Effect of Particle Size on Silicon Nitride Ceramic Slurry by Stereolithography

The effects of particle size,gradation and solid loading of silicon nitride (Si_(3)N_(4)) on the rheological behavior and curing properties of ceramic slurry are studied by stereolithography (SLA).The results show that the particle size of Si_(3)N_(4) powder has a signif icant influence on the rheological properties and stability of the slurry.When m_(D50=1.3μm):m_(D50=2.3μm)=3:7,the slurry viscosity is low and the sedimentation is slow.The most important thing is that with the increase of the solid loading of the slurry,the viscosity of the slurry increases,the stability becomes higher,and the curing thickness decreases.The curing thickness of Si_(3)N_(4) ceramic slurry with solid loading of 50 vol% can reach nearly 50μm.The above results finally show that the process optimizes the formulation of the slurry in rheological and curing properties.

Development and Application of Multi-phase Nitrides Bonded Silicon Carbide Lintel Blocks for Dry Quenching Furnaces

Multi-phase nitrides bonded silicon carbide lintel blocks were prepared using industrial SiC(SiC≥98 mass%,3-0.5,≤0.5 and≤0.044 mm),Si powder(Si≥98 mass%,≤0.044 mm),and SiO2 micropowder(SiO2≥96 mass%,d50=0.15 pm)as raw materials,and calcium lignosulfonate as the additive,batching,mixing,and molding on a vibration pressure molding machine,drying and then firing at 1420℃for 10 h in high-purity N2.The apparent porosity,the bulk density,the cold modulus of rupture,the hot modulus of rupture,and the linear expansion coefficient of the samples were tested.The phase composition and the microstructure of the samples at different nitriding depths(50,100,and 150 mm)were analyzed by XRD and SEM.The field application effects of the blocks were studied.The results show that:(1)the multi-phase nitrides bonded silicon carbide refractories can dynamically adjust their own phase composition and minimize structural and thermal stresses,improving the service life of key parts of dry quenching furnaces;(2)calcium lignosulfonate can improve the nitriding micro-environment of multi-phase nitrides bonded silicon carbide lintel blocks,successfully increasing the effective nitriding thickness of the blocks to 300 mm;(3)Sinosteel LI RR provides a unique concept in the design of materials and block types as well as the stable and scientific overall structure,promoting the industrialization process of dry quenching furnaces with long service life in China.

Effect of Additives on the Sintering of Amorphous Nano-sized Silicon Nitride Powders

Amorphous nano-sized silicon nitride powders were sintered by liquid phase sintering. The influences of the additives of Y2O3 and Al2O3 prepared by two different ways, the polyacrylamide gel method and the precipitation method, were investigated. The grain sizes of the additives prepared by the first method were finer than those of prepared by the latter method. When sintered at the same temperature, 1700 ℃, the average grain size of the silicon nitride is 0.3 um for the sample with the former additives, which is much finer than the one with the latter additives. The density of additives prepared by precipitation method is clearly lower than those of prepared by polyacrylamide gel method.

Fabrication of Fine-Grained Si_3N_4-Si_2N_2O Composites by Sintering Amorphous Nano-sized Silicon Nitride Powders

Si3N4-Si2N2O composites were fabricated with amorphous nano-sized silicon nitride powders by the liquid phase sintering （ LPS ）. The Si2 N2O phase was generated by an in-situ reaction 2 Si3 N4 （ s ） ＋ 1.5 02 （ g ） = 3 Si2 N2O （ s ） ＋ N2 （ g ） . The content of Si2 N2 O phase up to 60% in the volume was obtained at a sintering temperature of 1 650℃ and reduced when the sintering temperature increased or decreased, indicating the reaction is reversible. The mass loss, relative density and average grain size increased with increasing the sintering temperature. The average grain size was less than 500 nm when the sintering temperature was below 1 700 ℃. The sintering procedure contains a complex crystallization and a phase transition ： amorphous silicon nitride→equiaxial α- Si3 N4→ equiaxial β- Si3 N4→ rod- like Si2 N2O→ needle- like β- Si3N4 . Small round-shaped β→ Si3 N4 particles were entrapped in the Si2 N2O grains and a high density of staking faults was situated in the middle of Si2 N2O grains at a sintering temperature of 1 650 ℃. The toughness inereased from 3.5 MPa·m^1/2 at 1 600 ℃ to 7.2 MPa· m^1/2 at 1 800 ℃ . The hardness was as high as 21.5 GPa （Vickers） at 1 600 ℃ .

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.

Influence of Yb_2O_3-MgO on Mechanical Properties and Thermal Conductivity of Silicon Nitride Ceramics via Gas Pressure Sintering

In this work,Yb2O3 and Mg O were used as sintering aids in preparing silicon nitride ceramics by gas pressure sintering（ 0. 6 MPa N2atmosphere） to investigate how the amounts of Yb2O3- Mg O influence the mechanical properties and thermal conductivity of silicon nitride ceramics. The total contents of Yb2O3- Mg O added were 1 mol%,2 mol%,4 mol%,6 mol%,8 mol%,10 mol%,12 mol%,14 mol%,keeping the Yb2O3-Mg O molar ratio of 1 ∶ 1 steadily. Curves of the relative density,thermal conductivity and bending strength plotted against the aids content present a ‘mountain＇shape with a maximum at nearly 10 mol% aids. The fracture toughness increased with the amounts of additives up to10 mol% and decreased slightly thereafter. The mechanical properties and thermal conductivity were almost proportional to the amount of the additives before10 mol%. When the content of aids exceeded 10 mol%,it would weaken the mechanical properties and thermal conductivity of the ceramics. The optimum content of Yb2O3- Mg O was 10 mol% by gas pressure sintering（ 0. 6MPa） at 1 850 ℃ for 4 h,which led to a relative density of 98. 9%,a flexural strength of（ 966 ± 38）MPa as well as a fracture toughness of（ 6. 29 ± 0. 29）MPa·m1 /2and thermal conductivity of 82 W /（ m·K）.

PREPARATION OF NANOSIZED SILICON NITRIDE POWDERS BY AMMONO SOL-GEL PROCESSING

ＰＲＥＰＡＲＡＴＩＯＮＯＦＮＡＮＯＳＩＺＥＤＳＩＬＩＣＯＮＮＩＴＲＩＤＥＰＯＷＤＥＲＳＢＹＡＭＭＯＮＯＳＯＬＧＥＬＰＲＯＣＥＳＳＩＮＧ①ＧａｏＪｉｍｉｎｇ，ＸｉａｏＨａｎｎｉｎｇ，ＺｈａｎｇＬｉ，ＤｕＨａｉｑｉｎｇＣｈｅｍｉｓｔｒｙａｎｄＣｈｅｍｉ...

Experimental investigation of laser surface processing of flexure silicon nitride ceramic

A continuous wave carbon dioxide (CO2) laser (λ=10.6μm) was employed to treat the surface of Si3N4 MOR (modulus of rupture) bars. The effects of the CO2 laser process on physical and mechanical properties of ground Si3N4 samples were investigated. Scanning electron microscopy (SEM) analysis shows that the area occupied by cavities and fracture is decreased by about 49.4% after laser treatments. Cross-sectional metallography results indicate that the secondary YSiAlON phase in the Si3N4 ceramic is softened/melted and flowed into the defects. Four-point bending tests show that the flexural strength of the treated samples is improved to 10.9%. Fractographic analysis show that the fracture origins move from the surface to subsurface. It is concluded that laser surface processing have significant effects on fracture behavior of flexure Si3N4 ceramic.

Structural and Electrical Characterization of Sintered Silicon Nitride Ceramic

The electrical conduction phenomena, dielectric response and microstructure have been discussed in sintered silicon nitride ceramics at different temperature and frequencies. Microstructure and phase of the sintered samples was investigated by Scanning Electron Microscope (SEM) and X-ray diffractometer (XRD). The electrical conductivity, dielectric constant and dielectric loss increases exponentially with temperature greater than 600 K. The dielectric constant and loss have been measured in the frequency range 100 Hz to 1 MHz. The a.c. conduction studies in the audio frequency range 500 Hz to 1 MHz indicates that the conduction may be due to the electronic hopping mechanism. Silicon Nitride ceramics became dense after sintering. The effect of grain size and role of phase on electrical and dielectric properties have been discussed. These types of samples can be used as a high temperature semi conducting materials for device packaging.

Comparison of Silicon Nitride Nanofibers Synthesized Using Silica Nanopowders and Silica Gel

Nanofibers of alpha silicon nitride were grown by a vapor-solid mechanism at 1450?C, through the carbothermal reduction process. Two different precursor silica sources were used: silica nanopowders and silica gel. The effect of processing geometry, particularly the stacking orientations of the graphite substrates, silica pellets, and crucibles, on the density of nanofiber growth was also explored. The silicon nitride nanofibers appear with a predominantly rectangular cross section from silica nanopowder precursors and with a circular cross section for silica gel precursors. Silica gel precursors produce nanofiber products that are smaller in cross section but greater in length than the products from silica nanopowder precursors. The processing geometry must be suitably designed such that the vapor-solid mechanism that is responsible for the formation of the nanofibers is not disrupted.

Mechanical Properties of Composite SiNx/DLC Films Prepared by Filtered Cathodic Arc of Graphite Incorporated with RF Sputtering of Silicon Nitride

Composite SiNx/DLC films were deposited on Si substrate by RF magnetron sputtering of silicon nitride (Si3N4) target simultaneously with filtered cathode arc (FCA) of graphite. The RF power was fixed at 100 W whereas the arc currents of FCA were 20, 40, 60 and 80 A. The effects of arc current on the structure, surface roughness, density and mechanical properties of SiNx/DLC films were investigated. The results show that the arc current in the studied range has effect on the structure, surface roughness, density and mechanical properties of composite SiNx/DLC films. The composite SiNx/DLC films show the sp3 content between 53.5% and 66.7%, density between 2.54 and2.98 g/cm3, stress between 1.7 and 2.2 GPa, and hardness between 35 and 51 GPa. Furthermore, it was found that the density, stress and hardness correlate linearly with the sp3 content for composite SiNx/DLC films.

IR Spectroscopic Study of Silicon Nitride Films Grown at a Low Substrate Temperature Using Very High Frequency Plasma-Enhanced Chemical Vapor Deposition

Hydrogenated amorphous silicon nitride (a-SiNx:H) films have been grown from a SiH4–N2 gas mixture through very high frequency (VHF) plasma-enhanced chemical vapor deposition (PECVD) at 50℃. The films are dense and transparent in the visible region. The peak frequency of the Si–N stretching mode in the IR absorption spectrum increases with increasing N–H bond density, which is similar to the behavior of a-SiNx:H films grown from SiH4–NH3 gas. During storage in a dry air atmosphere, the Si–O absorption increases. A large shift in the peak frequency of the Si–N stretching mode in the initial stage of oxidation, which is higher than the shift expected from the increase in the N–H bond density, is mainly caused by the change in the sum of electronegativity of nearest neighbors around the Si–N bond due to the increase in the Si–O bond density.

Liquid Phase Sintering (LPS) and Dielectric Constant of α-Silicon Nitride Ceramic

The spark plasma sintering （SPS） was applied to prepare α-Si3 N4 ceramics of different densities with magnesia, silicon dioxide, alumina as the sintering aids. The mechanism of liquid phase sintering （LPS） wus discussed and the factors influencing the density of the prepared samples were analyzed. The dielectric constant of sintered samples was tested. The experimental results show that the density can be controlled from 2.48 g/ cm^3 to 3.09 g/ cm^3 while the content of the sintering aids and the sintering temperature alter and the dielectric constant is closely dependent on the density of obtained samples.

Cutting performance of multilayer diamond coated silicon nitride inserts in machining aluminum-silicon alloy

Aluminum-silicon （Al-Si） alloy is very difficult to machine and diamond tools are considered by far the best choice for the machining of these materials. Experimental results in the machining of the Al-Si alloy with diamond coated inserts are presented. Considering the fact that high adhesive strength and fine surface morphology play an importance role in the applications of chemical vapor deposition （CVD） diamond films, multilayer technique combining the hot filament CVD （HFCVD） method is proposed, by which multilayer diamond-coating on silicon nitride inserts is obtained, microcrystalline diamond （MCD）/ nanocrystalline diamond （NCD） film. Also, the conventional monolayer NCD and MCD coated inserts are produced for comparison. The as-deposited diamond films are characterized by field emission scanning electron microscopy （FE-SEM） and Raman spectrum. All the CVD diamond coated inserts and uncoated insert endure the aluminum-silicon alloy turning to estimate their cutting performances. Among all the tested inserts, the MCD/NCD coated insert exhibits the perfect behavior as tool wear due to its very low flank wear and no diamond peeling.

DESIGN AND PREPARATION OF SILICON NITRIDE COMPOSITE WITH HIGH FRACTURE TOUGHNESS AND NACRE STRUCTURE

A new way of designing and preparing silicon nitride ceramic composite with high fracture toughness and nacre structure has been proposed. To mimic the laminated structure of nacre, Si_3N_4 matrix ceramic layer can be obtained through compacting rolling method. To mimic the secondary toughening of nacre structure, SiC whisker is added into Si_3N_4 and acts as the secondary toughening phase. Boron nitride (BN)is selected to mimic the organic layer in nacre so as to form the weak interfaces between Si_3N_4 layers. Alumina is added into BN to adjust the bonding strength of the interface.The Si_3N_4 sheets are stacked into the die after coating with BN. After the removal of the organic matter in them, the green body is hot pressed at 1820℃for 1.5 hours under N_2 atmosphere. The fracture toughness of the so-made Si_3N_4 composite at room temperature is 20.36MPa m￣(1/2), the three-point bending strength at room temperature is 651.47MPa. The crack spreads and deflects along the interface between BN and Si_3N_4 layer and extends through the BN layer into Si_3N_4 layer. The improvement of the fracture toughness may be due to the staircase-shape-like crack which provides the long crack path, the fracture and deformation of Si_3N_4 layer, and the pullout of SiC whiskers from the Si_3N_4 layer.

Research on Abrasives in the Chemical Mechanical Polishing Process for Silicon Nitride Balls

Silicon nitride (Si 3N 4) has been the main material for balls in ceramic ball bearings, for its lower density, high strength, high hardness, fine thermal stability and anticorrosive, and is widely used in various fields, such as high speed and high temperature areojet engines, precision machine tools and chemical engineer machines. Silicon nitride ceramics is a kind of brittle and hard material that is difficult to machining. In the traditional finishing process of silicon nitride balls, balls are lapped by expensive diamond abrasive. The machining is inefficiency and the cost is high, but also lots of pits, scratch subsurface micro crazes and dislocations will be caused on the surface of the balls, the performance of the ball bearings would be declined seriously. In these year, a kind of new technology known as chemical mechanical polishing is introduced in the ultraprecision machining process of ceramic balls. In this technology, abrasives such as ZrO 2, CeO 2 whose hardness is close to or lower than the work material (Si 3N 4) are used to polishing the balls. In special slurry, these abrasives can chemo-mechanically react with the work material and environment (air or water) to generate softer material (SiO 2). And the resultants will be removed easily at 0.1 nm level. So the surface defects can be minimized, very smooth surface (Ra=4 nm) and fine sphericity (0.15～0.25 μm ) can be obtained, and the machining efficiency is also improved. The action mechanism of the abrasives in the chemical mechanical polishing process in finishing of silicon nitride ball will be introduced in this paper.

Study on the Performance of PECVD Silicon Nitride Thin Films

Mechanical properties and corrosion resistance of Si3N4 films are studied by using different experiment parameters, such as plasma enhanced chemical vapor deposition(PECVD) RF power, ratio of reaction gas, reaction pressure and working temperature. The etching process of Si3N4 is studied by inductively coupled plasma (ICP) with a gas mixture of SF6 and O2. The influence of the technique parameters, such as ICP power, DC bias, gas composition, total flow rate, on the etching selectivity of Si3N4/EPG533 which is used as a mask layer and the etching rate of Si3N4 is studied, in order to get a better etching selectivity of Si3N4/EPG533 with a faster etching rate of Si3N4. The optimized process parameters of etching Si3N4 by ICP are obtained after a series of experiments and analysis. Under the conditions of total ICP power of 250 W, DC bias of 50W, total flow rate of 40 sccm and O2 composition of 30%, the etching selectivity of 2.05 can be reached when Si3N4 etching rate is 336 nm/min.

Preparation and Properties of Macroporous Silicon Nitride Ceramics by Gelcasting and Carbonthermal Reaction

Macroporous silicon nitride （Si3N4） ceramics with high strength, uniform structure and relatively high porosity were obtained by gelcasting and carbonthermal reaction in a two-step sintering technique. Microstructure and composition were investigated by scanning electron microscopy （SEM）, transmission electron microscopy （TEM）, X-ray diffraction （XRD）. Open porosity, pore size distribution and basic mechanical performance were measured by Archimedes method, mercury intrusion porosimetry and three-point bending methods, respectively. SEM and TEM results revealed that pores were formed by elongated β-Si3N4. SADP measurement proved the formation of SiC particles. The SiC granules were beneficial for the formation of high ratio elongated β-Si3N4, and at proper amount, they also acted as reinforcement phase. Thermodynamic analysis indicated that the mechanisms of the reactions were mainly associated with liquid-solid reaction and gas-liquid reaction.

LASER PLASMA ASSISTED CHEMICAL VAPOR DEPOSITIONOF SILICON NITRIDE ON STAINLESS STEEL

This study raised a new assisted technique used for chemical vapor deposition (CVD) in which a laser beam irradiated the surface of substrate and simultaneously the plasma surroundings created in the reactive room, but both laser and plasma were at lower energy level in order to perform easily. The chemical vapor deposition reaction could be performed only just using simultaneously above two assisted methods. If not, the reaction could not be performed, too. It is laser plasma assisted chemical vapor deposition (LPCVD). For these reasons, a LPCVD device had been designed and manufactured, and was carried on practical operation. The results indicated that this technique is successful and feasible. Acting on the system of SiH 4 NH 3 N 2 with both CO 2 laser and RF plasma, expectant film of silicon nitride had been obtained on the surface of stainless steel.

Microhardness and Biocompatibility of Silicon Nitride Ceramic Developed for Dental Applications

Silicon nitride (Si3N4) ceramic is an attractive material for dental applications, especially used as a dental core material, due to its unique properties including high fracture toughness, high strength, high wear resistance and non-cytotoxicity. In this study, the Si3N4 ceramic was fabricated by a non-pressure sintering technique at a relatively low sintering temperature of 1650℃ in nitrogen atmosphere. Borosilicate glass and 5 wt% ZrO2-added borosilicate glass were used for coating on the Si3N4 core surface because of their compatibility in thermal expansion, high chemical resistance and bio-inert. The specimens were then fired in electric tube furnace at 1100℃. The Vickers microhardness of borosilicate glass and 5 wt% ZrO2-added borosilicate glass veneering materials were measured and compared with the commercial dental veneer porcelain as a control (VITA VMK 95). The cytotoxicity of the Si3N4 ceramic and the veneering materials were tested by MTT assay, using human gingival fibroblasts (HGF) and periodontal ligament fibroblasts (HPDLF). The results indicate that the Si3N4 ceramic and Si3N4 ceramic veneered with borosilicate glass or 5 wt% ZrO2-added borosilicate glass veneering materials tested in this study are not toxic to oral tissue and can be used to produce dental prostheses.