Improvement of toughness of reaction bonded silicon carbide composites reinforced by surface-modified SiC whiskers

To improve the reliability, especially the toughness, of the reaction bonded silicon carbide (RBSC) ceramics, silicon carbide whiskers coated with pyrolytic carbon layer (PyC-SiC_w) by chemical vapor deposition (CVD) were introduced into the RBSC ceramics to fabricate the SiC_w/RBSC composites in this study. The microstructures and properties of the PyC-SiC_w/RBSC composites under different mass fraction of nano carbon black and PyC-SiC_w were investigated methodically. As a result, a bending strength of 550 MPa was achieved for the composites with 25 wt% nano carbon black, and the residual silicon decreased to 11.01 vol% from 26.58 vol% compared with the composite of 15 vol% nano carbon black. The fracture toughness of the composites reinforced with 10 wt% PyC-SiC_w, reached a high value of 5.28 MPa m^1/2, which increased by 39% compared to the RBSC composites with 10 wt% SiC_w. The residual Si in the composites deceased below to 7 vol%, resulting from the combined actively reaction of nano carbon black and PyC with more Si. SEM and TEM results illustrated that the SiC_w were protected by PyC coating. A thin SiC layer formed of outer surface of whiskers can provide a suitable whisker-matrix interface, which is in favor of crack deflection, SiC_w bridging and pullout to improve the bending strength and toughness of the SiC_w/RBSC composites.     

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。     

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.     

Shear strength enhancement of SiC-coated 3D C/SiC composite joints with a Ni-Ti-Nb multi-interlayer by interfacial microstructure tailoring

SiC-coated three-dimensional (3D) C/SiC composites were successfully joined with a Ni-Ti-Nb multi-interlayer by spark plasma sintering (SPS). The interfacial microstructure, phase evolution, and mechanical properties of the as-prepared joints were investigated. A sawtooth-like interfacial structure was generated as a result of the non-uniform dissolution behavior of SiC during the joining process. This interfacial structure substantially enhanced the interfacial bonding strength of the composites. The evolution of the interfacial microstructure was correlated with the mechanical properties of the joints. Finally, a reliable joint free of microdefects with a shear strength of 108 ± 5 MPa was obtained by precise tailoring of the interfacial microstructure.     

Combination of direct ink writing and reaction bonded for rapid fabrication of SiCw/SiC composites

Silicon carbide ceramic matrix composites are widely used in aerospace field due to their advantages of high temperature resistance, high strength and corrosion resistance. However, its application is greatly limited because of the difficulty in preparing complex shape structures by traditional machining methods. Here, a new strategy for preparing SiC_w/SiC complex structure by combining direct ink writing with reaction bonding is proposed. A water-based slurry consisting of silicon carbide, carbon powder and silicon carbide whisker was developed. The influence laws of C content and SiC_w content in slurry on sintering properties of direct-written samples were studied. The reaction bonding mechanism and whisker reinforcing and toughening mechanism were analyzed by means of microstructure and phase composition. The results show that the slurry exhibits shear thinning behavior with stress yield point, and its flow behavior and plasticity meet the requirements of direct writing. When the carbon content is 6.4 wt%, the maximum flexural strength is 239.3 MPa. When 15 wt% SiC_w was added, the flexural strength of the composite reached 301.6 MPa, and when 20 wt% SiC_w was added, the fracture toughness of the composite reached 4.02 MPa m^1/2, which was increased by 26% and 18% compared with single-phase SiC, respectively. The reinforcing and toughening mechanisms of the whiskers mainly include whisker pullout, crack deflection and whisker bridging. After direct ink writing and reaction bonded, the whole process shows good near net forming ability. 3D printed SiC_w/SiC composites have great application prospects in aerospace field.     

Synthesis of SiC Whiskers from Silicon Nitride in Argon Atmosphere

SiC whiskers were synthesized by carbothermal reduction of silicon nitride. α-Si3N4 and β-Si3N4 powders were used as silicon sources, and graphite, active carbon and black carbon as carbon sources, as well as boron oxide as catalyst. The synthesized SiC whiskers were characterized by XRD and SEM. The results showed that the synthesizing temperature should be above 1 716 K; the decomposition of Si3N4 was the limited step in the synthesis of SiC whiskers; and catalyst not only offered the liquid condition, bu...     

Effect of crystallisation on the reaction kinetics of nickel reduction by hydrogen

The reaction kinetics of precipitation from aqueous solution is not only a function of the concentration of reagents but also depends on the properties of the solid particles formed in the process. These property changes arise from the increasing influence of surface properties in comparison to volumetric bulk-properties as the particle size decreases. The ratio α of the active surface area to the actual surface area of the particles in the system is used in this work to evaluate the reaction activity of the particles. The investigation of the reaction kinetics of nickel reduction without sampling during the process of the reaction was successfully carried out in the experiment. The overall kinetics of nickel reduction have been suggested, where the constants relate to the main processes of nickel precipitation from the solution. The significant agglomeration reduces the deactivation of the nickel particles in the precipitation process, while breakage and crystal growth decrease the activation. The activations of dry and wet seeds are insignificantly different.     

Enhancement of the microwave absorption properties of PyC-SiCf/SiC composites by electrophoretic deposition of SiC nanowires on SiC fibers

The employment of coating technique on the silicon carbide fibers plays a pivotal role in preparing SiC fiber-reinforced SiC composites (SiC_f/SiC) toward electromagnetic wave absorption applications. In this work, SiC nanowires (SiCNWs) are successfully deposited onto the pyrolytic carbon (PyC) coated SiC fibers by an electrophoretic deposition method, and subsequently densified by chemical vapor infiltration to obtain SiCNWs/PyC-SiC_f/SiC composites. The results reveal that the introduction of SiCNWs could markedly enhance the microwave absorption properties of PyC-SiC_f/SiC composites. Owing to the increasing of SiCNWs loading, the minimum reflection loss of composites raises up to −58.5 dB in the SiCNWs/PyC-SiC_f/SiC composites with an effective absorption bandwidth (reflection loss ≤ −10 dB) of 6.13 GHz. The remarkable enhancement of electromagnetic wave absorption performances is mainly attributed to the improved dielectric loss ability, impedance matching and multiple reflections. This work provides a novel strategy in preparing SiC_f/SiC composites with excellent electromagnetic wave absorption properties.     

Advanced technology for fabrication of reaction-bonded SiC with controlled composition and properties

An advanced fabrication technology of reaction-bonded SiC is developed, which includes the preparation of a C/SiC preform by repeated cycles of phenolic resin impregnation and pyrolysis, followed by infiltration with silicon melt. The use of different number of impregnation stages provides control of carbon content in the preform and the corresponding SiC content in final ceramics. The effect of the impregnation number on the preform characteristics and ceramics composition, thermal and mechanical properties are investigated comprehensively. With an increase of impregnation number up to four, SiC fraction in the ceramics enlarges to 93 vol%, thermal conductivity and Young’s modulus increase to 186 W/(m?K) and 427 GPa respectively, which are superior to most reaction-bonded SiC. Flexural strength (225 MPa) and thermal expansion coefficient (2?10^?6 K^-1) are not dependent on the impregnation number. The obtained results provide an opportunity to design and fabricate reaction-bonded SiC ceramics with a given set of properties.     

Interfacial zone surrounding the diamond in reaction bonded diamond/SiC composites: Interphase structure and formation mechanism

Diamond/SiC composites have attracted considerable research interests due to their outstanding properties sought for a wide range of applications. Among a few techniques used for the fabrication of diamond/SiC composites, molten Si infiltration is an approach highly favored due to its cost-effectiveness and process flexibility. This study critically evaluated the interfacial zone surrounding the diamond in a reaction bonded (RB) diamond/SiC composite. XRD suggests that the composite consists of diamond, α-SiC, β-SiC, Si, and graphite. TEM reveals that a thin layer of graphite surrounds the diamond grain and it appears to form through a process of diamond graphitization and amorphous carbon transformation during the fabrication. In addition, a carbon dissolution and saturation process is proposed as a predominant mechanism for the formation of nano-crystalline SiC near the interface as well as the defects inside the SiC grits. A minor Al₄C₃ phase is occasionally detected near the interface region.     

SiC超细粉的化学分析(Ⅰ)──示差分光光度法测定SiC超细粉末中的总硅量

在碳化硅的总硅量测定中，样品的分解是其关键之一。本文采用NaOH和Na2O2（2：1）的混合溶剂，在银坩埚中于700℃下熔融20分钟来分解SiC超细粉末。由于SiC中的总硅量高达70％左右，所以用500μg／100ml的标准SiO2溶液作为参比溶液，以硅钼蓝示差分光光度法测定SiC超细粉末中的总硅量。本方法的最大吸收波长λ=800nm，在该波长处的表观摩尔吸光系数ε=2．51×104。     

Ultra-high creep resistant SiC ceramics prepared by rapid hot pressing

The high-temperature compression creep of additive-free β/α silicon carbide ceramics fabricated by rapid hot pressing (RHP) was investigated. The creep tests were accomplished in vacuum at temperature range 1500 °C–1750 °C and compressive loads of 200 MPa to 400 MPa. Under investigated condition the RHP ceramics possessed the lowest creep rate reported in the literature. The observed strain rates changed from 2.5 × 10^?9 s^?1 at 1500 °C and a lowest load of 275 MPa to 1.05 × 10^?7 s^?1 at 1750 °C and a highest load of 400 MPa. The average creep activation energy and the stress exponent remain essentially constant along the whole range of investigated parameters and were 315 ± 20 kJ?mol^?1, and 2.22 ± 0.17, respectively. The suggested creep mechanism involves GB sliding accommodated by GB diffusion and β?α SiC phase transformation.     

Tribological study of Ni matrix composite coatings containing nano and micro SiC particles

Nickel matrix composite coatings containing micro and nano-sized SiC particles were prepared from an additive-free Watts’ type solution under direct and pulse current conditions, in order to study the correlation between SiC particles embedding and the tribological behaviour of deposits. The wear properties of Ni/SiC composite coatings were shown to depend on the type of current, the size of the embedded particles, the weight fraction of codeposited particles, the microstructural modifications induced by codepositing SiC particles and the plating conditions. It was proved that the presence of SiC particles influences the adsorption-desorption phenomena occurring at the metal-catholyte interface during electrocrystallization and, synergically with the plating conditions, modifies the deposits microstructure thus affecting wear properties.     

Direct laser sintering of reaction bonded silicon carbide with low residual silicon content

Additive manufacturing (AM) techniques are promising manufacturing methods for the production of complex parts in small series. In this work, laser sintering (LS) was used to fabricate reaction bonded silicon carbide (RBSC) parts. First, silicon carbide (SiC) and silicon (Si) powders were mixed in order to obtain a homogeneous powder. This powder mixture was subsequently laser sintered, where the Si melts and re-solidifies to bind the primary SiC particles. Afterwards, these SiSiC preforms were impregnated with a phenolic resin. This phenolic resin was pyrolysed yielding porous carbon, which was transformed into secondary reaction formed SiC when the preforms were infiltrated with molten silicon in the final step. This resulted in fully dense RBSC parts with up to 84?vol% SiC. The optimized SiSiC combined a Vickers hardness of 2045?HV, an electrical conductivity of 5.3?×?10³?S/m, a Young's modulus of 285?GPa and a 4-point bending strength of 162?MPa.     

Room temperature impact-induced deposition of pure SiC coating layer by vacuum kinetic spraying

This study successfully manufactured a thick, pure SiC coating layer with a thickness of 83.3 μm using vacuum kinetic spray process and investigated the unique impact-induced deposition behavior at room temperature. The simulated result of SiC particle collides with the metallic matrix, or predeposited SiC layer confirmed that particle shock pressure could increase up to the maximum pressure of 27.2 GPa. Moreover, the particles were predicted to fracture to submicrometer size after plastic deformation and those characteristics also matched microstructural observations made with a transmission electron microscope. The SiC coating layer formed an unexpected microstructure composed of bent lattices, fractured submicrometer-sized particles, and amorphous layers. Correlating the microstructure and simulation results suggested that a pure SiC coating layer could be formed using mechanical anchoring and amorphous bonding at room temperature.     

Electrochemical preparation and characterization of Ni/SiC compositionally graded multilayered coatings

In our study, Ni/SiC functionally graded coatings have been obtained by electrochemical deposition of silicon carbide microparticles (mean diameter 2 μm) from nickel Watts baths with different concentrations of SiC particles in solution. The SiC particles were characterized by electroacustics technique in order to determine zeta potential and particle size. Moreover, the effect of the concentration of SiC particles in solution on the amount of SiC deposited in the nickel layer was investigated. Further experiments showed that the degree of particle incorporation provoked changes in the texture of the nickel matrix. The characterization of the coatings proved that the Ni/SiC graded composite coatings were bright and compact, presented good adhesion and improved the hardness and wear resistance of pure nickel electrodeposits.     

Effect of technological parameters on densification of reaction bonded Si/SiC ceramics

Si/SiC composite ceramics was produced by reaction sintering method in process of molten silicon infiltration into porous C/SiC preform fabricated by powder injection molding followed by impregnation with phenolic resin and carbonization. To optimize the ceramics densification process, effect of slurry composition, debinding conditions and the key parameters of all technological stages on the Si/SiC composite characteristics was studied. At the stage of molding the value of solid loading 87.5% was achieved using bimodal SiC powder and paraffin-based binder. It was found that the optimal conditions of fast thermal debinding correspond to the heating rate of 10?°C/min in air. The porous C/SiC ceramic preform carbonized at 1200?°C contained 4% of pyrolytic carbon and ～25% of open pores. The bulk density of Si/SiC ceramics reached 3.04?g/cm³, silicon carbide content was 83–85?wt.% and residual porosity did not exceed 2%.     

旋风炉SiC质炉衬损毁机理研究

热电厂旋风炉ＳｉＣ炉衬，由于受液态渣的侵蚀，在短期内损毁。本文研究了液态渣的物相、渣村的相互关系，认为ＳｉＣ炉衬的侵蚀机理：一方面由于增钙，液态渣变稀，渣中多钙、铝而少硅，对炉衬的渗透力强，能夺取ＳｉＣ中的硅，造成化学侵蚀；另一方面是由于旋风燃烧的作用，液态渣对炉衬的机械侵蚀。该研究结果为研制新炉衬提供了依据。     

Effect of Carbon Containing Materials on Pure Carbon Reaction-bonded SiC

Petroleum coke, graphite, gas carbon and lower sulfur carbon black were used to prepare reaction-bonded silicon carbide. The influences of different carbon containing materials on properties of carbonaceous precursors, sintering process, and microstructure of the prepared SiC were researched. The results show that ： （ 1 ） With the density of carbon containing materials increasing, the porosity of carbonaceous precursors decreases and the infiltrating process of liquid silicon is more difficult. （2） The reaction between carbon containing materials and liquid silicon, the volume effect is more obvious with the density of carbon containing materials increasing. （3） As the carbon containing materials density decreasing, residual carbon in reaction bonded SiC also decreases.