Insight into microstructure and flexural strength of ultra-high temperature ceramics enriched SICARBON™ composite

Research efforts on Ceramic Matrix Composites (CMCs) are aimed to increase the operating temperature in oxidizing environments by adding Ultra-High Temperature Ceramic (UHTC) phases to the matrix. The structural performances of UHTC-enriched CMCs are generally investigated through bending test because it requires simple fixture and specimen geometry with small quantity of plate material. However, there are hardly any scientific studies which bring out what bending test conditions are required to determine reliable flexural strength of these composites. In this study, the effect of span length and specimen orientation on the flexural strength of UHTC-enriched SICARBON™ material, produced by Airbus, was comprehensively evaluated and reported. Transition of the failure mode was obtained by tilting the specimens with horizontal build direction instead of lay-up configuration (vertical build direction). The tilted configuration allowed to get a valid flexural strength of 370 MPa even with small specimens of about 30 mm. To assess failure mode in different test configurations, virtual microstructure was generated on the base of cumulative distribution functions of observed microstructural features. Tsai-Wu failure criterion was extended in order to evaluate direction dependent failure indices for different lay-up configurations

Influence of Y2O3 addition on the mechanical and oxidation behaviour of carbon fibre reinforced ZrB2/SiC composites

The influence of Y2O3 addition on the microstructure, thermo-mechanical properties and oxidation resistance of carbon fibre reinforced ZrB2/SiC composites was investigated. Y2O3 reacted with oxide impurities present on the surface of ZrB2 and SiC grains and formed a liquid phase, effectively lowering the sintering temperature and allowing to reach full density at 1900 °C. The presence of a carbon source (fibres) led to additional reactions which resulted in the formation of new secondary phases such as yttrium boro-carbides. Mechanical properties were significantly enhanced compared to the un-doped composite. Further tests at high temperatures resulted in strength increase up to 700 MPa at 1500 °C which was attributed to stress relaxation. Oxidation tests carried out at 1500 °C and 1650 °C in air showed that the presence of the Y-based secondary phases enhanced the growth of ZrO2 grains, but offered limited protection to oxygen due to the lower availability of surficial SiO2 formed from SiC

Ti3SiC2-Cf composites by spark plasma sintering: Processing, microstructure and thermo-mechanical properties

MAX phases, and particularly Ti3SiC2, are interesting for high temperature applications. The addition of carbon fibers can be used to reduce the density and to modify the properties of the matrix. This work presents the densification and characterization of Ti3SiC2 based composites with short carbon fibers using a fast and simple fabrication approach: dry mixing and densification by Spark Plasma Sintering. Good densification level was obtained below 1400 °C even with a high amount of fibers. The reaction of the fibers with the matrix is limited thanks to the fast processing time and depends on the amount of fibers in the composite. Bending strength at room temperature, between 437 and 120 MPa, is in the range of conventional CMCs with short fibers and according to the resistance of the matrix and the presence of residual porosity. Thermo-mechanical properties of the composites up to 1500 °C are also presented.This work has received funding from the European Union’s Horizon2020 “Research and innovation programme” under grant agreement No 685594 (C3HARME

Toughening effect of non-periodic fiber distribution on crack propagation energy of UHTC composites

Different configurations of continuous carbon fiber-reinforced ultrahigh temperature ceramics (UHTCs), by combining coatings and matrix, were produced via electrophoretic deposition (EPD) and slurry infiltration. The toughening of non-periodic fiber distribution induced by the EPD process was investigated through work of fracture analysis. The results show that a non-periodic fiber distribution results in toughness increase from 8 MPa√m to 11 MPa√m with respect to a periodic fiber distribution. This toughness improvement does not strongly affect the flexural strength, which is mainly related to the fiber volumetric amount. It is shown that the assembling of carbon fibers into bundles (i.e. by dispersing the fibers with a non-periodic distribution) increases the crack propagation energy dissipated on the crack-wake from 0.5 kJ/m2 to 1 kJ/m2, which can be mainly ascribed to the fiber/bundle pull-out. On the other hand, the energy dissipated on the crack-tip (as fiber/matrix debonding) is fiber distribution-independent and increases from 0.3 kJ/m2 to 0.4 kJ/m2 with increasing the fiber amount from 33 vol% to 40 vol%. Finally, WoF analysis is proposed as test to evaluate pull-out toughening instead of push-in and push-out tests

Reactive melt infiltration of carbon fibre reinforced ZrB2/B composites with Zr2Cu

The microstructure and mechanical properties of carbon fibre reinforced ZrB2 composites produced by slurry infiltration and consolidated by reactive melt infiltration were investigated. Fibres were preliminary infiltrated with ZrB2/B slurries with varying ZrB2/B ratios. Then the composites were infiltrated with Zr2Cu melt at 1200 °C under vacuum. Boron was chosen as the reactant phase, while raw ZrB2 was added as a filler to prevent excessive swelling. With increase of boron content the infiltration becomes more difficult due to the reaction of alloy and boron. The boron is completely converted to nano ZrB2 grains. Some ZrC is produced from the side reaction between Zr2Cu and the carbon fibre, resulting in reduction of fibre diameter. The flexural strength increased from 360 to 560 MPa with the increase of boron content, while KIc amounted to 10 MPa⋅m0.5 but was affected by large scatter. The mechanical behaviour was mostly dominated by matrix properties

Formation of high entropy metal diborides using arc-melting and combinatorial approach to study quinary and quaternary solid solutions

High entropy metal diborides (HEBs) represent a radically new approach to extend the chemical composition window of ultra-high temperature ceramics (UHTCs). In this work, arc-melting was used to produce dense HEBs starting from UHTC powders. In order to understand the influence of each individual diboride within the quinary system (HfB2, ZrB2, TiB2, TaB2 and CrB2), we investigated five quaternary equimolar solid solutions e.g. Hf-Zr-Ti-Ta, Hf-Zr-Ti-Cr, Hf-Zr-Ta-Cr, Hf-Ti-Ta-Cr, Zr-Ti-Ta-Cr and the overall quinary equimolar combination. Arc-melting allowed a rapid screening of favorable and unfavorable combinations. The produced HEBs were free from undesired oxides and characterized by linear variation of lattice parameters typical of diborides and binary solid solutions. Because of evaporation during arc melting, CrB2 was hardly found in the solid solution, suggesting that vapor pressure should be taken into account when designing HEB compositions especially for operating temperatures exceeding 2000 °C. Finally, Vickers microhardness ranged between the typical values of starting diborides

Development of UHTCMCs via water based ZrB2 powder slurry infiltration and polymer infiltration and pyrolysis

Cf/ZrB2-SiC ultra-high temperature composites were manufactured via aqueous slurry impregnation coupled with polymer infiltration and pyrolysis, using a allylhydrido polycarbosilane precursor. For the first time we used ultra-high modulus pitch-based carbon fibres for the PIP process, investigating three different architectures, 0/0°, 0/90°, and 2D. Microstructure, mechanical properties and oxidation resistance in air at 1650 °C were investigated. As expected, the mechanical properties showed the tendency to decrease with increase of the preforms complexity, due to the higher amount of flaws and residual stresses. For instance, the flexural strength was approaching 500 MPa for 0/0°, 370 MPa for 0/90° and 190 MPa for 2D. The materials showed an optimal resistance to oxidation at 1650 °C thanks to formation of a viscous borosilicate glass that guaranteed a self-healing functionality

Effect of PAN-based and pitch-based carbon fibres on microstructure and properties of continuous Cf/ZrB2-SiC UHTCMCs

In this paper the microstructure and mechanical properties of two different Cf/ZrB2-SiC composites reinforced with continuous PyC coated PAN-derived fibres or uncoated pitch-derived fibres were compared. Pitch-derived carbon fibres showed a lower degree of reaction with the matrix phase during sintering compared to PyC/PAN-derived fibres. The reason lies in the different microstructure of the carbon. The presence of a coating for PAN-derived fibres was found to be essential to limit the reaction at the fibre/matrix interface during SPS. However, coated bundles were more difficult to infiltrate, resulting in a less homogeneous microstructure. As far as the mechanical properties are concerned, specimens reinforced with coated PAN-derived fibres provided higher strengths and damage tolerance than uncoated pitch-derived fibres, due to the higher degree of fibre pull-out. On the other hand, the weaker fibre/matrix interface resulted in lower interlaminar shear, off-axis strength and ablation resistance

Is spark plasma sintering suitable for the densification of continuous carbon fibre - UHTCMCs?

For the first time we show that spark plasma sintering can efficiently replace hot pressing for the densification of UHTCMCs, in the present case ZrB2/SiC composites reinforced with continuous carbon fibres. To this purpose, the same materials were first produced by hot pressing as baseline samples and then by spark plasma sintering (SPS) to compare microstructure and basic mechanical properties. A special emphasis was given to the study of interfaces, in case of both coated and uncoated carbon fibres. SPS allowed for faster sintering but required an adjustment of the temperature to avoid fibre degradation compared to hot pressing. With similar porosity levels, we observed a slight decrease of flexural strength (300 vs 470 MPa), and an improvement of fracture toughness (15 vs 10 MPa√m) for SPSed samples. SPS was proved to be an effective method for the consolidation of continuous fibre reinforced UHTC composites