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     

The influence of amount and type of additives on α → β Si3N4 transformation

During the liquid-phase sintering of silicon nitride-based ceramics, the dissolution of the Si3N4 is inferred from the tendency of the -Si3N4 to transform to -Si3N4. In order for this to correlate with densification it is necessary for the dissolved material to diffuse and precipitate, allowing contraction. In the present work the influence of the amount, quantity and type of additives on the transformation has been analysed. Two systems have been studied: Si3N4–SiO2 and Si3N4–Y2O3–SiO2. All samples were densified through hot isostatic pressing (HIP) of encapsulated compacts. In the Si3N4–SiO2 system the dissolution of -phase follows a zero-order kinetics and the amount of intergranular phase increases uniformly as a function of time, in this way eliminating dissolution as the rate-controlling mechanism in the transformation kinetic. In the Si3N4–Y2O3–SiO2 system, the kinetics of dissolution are first-order and the amount of intergranular phase remains constant with time. This is a sufficient and necessary condition to establish that transformation in this system is a process whose kinetics are controlled by the dissolution of -Si3N4 in the liquid phase.     

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。     

Study on the structures of N-containing melilite Y2Si3O3N4 and Nd2Si2.5Al0.5O3.5N3.5

Rietveld refinements have been used to determine the structure of Y2Si3O3N4 from X-ray data and Nd2Si2.5Al0.5O3.5N3.5 from neutron powder diffraction data. The refinements show that in the melilite phase Y2Si3O3N4 and melilite solid solution Nd2Si2.5Al0.5O3.5N3.5 the distributions of cations and anions are almost identical. They are analogous to the akermanite (Ca2MgSi2O7) structure, with Si/Si,Al atoms at the origin and centre of the unit cell and with four N/N,O atoms forming the SiN4/(Si,Al)(N3.5O0.5) tetrahedra which share corners with SiO2N2/(Si,Al)O2.25N1.75 tetrahedra to form a continuous sheet structure. Each Y3+ or Nd3+ ion is surrounded by eight N/O atoms forming the coordination polyhedron in Y2Si3O3N4 and Nd2Si2.5Al0.5O3.5N3.5 respectively. The arrangement of Al, Si atoms in the tetrahedra in Nd2Si2.5Al0.5O3.5N3.5 structure is also discussed. This revised version was published online in November 2006 with corrections to the Cover Date.     

包覆和凝胶注模成型对氮化硅陶瓷性能的影响

利用含 Al (NO3) 3,Y (NO3) 3和尿素的水溶液中无机盐的沉淀再经煅烧在 Si3N4粉料的表面包覆 Y2 O3- Al2 O3层 ,作为氮化硅烧结的助烧剂。包覆层改变了 Si3N4粉料的电动性和胶态特性 ,从而提高了 Si3N4的分散性。研究表明 ,经包覆和凝胶注模成型的方法所制备的氮化硅烧结体较冷等静压方法所获得的烧结体的抗弯强度和 Weibull模数都大大提高     

A fine cobalt-toughened Al2O3-TiC ceramic and its wear resistance

Mechanical ball milling is the most common method for mixing ceramic powders with a ductile phase such as metal particles. In this paper, a new powder processing way is presented. Al2O3 and TiC powders are coated with a layer of metal cobalt using the chemical deposition process. The thickness of the metal cobalt film can be controlled by adjusting the deposition conditions. The Co-coated Al2O3 (Al2O3–Co) and TiC (Tic–Co) powders are mixed at the rate of 7:3 and hot-press sintered into a fine Al2O3–TiC–Co (ATC) ceramic. The main properties, erosion behaviour, abrasion behaviour, wear mechanism and wear resistance of Al2O3-TiC-Co and Al2O3–30 wt% TiC (AT30) ceramics are determined by transmission electron microscopy, scanning electron microscopy, energy dispersive X-ray spectroscopy, etc. It is shown that the ATC ceramic possesses improved mechanical properties. Because of the existence of metal cobalt in the grain boundaries, the bonding strength between grains is increased, and this prevents spalling of grains during wear. Experimentation indicates that ATC is more resistant to wear than Al2O3–TiC ceramic. The relationship between their mechanical properties and wear resistance is also discussed in this paper.     

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…     

Toughening effects of WC/Co particles and compressive surface stress on (Al2O3–WC/Co)/TiC/Ni graded materials

A graded material of the (Al2O3–WC/Co)/TiC/Ni was prepared by using the self-propagating high-temperature synthesis-aided hot isostatic pressing process. The WC/Co particles were added to the outer Al2O3 layer in order to activate the heterophase toughening effects and control the thermal expansion mismatch between the outer and inner layers. SEM and TEM observations show a clustering structure of the WC/Co cermet in the Al2O3 matrix. The residual stress introduced by the compositionally graded structures was analysed using FEM calculation and X-ray diffraction. Measurements of the indentation toughness and R-curve behaviour indicated that the compressive surface stresses and WC/Co particles can significantly strengthen and toughen the Al2O3 ceramics. The indentation toughness of the (Al2O3–WC/Co)/TiC/Ni at the surface was 13.1 MPa m1/2, while those of the (Al2O3–WC/Co) uniform composite and the monolithic Al2O3 were 7.3 and 4.0 MPa m1/2, respectively. It was found by SEM observation of the crack propagation induced by indentation, thatthe crack deflection, bridging, blunting and arresting occurred at the WC/Co clusters. © 1998 Chapman & Hall     

Physico-chemistry and cytotoxicity of ceramics: Part I – Characterization of ceramic powders

The morphology of Al2O3, ZrO2/Y2O3, AIN, B4C, BN, SiC, Si3N4, TiB2, TiC, TiN ceramic, graphite and diamond powders has been studied by scanning electron microscopy (SEM) and the specific area of each powder was determined with the BET method. X-ray diffraction (XRD) investigations have been carried out in order to evaluate the crystallinity and determine the constitutive phases. The chemical composition was assessed by classical chemical analyses and by X-ray microprobe; some powders were studied by the laser micro-Raman technique. Correlations have been established between all these results.     

The oxidation of TiC in dry oxygen, wet oxygen, and water vapor

Isothermal oxidation of TiC was studied using powder sample at 300–400°C in Ar/O₂ = 95/5 kPa (dry oxidation) and Ar/O₂/H₂O = 90/5/5–10 kPa (wet oxidation), and at 520–650°C in Ar/H₂O = 95/5–15 kPa (H₂O oxidation) by monitoring weight changes. The phases produced were identified by X-ray analysis and the oxidized sample was observed by scanning and transmission electron microscopy. The dry, wet and H₂O oxidation of TiC was found to be described by a one-dimensional diffusion-controlling equation. It was revealed that the oxidation was divided into three steps, slow step I, fast step II, and slow step III. Water vapor in the wet oxidation accelerated these three steps, particularly step II. Non-isothermal oxidation of TiC was also performed to simultaneously monitor the evolved gases (CO/CO₂, H₂, CH₄) with weight changes by thermogravimetry and mass analysis. The accelerating effect of water vapor on oxidation of TiC was discussed from kinetic and thermoanalytical viewpoints.     

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。      

Oxidation mechanism of Si3N4-bonded SiC ceramics by CO, CO2 and steam

This paper presents a theoretical and experimental investigation into the oxidation reactions of Si3N4-bonded SiC ceramics. Such ceramics which contain a small amount of silicon offer increased oxidation and wear resistance and are widely used as lining refractories in blast furnaces. The thermodynamics of oxidation reactions were studied using the JANAF tables. The weight gain was measured using a thermogravimetric analysis technique to study the kinetics. The temperature range of oxidation measurements is from 1073 to 1573 K and the oxidation atmosphere is water vapour, pure CO and CO–CO2 gas mixtures with various CO-to-CO2 ratios. Thermodynamic simulations showed that the oxidation mechanism of Si3N4-bonded SiC ceramics is passive oxidation and all components contribute to the formation of a silica film. The activated energies of the reactions follow the sequence Si3N4>SiC>Si. The kinetic study revealed that the oxidation of Si3N4-bonded SiC ceramics occurred in a mixed regime controlled by both interface reaction and diffusion through the silica film. Under the atmosphere conditions prevailing in the blast furnace, this ceramic is predicted to be passively oxidized with the chemical reaction rate becoming more dominant as the CO concentration increases. © 1998 Chapman & Hall     

微波烧结TiC/Ti6Al4V复合材料的高温氧化行为

采用微波烧结法制备TiC/Ti6Al4V复合材料,研究TiC/Ti6Al4V复合材料在550、650和750℃空气中的恒温氧化行为,并对氧化膜的表面、截面形貌及相组成进行了分析。结果表明:TiC/Ti6Al4V复合材料由TiC、ɑ-Ti+β-Ti三种物相组成。随着氧化温度的增加,TiC/Ti6Al4V复合材料的氧化规律由抛物线型转变为直线型,在650℃温度以下,复合材料的氧化产物主要由TiO_2组成,而750℃时氧化层主要有外层极薄的TiO_2、中间层Al_2O_3和TiO_2混合区及大部分内层TiO_2三部分组成。随着TiC含量增加,氧化激活能增大,氧化物粒径减小,TiC/Ti6Al4V复合材料的抗氧化性能也越好。     

Oxidation behavior of hot-pressed MoSi2-TiC composite

The oxidation behavior of a hot-pressed MoSi₂-TiC composite was investigated in air over the temperature range of 500 °C–1400 °C. The composite exhibits parabolic oxidation kinetics between 500 °C–800 °C, where the activation energy was calculated to be 32 kJ/mol. However, above 800 °C, it shows two-step parabolic oxidation kinetics, where the first stage (step I) was proposed to be dominated by the oxidation of surface TiC particles. After all the surface TiC particles are oxidized, the oxidation of the composite turns into the second stage (step II) which was controlled by the oxidation of MoSi₂. The activation energy was determined to be 130 kJ/mol and 141 kJ/mol for step I and step II, respectively. A dense cristobalite scale with TiO₂ in lath shapes on the top was observed after oxidation at 1400 °C.     

High temperature strength and oxidation behaviour of hot-pressed silicon nitride-disilicate ceramics

Twelve different silicon nitride-disilicate ceramics have been fabricated by hot-pressing Si3N4 with the oxides of Y, Yb, Ho, Dy, Er, Sm, Ce, Lu, La, Pr, Gd, and Sc that are used as sintering additives. The high temperature strength and oxidation behaviour of the hot-pressed ceramics were investigated and correlated with the cationic radii of the oxide additives. The flexural strength at 1200°C increased, from 666 MPa for Si3N4-La2Si2O7 to 965 MPa for Si3N4-Sc2Si2O7 which is correlated with a decreasing cationic radius of the oxide additive. The weight gain during oxidation at 1400°C for 192 h in air decreased, from 0.8732 mg cm-2 for a Si3N4-Sm2Si2O7 ceramic to 0.1089 mg cm-2 for a Si3N4-Sc2Si2O7 ceramic, which is a function of the decreasing cationic radius of the oxide additive. This revised version was published online in November 2006 with corrections to the Cover Date.     

Self-sustaining oxidation of liquid aluminium and its alloys containing magnesium and silicon

An experimental investigation has been conducted into factors affecting the self-sustaining air oxidation of liquid aluminium and its alloys containing magnesium and silicon. Thermogravimetry and optical microscopy, scanning electron microscopy, and X-ray diffraction analysis have been performed to characterize the progress of oxidation and the nature of the products produced. On the basis of the results obtained, a comprehensive model is proposed capable of explaining the observed capability of producing an alumina composite material by a self-sustaining oxidation mechanism. It is proposed that aluminium/alumina transport occurs by means of the formation of gas-phase aluminium-bearing species which are then encapsulated by a liquid MgO–SiO2–Al2O3 slag phase. Subsequent precipitation of alumina from the slag phase provides the means by which alumina is continuously distributed throughout a growing alumina composite material. © 1998 Chapman & Hall     

Y_2O_3和TiO_2烧结剂对制备β-Sialon陶瓷烧结性能的影响

以金属Al粉、单质Si粉、α-Al_2O_3微粉为主要原料,高温氮化反应制备β-Sialon陶瓷。通过在反应物中分别添加不同含量的Y_2O_3和TiO_2烧结剂,研究分析和对比了Y~(3+)和Ti~(4+)对β-Sialon陶瓷晶相组成、晶格常数、微观结构及烧结性能的影响。采用SEM及EDS对试样的微观形貌进行观察与分析,利用X'Pert Plus软件分析晶相的晶格常数,采用半定量法计算试样晶相组成。结果表明:Y_2O_3和TiO_2可显著降低高温氮化法制备β-Sialon陶瓷试样中β-Sialon相的生成温度。伴随着Y_2O_3和TiO_2的引入,Al_2O_3在Si3N4中的固溶度提高,β-Sialon晶相的生成量增加,晶格常数和晶胞体积增大,烧结性能得到改善。综合对比分析,Y_2O_3和TiO_2均对制备β-Sialon陶瓷具有良好的促烧结作用,用成本较低的TiO_2代替传统的稀土氧化物作为助烧结剂无压烧结制备β-Sialon陶瓷是可行的。     

SiO2对铝合金熔体直接氧化的影响

本文研究了在高温空气氛中涂覆在Al-Mg-Si合金表面的SiO₂对铝合金直接氧化的影响规律。实验揭示了SiO₂对Al-Mg-Si合金熔体直接氧化生长表面的形态的影响规律,发现SiO₂有助于Al₂O₃/Al复合材料以光滑的方式进行氧化生长,提高了材料的致密度。实验还发现,SiO₂可消减Al-Mg-Si合金熔体直接氧化所需的孕育期,缩短Al₂O₃/Al复合材料的生长时间。     

Electrochemical Al2O3–ZrO2 composite coatings on non-oxide ceramic substrates

Aqueous solutions of xAl(NO3)3+(1–x)ZrO(NO3)2 were used for electrodeposition of ceramic Al2O3–ZrO2 composite on TiC, TiB2 and SiC sunstrates. The weight of the deposit was studied versus the duration of deposition, the current density and the temperature of the bath for Al-rich (x=0.9), Zr-rich (x=0.4) and eutectic (x=0.75) electrolyte compositions. Optimal current densities and durations of deposition were determined to obtain maxima weights of deposits. Amorphous deposits with thicknesses up to 10 m were formed. The microstructure and microchemical composition of the as-deposited and sintered deposits were characterized. Increase in the temperature of the bath inhibited microcracking due to shrinkage during drying. Coated TiC substrates exhibited enhanced oxidation resistance in air at 1100°C.     

Effect of Y_2O_3-MgO Addition on Heterogeneous Precipitation-Thermal Reduction Synthesis and Sintering of FeeMo/Si_3N_4 Powders

Effect of Y2O3e-MgO addition on heterogeneous precipitation-thermal reduction synthesis and the sintering of Fee Mo/Si3N4 powders has been investigated. It was found that the whiskers-like b-Si3N4, good wettability phases on Si3N4 surface, and high toughness Fe phase appeared in Fee Mo/Si3N4 cermets with Y2O3-MgO additives. The results show that Y2O3-MgO additives can effectively optimize the microstructures of Fee Mo/Si3N4 cermets, and improve the material mechanical properties. Therefore, it indicated that Y2O3-MgO additives can be used for strengthening of sintered cermets, and the dual function of whiskers self-toughening and different metal-composition toughening can be achieved in Fee Mo/Si3N4 cermets with Y2O3-MgO additives.