Microstructure evolution and phase transformation of TiB2/SiC/B4C composites synthesized from Ti‐SiC‐B4C ternary system

Bulk TiB₂/SiC/B₄C composites have been synthesized from Ti‐SiC‐B₄C ternary system with different Ti weight percentages via reactive hot pressing at 1800°C under an applied pressure of 30 MPa for 1.5 h. By Ti amount increasing, the flexural strength curve exhibited an “M‐like” tendency reaching the maximum value of 512.36 MPa for 30 wt.% Ti. Microstructural evolution of the composites from conterminously large matrix grains to finely clear‐edged particles was observed by scanning electron microscopy. The phase transformation and element diffusion were analyzed by XRD and Energy Disperse Spectroscopy. A hybrid reinforcing mechanism of fracture and crack deflection is proposed to illustrate the change in flexural strength.     

The effect of microwave heating on the microstructure and the mechanical properties of reaction-bonded boron carbide

Reaction-bonded boron carbide composites were fabricated by both microwave (under Ar/10% H₂) and conventional heating (under vacuum or Ar/10% H₂). Silicon carbide (SiC) formation occurred in all cases and was slightly favored in the case of microwave heating under Ar/H₂. The resulting microstructures were influenced by the heating process and atmosphere; the SiC existed in the form of needles with conventional heating under vacuum. SiC small polygonal grains were present after microwave heating under Ar/H₂. Both the atmosphere and the electromagnetic field influence the SiC morphology. Despite this difference, the hardness and toughness of composites obtained by both heating techniques were similar.     

热压烧结工艺制备SiC/B4C复合材料

以Si粉为烧结助剂,采用真空热压烧结工艺制备了SiC/B4C陶瓷基复合材料.研究了Si的加入和烧结压力对复合材料力学性能的影响.借助X射线衍射、扫描电镜分析了复合材料的物相组成和微观结构.研究结果表明:Si与B4C粉料中的游离碳反应,随后固溶到B4C晶体结构中.当Si质量百分含量为8%时,经18.50℃、60 MPa真空热压烧结的复合材料主晶相为B4.C、SiC,相对密度达到99.8%,断裂韧性和弯曲强度分别达到5.04 MPa·m1/2和354 MPa.复合材料力学性能的提高主要是由于烧结体的高致密度以及断裂方式的转变.     

(SiC,TiB2)/B4C复合材料的微观结构及性能

以B4C与Si3N4和少量SiC,TiC为原料,Al2O3和Y2O3为烧结助剂,烧结温度为1 800～1 880℃,压力为30 MPa的热压条件下制备(SiC,TiB2)/B4C复合材料.用透射电子显微镜、扫描电子显微镜和能谱分析进行显微结构分析.结果表明:在烧结过程中反应生成了SiC,TiB2和少量的BN.复合材料的主晶相之间有长棒状架构弥散相和束状弥散相,在部分B4C晶粒内部出现了内晶结构.结合对复合材料性能的分析表明:新形成相、均匀细晶和棒状结构对提高材料的性能具有重要作用.通过对材料断口形貌和裂纹扩展模式分析认为,复合材料的断裂机制主要为裂纹偏转.     

LiFePO4/C cathode materials synthesized by co-precipitation and microwave heating

LiFePO₄/C cathode materials were synthesized by a combination of co-precipitation and microwave heating using polyethylene glycol (PEG) as a carbon resource and the influence of microwave heating time on the structure and electrochemical performance of the materials was also discussed. The samples were characterized by X-ray diffraction (XRD), TEM, particle-size analysis and constant current charge-discharge experiment. The results show that the LiFePO₄/C heated for 9 min has a pure olive-type phase and excellent electrochemical performance. The initial discharge capacities of this sample are 154.3, 139.7, 123.9 mAh/g at the rates 0.1C, 0.2C, 1C at room temperature, respectively, and after 20 cycles remain 152.3, 134.3, 118.5 mAh/g, respectively. __________ Translated from New Chemical Materials, 2008, 36(2): 21–24 [译自:化工新型材料]     

Flexural modulus of SiC/SiC composites sintered by microwave and conventional heating

To deeply study the variation mechanisms of mechanical properties, flexural modulus of SiC fibers reinforced SiC matrix (SiC/SiC) composites prepared by conventional and microwave heating at 800?°C–1100?°C was discussed in detail. The elastic modulus of fibers and matrix, interface bonding strength and porosity of SiC/SiC composites were considered together to analyze the changing tendencies and differences in their flexural modulus. The elastic modulus of fiber and matrix was determined by nanoindentation technique and interface characteristics applying fiber push-out test. The porosity and microstructure examinations were characterized by mercury intrusion method, X-ray Diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscope (TEM). Moreover, two conflicts between the changing trends of elastic modulus and chemical compositions of composite components were focused and explained. Results indicate that three factors played different roles in the flexural modulus of SiC/SiC composites and residual tensile stress in composite components led to the conflicts between their elastic modulus and chemical compositions.     

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.     

SiC／B复合超细粉末的溶胶—凝胶法合成

以硅溶胶、炭黑和硼酸或硼粉为原料,用溶胶-凝胶法合成了SiC/B复合超细粉末。粉末中硼的含量取决于硼源的种类和用量。硼的引入促进了粉末的昌粒长大并抑制了α-SiC相的生成。     

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.     

LiFePO/C cathode materials synthesized by co-precipitation and microwave heating

LiFePO₄/C cathode materials were synthesized by a combination of co-precipitation and microwave heating using polyethylene glycol (PEG) as a carbon resource and the influence of microwave heating time on the structure and electrochemical performance of the materials was also discussed. The samples were characterized by X-ray diffraction (XRD), TEM, particle-size analysis and constant current charge-discharge experiment. The results show that the LiFePO₄/C heated for 9 min has a pure olive-type phase and excellent electrochemical performance. The initial discharge capacities of this sample are 154.3, 139.7, 123.9 mAh/g at the rates 0.1C, 0.2C, 1C at room temperature, respectively, and after 20 cycles remain 152.3, 134.3, 118.5 mAh/g, respectively.     

Microstructure and mechanical properties of B4C–TiB2–SiC composites toughened by composite structural toughening phases

B₄C–TiB₂–SiC composites toughened by composite structural toughening phases, which are the units of (TiB₂–SiC) composite, were fabricated through reactive hot pressing with B₄C, TiC, and Si as raw materials. The units of (TiB₂–SiC) composite with the size of 10‐20 μm are composed of interlocking TiB₂ and SiC with the size of 1‐5 μm. The addition of TiC and Si can effectively promote the sintering of B₄C ceramics. The relative densities of all the B₄C composites with different contents of TiB₂ and SiC are close to completely dense (98.9%‐99.4%), thereby resulting in superior hardness (33.1‐36.2 GPa). With the increase in the content of TiB₂ and SiC, the already improved fracture toughness of the B₄C composite continuously increases (5.3‐6.5 MPa·m^1/2), but the flexure strength initially increases and then decreases. When cracks cross the units of the (TiB₂–SiC) composite, the cracks deflect along the interior boundary of TiB₂ and SiC inside the units. As the crack growth path is lengthened, the crack propagation direction is changed, thereby consuming more crack extension energy. The cumulative contributions improve the fracture toughness of the B₄C composite. Therefore, the composite structural toughening units of the (TiB₂–SiC) composite play an important role in reinforcing the fracture toughness of the composites.     

Optimizing the fiber push-out method to evaluate interfacial failure in SiC/BN/SiC ceramic matrix composites

The investigation of several parameters during fiber push-out micromechanical tests on the interfacial shear strength (ISS) of the BN interphase in SiC_f/SiC ceramic matrix composites (CMC) was undertaken to optimize experimental work. The SiC_f/SiC composites—candidate materials for jet engine components—were manufactured with varying fiber types and interlayer thicknesses. Experimental parameters explored included analyzing the effect of sample thickness on the success rate of micromechanical tests, the effect of fiber local environment whether at tow-level (intra-tow variability in ISS) or CMC architecture-level (inter-tow variability), the effect of nanoindenter flat-punch tip size, and the effect of the interphase thickness itself. Over 1000 fiber push-outs were performed and analyzed in this work—with data presented as cumulative distribution functions to compare and contrast samples. It was found that the ISS measured was strongly and statistically influenced by the underlying fiber roughness (interphase adherence), as well as its local fiber environment (e.g., number of nearest neighbors) only if the thickness of the interphase itself surpassed a threshold of 200 nm. Finally for thinner interphases, limited value was added to the CMC as the ISS measured was high and there was no effect from any local environment.     

热压烧结制备高致密度B4C陶瓷及其致密化

以B4C粉末为原料,以酚醛树脂热解碳为烧结助剂,采用真空热压烧结工艺制备出高致密度的B4C陶瓷材料,探讨了酚醛树脂含量和烧结温度对材料致密化的影响,对比分析了纯B4C和掺碳B4C的热压烧结致密化过程.研究显示,烧结温度的升高有利于材料的致密化,酚醛树脂的添加则显著活化了B4C的烧结.实验条件下酚醛树脂的最优添加量为3％（质量分数）,烧结过程中热解碳固溶于B4C晶格,显著加速了其在1600℃至1800℃区间的致密化速率.     

可加工BN/B_4C复相陶瓷的制备与其抗热震性能

采用热压烧结工艺制备了BN/B4C微米复相陶瓷和BN/B4C纳米复相陶瓷。由淬水法测试了单相B4C陶瓷,BN/B4C微米复相陶瓷和BN/B4C纳米复相陶瓷的抗热震性能,用三点弯曲法测试了热震后样品的抗弯强度。结果表明:BN/B4C微米复相陶瓷和BN/B4C纳米复相陶瓷的抗热震性能明显高于单相B4C陶瓷的抗热震性能,而且BN/B4C纳米复相陶瓷的抗热震性能明显高于BN/B4C微米复相陶瓷的抗热震性能。BN/B4C微米复相陶瓷和BN/B4C纳米复相陶瓷具有良好的抗热震性能主要是由于具有较高的抗弯强度和较低的弹性模量;同时BN/B4C复相陶瓷中的BN/B4C弱界面和层状结构的h-BN晶粒能够显著提高复相陶瓷的抗热震性能。     

Preparation of Machinable B4C/BN Composites and Their Oxidation Resistances at High Temperature

采用热压烧结工艺制备单相 B4C 陶瓷、B4C/BN 微米复相陶瓷和 B4C/BN 纳米复相陶瓷。研究了其在 1 000～1 300 ℃的等温氧化性能,通过对氧化后试样表面的物相组成和显微结构的分析,探讨了氧化机理。结果表明：单相 B4C 陶瓷、B4C/BN 微米复相陶瓷和 B4C/BN 纳米复相陶瓷的高温抗氧化性能随氧化温度提高和氧化时间增加而逐渐降低,试样氧化过程中质量损失逐渐明显。对试样在不同氧化温度下得到的氧化曲线进行了线性拟合分析,试样在 1 000 ℃时抗氧化性能较好,但在 1 300 ℃时抗氧化性能较差。氧化后试样表面的物相组成主要为 B4C 相、h-BN 相,以及少量的B2O3 相和 Al4B2O9 或 Al18B4O33 相。氧化后试样表面存在一层厚度约为 100 μm 的氧化层,氧化层中存在许多微孔和少量玻璃相物质。氧化生成的 B2O3挥发是导致试样质量随着氧化温度和氧化时间增加而显著减少的主要原因。     

Synthesis and properties of conductive B4C ceramic composites with TiB2 grain network

High electrical resistance and low fracture toughness of B₄C ceramics are 2 of the primary challenges for further machining of B₄C ceramics. This report illustrates that these 2 challenges can be overcome simultaneously using core‐shell B₄C‐TiB₂&TiC powder composites, which were prepared by molten‐salt method using B₄C (10 ± 0.6 μm) and Ti powders as raw materials without co‐ball milling. Finally, the near completely dense (98%) B₄C‐TiB₂ interlayer ceramic composites were successfully fabricated by subsequent pulsed electric current sintering (PECS). The uniform conductive coating on the surface of B₄C particles improved the mass transport by electro‐migration in PECS and thus enhanced the sinterability of the composites at a comparatively low temperature of 1700°C. The mechanical, electrical and thermal properties of the ceramic composites were investigated. The interconnected conductive TiB₂ phase at the grain boundary of B₄C significantly improved the properties of B₄C‐TiB₂ ceramic composites: in the case of B₄C‐29.8 vol% TiB₂ composite, the fracture toughness of 4.38 MPa·m^1/2, the electrical conductivity of 4.06 × 10⁵ S/m, and a high thermal conductivity of 33 W/mK were achieved.     

Multiple nonlinear regression model of cutting force for C/SiC composites by laser-assisted micromachining

Based on the response surface methodology (RSM), laser-assisted micromachining (LAMM) experiments of carbon fiber reinforced silicon carbide matrix(C/SiC) composites have been carried out to obtain the data of three-direction cutting forces Fx, Fy, Fz, and result-force F in the cutting process. A stepwise regression method is used to screen out the factors that significantly affected the cutting force, and hence a multivariate nonlinear mathematical regression model has been established. Through the analysis of variance and regression analysis, the R2 of the regression model is the cutting force Fx: 0.975, the cutting force Fy: 0.970, the cutting force Fz: 0.972, the resultant force F: 0.987, and the probability p > F-values are all less than 0.001. The model analysis results show that the main effects and interactions of the three factors of laser power, cutting speed, and cutting depth significantly influence the cutting force. The main effect of the most considerable influence on the resultant F is cutting depth, followed by cutting speed and laser power, and the interactive effect is cutting speed and cutting depth. The experimental results show that the model prediction results are in good agreement with the experimental results.     

Thermal conductivity mapping of oxidized SiC/SiC composites by time-domain thermoreflectance with heterodyne detection

Silicon carbide/silicon carbide (SiC/SiC) composites are often used in oxidizing environments at high temperatures. Measurements of the thermal conductance of the oxide layer provide a way to better understand the oxidation process with high spatial resolution. We use time-domain thermoreflectance (TDTR) to map the thermal conductance of the oxide layer and the thermal conductivity of the SiC/SiC composite with a spatial resolution of 3 μm. Heterodyne detection using a 50-kHz-modulated probe beam and a 10-MHz-modulated pump suppresses the coherent pick-up and enables faster data acquisition than what has previously been possible using sequential demodulation. By analyzing the noise of the measured signals, we find that in the limit of small integration time constants or low laser powers, the dominant source of noise is the input noise of the preamplifier. The thermal conductance of the oxide that forms on the fiber region is lower than the oxide on the matrix due to small differences in thickness and thermal conductivity.     

Nanowire-decorated SiC foam from tissue paper and silicon powder by filter-pressing

A facile and scalable method for the preparation of low-density SiC foam from tissue paper and silicon powder is reported. The co-dispersion of pulp-containing tissue paper micro-ribbons and silicon powder is coagulated by adjusting the pH to 3.5. The silicon particles adhere to the tissue paper micro-ribbons during the coagulation. The coagulated co-dispersion on filter-pressing consolidates the silicon particle-decorated tissue paper micro-ribbons and orients them perpendicular to the filter-pressing direction. The filter-pressed body on drying followed by heat treatment at 1600°C in inert atmosphere produces SiC foam. The tissue paper micro-ribbons retain their morphology during carbonization as well as high-temperature reaction with the silicon. The enormous growth of carbon-rich SiC nanowires is observed on the SiC micro-ribbons. The random orientation of SiC micro-ribbons in the X-Y plane with the hairy nanowires on the surface and their stacking in the Z-direction produces a porosity of ~94 vol.% with pore sizes in the range of 0.08 to 20 µm. The SiC foam shows a compressive strength and Young's modulus of 0.22 and 5.5 MPa, respectively. The thermal conductivity decreases from 0.11 to 0.07 W m⁻¹ K⁻¹ when temperature increases from 25°C to 350°C.     

Seeds-induced synthesis of SiC by microwave heating

α-SiC particles were used as heating seeds to prepare SiC from coal minerals with microwave heating method. Coating technique was carried out to prepare composite raw powders in three different methods. Heating temperatures were at 1000?°C, 1050?°C, 1100?°C, 1150?°C, 1200?°C for 10min, respectively. XRD, SEM techniques were carried out to characterize samples. It was found that different distribution between C and α-SiC particles from different mixing method leads to different microwave heating behavior and growth mechanisms. V-V reaction leads to in situ nucleation and grain growth on the surface of α-SiC seeds which contact with C particles. Well-grown β-SiC particulates appear. Hybrid V-V reaction V-L reaction lead to local microwave plasma and diffusion-precipitation with a very thin layer of SiO₂ between raw C particles and α-SiC seeds. Local fine β-SiC whiskers and particulates on the surface of α-SiC seeds co-exist. Primary V-V reaction leads to nucleation and grain growth along reacted C-SiO₂ interface with very thick layer of SiO₂ between raw C and α-SiC seeds. Substantial β-SiC whiskers appear. Transformation from β-SiC to α-SiC on the surface of as-formed whiskers will be enhanced by microwave plasma at high temperature.