The Role of Nanodispersed Nitrides in the Sintering of Silicon Nitride Ceramics

The synthesis of ceramics based on silicon nitride using nanopowders of TiN and Si3N4 as additives was studied. The ceramic compositions were pressurelessly sintered under ni- trogen atmosphere at different temperatures （1550℃, 1650℃ and 1750℃） with a heating rate of 10℃/min and a holding time of 2 h. The nanodispersed nitrides （NDN） were produced by electric-arc plasma synthesis and characterized. The ceramic composites obtained with nanoparticles of 1wt% to 5wt% TiN and 20wt% Si3N4 were characterized by scanning electron microscopy （SEM）, atom force microscopy （AFM） and energy-dispersive spectrometry （EDX）. The effect of the addition of nanodispersed powders on the mechanical properties and microstructure of Si3N4 ceramics was investigated.

Promising high-thermal-conductivity substrate material for high-power electronic device:silicon nitride ceramics

High-thermal-conductivity silicon nitride ceramic substrates are indispensable components for nextgeneration high-power electronic devices because of their excellent mechanical properties and high thermal conductivities, which make them suitable for applications in complex and extreme environments. Here, we present an overview of the recent developments in the preparation of high-thermal-conductivity silicon nitride ceramics. First,the factors affecting the thermal conductivity of silicon nitride ceramics are described. These include lattice oxygen and grain boundary phases, as well the oxygen content of the crystal lattice, which is the main influencing factor.Then, the methods to prepare high-thermal-conductivity silicon nitride ceramics are presented. Recent work on the preparation of high-thermal-conductivity silicon nitride is described in detail, including the raw materials used and the forming and sintering processes. Although great progress has been made, the development of a high-quality,low-cost fabrication process remains a challenge. Nevertheless, we believe that high-thermal-conductivity silicon nitride substrates are promising for massive practical applications in the next generation of high-power electronic devices.

Porosity and Oxide Layer Dependence of Thermal Shock Behavior of Porous Silicon Nitride Ceramics

A water-quenching technique has been adopted to evaluate thermal shock fracture and fatigue behaviors of porous Si3N4 ceramics in an air atmosphere. The high-porosity Si3N4 ceramics exhibit a higher strength retention and a better resistance to thermal shock fatigue because of its role of the pores as crack arresters.A dense and coherent surface oxide layer leads to a significant benefit in residual strength during thermal fatigue, however, an increased fatigue number to 30 th cycle cannot cause a further influence although a thicker oxide layer presents, which is attributed to holes defect and disappearance of part intergranular phase.

Effects of Phase Composition on Microstructure and Mechanical Properties of Lu_2O_3-doped Porous Silicon Nitride Ceramics

Porous silicon nitride ceramics（Si3N4） were fabricated by pressureless sintering using different particle size of silicon nitride powder.Lu2O3 was used as sintering additive.According to phase relationships in the ternary system Si3N4-SiO2-Lu2O3,porous Si3N4 ceramics with different phase composition were designed through the change of the content of SiO2 which was formed by the oxidation at 800℃ in air.Porous Si3N4 with different phase compositions was obtained after sintering at 1800℃ in N2atmosphere.A small content of SiO2 favored the formation of secondary phase Lu4Si2O7N2,while large content of SiO2 favored the formation of secondary phase Lu2Si2O7 and Si2N2O.Porous Si3N4 ceramics with secondary phase Lu4Si2O7N2 had a flexural strength of 207 MPa,while that with secondary phase Si2N2O and Lu2Si2O7 had lower flexural strength.

Dielectric Properties of Porous Reaction-boned Si_3N_4 Ceramics with Controlled Porosity and Pore Size

This paper presents the microwave dielectric properties of reaction bonded porous silicon nitride ceramics with variant porosity and pore size, which were prepared by adding pore-forming agent grains into the silicon powders. The experimental results show that the dielectric constant and the dielectric loss of the samples reduce evidently with increasing porosity in the sample. When the porosity is constant, the dielectric constant and the dielectric loss of the ceramics decrease visibly as the pore size increases. Among all the obtained samples, the minimum dielectric constant is about 2.4.

Densification mechanism of stereolithographical dense Si_(3)N_(4) ceramics with CeO_(2) as sintering additive by field assisted sintering

Combining sintering additive with field assisted sintering,stereolithographical dense Si3N4 ceramics was successfully fabricated.Owing to a large amount of polymer during the stereolithography,the green parts have the characteristics of low powder loading and high porosity.Adjusting the process parameters such as sintering temperature and soaking time can effectively improve the density of the specimens.The stress exponent n of all specimens is in a range of 1 and 2,which is derived from a modified sintering kinetics model.The apparent activation energy Qd of stereolithographic Si_(3)N_(4) ceramics sintered with applied pressures of 30 MPa,40 MPa,and 50 MPa is 384.75,276.61 and 193.95 kJ/mol,respectively,suggesting that the densification dynamic process is strengthened by raising applied pressure.The grain boundary slipping plays a dominating role in the densification of stereolithographic Si3N4 ceramics.The Vickers hardness and fracture toughness of stereolithographic Si3N4 ceramics are HV10/10(1347.9±2.4)and(6.57±0.07)MPaAbstract:Combining sintering additive with field assisted sintering,stereolithographical dense Si3N4 ceramics was successfully fabricated.Owing to a large amount of polymer during the stereolithography,the green parts have the characteristics of low powder loading and high porosity.Adjusting the process parameters such as sintering temperature and soaking time can effectively improve the density of the specimens.The stress exponent n of all specimens is in a range of 1 and 2,which is derived from a modified sintering kinetics model.The apparent activation energy Qd of stereolithographic Si3N4 ceramics sintered with applied pressures of 30 MPa,40 MPa,and 50 MPa is 384.75,276.61 and 193.95 kJ/mol,respectively,suggesting that the densification dynamic process is strengthened by raising applied pressure.The grain boundary slipping plays a dominating role in the densification of stereolithographic Si3N4 ceramics.The Vickers hardness and fracture toughness of stereolithographic Si3N4 ceramics are HV10/10(1347.9±2.4)and(6.57±0.07)MPa·m^(1/2),respectively.

The Influence of Yttrium Isopropoxide on the Mechanical Properties of SiC_w-reinforced AIN Ceramics

By using self-made metal-alkoxide yttrium isopropoxide as a sintering additive and disperser of whisker, the SiC whisker reinforced AIN ceramics was prepared. Its apparent density is 99.5 percent of the theoretical density; its flexural strength and fracture toughness are 681 MPa and 5.21 MPa·m1/2 respectively. Comparing the result with that by applying Y2O3 powder as a sintering additive, the flexural strength is increased by 25% and the fracture toughness is increased by 33% . The dispersity of whisker by increased yttrium isopropoxide is significantly better than that by Triton X-100.

Microstructure and properties of Si_3N_4 ceramics obtained from addition of β-phase seeds and celsian

The silicon nitride based ceramics obtained by the addition of β-Si3N4 seeds was fabricated using celsian as the additive and by pressureless sintering. The microstructure of the material was observed and analyzed using XRD, SEM, and TEM and the mechanical response of this array microstructure was characterized for flexural strength and fracture behavior. The result shows that the growth of the larger aspect ratio grains initiate mainly from the seeds through the heterogeneous nucleation mechanism during the process of phase transformation, and the intergranular phase BaAl2Si20s services as good refractory materials. In contrast to conventional processing, a stable bimodal microstructure and complicated component with a lower cost can be achieved using the abovementioned process theoretically and practically.

Effect of Nano-Al_2O_3 on Mechanical Properties and Microstructure of Si_3N_4 Ceramics

Si3N4 ceramics were prepared by pressureless sintering at 1 650 ℃ in nitrogen atmosphere using Si3N4 powder as main starting material and adding nano Al203 powder （3%, 6%, 9%, 12%, and 15% in mass, the same hereinafter）. The bending strength and fracture toughness （KIC） of the specimens were detected.The microstructure and phase compositions of the specimens were analyzed. The results show that SigN4 ceramics can be prepared by pressureless sintering when adding 9% -12% nano-A1203 as active reactant, which dissolves in Si3N4, in-situ forming non-oxide SiAION. The obtained Si3N4 ceramics have the maximum bending strength of 710. 86 MPa and KIC of 8. 61 MPa · m1/2 The exceUent properties come from many interwoven structures distributed uniformly in the ceramics matrix, u,hich is composed of big and firm plate-like β-Si3N., hexagonal SiAION and sheet Si2N2 0.

Experimental Research on Residual Stress in Surface of Silicon Nitride Ceramic Balls

The influence of the residual stress in surface of ceramic balls on the fatigue life is large, because the life of silicon nitride ball bearings is more sensitive to the load acted on the bearings than the life of all-steel ball bearings. In this paper, the influence of thermal stress produced in sintering and mechanical stress formed in lapping process on residual stress in surface of silicon nitride ceramic balls was discussed. The residual compress stress will be formed in the surface of silicon nitride ceramic balls after sintering. The residual tensile stress will be formed in surface of silicon nitride ceramic balls in lapping process, and the size of abrasive particle is smaller, such trend is stronger. In this paper the residual stress was measured by the xylometric measurement in which the material in surface was peeled with lapping. The distribution of residual stress in surface can be calculated with the variation in specific volume. The technological parameter with which the material was peeled by lapping was given, for minimizing the extra influence of the residual stress forming in peeling on the original residual stress in surface, the abrasive particle size would not be too small and the load impressed would not be too large. Some experimental researches on residual stress in surface of silicon nitride ceramic balls were made. The surface of silicon nitride ceramic balls presented residual compressive stress after sintering and the influence of the ball size on the residual stress is feeble. It is expected that the size of ball blank is same for achieving the same residual compressive stress in surface on balls after final machining. In lapping process, the surface of silicon nitride ceramic balls presented residual tensile stress, the larger the load which is impressed on single ball, the larger the amplitude of residual tensile stress is; the smaller the abrasive particle, the stronger the trend of plastic deformation is and the larger the amplitude of residual tensile stress is.

Design and Implementation of a System for Laser Assisted Milling of Advanced Materials

Laser assisted machining is an effective method to machine advanced materials with the added benefits of longer tool life and increased material removal rates. While extensive studies have investigated the machining properties for laser assisted milling（LAML）, few attempts have been made to extend LAML to machining parts with complex geometric features. A methodology for continuous path machining for LAML is developed by integration of a rotary and movable table into an ordinary milling machine with a laser beam system. The machining strategy and processing path are investigated to determine alignment of the machining path with the laser spot. In order to keep the material removal temperatures above the softening temperature of silicon nitride, the transformation is coordinated and the temperature interpolated, establishing a transient thermal model. The temperatures of the laser center and cutting zone are also carefully controlled to achieve optimal machining results and avoid thermal damage. These experiments indicate that the system results in no surface damage as well as good surface roughness, validating the application of this machining strategy and thermal model in the development of a new LAML system for continuous path processing of silicon nitride. The proposed approach can be easily applied in LAML system to achieve continuous processing and improve efficiency in laser assisted machining.

Injection molding of ultra-fine Si_3N_4 powder for gas-pressure sintering

The ceramic injection molding technique was used in the gas-pressure sintering of ultra-fine Si3N4 powder. The feedstock＇s flowability, debinding rate, defect evolution, and microstructural evolution during production were explored. The results show that the solid volume loading of less than 50vol% and the surfactant mass fraction of 6wt% result in a perfect flowability of feedstock; this feedstock is suitable for injection molding. When the debinding time is 8 h at 40°C, approximately 50% of the wax can be solvent debinded. Defects detected during the preparation are traced to improper injection parameters, mold design, debinding parameters, residual stress, or inhomogeneous composition distribution in the green body. The bulk density, Vickers hardness, and fracture toughness of the gas-pressure-sintered Si3N4 ceramic reach 3.2 g/cm^3, 16.5 GPa, and 7.2 MPa·m^1/2, respectively.

Reaction Mechanism and Microstructure Evolution of Reaction Sintered h-BN

Hexagonal boron nitride ceramic（h-BN） based on the nitridation of B powders was obtained by reaction sintering method. The effects of sintering temperature on the mechanical properties and microstructure of the resultant products were investigated and the reaction mechanism was discussed. Results showed that the reaction between B and N2 occurred vigorously at temperatures ranging from 1 000 ℃ to 1 300 ℃, which resulted in the generation of t-BN. When the temperature exceeded 1 450 ℃, transformation from t-BN to h-BN began to occur. As the sintering temperature increased, the spherical particles of t-BN gradually transformed into fine sheet particles of h-BN. These particles subsequently displayed a compact arrangement to achieve a more uniform microstructure, thereby increasing the strength.

Dynamic study in partial transient liquid phase bonding of Si_3N_4

Dynamics in partial transient liquid phase bonding (PTLP bonding) of Si_3N_4 ceramic with Ti/Cu/Ti multi-interlayer was systematically studied through micro-analysis of joint interfaces. The results show that growth of reaction layer and isothermal solidification procession do at the same time. Growth of reaction layer and moving of isothermal solidification interface obey the parabolic law governed by the diffusion of participating elements during the PTLP bonding. Coordination of the above two dynamics process is done through time and temperature. When reaction layer thickness is suitable and isothermal solidification process is finished, the high bonding strength at room temperature and high temperature are obtained.

Effect of CeO_2 on low temperature pressureless sintering of porous Si_3N_4 ceramics

Porous silicon nitride（Si_3N_4） ceramics were fabricated by low temperature pressureless sintering, using carbonized rice husk and α-Si_3N_4 powders as raw materials, and MgO-CeO_2 as sintering additives. The effects of CeO_2 concentration and sintering temperature on phase composition, microstructure, porosity and flexural strength of the sintered products were investigated by X-ray diffraction（XRD）, scanning electronic microscopy（SEM）, Archimedes＇ displacement method and three-point bending strength, respectively. The results suggested that MgO-CeO_2 was a much more effective sintering additive for Si_3N_4 than MgO alone. When CeO_2 concentration was 4 wt.%–5 wt.% and sintering temperatures were in a range of 1500 to 1550 oC, the obtained porous silicon nitride ceramics had the porosity of 45.78%–42.81% and flexural strength of 49.44–84.09 MPa. Moreover, when sintering temperature was 1550 oC and CeO_2 concentration was 5%, large elongated β-Si_3N_4 grains were well developed.

In-situ ZrB2-hBN ceramics with high strength and low elasticity

ZrB2 ceramics with various hexagonal BN(hBN)additions up to 37 vol%were reactively densified by spark plasma sintering using powder mixtures containing ZrB2,ZrN and boron.ZrN-boron based additives effectively promoted the densification process,ZrB2 ceramics reached>99%relative density at 2000℃and an applied pressure of 60 MPa with only 5 vol%in-situ formed hBN,whereas the relative density of pure ZrB2 was only 91.2%at the same conditions.Increasing thehBN contents,the morphology of hBN grains gradually changed from quasi-spherical to flake dominated,which has substantial influence on their mechanical properties.In-situ ZrB2-10 vol%hBN ceramics demonstrated high flexural strength of 597±22 MPa,relatively low Young’s modulus of 406 GPa and good machinability,especially for the impressively large strain to failure(1.47×10^-3)which is superior to most of their counterparts in the ZrB2 based particulate reinforced ceramics.

Numerical Simulation and Experimental Study of an Ultrasonic Waveguide for Ultrasonic Casting of 35CrMo Steel

To achieve ultrasonic casting of 35 CrMo steel,the waveguide unit for introducing ultrasound into liquid steel was studied numerically and experimentally.The structure and length of the ultrasonic waveguide were optimized by modal analysis.The simulation results showed that a T-shaped waveguide unit matched the vibrational system better than an L-shaped unit.The performance of T-shaped waveguide unit was optimized when the length of the ultrasound radiator was 135 mm.The performance of the T-shaped waveguide unit was investigated in ultrasonic casting experiments,and the effect of ultrasound on the microstructure of 35 CrMo steel was examined.The experimental results showed that the T-shaped waveguide was able to successfully introduce ultrasound into the 35 CrMo melt.In addition,the use of a silicon nitride ceramic radiator avoided high-temperature corrosion in the molten metal.The microstructure of the treated area was significantly refined and equiaxed grains were obtained.The results represented a novel method for ultrasonic casting of steel.