Microstructure and Oxidation Behavior of ZrB_(2)-SiC Ceramics Fabricated by Tape Casting and Reactive Melt Infiltration

ZrB_(2)-based ceramics typically necessitate high temperature and pressure for sintering,whereas ZrB_(2)-SiC ceramics can be fabricated at 1500℃using the process of reactive melt infiltration with Si.In comparison to the conventional preparation method,reactive synthesis allows for the more facile production of ultra-high temperature ceramics with fine particle size and homogeneous composition.In this work,ZrSi_(2),B4C,and C were used as raw materials to prepare ZrB_(2)-SiC via combination of tape casting and reactive melt infiltration herein referred to as ZBC ceramics.Control sample of ZrB_(2)-SiC was also prepared using ZrB_(2) and SiC as raw materials through an identical process designated as ZS ceramics.Microscopic analysis of both ceramic groups revealed smaller and more uniformly distributed particles of the ZrB_(2) phase in ZBC ceramics compared to the larger particles in ZS ceramics.Both sets of ceramics underwent cyclic oxidation testing in the air at 1600℃for a cumulative duration of 5 cycles,each cycle lasting 2 h.Analysis of the oxidation behavior showed that both ZBC ceramics and ZS ceramics developed a glassy SiO_(2)-ZrO_(2) oxide layer on their surfaces during the oxidation.This layer severed as a barrier against oxygen.In ZBC ceramics,ZrO_(2) is finely distributed in SiO_(2),whereas in ZS ceramics,larger ZrO_(2) particles coexist with glassy SiO_(2).The surface oxide layer of ZBC ceramics maintains a dense structure because the well-dispersed ZrO_(2) increases the viscosity of glassy SiO_(2),preventing its crystallization during the cooling.Conversely,some SiO_(2) in the oxide layer of ZS ceramics may crystallize and form a eutectic with ZrO_(2),leading to the formation of ZrSiO_(4).This leads to cracking of the oxide layer due to differences in thermal expansion coefficients,weakening its barrier effect.An analysis of the oxidation resistance shows that ZBC ceramics exhibit less increase in oxide layer thickness and mass compared to ZS ceramics,suggesting superior oxidation resistance of ZBC ceramics.

Ablation behaviour and mechanical performance of ZrB_(2)-ZrC-SiC modified carbon/carbon composites prepared by vacuum infiltration combined with reactive melt infiltration

The development of advanced aircraft relies on high performance thermal-structural materials,and carbon/carbon com-posites(C/C)composited with ultrahigh-temperature ceramics are ideal candidates.However,the traditional routes of compositing are either inefficient and expensive or lead to a non-uniform distribution of ceramics in the matrix.Compared with the traditional C/C-ZrC-SiC composites prepared by the reactive melt infiltration of ZrSi_(2),C/C-ZrB_(2)-ZrC-SiC composites prepared by the vacuum infiltration of ZrB_(2) combined with reactive melt infiltration have the higher content and more uniform distribution of the introduced ceramic phases.The mass and linear ablation rates of the C/C-ZrB_(2)-ZrC-SiC composites were respectively 68.9%and 29.7%lower than those of C/C-ZrC-SiC composites prepared by reactive melt infiltration.The ablation performance was improved because the volatilization of B_(2)O_(3),removes some of the heat,and the more uniformly distributed ZrO_(2),that helps produce a ZrO2-SiO2 continu-ous protective layer,hinders oxygen infiltration and decreases ablation.

Ti_3AlC_2-Al_2O_3-TiAl_3 composite fabricated by reactive melt infiltration

Porous preforms were fabricated by cold-pressing process using powder mixture of TiC,TiO2 and dextrin.After pyrolysis and sintering,Al melt was infiltrated into the porous preforms,leading to the formation of Ti3AlC2-Al2O3-TiAl3 composite.Effects of cold-pressing pressure of preforms on microstructures and mechanical properties of the composites were studied.Synthesis mechanism and toughening mechanism of composite were also analyzed.The results shows that TiO2 is reduced into Ti2O3 by carbon,the decomposition product of dextrin,which causes the spontaneous infiltration of Al melt into TiC/Ti2O3 preform.Then, Ti3AlC2-Al2O3-TiAl3 composite is in-situ formed from the simultaneous reaction of Al melt with TiC and Ti2O3.With the increase of cold-pressing pressure from 10 MPa to 40 MPa,the pore size distribution of the preforms becomes increasingly uniform after pre-sintering,which results in the reduction of defects,and the decrease of property discrepancy of composites.Nano-laminated Ti3AlC2 grains and Al2O3 particles make the fracture toughness of TiAl3 increase remarkably by various toughening mechanisms including stress-induced microcrack,crack deflection and crack bridging.

Theoretical study of reactive melt infiltration to fabricate Co-Si/C composites

Cobalt-silicon based carbon composites(Co–Si/C)have established a noteworthy consideration in recent years as a replacement for conventional materials in the automotive and aerospace industries.To achieve the composite,a reactive melt infiltration process(RMI)is used,in which a melt impregnates a porous preform by capillary force.This method promises a high-volume fraction of reinforcement and can be steered in such a way to get the good“near-net”shaped components.A mathematical model is developed using reaction-formed Co–Si alloy/C composite as a prototype system for this process.The wetting behavior and contact angle are discussed;surface tension and viscosity are calculated by Wang’s and Egry’s equations,respectively.Pore radii of 5μm and 10μm are set as a reference on highly oriented pyrolytic graphite.The graphs are plotted using the model,to study some aspects of the infiltration dynamics.This highlights the possible connections among the various processes.In this attempt,the Co–Si(62.5 at.%silicon)alloy’s maximum infiltration at 5μm and 10μm radii are found as 0.05668 m at 125 s and 0.22674 m at 250 s,respectively.

Particle erosion of C/C-SiC composites with different Al addition in reactive melt infiltrated Si

Particle erosion of C/C-SiC composites prepared by reactive melt infiltration with different Al addition was studied by gas-entrained solid particle impingement test.SEM,EDS and XRD were performed to analyze the composites before and after erosion.The results indicate that a U shape relationship curve presents between the erosion rates and Al content,and the lowest erosion rate occurs at 40 wt%Al.Except for the important influence of compactness,the increasing soft Al mixed with reactive SiC,namely the mixture located between carbon and residual Si also,plays a key role in the erosion of the C/C-SiC composites through crack deflection,plastic deformation and bonding cracked Si.

Microstructure and Mechanical Properties of ZrC_(x)-NbC_(y)-Cu Composites by Reactive Infiltration at 1300℃

ZrC_(x)-NbC_(y)-Cu composites were fabricated by pressure-less reactive infiltration of Zr-Cu binary melts into porous NbC preforms at 1300℃.The effect of Zr content in the infiltrator on microstructure of the as-synthesized composites was studied.Mechanical properties of the composites were reported.A partial displacement of Nb atoms in NbC by Zr atoms from Zr-Cu melt occurs during the reaction between Zr-Cu melt and porous NbC preform.The formation of a core-shell structure suggests the reaction is mainly a dissolutionprecipitation type.NbC dissolves into Zr-Cu melt,from which the(Nb,Zr)C_(z)phase precipitates and grows.With increasing Zr content in the Zr-Cu infiltrator,the reaction is enhanced and the infiltration is easily chocked.ZrC_(x)-NbC_(y)-Cu composite is synthesized using Zr_(14)Cu_(51)infiltrator.The flexural strength and fracture toughness of ZrC_(x)-NbC_(y)-Cu composite reach 637 MPa and 12.7 MPa·m^(1/2),respectively.And the improved toughness is probably attributed to residual Cu phase and plate-like Nb_(x)C_(y)phases.

Microstructure and Mechanical Properties of C/C-ZrC-SiC Composites Fabricated by Reactive Melt Infiltration with Zr,Si Mixed Powders

To meet the increasing demand for advanced materials capable of operation over 2000 ℃ for future thermal protection systems application, C/C-ZrC-SiC composites were fabricated by reactive melt infiltration （RMI） with Zr, Si mixed powders as raw materials. The structural evolution and formation mechanism of the C/C- ZrC-SiC composites were discussed, and the mechanical property of the as-prepared material was investigated by compression test. The results showed that after the RMI process, a special structure with ZrC-SiC multi-coating as outer layer and ZrC-SiC-PyC ceramics as inner matrix was formed. ZrC and SiC rich areas were formed in the composites and on the coating surface due to the formation of Zr-Si intermetallic compounds in the RMI process. Mechanical tests showed that the average compression strength of the C/C-ZrC-SiC composites was 133.86 MPa, and the carbon fibers in the composites were not seriously damaged after the RMI process.

Fabrication and microstructure of ZrB_2–ZrC–SiC coatings on C/C composites by reactive melt infiltration using ZrSi_2 alloy

ZrB_2–ZrC–SiC ternary coatings on C/C composites are investigated by reactive melt infiltration of ZrSi_2 alloy into pre-coatings. Two different pre-coating structures, including porous B_4C–C and dense C/B, are designed by slurry dip and chemical vapor deposition(CVD) process respectively. The coating prepared by reactive melt infiltration(RMI) into B_4C–C presents a flat and smooth surface with a three-layer cross-sectional structure, namely interior SiC transition layer, gradient ZrB_2–ZrC–SiC layer, and ZrB_2–ZrC exterior layer. In comparison, the coating prepared by RMI into C/B shows a more granular surface with a different three-layer cross-sectional structure, interior unreacted B–C pre-coating layer, middle SiC layer, and exterior ZrB_2–ZrC–ZrSi_2 layer. The forming mechanisms of the specific microstructures in two coatings are also investigated and discussed in detail.

CVI-RMI法制备C/SiC复合材料的微观结构与弯曲性能

以T700炭纤维准三维编织针刺整体毡为预制体,在炭纤维表面CVI预沉积热解炭涂层,利用化学气相渗透-反应熔体浸渗法(CVI-RMI)制备C/SiC复合材料,观察材料的微观形貌,并探讨界面对弯曲性能的影响。研究结果表明:利用CVI-RMI联合工艺制备的C/SiC复合材料致密度高,开孔率较小(10%),基体分布均匀;材料弯曲强度达133 MPa,呈逐层破坏机制,表现出良好的假塑性;热解炭涂层与CVI-SiC基体减少了RMI工艺过程对炭纤维的损伤,且热解炭涂层调节了炭纤维与基体之间的界面结合状况,有利于纤维的拔出。

C/C坯体对RMI C/C-SiC复合材料组织的影响

以PAN基炭纤维(Cf)针刺整体毡为预制体,用化学气相渗透(CVI)、浸渍炭化(IC)方法制备了不同炭纤维增强炭基体的多孔C/C坯体,采用反应熔渗(RMI)法制备C/C-SiC复合材料,研究了渗Si前后坯体的密度和组织结构。结果表明:不同C/C坯体反应溶渗硅后复合材料的物相组成为SiC相、C相及单质Si相;密度低的坯体熔融渗硅后密度增加较多;密度的增加与开口孔隙度并不是单调增加的关系,IC处理的坯体开口孔隙度低,但渗硅后复合材料的密度增加较多;IC坯体中分布分散的树脂C易与熔渗Si反应,CVI坯体中的热解C仅表层与熔渗Si反应,在Cf和SiC之间有热解C存在;坯体密度相同时,IC处理的坯体中SiC量较多,单质Si相含量少且分散较好,而CVI坯体中SiC量较少,单质Si相的量较多;制备方法相同时,高密度的C/C坯体,渗硅后C相较多。

SiC_(f)/SiC复合材料的RMI制备方法以及微观结构和性能优化

反应熔体渗透(RMI)是制备高密度陶瓷基复合材料的有效方法之一,而熔体的渗透和复合材料的形成主要取决于预制体的孔隙结构。本研究将硅熔体渗透到具有不同孔隙结构的含碳预制体中,制备了SiC纤维增强SiC基复合材料(SiC_(f)/SiC),并研究了孔隙结构对熔体浸润和SiC_(f)/SiC复合材料的影响。研究结果表明:具有较均匀孔径的预制体可以使熔体浸润更充分,制备的复合材料具有更少的残余孔隙及更优的力学性能。该研究对反应熔渗制备复合材料的孔结构调控具有指导意义。

CVI+RMI快速制备C/C-SiC复合材料的摩擦学性能

为了研究C/C坯体热处理温度对C/C-SiC复合材料微观结构和摩擦性能的影响,以针刺碳毡为预制体,经化学气相渗透法(CVI)制备C/C坯体,然后采用反应熔体浸渗法(RMI)制备C/C-SiC复合材料。结果表明:C/C坯体高温热处理未改变C/C-SiC复合材料的相组成。C/C坯体热处理温度对C/C-SiC复合材料的摩擦磨损性能产生一定的影响。与1 800℃相比,C/C坯体经2 000℃和2 200℃热处理后,C/C-SiC复合材料的摩擦面更易形成致密的润滑膜,摩擦系数逐渐增大;且随着制动次数的增加,摩擦系数变化幅度变小,刹车稳定。

ZrB_(2)超细粉体改性C/C-SiC-ZrC复合材料的微观结构和烧蚀性能

为进一步提升C/C-SiC-ZrC复合材料的抗烧蚀性能,采用反应熔渗法(reactive melt infiltration,RMI)制备ZrB_(2)超细粉体改性C/C-SiC-ZrC复合材料,考察ZrB_(2)超细粉体含量对改性复合材料的微观结构和烧蚀性能的影响。研究结果表明:相较于未改性的C/C-SiC-ZrC复合材料,ZrB_(2)超细粉体的引入使C/C-SiC-ZrC复合材料的密度由2.25 g/cm^(3)增至2.40~2.48 g/cm^(3);ZrB_(2)主要分布在ZrC基体中,且分布均匀;ZrB_(2)超细粉体的添加显著提升了复合材料的抗烧蚀性能;电火花等离子体烧蚀120 s后,当ZrB_(2)超细粉体摩尔分数为2%时,复合材料的质量烧蚀率和线烧蚀率最低,分别为6.90 mg/s和2.26μm/s;在烧蚀过程中,氧化生成的ZrO_(2)黏附在材料表面,与具有一定流动性的SiO_(2)形成龟壳状的ZrO_(2)-SiO_(2)氧化层,该氧化层减少了烧蚀过程中等离子体向基体的扩散和热传递,有效提升了改性复合材料的抗烧蚀性能。

多孔碳陶瓷化改进反应熔渗法制备陶瓷基复合材料研究进展

连续纤维增强陶瓷基复合材料具有高强韧、耐氧化的特性,现已成为航空航天领域重要的高温结构候选材料。反应熔渗法可实现陶瓷基复合材料的大规模、短周期和低成本制备,是目前最具有商业化前景的技术之一。然而,传统反应熔渗法制得陶瓷基复合材料存在着基体碳残留、纤维刻蚀等问题,导致材料力学与氧化-烧蚀性能不佳。为突破传统碳基体陶瓷化程度低的局限性,相关研究人员采用碳基体孔结构构筑方法,通过多孔碳基体取代传统熔渗预制体中致密碳基体,以促进碳基体的陶瓷化转变及反应熔体的消耗,进而实现陶瓷基复合材料的性能优化。本综述介绍了采用多孔碳陶瓷化策略制备SiC陶瓷、SiC/SiC复合材料、C/SiC复合材料及超高温陶瓷基复合材料的相关研究进展,并且通过与传统反应熔渗法对比,验证了多孔碳陶瓷化策略的优势,同时总结了相关多孔碳基体制备方法的发展演变过程,最后针对先进陶瓷基复合材料的基础理论与工艺技术需求,对多孔碳陶瓷化改进反应熔渗法的未来发展方向进行了展望。

ZrC纳米粉体改性C/C-SiC复合材料的微观结构和烧蚀性能

为改善C/C-SiC复合材料的抗烧蚀性能,以ZrC纳米粉体和Si粉为反应渗料,采用反应熔渗(reactive melt infiltration,RMI)法制备ZrC纳米粉体改性C/C-SiC复合材料。采用X射线衍射仪、扫描电镜和能谱仪等研究ZrC纳米粉体含量对C/C-SiC复合材料微观结构和烧蚀性能的影响。结果表明:随ZrC纳米粉体含量增加,复合材料的孔隙率增大,而密度变化不大。ZrC纳米粉体一部分弥散分布在SiC基体中,一部分则发生了团聚。烧蚀30 s后,ZrC纳米粉体摩尔分数为6%时,复合材料的质量烧蚀率和线烧蚀率最低,分别为2.0 mg/s和3.9μm/s。随ZrC纳米粉体含量增加,烧蚀过程中形成的ZrO_(2)含量增多,对SiO_(2)的钉扎作用明显增强,能有效提升C/C-SiC复合材料的抗烧蚀性能。

Microstructure and ablation behavior of Zr-based ultra-high-temperature gradient composites

To obtain high-performance Zr-based ultra-high-temperature composites,Zr-based ultra-high-temperature gradient composites were prepared by changing the laying method of the infiltrant via reactive melt infiltration.The effects of different infiltrant laying methods on the microstructure and ablative properties of Zr-based ultrahigh-temperature gradient composites were investigated.The results showed that the gradient structure of the Zr-based ultrahigh-temperature gradient composites differed when the composition ratio of the infiltrant was changed.When the thicknesses of the Zr/Mo/Si layers were 6/4/12 mm and 8/2/12 mm,the SiMoZrC solid solution content in the samples increased and decreased along the infiltration direction,respectively.The gradient samples were ablated in an oxyacetylene flame at 3000°C for 40 s.The ablation resistance of the sample was the highest when the infiltrant was a powder and the thickness of the Zr/Mo/Si layer was 6/4/12 mm.

反应熔渗法制备C/C-ZrC复合材料的微观结构及烧蚀性能

采用反应熔渗法(reactive melt infiltration,RMI)制备ZrC改性多孔C/C复合材料,研究不同孔隙度的C/C多孔体在熔渗过程中的增密行为和渗Zr后的相组成及微观形貌,探寻具有最佳熔渗效果的C/C多孔体,并研究所得C/C-ZrC复合材料在不同温度下的氧乙炔焰烧蚀行为。结果表明,随C/C多孔体密度增加,C/C-ZrC复合材料的密度降低;其中密度为1.40 g/cm3的多孔体熔渗效果最佳,开孔隙率由熔渗前的28.2%降低到6.6%。;熔渗的Zr液易与网胎层处的炭纤维和基体炭反应,生成的ZrC陶瓷相主要分布在原网胎层位置。择取原始密度为1.40 g/cm3的C/C多孔体熔渗后进行60 s的氧乙炔焰烧蚀实验,在3 000℃下的线烧蚀率和质量烧蚀率分别为0.003 3 mm/s和0.004 2 g/s,在2 500℃下的线烧蚀率和质量烧蚀率分别为0.008 0 mm/s和0.009 0 g/s,C/C-ZrC复合材料在3 000℃下的抗烧蚀性能明显优于2 500℃下的抗烧蚀性能。

碳/碳化硅摩阻复合材料的研究进展

碳/碳化硅是近年来发展起来的一种新型高性能陶瓷基摩阻材料,具有密度低,抗氧化性好,摩擦性能高且性能稳定等一系列优点,在高速列车、飞机和重型汽车等高能载制动领域具有广泛的应用前景。反应性熔体浸渗法是制备碳/碳化硅摩阻复合材料的有效途径。从碳/碳化硅摩阻复合材料的设计出发,深入分析了反应性熔体渗透过程的热力学条件,Si-C反应体系的基本特征以及动力学规律。针对短纤维模压和三维针刺等两种典型C/SiC复合材料的制备过程,对材料的微结构特征和摩擦磨损性能进行了系统论述。同时,对红外热成像、X射线透射和工业CT等先进工程检测方法在碳/碳化硅摩阻复合材料构件上的应用进行了分析。

SiC含量对C/C-SiC摩擦材料摩擦磨损性能的影响

以整体碳毡为预制体,经化学气相渗透法制得C/C多孔坯体,然后采用反应熔融浸渗法制得C/C-SiC摩擦材料,探究SiC含量对C/C-SiC摩擦材料摩擦磨损性能的影响。结果表明:C/C-SiC试样的摩擦因数随着SiC含量的增加呈现先上升后下降的趋势,当SiC含量为29.88%时摩擦因数达到最大值0.62。当SiC含量低于33.56%时磨损率的变化规律与摩擦因数比较一致,当SiC含量高于33.56%时磨损率的变化规律与摩擦因数则呈相反的变化趋势。因此,SiC含量为33.56%时是该摩擦材料摩擦磨损性能的拐点。

浆料浸渍结合反应熔渗法制备2D C/SiC-Zr B_2复合材料

利用XRD,SEM,EDS研究浆料浸渍结合反应熔渗法制备2D C/SiC-ZrB2复合材料的组成与结构,并测定了复合材料的弯曲强度。结果表明:采用单向加压依次渗入ZrB2微粉和酚醛树脂,能很好地将ZrB2微粉和树脂渗入到纤维束间,但熔融Si难以渗入到试样内部,复合材料的开气孔率和室温弯曲强度分别为18.3%和110MPa。采用ZrB2浆料真空浸渍,沉积碳基体后进行熔融渗Si,复合材料的开气孔率和室温弯曲强度分别为5.5%和230MPa。