Mechanical properties and microstructures of 2D Cf/ZrC–SiC composites using ZrC precursor and polycarbosilane

Two-dimensional C_f/ZrC–SiC composites were fabricated through mold-pressing and polymer infiltration and pyrolysis (PIP) using T700SC plain weave fiber fabrics as reinforcements with ZrC precursor and polycarbosilane. The mechanical properties and microstructures of the composites with 34, 45, and 56% fiber fraction were investigated. All composites showed a typical non-brittle fracture behavior and a large amount of pulled-out fibers were observed on the fracture surface. The bending strength and elastic modulus of the composite with 56 vol% fiber fraction increased up to 582 ± 80 MPa and 167 ± 25 GPa, with increasing fiber fraction. The mass loss and linear recession rate of the composites during the oxy-propane torch test were 0.008 g/s and ?0.003 mm/s, respectively. The formation of a ZrSiO₄ melt on the surface of the composite significantly contributed to the excellent ablative property of the 2D C_f/ZrC–SiC composites.     

Architectural engineering inspired method of preparing Cf/ZrC–SiC with graceful mechanical responses

Inspired by grouting technique in architectural engineering, an innovative method of slurry injection and vacuum impregnation was put forward to introduce nanosized ZrC–SiC ceramics into PyC modified 3-D needle-punched carbon fiber preform homogeneously and continuously, followed by spark plasma sintering to prepare C_f/ZrC–SiC with graceful mechanical responses. The composite possessed improved fracture toughness and work of fracture at 5.37 ± 0.25 MPa∙m^1/2 and 951 ± 12 J/m², 50% and nearly one order of magnitude higher than those of ZrC–SiC composite, respectively, with rivaling flexural strength at 177 ± 8 MPa synchronously. A graceful fracture mode was embodied in an obviously extended yield plateau with increased failure displacement by 300%. This enhancement was attributed to the uniform and continuous combination of ZrC–SiC with carbon fiber preform as well as protection and interface tailoring from PyC coating. The study offered an easy and effective method of preparing 3-D fiber reinforced ceramic matrix composites.     

Effect of PyC interphase thickness on mechanical and ablation properties of 3D Cf/ZrC–SiC composite

Three-dimensional (3D) C_f/ZrC–SiC composites were successfully prepared by the polymer infiltration and pyrolysis (PIP) process using polycarbosilane (PCS) and a novel ZrC precursor. The effects of PyC interphase of different thicknesses on the mechanical and ablation properties were evaluated. The results indicate that the C_f/ZrC–SiC composites without and with a thin PyC interlayer of 0.15 µm possess much poor flexural strength and fracture toughness. The flexural strength grows with the increase of PyC layer thickness from 0.3 to 1.2 µm. However, the strength starts to decrease with the further increase of the PyC coating thickness to 2.2 µm. The highest flexural strength of 272.3±29.0 MPa and fracture toughness of 10.4±0.7 MPa m^1/2 were achieved for the composites with a 1.2 µm thick PyC coating. Moreover, the use of thicker PyC layer deteriorates the ablation properties of the C_f/ZrC–SiC composites slightly and the ZrO₂ scale acts as an anti-ablation component during the testing.     

Cf/SiC复合材料生产工艺研究

Cf／SiC复合材料克服了单一SiC材料韧性低、烧结过程中晶粒长大造成强度下降等缺点，本文就Cf／SiC复合材料的生产工艺进行了综述。     

Co-reinforcing of ZrB2–SiC ceramics with optimized ZrC to Cf ratio

Characteristics of ZrB₂–SiC ultrahigh temperature ceramic matrix composites (UHTCMCs) reinforced with ZrC and carbon fiber (C_f) were investigated in this article. Spark plasma sintering (SPS) process was utilized to fabricate the samples at 1800 °C for 5 min under 30 MPa punch pressure and vacuumed atmosphere. In all samples, the volume ratio of ZrB₂: SiC was equal to 4:1, and the summation of ZrC and C_f reinforcements was 7.5 vol% with different ZrC: C_f ratios. Field emission scanning electron microscopy (FE-SEM), energy dispersive spectroscopy (EDS), densitometry, flexural strength, and hardness measurements were employed for characterization of the prepared samples. Microstructural inspection revealed the formation of SiC sheath around the carbon fibers due to several reactions in the surface SiO₂ layers existed on the SiC particles. Optimal flexural strength (628.4 MPa) and hardness (20.8 GPa) values were achieved for the sample co-reinforced with 6.5 vol% ZrC and 1 vol% C_f, with a relative density of 97.7%.     

Fabrication of Cf/ZrC–SiC composites using Zr–8.8Si alloy by melt infiltration

Cf/ZrC–SiC composites were fabricated by melt infiltration at 1800 °C using Zr–8.8Si alloy and carbon felt preforms. Microstructural analysis showed the formation of both ZrC and SiC phases in the matrix, in which ZrC acted as a main composition of the resulting composites. The results showed that carbon matrix reacted preferentially with Si of Zr–8.8Si alloy, which caused the formation of SiC first and then ZrC. The designed carbon coating by pyrolysis prevented the severe reaction between fibers and the melt. The composites could be more dense and uniform with the bending strength of 53.3 MPa, when preforms had a high open porosity (47.2%) with small size pores (10–40 μm).     

Spark plasma sintering of quadruplet ZrB2–SiC–ZrC–Cf composites

Spark plasma sintering (SPS) route was employed for preparation of quadruplet ZrB₂–SiC–ZrC–C_f ultrahigh temperature ceramic matrix composites (UHTCMC). Zirconium diboride and silicon carbide powders with a constant ZrB₂:SiC volume ratio of 4:1 were selected as the baseline. Mixtures of ZrB₂–SiC were co-reinforced with zirconium carbide (ZrC: 0–10 vol%) and carbon fiber (C_f: 0–5 vol%), taking into account a constant ratio of 2:1 for ZrC:C_f components. The sintered composite samples, processed at 1800 °C for 5 min and 30 MPa punch press under vacuumed atmosphere, were characterized by densitometry, field emission scanning electron microscopy, energy dispersive spectroscopy, X-ray diffractometry as well as mechanical tests such as hardness and flexural strength measurements. The results verified that the composite co-reinforced with 5 vol% ZrC and 2.5 vol% C_f had the optimal characteristics, i.e., it reached a relative density of 99.6%, a hardness of 18 GPa and a flexural strength of 565 MPa.     

热压烧结Cf/SiC复合材料的力学性能

以ＡｌＮ－Ｙ２Ｏ３为烧结助剂体系,采用先驱体转化－热压法制备出了Ｃｆ／ＳｉＣ复合材料。研究了烧结助剂及其用量和烧结温度对复合材料力学性能的影响。结果表明,由于ＡｌＮ－ＳｉＣ的固溶和液相烧结的作用;烧结温度为１８５０℃时,烧结助剂用量较少的复合材料具有很好的断裂韧性。随着烧结助剂用量的增加,虽然复合材料的抗弯强度不断提高,但由于晶界相和ＡｌＮ－ＳｉＣ固溶体量的增加,使纤维与基体的结合过程,从而导致纤     

Mechanical behaviour of carbon fibre reinforced TaC/SiC and ZrC/SiC composites up to 2100°C

The microstructure and elevated temperature mechanical properties of continuous carbon fibre reinforced ZrC and TaC composites were investigated. Silicon carbide was added to both compositions to aid sintering during hot pressing. Fibres were homogeneously distributed and no fibre degradation was observed at the interface with the ceramic matrix even after testing at 2100 °C. The flexural strength increased from 260 to 300 MPa at room temperature to ∼450 MPa at 1500 °C, which was attributed to stress relaxation. At 1800 °C, the strength decreased to ∼410 MPa for both samples. At 2100 °C plastic deformation resulted in lower strength at the proportional limit (210–320 MPa), but relatively high ultimate strength (370–440 MPa). The sample containing ZrC had a lower ultimate strength, but higher failure strain at 2100 °C due to the weak fibre/matrix interface that resulted in fibre-dominated composite behaviour.     

单向Cf/SiC复合材料的弯曲疲劳性能

对单向Cf/SiC复合材料进行了三点弯曲疲劳性能测试,得到了复合材料的应力－寿命曲线（S－N曲线）,并对其进行线性拟合,得到疲劳最大应力与复合材料疲劳寿命的关系;考察了疲劳过程中刚度下降和疲劳裂纹产生情况。结果表明在疲劳过程中复合材料的弯曲模量有3个变化阶段：首先在疲劳加载初期,弯曲模量的下降速度及幅度都较大;其次在弯曲模量下降到原始弯曲模量的85％（133GPa)后,其变化方式没有明显的规律可循,有时甚至可能上升;最后复合材料发生疲劳断裂时,模量将发生突变。显微结构分析表明：基体横向裂纹群的产生是疲劳断裂的独有特征。它的产生是由于基体SiC的断裂应变小于碳纤维的断裂应变,基体首先开裂并导致应力重新分布的结果。     

纤维类型对Cf/SiC复合材料力学性能的影响

本工作以AIN和Y2O3为烧结助剂,采用先驱体转化－热压烧结的方法制备出了Cf/SiC复合材料,研究了纤维类型影响复合材料力学性能的本质原因,由于T300纤维的制备温度明显低于M40JB纤维的制备温度,因此,与M40JB纤维相比,T300纤维的石墨化程度较低且含有较多的杂质,从而导致T300纤维表面的活性强,而M40JB纤维表面的活性较弱,正是这种结构和成分的差别,使T300纤维与基体的结合较强,而M40JB纤维与基体的结合较弱,因此以T300纤维为增强的复合材料呈现脆性断裂,而以M40JB纤维为增强相的复合材料则呈现韧性断裂,谈复合材料具有较好的力学性能。     

Cf/SiC复合材料的制备及性能的研究

采用料浆渗积-有机前躯体裂解工艺制备碳纤维增强碳化硅陶瓷基复合材料.制备材料的抗弯强度达283 MPa,断裂韧性达12.1 MPa·m1/2.     

三维编织Cf/SiC复合材料的拉伸破坏行为

通过三维编织碳纤维(carbon fiber，Cf)／SiC复合材料样品单向拉伸以及单向拉伸加卸载实验．结合样品断口观察．从宏观上分析了三维编织Cf／SiC复合材料单向拉伸时的力学响应，为进一步描述三维编织Cf／SiC复合材料力学行为奠定了实验基础。实验结果表明：三维编织Cf／SiC复合材料单向拉伸时，卸载模量衰减与应力呈线性关系，残余应变的增加与应力呈二次函数关系。微裂纹主要在编织节点处萌生，沿纤维束界面扩展，最终在编织节点处汇合，导致样品发生破坏。     

Cf/ZrB2–ZrC–SiC超高温陶瓷基复合材料的设计、制备及性能EI北大核心CSCD

提出了溶胶-凝胶孔道构建-反应熔渗制备新方法,首先通过溶胶凝胶方法在纤维预制体中引入B4C-C多孔体,获得Cf/B4C-C多孔预成型体结构;在此基础上,结合反应熔渗Si-Zr合金,获得Cf/ZrB2-ZrC-SiC超高温陶瓷基复合材料。研究了Cf/B4C-C多孔预成型体结构对RMI过程和材料性能的影响,并揭示了孔隙结构对基体分布和界面损伤及复合材料性能的影响规律。结果表明:通过灵活调控Cf/B4C-C孔隙结构可实现复合材料中ZrB2-ZrC-SiC基体分布改善和(PyC-SiC)2界面损伤缓解,大幅提升材料性能。当预成型体孔隙结构为25.9%和58.0μm时,制备的Cf/ZrB2-ZrC-SiC复合材料基体可均匀分布于纤维束间和束内,同时纤维能得到良好的保护,材料表现出最优的力学性能(抗弯强度231 MPa)。     

Effects of high-temperature annealing on the microstructure and properties of C/SiC–ZrC composites

C/SiC–ZrC composites were prepared by a combining slurry process with precursor infiltration and pyrolysis, and then annealed from 1200 °C to 1800 °C. With rising annealing temperature, their mass loss rate increased, and the flexural strength and modulus decreased from 227.9 MPa to 41.3 MPa and from 35.3 GPa to 22.7 GPa, respectively. High-temperature annealing, which elevated thermal stress and strengthened interface bonding, was harmful to the flexural properties. However, it improved the ablation properties by increasing the crystallization degree of SiC matrix. The mass loss rate and linear recession rate decreased with increasing annealing temperature and those of the samples annealed at 1800 °C were 0.0074 g/s and 0.0011 mm/s respectively. Taking mechanical and ablation properties into consideration simultaneously, the optimum annealing temperature was 1600 °C.     

Densification,microstructure, and mechanical properties of ZrC–SiC ceramics

ZrC–SiC ceramics were fabricated by high-energy ball milling and reactive hot pressing of ZrH₂, carbon black, and varying amounts of SiC. The ceramics were composed of nominally pure ZrC containing 0 to 30 vol% SiC particles. The relative density increased as SiC content increased, from 96.8% for nominally pure ZrC to 99.3% for ZrC-30 vol% SiC. As SiC content increased from 0 to 30 vol%, Young's modulus increased from 404 ± 11 to 420 ± 9 GPa and Vickers hardness increased from 18.5 ± 0.7 to 23.0 ± 0.5 GPa due to a combination of the higher relative density of ceramics with higher SiC content and the higher Young's modulus and hardness of SiC compared to ZrC. Flexure strength was 308 ± 11 MPa for pure ZrC, but increased to 576 ± 49 MPa for a SiC content of 30 vol%. Fracture toughness was 2.3 ± 0.2 MPa·m^1/2 for pure ZrC and increased to about 3.0 ± 0.1 MPa·m^1/2 for compositions containing SiC additions. The combination of high-energy ball milling and reactive hot pressing was able to produce ZrC–SiC ceramics with sub-micron grain sizes and high relative densities with higher strengths than previously reported for similar materials.     

High shear strength and ductile ZrC–SiC/austenitic stainless steel joints bonded with Ti/Ni foam interlayer

A transient-liquid-phase (TLP) diffusion bonding method was employed to join ZrC–SiC ceramic and austenitic stainless steel by using Ti foil and various density Ni foam as interlayer. The Ti–Ni TLP contributed to a firm bonding between ceramic and foam interlayer while avoiding liquid infiltration in foam structure. The influence of holding time on the microstructure of the TLP reaction layer was investigated. The shear tests showed the joints with foam interlayer exhibited ductile failure mode and improved fracture work in comparison with the one with dense Ni interlayer. A maximum shear strength of 117.2 MPa was reached when the relative density of Ni foam was 0.57. The fracture behaviors of the joints during shear test were in-situ observed.     

热压辅助先驱体裂解制备Cf/SiC复合材料的研究

以聚碳硅烷为先驱体 ,采用先驱体转化法制备三维编织Cf SiC复合材料。研究发现 ,第一次裂解时采用热压辅助可以明显提高材料的致密度和力学性能。第一次在 160 0℃、10MP的条件下热压裂解 60min ,后续真空浸渍—常压裂解处理五个周期所制得的材料具有较高的力学性能 ,其弯曲强度和断裂韧性分别为 5 64MPa、16MPa·m1 2 。讨论了制备工艺对材料结构和性能的影响     

Polymeric liquid precursor of multi-component ZrC–SiC ceramic

Polymeric liquid ceramic precursors for the production of multi-component ZrC–SiC ceramics were prepared by reactive blending of polyzirconoxanesal, phenylacetylene-terminated polysilane and bisphenol-A type benzoxazine. The polymeric liquid precursors of ZrC–SiC ceramic have the processing capability of Precursor-Infiltration-and-Pyrolysis technique in ceramic composites fabrication. The thermal cure reactions included by the catalytic polymerisation of ethynyl groups, the ring opening polymerisation of benzoxazine rings, and the condensation of zirconate with phenolic hydroxyl and Si–H at 200–350°C. The monolithic ceramics were formed upon pyrolysis at 1000, 1200 and 1600°C in a yield of 65, 62 and 40%, respectively. X-ray diffraction and SEM–EDS results revealed that almost pure, elemental, uniformly distributed ZrC–SiC multi-component ceramic monolith was obtained through pyrolysis at 1600°C via carbothermal reduction of ZrO₂.     

Cf/SiC复合材料抗氧化涂层的制备、性能与保护机理

用化学气相沉积法(chemical vapor deposit,CVD)在碳纤维增强碳化硅复合材料(carbon fiber reinforced silicon carbide composites,Cf／SiC)表面制备了CVD—SiC粘接层、自愈合功能层和CVD—SiC耐冲蚀层组成的3层涂层体系,并进行了氧化实验。结果表明：单层CVD—SiC涂层保护试样的氧化质量损失速率比无涂层试样的明显降低,含有自愈合层的3层涂层保护试样比单层CVD—SiC保护试样的氧化质量损失速率又有明显降低。3层涂层保护的试样800～1300℃的氧化质量损失率非常小,氧化288h后仍能保持较高的弯曲强度。通过扫描电镜观察到自愈合层的玻璃态物质进入涂层裂纹中,有效地填充裂纹并阻挡氧的通过。同时,因涂层不均产生的孔洞或玻璃态物质流失后产生的涂层裂纹等缺陷会导致其自愈合功能的失效,使Cf／SiC复合材料不均匀氧化。