Sintered reaction-bonded silicon nitrides with high thermal conductivity: The effect of the starting Si powder and Si3N4 diluents

Silicon nitride ceramics with high thermal conductivity were fabricated by employing the reaction bonding method. It was revealed that the addition of Si₃N₄ diluents affected both the nitriding reaction and the post-sintering behavior by changing the size of the silicon particle during the milling process. The reduced size of silicon particle led to an increased degree of nitridation. Further, narrower pore channels in the nitrided bodies caused by the reduced size of silicon particle enhanced the final density, by promoting the easier elimination of finer pores during post-sintering. The positive effect of the finer silicon particle was confirmed by a back-up experiment employing a variety of silicon particle sizes, produced by milling the raw silicon powder for different milling times. Thermal conductivity was dominated by material density rather than variation of the microstructure or oxygen content in the current research.     

Improvement in fracture strength of porous reaction-bonded silicon carbide with unique surface layer by incorporating α-silicon carbide powder as a secondary phase

This study investigated the effect of incorporating α-phase silicon carbide (α-SiC) powder as a secondary phase on the fracture strength of porous reaction-bonded silicon carbide with a surface layer (porous RB-SiC) mainly based on β-phase SiC (β-SiC). The porous RB-SiC was composed of a highly porous body and surface layer with lower porosity than the porous body. α-SiC powder was incorporated into the porous RB-SiC through powder-based direct foaming followed by reaction sintering. The fracture strength and porous structure of the porous RB-SiC were investigated by varying the amount and particle size of the α-SiC powder. The porous structure composed of β-SiC grain in the porous RB-SiC was strongly influenced by the incorporation of α-SiC powder. Fracture strength of porous RB-SiC increased from 27.1 ± 1.4 MPa (without α-SiC powder) to 39.9 ± 2.0 MPa as maximum by incorporation of α-SiC, resulting in fracture strength improvement by up to 1.5 times.     

Selective laser reaction synthesis of SiC,Si3N4 and HfC/SiC composites for additive manufacturing

Selective laser reaction sintering techniques (SLRS) techniques were investigated for the production of near net-shape non-oxide ceramics including SiC, Si₃N₄, and HfC/SiC composites that might be compatible with prevailing powder bed fusion additive manufacturing processes. Reaction bonded layers of covalent ceramics were produced using in-situ reactions that occur during selective laser processing and layer formation. During SLRS, precursor materials composed of metal and/or metal oxide powders were fashioned into powder beds for conversion to non-oxide ceramic layers. Laser-processing was used to initiate simultaneous chemical conversion and local interparticle bonding of precursor particles in 100 vol% CH₄ or NH₃ gases. Several factors related to the reaction synthesis process—precursor chemistry, gas-solid and gas-liquid synthesis mechanisms, precursor vapor pressures—were investigated in relation to resulting microstructures and non-oxide yields. Results indicated that the volumetric changes which occurred during in-situ conversion of single component precursors negatively impacted the surface layer microstructure. To circumvent the internal stresses and cracking that accompanied the conversion of Si or Hf (that expands upon conversion) or SiO_x (that contracts during conversion), optimized ratios of the precursor constituents were used to produce near isovolumetric conversion to the product phase. Phase characterization indicated that precipitation of SiC from the Si/SiO₂ melt formed continuous, crack-free, and dense layers of 93.7 wt% SiC that were approximately 35 µm thick_, while sintered HfC/SiC composites (84.2 wt% yield) were produced from the laser-processing of Hf/SiO₂ in CH₄. By contrast, the SLRS of Si/SiO_x precursor materials used to produce Si₃N₄ resulted in whisker formation and materials vaporization due to the high temperatures required for conversion. The results demonstrate that under appropriate processing conditions and precursor selection, the formation of near net-shape SiC and SiC composites might be achieved through single-step AM-compatible techniques.     

发动机用新材料──氮化硅陶瓷

高温陶瓷代替金属制造发动机，是目前国外研究的新课题。本文从提高效率、节约能源的角度出发，以氮化硅（Ｓｉ３Ｎ４）陶瓷发动机为例，介绍了其特点、制造方法及国外应用情况．     

Si3N4／纳米SiC复相陶瓷显微结构的研究

本研究通过采用纳米SiC粉体及有机前驱体两种途径,制备了Si_3N_4/纳米SiC粒子(Si_3N_4/纳米SiCp)复相陶瓷,研究了这些材料的显微结构特点,讨论了材料强化的机制与显微结构的关系。     

聚碳硅烷粘结法低温制备碳化硅多孔陶瓷

分别以平均粒径为10μm和20μm的两种规格碳化硅(SiC)粉末为原料、聚碳硅烷(PCS)为粘结剂,通过包混、过筛、模压成型、1000℃热解等工序制备了SiC多孔陶瓷,研究了PCS含量对SiC多孔陶瓷微观形貌、线收缩率、孔隙率与抗弯强度的影响,并对两种规格粉末制备的SiC多孔陶瓷性能进行了对比。结果表明:随着PCS含量的增加,两种规格粉末制备的SiC多孔陶瓷微观形貌都逐渐变得致密,当PCS含量为13%时,两种规格粉末制备的多孔陶瓷都出现了微观裂纹。随着PCS含量的增加,两种规格粉末制备的SiC多孔陶瓷孔隙率都逐渐降低,线收缩率都逐渐增大,抗弯强度先增大后降低,在PCS含量为10%时,平均粒径为10μm与20μm的SiC粉末制备的多孔陶瓷抗弯强度取得最大值,分别为31.6MPa与29.0MPa。     

SiC含量对反应烧结SiC-Si3N4复合材料性能的影响

以粒度均≤0.044mm的工业Si粉和α-SiC粉为原料,酚醛树脂为结合剂(占总粉末质量的6.5%),配成SiC含量(质量分数)分别为10%、30%、50%和70%的4组试样,经200MPa冷等静压成型后,在N2气氛中(压力为1.25MPa)于1395℃反应烧结制备了SiC-Si3N4复合材料,并采用SEM、XRD和EDS等测试手段对试样进行了观察和测试。结果表明:随着粉料中SiC含量的增加,烧后试样的体积密度下降,显气孔率提高,抗折强度降低,以SiC加入量为10%的试样性能最优;4组试样经800℃～室温空冷热震15次后的抗折强度保持率均在90%以上,表明材料具有良好的抗热震性能。     

工艺参数对反应烧结AIN陶瓷的影响

以Al,AlN粉为原料，采用反应烧结技术制备AlN陶瓷。Al粉含量、Al粉粒径、成型压力和升温制度是RBAN的重要工艺参数，优化工艺参数可制备出性能良好的AlN陶瓷。Al体积分数45％,1700℃温度下可制备出烧结密度为93％，抗弯强度为292MPa的AlN陶瓷。     

Fabrication of mullite-bonded porous SiC ceramics via a sol–gel assisted in situ reaction bonding

In the present work, mullite-bonded porous SiC ceramics were fabricated using reaction bonding techniques. The morphologies, phase composition, open porosity, pore size distribution and mechanical strength of porous ceramics were examined as a function of alumina sources (calcined nano-sized alumina powder and alumina sol prepared from hydrolysis of aluminum isopropoxide) and contents. It was found that the addition of alumina in powder form effectively enhanced the strength and decreased the porosity. In contrast, when alumina was added in sol form, a reverse effect was observed. Moreover, it was revealed that when a portion of calcined alumina was replaced by alumina sol, the mechanical properties improved significantly (more than 30%) as well as porosity compared to the traditional method. Pore size distribution analysis showed that the dispersion of nanosize alumina powder and SiC micro-particles in alumina sol is strongly improved compared to mixing in ethanol.     

氮化硅陶瓷注射成型体脱脂过程的研究

陶瓷注射成型是制备复杂形状陶瓷部件的一种有效方法。在这一陶瓷制备技术中,注射成型体的脱脂过程是关键一环。本文针对尺寸较大、形状复杂的陶瓷涡轮转子、研究了坯体中有机物排出的脱脂过程。结果表明:在低温段(RT～300℃左右),埋粉性质对脱脂速率和坯体质量影响显著,而高温段有机物的排除主要以裂解形式,脱脂气氛和压力起着重要作用;对于尺寸较大,形状复杂的陶瓷注射坯体在氮气中加压脱脂更为有利。     

Porous SiC/SiCN composite ceramics fabricated by foaming and reaction sintering

Porous SiC/SiCN composite ceramics with heterogeneous pore structure and rod-like SiCN grains were fabricated by foaming and reaction sintering. The mixture slurry containing SiC and silicon as raw materials, cornstarch as binder, Y₂O₃ as sintering additive and an electrosteric dispersant was stirred with foams derived from pre-foaming using foaming agent. The casted green body was sintered at 1650 °C under nitrogen atmosphere. The results demonstrated that the porous SiC/SiCN ceramics exhibited hierarchical vias ranging from 1 μm to 1 mm and the rod-like crystalline SiCN grains generated in the SiC matrix.     

反应结合氧化铝陶瓷制备新工艺

本文评述了反应结合氧化铝陶瓷的制备工艺原理,配料组成,研磨与原料细度,成形压力和升温速率等对陶瓷性能的影响。介绍了几种反应结合氧化铝陶瓷制造实例。