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 ℃ .

Synthesis and characterization of high strength polyimide/silicon nitride nanocomposites with enhanced thermal and hydrophobic properties

Polyimide(PI)composite films were synthesized incorporating amino modified silicon nitride(Si_(3)N_(4))nanoparticles into PI matrix via in situ polymerization technique.The mechanical and thermal performances as well as the hydrophobic properties of the as prepared composite films were investigated with respect to the dosage of the filler in the PI matrix.According to Thermogravimetric(TGA)analysis,meaningful improvements were achieved in T5(5%weight loss temperature)and T10(10%weight loss temperature)up to 54.1℃ and 52.4℃,respectively when amino functionalized nano Si_(3)N_(4) particles were introduced into the PI matrix.The differential scanning calorimetry(DSC)results revealed that the glass transition temperature(Tg)of the composites was considerably enhanced up to 49.7℃ when amino functionalized Si_(3)N_(4) nanoparticles were incorporated in the PI matrix.Compared to the neat PI,the PI/Si_(3)N_(4) nanocomposites exhibited very high improvement in the tensile strength as well as Young’s modulus up to 105.4%and 138.3%,respectively.Compared to the neat PI,the composites demonstrated highly decreased water absorption behavior which showed about 68.1%enhancement as the content of the nanoparticles was increased to 10 wt%.The SEM(Scanning electron microscope)images confirmed that the enhanced thermal,mechanical and water proof properties are essentially attributed to the improved compatibility of the filler with the matrix and hence,enhanced distribution inside the matrix because of the amino groups on the surface of Si_(3)N_(4) nanoparticles obtained from surface functionalization.

Effects of precoating and calcination on microstructure of 3D silica fiber reinforced silicon nitride based composites

Three-dimensional silica fiber reinforced silicon nitride based composites were fabricated by preceramic polymer infiltration and pyrolysis method using perhydropolysilazane as a precursor. The effects of precoating and high temperature calcination on the microstructures of the composites were investigated by scanning electron microscopy. For the composite without a precoating, the fracture surface is plain, and the fiber/matrix interfaces become very unclear after calcination at 1 600 ℃ due to intense interfacial reactions. The composite with a precoating shows tough fracture surface with distinct fiber pull-outs, and the fiber/matrix interfaces are still clear after calcination at 1 600 ℃. It is the appropriate precoating process that contributes to the good interfacial microstructures for the composite.

TiC Particle Reinforced Silicon Nitride Composite Joined With Y_2O_3-Al_2O_3-SiO_2 Mixture

Silicon nitride composite is joined to itself by heating interlayer of Y2 O3 -AL2O3 -SiO2 mixtures above their liquidus temperatures in flowing nitrogen. The joined specimens are tested in four point flexure from room temperature to 1373 K. The interface microstruclure and fractured surfaces after testing are observed and analyzed by SEM, EPMA and XRD respectively. The results show that F2 O3 -A12 O3 -SiO2 glass reacts with Si3 N4 at interface, forming the Si3 N4/Si2 N2 O( Y-AlrSi-O-N glass/ Y-Al- Si-O glass gradient interface. With the increase of bonding temperature and holding time, the joint strength first increases, reaching a peak, and then decreases . According to interfacial analyses , the bonding strength depends on joint thickness .

High Performance Silicon Nitride-based Composite Materials with Rare-earth Oxides Additives

In the present paper,a silicon nitride-based composite processed with rare-earth oxidesadditives is presented.Its bend strength can be maintained at a value as high as 1000 MPafrom 1000 to 1370℃ and the fracture toughness measures 9-10 MPa·m1/2.The static fa-tigue behavior at 1370℃ of this material is also encouraging.Besides,two another α′/β′sialon composites doped with rare-earth oxides are also described.The effects of processingparameters on the microstructure and the properties of the materials are discussed in somedetails.

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.

Synthesis of ZrN-Si_3N_4 Composite by Carbothermal Reduction and Nitridation of Zircon

Zircon （ ≤44 μm） and carbon black （≤30μm） were used as starting materials and mixed for 24 h using anhydrous ethanol as medium with the mass ratio of 100：40, dried fully at 60 ℃ and then dry mixed for 10 h. Specimens with size of Ф20 mm × 5 mm were pressed under 60 MPa, then dried fully at 120 ℃ , put into a furnace with 1. 0 L ·min^-1 nitrogen gas and fired at 1 400, 1 450, 1 480 and 1 500℃ for 6, 9 and 12 h, respectively. The phase composition and microstructure of the specimens were studied by XRD and SEM, and the carbothermal reduction and nitridation reaction process was thermodynamically analyzed. The results show that using zircon and carbon black as starting materials, ZrN - Si3N4 composite is synthesized by carbothermal reduction and nitridation reaction in nitrogen atmosphere. The composites with different compositions are obtained by controlling the firing temperature and partial pressure of CO gas. The proper firing temperature and holding time to synthesize ZrN - Si3N4 composite are 1 500 ℃ for 12 h.

Dielectric properties of spark plasma sintered AlN/SiC composite ceramics

In this study, we have investigated how the dielectric loss tangent and permittivity of AlN ceramics are affected by factors such as powder mixing methods, milling time, sintering temperature, and the addition of a second conductive phase. All ceramic samples were pre-pared by spark plasma sintering （SPS） under a pressure of 30 MPa. AlN composite ceramics sintered with 30wt%-40wt%SiC at 1600℃ for 5 min exhibited the best dielectric loss tangent, which is greater than 0.3. In addition to AlN and β-SiC, the samples also contained 2H-SiC and Fe5Si3, as detected by X-ray difraction （XRD）. The relative densities of the sintered ceramics were higher than 93%. Experimental results indicate that nano-SiC has a strong capability of absorbing electromagnetic waves. The dielectric constant and dielectric loss of AlN-SiC ce-ramics with the same content of SiC decreased as the frequency of electromagnetic waves increased from 1 kHz to 1 MHz.

Effect of Sintering Additives on Properties of Si_3N_4BN Composites Fabricated via Die Pressing and Precursor Infiltration and Pyrolysis Route

The Si3N4-BN composites have been prepared via die pressing and precursor infiltration and pyrolysis route using borazine as precursor, and the effect of sintering additives on properties of the composites has been investigated. After sintering additives are adopted, the a to β phase transition of Si3N4 and the mechanical properties of the composites at both room temperature and high temperature are all increased with small extent. When using Y2O3＋Al2O3 as additives, the phase transition of Si3N4 and the mechanical properties of the composites have better results. The β-Si3N4 content is 17.47%. The flexural strength, elastic modulus and fracture toughness of the composites are 188.74 MPa, 84.34 GPa and 2.96 MPa.m1/2, respectively. After exposed at 1 000 ℃ in the air for 15 min, the flexural strength of the composites is 154.62 MPa with a residual ratio of 81.92%. The elongated β-Si3N4 grains appear in all composites with different sintering additives. Relatively more rod like β-Si3N4 grains can be observed in composites with Y2O3＋Al2O3 as additives, making it to possess better mechanical properties.

Effects of Admixtures on the Anti-oxidation Property of MgO/Si_3N_4 Composite Refractory

The effect of the admixtures of Al and Si metals and B4 C and MgAlON compounds on the oxidation of MgO/ Si3N4 composite refractory has been studied, which is a promising carbon free refractory for steel-making application . The four kinds of admixtures can be used as anti-oxi-dants for Si3N4, but the mixture of Al and Si achieved the best result. The mixture can not only play the role as anti-oxidant, but also assist the sintering process and help form dense sintering layer, improving the property of the composite.

Thermal Shock Resistance of Nano SiC-BN Composites

Nano SiC - BN composite powders were prepared by dissolving analytically pure H3BO3 and CO（ NH2 ）2 with the mole ratio of 1：2.5 in the absolute alcohol, adding 80% E-SiC with 0. 2 μm average grain size while stirring, firing at 850 ℃ in nitrogen （purity： 99. 99%, pressure： O. 92 -0. 93 MPa） for 15 h. Nano SiC -BN composite specimens were prepared by hot-pressed sintering the nano SiC - BN composite powder in N2 atmosphere with 0. 92 - 0. 93 MPa and at 30 MPa axial pressure for 0. 5 - 1 h at 1 750 - 1 800 ℃. The thermal shock resistance of nano SiC -BN composites was studied by three-point bending, TEM and SEM. The results show that, adding BN can decrease the modulus of elasticity of SiC materials, which improves thermal shock resistance;furthermore, because of the large difference of thermal expansion coefficient between matrix SiC and second phase hexa-BN, thermal mismatch effect results in intercrystalline delamination of h-BN grains and forming many micropores in composite ceramic, which can relax the thermal expansion caused by high tempera- ture effectively, and improve the thermal shock resistance significantly.

Fabrication of silicon nitride/ boron nitride nanocomposite powder

Si3N4/BN nanocomposite powders with the mi-crostructure of the micro-sized a-Si3N4 particles coated with nano-sized BN particles were synthesized via the chemical reaction of boric acid, urea, and a-Si3N4 powder in a hydro-gen gas. The results of XRD, TEM, and selected area elec-tron diffraction showed that amorphous BN and a little amount of turbostratic BN(t-BN) were coated on Si3N4 parti-cles as the second phase after reaction at 1100℃. After re-heating the composite powders at 1450℃ in a nitrogen gas, the amorphous and turbostratic BN is transformed into h-BN. These nanocomposite powders can be used to prepare Si3N4/BN ceramic composites by hot-pressing at 1800℃, which have perfect machinability and can be drilled with normal metal tools.

ZDMA改性Si_(3)N_(4)制备ZDMA@Si_(3)N_(4)/EPDM复合材料及性能研究

以羧酸锌盐二甲基丙烯酸锌(ZDMA)为改性剂,湿法改性处理陶瓷纳米氮化硅粉体(n-Si_(3)N_(4)),制备ZDMA@Si_(3)N_(4)/EPDM复合材料,研究ZDMA@Si_(3)N_(4)对复合材料力学性能、耐磨性能及耐油性能的影响。实验结果表明,ZDMA对Si_(3)N_(4)具有很好的表面有机化改性效果,改善了其在EPDM基体中的分散性,同时结构中不饱和键与橡胶大分子链形成共硫化,有效提高了复合材料的交联密度和极性,二者具有良好的协同作用。当ZDMA@Si_(3)N_(4)添加量为15 phr时,ZDMA@Si_(3)N_(4)/EPDM复合材料的拉伸强度和撕裂强度分别提高24.2%和42.8%,阿克隆磨耗磨损体积由0.52 cm^(3)/1.6 km降低至0.14 cm^(3)/1.6 km,100℃*70 h耐热油质量变化率由102%降至87%。

氮化硅晶须骨架增强环氧复合材料导热与介电性能

含有高导热系数的环氧树脂复合材料在电子封装和电气设备领域具有广泛的应用前景,但复合材料导热性能的提升往往伴随介电性能的劣化。该文旨在解决环氧复合材料热性能与介电性能之间的矛盾。以氮化硅晶须(Si_(3)N_(4w))和气相二氧化硅(SiO_(2))为原料,通过改进后的聚苯乙烯(polystyrene,PS)模板法制备得到坚固、多孔且绝缘的Si3N4w骨架,在真空浸渍后得到环氧复合材料并研究其热性能。同时,在不同电场强度(10^(3)~10^(6) V/m)与温度范围下系统研究复合材料的介电性能。结果表明,含有Si3N4w骨架的复合材料在7.80%的低填料负载下获得1.05 W/(m·K)的导热系数,相比纯环氧提升525%。得益于绝缘骨架,复合材料在120℃以下保持介电常数低于5.5、损耗角正切低于0.05,表现出优良的介电性能。结果表明,复合材料介电常数与损耗角正切随电场强度的上升而有小幅度上升,这源于电场强度增大时材料极化增强;同时,两者均随温度上升而增加,并在玻璃化转变温度附近出现跃升,其绝缘性能失效。该文结果可为解决环氧复合材料热性能与介电性能的矛盾提供新的思路。

Ti-Si-Fe添加量与氮气压强对BN/SiC/Si_(3)N_(4)复相陶瓷材料的影响

以BN粉、Si粉、SiC粉、Ti-Si-Fe合金、助烧剂B_(2)O_(3)及外加结合剂酚醛树脂(PFF)为原料,采用原位氮化反应烧结制备BN/SiC/Si_(3)N_(4)复相陶瓷材料。探讨了在氮气气氛中添加不同含量Ti-Si-Fe合金部分替代硅粉及不同的气压下制得试样的力学性能差异。结果表明,Ti-Si-Fe合金中的Fe、Mn等元素促进了硅粉的氮化和氮化硅晶须的生长,所有的氮化产物均可以更好地填充气孔并提高试样的致密化程度以及调控材料的力学性能。当Ti-Si-Fe合金添加量为1.5 wt.%时,常压下试样的显气孔率最低为25.3%、体积密度最高为1.97 g·cm^(-3),常温抗弯强度最高为33.8 MPa;气压下试样的显气孔率最低为20.8%,体积密度最高为2.15 g·cm^(-3),常温抗弯强度最高为43.4 MPa。与常压相比,2 MPa气氛压力烧成的试样,纤维状的Si_(3)N_(4)晶须明显偏少,柱状的Si_(3)N_(4)晶须明显偏多。

Tribological performance of novel nickel-based composite coatings with lubricant particles

The present study is focused on the evaluation of the tribological performance of novel Ni/h BN and Ni/WS_2 composite coatings electrodeposited from an additive-free Watts bath with the assistance of ultrasound. Lubricated and non-lubricated scratch tests were performed on both novel composite coatings and on standard Ni deposits used as a benchmark coating to have an initial idea of the effect of the presence of particles within the Ni matrix. Under lubricated conditions, the performance of the Ni/h BN composite coating was very similar to the benchmark Ni coating, whereas the Ni/WS_2 behaved quite differently, as the latter did not only show a lower coefficient of friction, but also prevented the occurrence of stick-slip motion that was clearly observed in the other coatings. Under non-lubricated conditions, whereas the tribological performance of the Ni/hBN composite coating was again very similar to that of the benchmark Ni coating, the Ni/WS_2 composite coatings again showed a remarkable enhancement, as the incorporation of the WS_2 particles into the Ni coating not only resulted in a lower coefficient of friction, but also in the prevention of coating failure.

铝基碳化硅复合材料镍镀层氢释放规律

铝基碳化硅复合材料具有高导热率、低热膨胀以及尺寸稳定性好等特点,广泛应用于空间微波组件管壳产品。为满足其应用于天线微波组件时的导电、焊接、散热等功能特性要求,铝基碳化硅复合材料需要进行化学镀镍,此过程会引入氢,由此对释氢、控氢提出明确需求。基于此,对铝基碳化硅镀镍的氢分布进行研究,采用SEM、XRD等方法分析材料微观结构表征,结果表明,基材与镀层均存在一定的孔隙结构,为氢的存贮提供场所;采用氢微印的实验方法表征氢的分布,结果表明铝基碳化硅镀镍中的氢规律为:铝基碳化硅镀镍后,氢分布在镀镍层和镀层下浅层基体中,且随着时间的延长,氢自发向深层基体扩散;氢主要分布在Al基体中,SiC颗粒上较少,且主要分布在基材及镀层中的微孔及位错缺陷处。采用TDS对不同温度除氢后的铝基碳化硅镀镍的氢释放量进行测试,表明高温除氢后释氢明显降低,且温度高有利于氢释放。

氮化硅层状陶瓷界面性能对力学性能的影响

通过加入Ｓｉ３Ｎ４调节隔离层的性质，研究了Ｓｉ３Ｎ４／ＢＮ层状复合材料在不同界面结合情况下的力学性能变化规律。结果表明，随着隔离层中Ｓｉ３Ｎ４含量的提高，基体片层之间的结合力不断增强。在结合力很强时，层状材料具有与块状材料相同的破坏方式，强度出现极值，达到１０００ＭＰａ以上；在结合力较弱时，隔离层能够反复偏折裂纹，层状材料表现出高达２０ＭＰａｍ１／２的表观断裂韧性和约６００ＭＰａ的强度。

SiO_2-Si_3N_4复合材料的力学性能及其增韧机理

采用热压工艺制备了SiO2－Si3N4复合材料，其抗弯强度和断裂韧性达到143MPa和1.7MPa·m1／2.比基体SiO2材料分别提高107％和70％.复合材料性能的改善是由于高弹性模量的Si3N4引入以及SiO2和Si3N4热膨胀系数不匹配导致的残余应力.

可加工Si_3N_4/BN复相陶瓷的制备及性能研究

采用化学溶液法混料,然后用氢还原氮化法制备出具有包覆结构的Si3N4/BN纳米复合粉体,复合粉热压后获得较高强度,同时又具有良好加工性能的复相陶瓷。扫描电镜(SEM),X射线衍射(XRD)分析表明:复相陶瓷中氮化硼以六方晶(h-BN)均匀分布于以α-Si3N4为基体相的晶界与晶内,并抑制α-Si3N4的晶粒长大使基体晶粒细化。良好加工性能的获得是由于h-BN易沿其层间解理以及h-BN与α-Si3N4两相由于热膨胀失配产生的弱界面易在剪切方向剥层所致。