive. After sintering, only an amorphous secondary phase was observed in the material doped with 5 vol% Yb2O3. The material with the higher Yb2O3 volume fraction underwent a further heat treatment after the densification, in order to crystallize pockets of the secondary phase. This heat treatment resulted in the formation of Yb2Si2O7 at multi-grain junctions, with however, amorphous phases remaining along the grain and phase boundaries. The EXAFS data obtained from the two doped Si3N4 materials were compared with reference spectra obtained on pure Yb2O3 and synthetic Yb2Si2O7. No residual Yb2O3 was determined in the doped Si3N4 materials, independent of the Yb2O3 volume fraction. Compared to synthetic Yb2Si2O7, the secondary phase formed in the 10 vol% Yb2O3 containing material showed only subtle changes in the EXAFS data. A clear distinction between purely amorphous and a combination of crystalline plus amorphous Yb secondary phases was possible, when both doped Si3N4 materials were compared. However, no distinction between the glass phase present at triple junctions and the amorphous residue along grain/phase boundaries was feasible, since a full numerical data evaluation could not be performed.     

Heat treatment of wollastonite-type Y–Si–Al–O–N glasses

Cumulative work over the last twenty years has defined the glass-forming regions in several M–Si–Al–O–N systems (M = Mg, Ca, Y, Ln) with the resulting crystalline products identified after heat treatment. Glass-forming regions in nitrogen-rich sialon glasses have been recently reported and heat treatment of some of these glasses in the Y–Si–Al–O–N system has been performed. The crystallization of yttrium-containing glasses is particularly sensitive to small variations in composition and heat treatment temperature and in the current work the results of three series are discussed: (1) a single composition, Y15.2Si14.6Al8.7O54.6N6.9 (16 e/oN), treated at 30 °C intervals between 875–1410 °C; (2) compositions of a constant Y: Si:Al ratio of 3:3:2 and up to 32 e/oN and (3) selected compositions lying on the 28 e/o N plane. Two different sets of crystalline products are found to form above and below 1200 °C. This revised version was published online in November 2006 with corrections to the Cover Date.     

粉料粒度对氮化硅陶瓷性能的影响

用球磨的方式将平均粒径为6.46μm的β-氮化硅原料粉细化为不同粒度的亚微米级起始粉料,加入适宜的添加剂,以无压液相烧结的方法研究起始粉料粒度对氮化硅陶瓷的强度、硬度等机械性能的影响。用扫描电镜、X射线衍射等方法测试分析试样的显微结构、相组成等。结果表明,试样密度、强度、硬度等均随起始粉料粒度的减小而增大;试样显微结构显示了烧结体晶粒尺寸随起始粉料粒度的减小而减小,且粒度小的试样烧结的晶粒均匀、致密;烧结后试样的物相主要是β-氮化硅和少量黄长石,粉料的粒度对烧结后样品的物相没有影响。     

制备工艺对原位合成(Al_2O_3+Si)_p/Al复合材料显微组织影响及体系分析

以Al-SiO_2为反应体系,通过烧结反应原位合成了(Al_2O_3+Si)_p/Al复合材料。研究了第二相含量、烧结时间以及热锻压等工艺对(Al_2O_3+Si)_p/Al复合材料的第二相形貌、尺寸及分布的影响,探讨了原位合成(Al_2O_3+Si)_p/Al复合材料的生成机制。研究表明,Si相含量随着第二相含量的增多而增多且与Al和Al_2O_3相界限相对明显;随着烧结时间的延长,Si相面积相对减小,Al_2O_3相的数量相对增加;锻压后,Si相和Al_2O_3分布更加均匀且尺寸减小。复合材料在液相烧结的过程中,高温下的液相粘性流动以及在原位反应时发生的颗粒重排与固相的溶解和沉淀对材料的致密化产生了较大的作用,当烧结温度达到1000℃时,Al_2O_3颗粒数量、分布情况都得到明显地改善。     

Microstructure and Toughness of Seeded Hot-Pressed Si3N4 Ceramics

Densification, phase transformation and fracture toughness were studied in hot-pressed Si_3N_4 seeded by in-houseproduced large, elongated β-Si_3N_4 seeds. A mixture of Y_2O_3-Al_2O_3 was used as the sintering aid. Concentration ofseeds were varied from 0 to 6 wt pct and the sintering time at 1700℃ was varied from 1 to 4 h. Maximum fracturetoughness of 9.0 MPam~(1/2) was measured in samples containing 5 wt pct seeds, hot pressed at 1700℃ for 4 h.     

SiC_W含量对SiC_W/Si_3N_4复合陶瓷力学及高温微波性能影响

以α-Si_3N_4粉、β-SiC_W为原料,Al_2O_3、Y_2O_3为烧结助剂,采用凝胶注模工艺制备了SiC_W/Si_3N_4复合陶瓷材料,烧结温度为1 650℃,保温1.5h。研究了SiC_W加入含量对SiC_W/Si_3N_4复合陶瓷的微观结构、力学及常温/高温微波吸收性能的影响。结果表明:随着SiC_W含量的增加,SiC_W/Si_3N_4复合陶瓷的抗弯强度和断裂韧性都有先増后减的趋势,当含量为10wt%时,抗弯强度达到最大值505MPa,断裂韧性达9.515MPa·m1/2。常温介电常数在SiC_W含量为10wt%时,实部达最大值12,在12GHz最大吸收值为-21dB。高温介电常数随着SiC_W含量的增加有先增后减的趋势,在含量为10wt%时,实部达到最大值12.5。相比于纯Si_3N_4陶瓷,当SiC_W含量为10wt%时,SiC_W/Si_3N_4复合陶瓷在11.7GHz左右最大吸收可达-27dB,有效吸收频带(小于-5dB)为11.2~12.3GHz。     

Microstructure and mechanical properties of a Si3N4/Al2O3 nanocomposite

A nanocomposite material fabricated by hot pressing in the form of nanometre-sized Si3N4 particles dispersed in an Al2O3 matrix has been shown to exhibit enhanced mechanical properties compared with monolithic matrix material. It was observed by transmission electron microscopy (TEM) for the first time that the alumina grains were in the shape of elongated columns with aspect ratios in the range 2.5–4. The presence of liquid phase during sintering was found to be responsible for the appearance of columnar grains. Regular hexagon-shaped larger -Sialon grains formed during sintering were mainly situated at grain boundaries of the matrix material while irregular smaller dispersoids were trapped within the alumina grains. The improvement in the mechanical properties of the nanocomposite is attributed to the change in fracture mode from intergranular fracture to transgranular fracture, the self-reinforcement effect arising from the elongated columnar grains of the matrix, as well as the pinning effect due to the existence of intergranular -sialon particles. It was revealed that the trapped particles have an -Al2O3 structure with partial sites of aluminium and oxygen atoms substituted by silicon and nitrogen atoms, which is also likely to lead to the strengthening of the composite.     

Al_6Si_2O_(13)晶须和TiC颗粒复合强化多孔Al_2TiO_5基复合材料

以γ-AlOOH和TiO_2为原料,添加不同质量分数SiC晶须(SiCw),采用无压反应烧结法制备多孔(Al_6Si_2O_(13)+TiC)/Al_2TiO_5复合材料,分析了SiCw质量分数对(Al_6Si_2O_(13)+TiC)/Al_2TiO_5复合材料孔隙率和抗压强度的影响,讨论了SiCw的强化机制。结果表明:不添加SiCw时,产物主要为Al_2TiO_5和少量Al_2O_3,还有少量未反应的TiO_2;加入SiCw之后,还形成了Al_6Si_2O_(13)和TiC相,TiC和Al_6Si_2O_(13)分别以规则颗粒状和晶须形态存在于Al_2TiO_5基体中。TiC颗粒与Al_6Si_2O_(13)晶须通过细化显微组织、裂纹偏转和晶须桥连机制,起到协同强化作用。SiCw的添加使孔隙率和抗压强度同时大幅度提高,随着SiCw质量分数的增加,(Al_6Si_2O_(13)+TiC)/Al_2TiO_5复合材料孔隙率降低,抗压强度提高的速率减小,当SiCw的质量分数为7.2%时,抗压强度最高,达到301.81 MPa。     

氮化硅-铼嬗变模拟靶材的制造和性能研究

采用无压烧结的方法(在1550℃保温3小时)添加5wt.％MgO,5wt.％Y2Oa和不同含量的Re制造出了Si3N4-Re嬗变模拟靶材.研究了Re含量的不同对嬗变靶材致密度和抗弯强度的影响,并通过物相分析,显微组织和断口形貌观察对相关机理进行了分析.     

Crystal structure and optical properties of oxynitride rare-earth tantalates RTa-(O, N) (R = Nd, Gd, Y)

X-ray absorption and photoluminescence were used to investigate the structure of rare-earth tantalum oxynitrides RTa-(O, N) (R = Nd, Gd, Y). Owing to the size of the rare-earth element, the crystal structure tends towards the pyrochlore or defect fluorite-type structure. EXAFS suggested neodymium and yttrium atoms are coordinated either by 6 + 2 or 6 oxygen/nitrogen atoms in the Nd or Y respective oxynitrides although the coordination number of tantalum is six in both compounds. Photoluminescence for 5 at.% doped europium showed the spectra compatible with the point symmetry C_3v lower than O_h in fluorite and D_3d in pyrochlore structure type for both the Gd and Y tantalum oxynitrides. These measurements supported that their structure types were basically pyrochlore for Nd and Gd tantalum oxynitrides and defect fluorite for Y tantalum oxynitride but they are highly defective.     

PMMA/硅铝包覆铝酸锶复合发光材料的制备和发光性能

采用原位乳液聚合法制备了聚甲基丙烯酸甲酯(PMMA)/硅铝包覆(SrAl2O4:Eu,Dy)复合发光材料。通过傅立叶变换红外光谱(FT-IR)和热失重(TGA)测定,研究了复合发光材料的结构,结果表明,复合发光材料中聚合物分子与硅铝包覆(SrAl2O4:Eu,Dy)之间是通过键合的方式结合;通过荧光光谱和发光亮度测试,研究了复合发光材料的发光特性和余辉性能,结果表明,在硅铝包覆(SrAl2O4:Eu,Dy)表面共价结合上PMMA后仍能保持SrAl2O4:Eu,Dy原有的发光性能。