PyC/SiC界面相对PIP法制备3D HTA C/SiC复合材料性能的影响

利用三维编织炭纤维预制件通过先驱体浸渍裂解法制备C／SiC复合材料。研究了热解碳（PyC）／SiC界面相对复合材料的微观结构和力学性能的影响。弯曲性能通过三点弯曲法测试，复合材料的断口和抛光面通过扫描电镜观察。结果表明：通过等温化学气相沉积法在纤维表面沉积PyC／SiC界面相以后，复合材料的三点抗弯强度从46MPa提高到247MPa。沉积界面的复合材料断口有明显的纤维拔出现象，纤维与基体之间的结合强度适当，起到了增韧作用；而未沉积界面相复合材料的断口光滑、平整，几乎没有纤维拔出，纤维在热解过程中受到严重的化学损伤，性能下降严重，材料表现为典型的脆性断裂。     

裂解碳涂层对碳纤维增强碳化硅复合材料力学性能的影响

采用先驱体裂解－热压烧结方法制备出Cf/SiC复合材料,探讨了裂解碳涂层和烧结温度对复合材料纤维／基体界面和力学性能影响,烧结温度为1800度时,由于其中由富碳界面相构成的纤维／基体界面相使纤维／基体界面结合适中,具有较好的力学性能。     

Fabrication of SiCf/SiC composites by chemical vapor infiltration and vapor silicon infiltration

Three-dimensional (3D) silicon carbide fiber reinforced silicon carbide matrix (SiC_f/SiC) composites, employing KD-1 SiC fibers (from National University of Defense Technology, China) as reinforcements, were fabricated by a combining chemical vapor infiltration (CVI) and vapor silicon infiltration (VSI) process. The microstructure and properties of the as prepared SiC_f/SiC composites were studied. The results show that the density and open porosity of the as prepared SiC_f/SiC composites are 2.1 g/cm³ and 7.7%, respectively. The SiC fibers are not severely damaged during the VSI process. And the SiC fibers adhere to the matrix with a weak interface, therefore the SiC_f/SiC composites exhibit non-catastrophic failure behavior with the flexural strength of 270 MPa, fracture toughness of 11.4 MPa·m^1/2 and shear strength of 25.7 MPa at ambient conditions. Moreover, the flexural strength decreases sharply at the temperature higher than 1200 °C. In addition, the thermal conductivity is 10.6 W/mk at room temperature.     

Microstructure, mechanical properties and reaction mechanism of KD-1 SiCf/SiC composites fabricated by chemical vapor infiltration and vapor silicon infiltration

Three-dimensional (3D) KD-1 silicon carbide fiber reinforced silicon carbide matrix (KD-1 SiC_f/SiC) composites were fabricated by a combining chemical vapor infiltration (CVI) and vapor silicon infiltration (VSI) process. The microstructure and mechanical properties of the resulting KD-1 SiC_f/SiC composites were studied. The results show that the resulting SiC_f/SiC composites have high bulk density and low open porosity (<6%). The mechanical properties of the resulting SiC_f/SiC composites firstly increase and then decrease with decreasing the open porosity of the SiC_f/C composites. The KD-1 SiC fibers were not severely deformed and adhered to the matrix with a weak interface during the VSI process. As a result, the composites exhibit non-catastrophic failure behavior. Additionally, the diffusion mechanism for the VSI process was also investigated in our work.     

SiCf/SiC陶瓷复合材料的研究进展

SiCf/SiC陶瓷复合材料具有良好的力学性能、高温抗氧化性和化学稳定性，是航空航天和原子能等领域理想的新一代高温结构材料。本文概述了增强体SiCt的发展状况及存在的问题，对SiCt/SiC材料的制备工艺、界面相的研究状态、材料的损伤破坏机理和目前的应用研究进展做了综述，并分析了SiCf/SiC陶瓷复合材料的研究重点和发展前景。     

炭/炭-陶瓷/炭多元复合材料的原位热压制备与性能

以纤维素和凹凸棒石(PG)为原料,在220℃下水热24h制备凹凸棒石/炭(PG/C)复合材料。采用浸渍-炭化工艺在炭/炭(C/C)复合材料中引入PG/C作为添加剂,一步热压对材料最终成型,原位获得C/C-陶瓷/C复合材料。研究了添加PG/C对C/C力学性能和抗氧化性能的影响。结果表明:PG/C在热压过程中转变为顽辉石/C,顽辉石/C通过"填充"和"桥联"起增强作用,顽辉石陶瓷表面负载纳米炭层有效避免了陶瓷相与基体炭间弱结合的产生。随着PG/C中表面负载纳米炭含量的减少,C/C的强度逐渐增加。当炭含量为13%的PG/C作为添加剂时,C/C的抗弯强度为263MPa,弹性模量为47GPa,相对于没有添加剂的C/C抗弯强度提高了45%,弹性模量提高了42%;相对于以PG作为添加剂的C/C抗弯强度提高了16%,弹性模量提高了27%。添加PG/C使C/C抗氧化性得到了提高;1 000℃下C/C的质量损失降低了12%~18%。     

碳化硅纳米线增韧碳化硅纤维/碳化硅基体损伤行为研究

通过在碳化硅纤维表面原位生长纳米线得到具有多级增强结构的碳化硅复合材料, 对复合材料引入纳米线后的微观结构、弯曲强度以及损伤的变化过程进行了研究。研究结果表明, 相较于原始的碳化硅纤维增强碳化硅复合材料, 碳化硅纳米线可以明显提高基体沉积效率并改善材料的弯曲力学性能。从声发射技术和维氏硬度压痕测试结果可以看出, 纳米线通过抑制微裂纹的产生和在微裂纹之间发生桥联来抑制早期损伤的发展。此外, 在纳米线表面沉积一层氮化硼界面相, 纳米线与基体之间的结合力变弱, 复合材料对微裂纹的抑制和偏转得到进一步增强, 弯曲性能大幅提升。     

Proportional Limit Stress and Residual Thermal Stress of 3D SiC/SiC Composite

Proportional limit stress （PLS） and residual thermal stresses （RTS） of 3D SiC/SiC composite were investigated. PLS was obtained by four different methods from the monotonic stress-strain response curve to get a convincing value. RTS in the SiC matrix was quantified by solving the geometric intersection point of the regression lines of hysteresis loops from the periodical loading-unloading-reloading cycle test curve. Classical ACK model and analytical formulas were used to analytically calculate the PLS and RTS of 3D SiC/ SiC composite. Good agreement between the experimental results and the analytical calculation was observed. And relationship between the PLS and the RTS of 3D SiC/SiC was discussed.     

PIP法制备Cf／SiC和SiCf／SiC复合材料的研究进展

先驱体浸渍-热解（PIP）法是制备连续纤维增强SiC基陶瓷的主要方法之一。介绍了PIP工艺的特点、对PIP工艺制备G／SiC和SiCJSiC复合材料的工作结果做了统计,概括了PIP工艺优化、填充剂、纤维预处理和表面涂层、低成本制造路线、陶瓷先驱体选择和合成方面的研究进展,分析了现有PIP工艺存在的问题,提出了在现有工艺水平上可以显著提高产品性能和产能的设备设施改进措施,包括建立高等级净化室和浸渍-固化-热解设备-体化。     

Fabrication and technological properties of nanoporous spinel/forsterite/zirconia ceramic composites

In this work, nanoporous spinel/forsterite/zirconia ceramic composites were fabricated at 1600 °C for 2 h. The influence of zirconia content (up to 10 mass%) on the technological properties, nanopores formation, phase compositions, microstructure and thermal diffusivity of nanoporous ceramic composites was investigated. Nanospinel and nanoforsterite powders were synthesized via a modified co-precipitation and sol–gel techniques, respectively. Results indicated that apparent porosity of the fired nanoporous ceramic composites is mostly in the range 14.26–56.14% with the average pores diameter 35.8 nm. Using of nanopowders (spinel and forsterite) as the staring materials were achieved high mechanical (cold crushing strength ∼ 235–164 MPa) and elastic (Young’s modulus ∼ 123.6–4.5 GPa) properties of the prepared nanoporous ceramic composites. Microstructure analysis exhibited all of the crystalline phases and pores of the nanoporous ceramic composites are in the nanosize (35–40 nm). These nanoporous ceramic composites are promising porous ceramic materials for using in advanced applications due to their excellent combination properties.     

Correlation of elastic properties of melt infiltrated SiC/SiC composites to in situ properties of constituent phases

The ability to correlate the elastic properties of melt infiltrated SiC/SiC composites to properties of constituent phases using a hybrid Finite Element approach is examined and the influence of material internal features, such as the fabric architecture and intra-tow voids, on such correlation is elucidated. Tensile testing was carried out in air at room temperature and 1204 °C. Through-thickness compressive elastic modulus utilizing the stacked disk method was measured at room temperature. In situ moduli of constituent materials were experimentally evaluated using nano-indentation techniques at room temperature. A consistent relationship is observed between constituent properties and composite properties for in-plane normal and shear moduli and Poisson’s ratio at room temperature. However, experimental data for through-thickness compressive elastic modulus is lower than the calculated value. It is hypothesized that the existence of voids inside the fiber tows and their collapse under compressive loads is the cause of such discrepancy. Estimates for the change in elastic moduli of constituent phases with temperature were obtained from literature and used to calculate the elastic properties of the composites at 1204 °C. A reasonable correlation between the in-plane elastic moduli of the composite and the in situ elastic properties of constituent phases is observed.     

SiCf/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。     

SiC纤维表面碳涂层及其SiCf／SiC复合材料性能研究

采用先驱体转化法（PIP）以酚醛和沥青为先驱体在SiC纤维表面涂覆碳层，并制备SiCf／SiC复合材料；优化了两种碳涂层制备工艺；分析了涂层后纤维的表面形貌并测试涂层厚度；研究了两种碳涂层对两种SiC纤维（普通和含铝）及复合材料力学性能的影响。     

SiCf/Ti复合材料的研制

概述了国外碳化硅连续纤维增强钛基复合材料的研制、性能及应用情况，并对箔压法制备SiCf/Ti复合材料的工艺及材料性能进行了研究。结果表明，本研究采用FFF法制作的SiCf/Ti复合材料能达到国外同类材料水平。此外，本研究还对SiCf/Ti复合材料各主要制作工艺进行了分析比较，认为真空等离子喷涂工艺是较有前途的。     

SiC引入方式对反应熔渗原位纳米SiC/MoSi_2复合材料组织性能的影响

探讨了SiC引入方式对反应熔渗原位20wt%纳米SiC/MoSi_2复合材料TEM组织及力学性能的影响。结果表明:完全原位反应熔渗硅可获得基体相和增强相均为纳米尺度的SiC/MoSi_2复合材料,其组织中存在大量晶内层错等缺陷,可能会使纳米SiC/MoSi_2复合材料力学性能的提高不十分显著;而部分原位反应熔渗法中,SiC初始粉末的引入可缓解剧烈物相反应,所得纳米SiC/MoSi_2复合材料晶内缺陷消失,断口出现大量撕裂棱,复合材料力学性能大幅提高。     

Improvement of SiCf/SiC density by slurry infiltration and tape stacking

SiC fiber-reinforced SiC–matrix ceramic composites (SiC_f/SiC) were fabricated by vacuum infiltration of a SiC slurry into Tyranno™-SA grade-3 fabrics coated with a 200 nm-thick pyrolytic carbon (PyC) layer followed by hot pressing using a transient eutectic-phase. The density of the composite was improved using a special infiltration apparatus with a pressure gradient and alternating tape insertion between fabrics. Their overall properties were compared with those of monolithic SiC and composite containing chopped fibers. Although the density of the composites decreased with increasing fiber fraction, SiC_f/SiC containing 50 vol.% fibers had a density of 3.13 g/cm³, which is the highest reported thus far. The composites containing continuous fibers had a maximum flexural strength of 607 MPa and a step increase in the stress–displacement behavior during the three-point bending test due to fiber reinforcement, which was not observed in the monolith.     

复合材料热压成型过程的树脂压力测试系统

在树脂基复合材料的成型工艺中大多涉及到树脂的流动过程, 而树脂压力是反映这一过程的重要参数, 监测成型过程中树脂压力的变化可以为工艺参数的选择和构件质量的控制提供指导。本文中针对热压工艺, 根据液体传压原理和特点, 自行研制了复合材料成型过程树脂压力测试系统, 对系统的精度和动态响应性能进行了研究, 并以该系统为测试手段, 初步研究了玻璃纤维单向层板中树脂压力的变化规律。结果表明, 该系统具有准确度高和动态响应敏感的特点, 满足热压成型过程树脂压力的测试要求, 为研究工艺过程树脂流动行为提供了有力的测试与验证手段。      

FCVI工艺制备SiCf/SiC复合材料结构与性能研究

采用热梯度强制流动化学气相渗积（FCVI）工艺制备SiCf/SiC复合材料，测试了复合材料的性能。制备的复合材料密度达到2.3g/cm3，强度为291 MPa，断裂韧性为11.4 MPa*m1/2。运用SEM，TEM，X射线衍射等分析手段对复合材料的微观结构进行了表征。结果表明：渗积的基体材料为β-SiC，晶粒尺寸为亚微米级，结晶度良好。通过对断口形貌的观察，分析了增韧机制。，SiCf/SiC composite was fabricated by forced flow thermal-gradient chemical vapor infiltration (FCVI). The density of composite is 2.3g/cm3.The flexural strength and fracture toughness of SiCf/SiC compsites were tested: the flexural strength is 291 MPa, the fracture toughness is 11.4 MPa*m1/2. The microscopy structure was characterized by SEM, TEM and X-ray diffraction. The results show that SiC matrix fabricated by FCVI is β-SiC, which has sub-micron grain size and good crystallinity.And the toughening mechanism was also investigated by morphology of the fractrue surface.     

Oxidation and Mechanical Properties of SiC/SiC-MoSi2-ZrBa Coating for Carbon/Carbon Composites

To improve oxidation resistance of carbon/carbon （C/C） composites, a SiC/SiC-MoSi2-ZrB2 double-layer ceramic coating was prepared on C/C composites by two-step pack cementation. The phase compositions and microstructures of as-prepared multilayer coating were characterized by X-ray diffraction and scanning electron microscopy. The oxidation resistance at 1773 K and the effect of thermal shock between 1773 K and room temperature on mechanical performance of coated specimens were investigated. The results show that the SiC/SiC-MoSi2-ZrB2 coating exhibits dense structure and is composed of SiC, Si, MoSi2 and ZrB2. It can protect C/C composites from oxidation at 1773 K for more than 510 h with weight loss of 0.5%. The excellent anti-oxidation performance of the coating is due to the formation of SiO2-ZrSiO4 complex glassy film. The coating can also endure the thermal shocks between 1773 K and room temperature for 20 times with residual flexural strength of 86.1%.     

High mechanical performance SiC/SiC composites by NITE process with tailoring of appropriate fabrication temperature to fiber volume fraction

Unidirectional SiC/SiC composites are prepared by nano-powder infiltration and transient eutectic-phase (NITE) process, using pyrolytic carbon (PyC)-coated Tyranno-SA SiC fibers as reinforcement and SiC nano-powder with sintering additives for matrix formation. The effects of two kinds of fiber volume fraction incorporating fabrication temperature were characterized on densification, microstructure and mechanical properties. Densification of the composites with low fiber volume fraction (appropriately 30 vol%) was developed even at lower fabrication temperature of 1800 °C, and then saturated at 3rd stage of matrix densification corresponding to classic liquid phase sintering. Hence, densification of the composites with high volume fraction (above 50 vol%) became restricted because the many fibers retarded the infiltration of SiC nano-powder at lower fabrication temperature of 1800 °C. When fabrication temperature increased by 1900 °C, densification of the composites was effectively enhanced in the intra-fiber-bundles and simultaneously the interaction between PyC interface and matrix was strengthened. SEM observation on the fracture surface revealed that fiber pull-out length was accordingly changed with fabrication temperature as well as fiber volume fraction, which dominated tensile fracture behaviors. Through NITE process, SiC/SiC composites with two fracture types were successfully developed by tailoring of appropriate fabrication temperature to fiber volume fraction as follows: (1) high ductility type and (2) high strength type.