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A special issue of Journal of Composites Science (ISSN 2504-477X).

Deadline for manuscript submissions: closed (30 June 2021) | Viewed by 32279

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Prof. Gérard L. Vignoles

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Guest Editor

University of Bordeaux, CNRS: LCTS – Lab. For ThermoStructural Composites, France
Interests: thermostructural composites; image processing; carbon science

Special Issue Information

Dear Colleagues,

Ceramic-Matrix Composites (CMCs) are made of fibrous reinforcements made of carbon, carbide, or oxide fibers, with a ceramic matrix and an intentional or spontaneous interphase between them, providing them with a non-brittle character although all constituents are fragile. Therefore, they are capable of overcoming the usual limitations of more classical refractory materials.

They are high-tech, high-performance materials, with applications in many domains like: aerospace propulsion; atmospheric re-entry of space objects; high-performance braking of aircraft and automobiles; high-temperature heat exchange in power plants and industry; nuclear technology, etc.

They bring the attention of scientists and engineers to many aspects of their processing, structure, properties, applications.

As compared to many other types of materials, CMCs present some better capabilities; however, their relative novelty makes them sometimes difficult to monitor and control. Issues in material reliability, knowledge of actual parameter domain of use, fabrication costs and value chain, new potential applications, etc. need to be solved; addressing the underlying scientific bottlenecks is of utmost importance. Indeed, technological challenges are frequently related to more fundamental materials science & engineering issues.

Potential contributors are welcome to submit their most recent results in fundamental and applied science relevant to the field of ceramic-matrix composites, covering experimental and modeling aspects focused either on newly found relationships between materials processing, structure and properties, on cutting-edge characterization and test interpretation methods, or, on materials and process modeling.

Prof. Gérard L. Vignoles
Guest Editor

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Keywords

Ceramic-matrix composites
Ceramic fibres
Interphases
EBC/TBC
Processing methods
Structural characterization
Mechanical testing
Thermal testing
Ablation
Corrosion and oxidation
Modelling

Published Papers (14 papers)

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Research

17 pages, 6413 KiB

Open AccessArticle

Validation of Deep Learning Segmentation of CT Images of Fiber-Reinforced Composites

by Aly Badran, Dula Parkinson, Daniela Ushizima, David Marshall and Emmanuel Maillet

J. Compos. Sci. 2022, 6(2), 60; https://doi.org/10.3390/jcs6020060 - 18 Feb 2022

Cited by 8 | Viewed by 2656

Abstract

Micro-computed tomography (µCT) is a valuable tool for visualizing microstructures and damage in fiber-reinforced composites. However, the large sets of data generated by µCT present a barrier to extracting quantitative information. Deep learning models have shown promise for overcoming this barrier by enabling automated segmentation of features of interest from the images. However, robust validation methods have not yet been used to quantify the success rate of the models and the ability to extract accurate measurements from the segmented image. In this paper, we evaluate the detection rate for segmenting fibers in low-contrast CT images using a deep learning model with three different approaches for defining the reference (ground-truth) image. The feasibility of measuring sub-pixel feature dimensions from the µCT image, in certain cases where the µCT image intensity is dependent on the feature dimensions, is assessed and calibrated using a higher-resolution image from a polished cross-section of the test specimen in the same location as the µCT image. Full article

(This article belongs to the Special Issue Ceramic-Matrix Composites)

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15 pages, 12657 KiB

Open AccessFeature PaperArticle

Organomorphic Carbon Preform Formation Mechanism

by Evgeny Bogachev

J. Compos. Sci. 2022, 6(2), 50; https://doi.org/10.3390/jcs6020050 - 6 Feb 2022

Cited by 1 | Viewed by 1750

Abstract

Looking for ways to increase the structural uniformity of ceramic matrix composites (CMC) resulted in the development of organomorphic composites (C/C, C/SiC, SiC/SiC) where the filament diameter is comparable to the space between the filaments. The structural uniformity of the aforesaid CMCs is determined by their reinforcing preform; however, the mechanism of formation of this structure from polymer fibers remains unclear. This paper discusses an investigation of pressed specimens of the OKSIPAN^® nonwoven fabric based on Pyron^® polyacrylonitrile (PAN) fibers that were underoxidized as was determined using the electron paramagnetic resonance and microtomography methods. Using electron scanning microscopy, thermomechanical analysis and X-ray tomography, cementation of the preform due to the release and condensation of readily-polymerizing resin-like substances on the fiber surface after pressing at 180 °C was shown to be mainly responsible for retaining the mutual positions occupied by the fibers during pressing. The carbonized residue of the resin-like substances binds the fibers after pyrolysis. The other reason for organomorphic carbon preform consolidation is autohesive interaction of insufficiently cross-linked cores of the PAN fibers, since their thermal oxidation during pyrolysis at up to 1000 °C is hindered by the relatively high density of the compressed polymer preforms. The combination of pressing, thermal stabilization and pyrolysis results in the formation of the organomorphic carbon preform that features a relative density of at least 0.3 and a collection of pores, their normalized diameter ranging between 4 and 40 μm. Full article

(This article belongs to the Special Issue Ceramic-Matrix Composites)

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14 pages, 7926 KiB

Open AccessArticle

Thermal Qualification of the UHTCMCs Produced Using RF-CVI Technique with VMK Facility at DLR

by Vinothini Venkatachalam, Sergej Blem, Ali Gülhan and Jon Binner

J. Compos. Sci. 2022, 6(1), 24; https://doi.org/10.3390/jcs6010024 - 11 Jan 2022

Cited by 8 | Viewed by 2274

Abstract

Ultra high-temperature ceramic matrix composites (UHTCMCs) based on carbon fibre (Cf) have been shown to offer excellent temperature stability exceeding 2000 °C in highly corrosive environments, which are prime requirements for various aerospace applications. In C³Harme, a recent European Union-funded Horizon 2020 project, an experimental campaign has been carried out to assess and screen a range of UHTCMC materials for near-zero ablation rocket nozzle and thermal protection systems. Samples with ZrB₂-impregnated pyrolytic carbon matrices and 2.5D woven continuous carbon fibre preforms, produced by slurry impregnation and radio frequency aided chemical vapour infiltration (RF-CVI), were tested using the vertical free jet facility at DLR, Cologne using solid propellants. When compared to standard CVI, RFCVI accelerates pyrolytic carbon densification, resulting in a much shorter manufacturing time. The samples survived the initial thermal shock and subsequent surface temperatures of >2000 °C with a minimal ablation rate. Post-test characterisation revealed a correlation between surface temperature and an accelerated catalytic activity, which lead to an understanding of the crucial role of preserving the bulk of the sample. Full article

(This article belongs to the Special Issue Ceramic-Matrix Composites)

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20 pages, 3829 KiB

Open AccessArticle

Chemical Supercritical Fluid Infiltration of Pyrocarbon with Thermal Gradients: Deposition Kinetics and Multiphysics Modeling

by Gerard L. Vignoles, Gaëtan Talué, Quentin Badey, Alain Guette, René Pailler, Yann Le Petitcorps and Laurence Maillé

J. Compos. Sci. 2022, 6(1), 20; https://doi.org/10.3390/jcs6010020 - 7 Jan 2022

Cited by 1 | Viewed by 2246

Abstract

The chemical supercritical fluid infiltration process is a recent variation of the chemical vapor infiltration (CVI) process that allows rapid and efficient manufacturing of ceramic-matrix composites (CMCs), albeit still needing optimization. This article proposes a quantitative assessment of the process dynamics through experiments and modeling. The kinetics of carbon deposition were determined through two sets of experiments: CVD on a single filament at pressures between 10 and 50 bar and infiltration at pressures ranging between 50 and 120 bar. The CVI experiments were conducted under important thermal gradients and were interpreted using a model-based reconstitution of these gradients. We found that (i) the kinetic law has to incorporate the potential effect of the reverse reaction (i.e., etching of C by H

_{2}

); (ii) the activation energy and pre-exponential factor both decrease with pressure up to 50 bar, then remain roughly constant, and (iii) although the apparent activation energy is modest, a favorable situation occurs in which an infiltration front builds up and travels from the hottest to the coldest part of the preform due to the presence of sufficient heat flux. A numerical simulation of the process, based on the solution of momentum, heat, and mass balance equations, fed with appropriate laws for the effective transfer properties of the porous medium and their evolution with infiltration progress, was performed and validated by comparing the simulated and actual infiltration profiles. Full article

(This article belongs to the Special Issue Ceramic-Matrix Composites)

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14 pages, 4580 KiB

Open AccessArticle

Automated Damage Detection of (C/C)/Si/SiC Composite Using Vibration Modes with Deep Neural Networks

by Chihiro Shibata, Naohiro Shichijo, Johei Matsuoka, Yuriko Takeshima, Jenn-Ming Yang, Yoshihisa Tanaka and Yutaka Kagawa

J. Compos. Sci. 2021, 5(11), 301; https://doi.org/10.3390/jcs5110301 - 16 Nov 2021

Cited by 1 | Viewed by 2450

Abstract

Discontinuous carbon fiber-carbon matrix composites dispersed Si/SiC matrix composites have complicated microstructures that consist of four phases (C/C, Si, SiC, and C/SiC). The crack stability significantly depends on their geometrical arrangement. Nondestructive evaluation is needed to maintain the components in their safe condition. Although several nondestructive evaluation methods such as the Eddy current have been developed, any set of them is still inadequate in order to cover all of the scales and aspects that (C/C)/Si/SiC composites comprise. We propose a new method for nondestructive evaluation using vibration/resonance modes and deep learning. The assumed resolution is mm-order (approx. 1–10 mm), which laser vibrometers are generally capable of handling sufficiently. We utilize deep neural networks called convolutional auto-encoders for inferring damaged areas from vibration modes, which is a so-called inverse problem and infeasible to solve numerically in most cases. We solve this inference problem by training convolutional auto-encoders using vibration modes obtained from a non-damaged specimen with various frequencies as the dataset. Experimental results show that the proposed method successfully detects the damaged areas of validation specimens. One of the noteworthy points of this method is that we need only a few specimens for training deep neural networks, which generally require a large amount of data. Full article

(This article belongs to the Special Issue Ceramic-Matrix Composites)

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15 pages, 5554 KiB

Open AccessArticle

Mechanical and Microstructural Assessment of Inhomogeneities in Oxide Ceramic Matrix Composites Detected by Air-Coupled Ultrasound Inspection

by Jan Roßdeutscher, Peter Mechnich, Ferdinand Flucht, Yuan Shi and Raouf Jemmali

J. Compos. Sci. 2021, 5(11), 286; https://doi.org/10.3390/jcs5110286 - 23 Oct 2021

Cited by 1 | Viewed by 2121

Abstract

Ceramic Matrix Composites (CMC) are promising materials for high-temperature applications where damage tolerant failure behavior is required. Non-destructive testing is essential for process development, monitoring, and quality assessment of CMC parts. Air-coupled ultrasound (ACU) is a fast and cost-efficient tool for non-destructive inspections of large components with respect to the detection of material inhomogeneities. Even though ACU inspection is usually used for visual inspection, the interpretation of C-scan images is often ambiguous with regard to critical defects and their impact on local material properties. This paper reports on a new approach to link the local acoustic damping of an oxide CMC plate obtained from ACU analysis with subsequent destructive mechanical testing and microstructural analyses. Local damping values of bending bars are extracted from ACU maps and compared with the results of subsequent resonant frequency damping analysis and 3-point bending tests. To support data interpretation, the homogeneous and inhomogeneous CMC areas detected in the ACU map are further analyzed by X-ray computed tomography and scanning electron microscopy. The results provide strong evidence that specific material properties such as Young’s modulus are not predictable from ACU damping maps. However, ACU shows a high, beneficial sensitivity for narrow but large area matrix cracks or delaminations, i.e., local damping is significantly correlated with specific properties such as shear moduli and bending strengths. Full article

(This article belongs to the Special Issue Ceramic-Matrix Composites)

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19 pages, 121822 KiB

Open AccessArticle

Cumulative Shear Damage Mechanism to Short Fiber Type C/SiC

by Yuta Tobata, Shinsuke Takeuchi and Ken Goto

J. Compos. Sci. 2021, 5(9), 230; https://doi.org/10.3390/jcs5090230 - 30 Aug 2021

Viewed by 1439

Abstract

A cumulative damage mechanism for short fiber type C/SiC during shear loading–unloading testing was examined and quantified using Iosipescu specimens parallel in the in-plane and through-thickness plane, and by using modified fracture and damage mechanics theory referring to measured damage characteristics (crack length, number and angle). A nonlinear stress–strain relation was found for both specimens. Decrease in the apparent modulus was confirmed with increased peak stress, although permanent strain increased. Inelastic strain of the decomposed tensile direction derived from shear stress was greater than that of the compressive one. Cracks propagated perpendicularly to the tensile direction, intruding on the boundary of the transverse fibers and connecting to other cracks. The theoretical damage mechanics model succeeded to predict the stress–strain relation, proposing that the shear mechanical properties are predictable by measuring the damage characteristics. Full article

(This article belongs to the Special Issue Ceramic-Matrix Composites)

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19 pages, 7574 KiB

Open AccessArticle

The Versatility of HVOF Burner Rig Testing for Ceramic Matrix Composite Evaluation

by Gregory N. Morscher, Ragav P. Panakarajupally and Leland Hoffman

J. Compos. Sci. 2021, 5(8), 223; https://doi.org/10.3390/jcs5080223 - 20 Aug 2021

Cited by 5 | Viewed by 2906

Abstract

Effective testing of ceramic matrix composites (CMCs) and CMC/coating systems for high temperature, high stress, high velocity and/or severe oxidation/corrosion environments is a critical need in materials/coatings evaluation for extreme environments of hot section parts in jet engine and hypersonic applications. Most current technology can evaluate two or three of the extreme conditions for a given application; however, incorporating as many of the extreme thermo-mechanical-environmental factors is highly advantageous to understand combinatorial effects. A high velocity oxygen fuel (HVOF) burner rig offers an excellent platform to evaluate many of these extreme conditions. In this work, the following three different thermo-mechanical-environmental test conditions using an HVOF rig on SiC-based CMCs are highlighted: (1) fatigue at temperature for >Mach 1 velocity and high temperature compared to typical stagnant air test environment, (2) high temperature hard particle erosion at temperature for ≤Mach 1 conditions and (3) ~Mach 5 near-hypersonic velocity conditions at very high temperature exposure. Full article

(This article belongs to the Special Issue Ceramic-Matrix Composites)

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12 pages, 7939 KiB

Open AccessArticle

Correlation of Process Conditions, Porosity Levels and Crystallinity in Atmospherically Plasma Sprayed Yb₂Si₂O₇ Environmental Barrier Coatings

by Robert Vaßen, Emine Bakan, Doris Sebold and Yoo Jung Sohn

J. Compos. Sci. 2021, 5(8), 198; https://doi.org/10.3390/jcs5080198 - 28 Jul 2021

Cited by 15 | Viewed by 2082

Abstract

Environmental barrier coatings are necessary to protect fibre reinforced ceramics from high recession rates in fast and hot water vapor-containing gases as they typically are found in the hot gas sections of gas turbines. A standard material to protect SiC/SiC composites is atmospherically plasma sprayed (APS) Yb₂Si₂O₇. For this material, it is difficult to obtain at reasonable substrate temperatures both low porosity and high crystallinity levels during APS. In this paper results of coatings prepared by a so-called high velocity APS process and also more conventional processes are presented. All coatings have been prepared by a single layer deposition method which avoids inter passage porosity bands. Furthermore, the samples were heat-treated in air at 1300 °C for 100 h and the influence of the topcoat density on the growth of the silica scale on the used silicon bond coat was studied. Full article

(This article belongs to the Special Issue Ceramic-Matrix Composites)

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16 pages, 3327 KiB

Open AccessArticle

Micromechanical Modeling Tensile and Fatigue Behavior of Fiber-Reinforced Ceramic-Matrix Composites Considering Matrix Fragmentation and Closure

by Longbiao Li

J. Compos. Sci. 2021, 5(7), 187; https://doi.org/10.3390/jcs5070187 - 16 Jul 2021

Cited by 1 | Viewed by 1686

Abstract

In this paper, micromechanical constitutive models are developed to predict the tensile and fatigue behavior of fiber-reinforced ceramic-matrix composites (CMCs) considering matrix fragmentation and closure. Damage models of matrix fragmentation, interface debonding, and fiber’s failure are considered in the micromechanical analysis of tensile response, and the matrix fragmentation closure, interface debonding and repeated sliding are considered in the hysteresis response. Relationships between the matrix fragmentation and closure, tensile and fatigue response, and interface debonding and fiber’s failure are established. Experimental matrix fragmentation density, tensile curves, and fatigue hysteresis loops of mini, unidirectional, cross-ply, and 2D plain-woven SiC/SiC composites are predicted using the developed constitutive models. Matrix fragmentation density changes with increasing or decreasing applied stress, which affects the nonlinear strain of SiC/SiC composite under tensile loading, and the interface debonding and sliding range of SiC/SiC composite under fatigue loading. Full article

(This article belongs to the Special Issue Ceramic-Matrix Composites)

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12 pages, 4762 KiB

Open AccessArticle

Use of Zr–Ti Alloy Melt Infiltration for Fabricating Carbon-Fiber-Reinforced Ultrahigh-Temperature Ceramic Matrix Composites

by Yutaro Arai, Tomoki Marumo and Ryo Inoue

J. Compos. Sci. 2021, 5(7), 186; https://doi.org/10.3390/jcs5070186 - 16 Jul 2021

Cited by 9 | Viewed by 2362

Abstract

Carbon-fiber-reinforced ultrahigh-temperature ceramic (C/UHTC) matrix composites are an attractive candidate for fabricating various hot structures. The present study aimed to establish a Si-free Zr–Ti melt-infiltration method for fabricating C/UHTC matrix composites. To achieve this, the wettability of Zr–Ti alloys on carbon and their reactivity to carbon were examined. The alloys were melted on graphite plates and infiltrated into model preforms, which were made of porous carbon and had median pore diameters of 3 μm. The results showed that the apparent contact angle between Zr–Ti and C measured from melted alloys on carbon in room temperature was ~20–42° and that the alloys infiltrated into the preforms regardless of the Zr or Ti content. However, with an increase in the Zr content in the alloys, carbon disappeared and was absorbed into the alloys since the reactivity of Zr was higher than that of Ti and the specific surface area of the porous preform was higher than that of carbon-fiber-reinforced carbon composites, which are a typical preform of C/UHTC matrix composites. These results clearly indicate that not only the capillary flow during infiltration but also the reactivity of alloys to preforms should be considered in the process design for fabricating high-density composites via Zr–Ti infiltration. Full article

(This article belongs to the Special Issue Ceramic-Matrix Composites)

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16 pages, 9980 KiB

Open AccessArticle

Densification of Ceramic Matrix Composite Preforms by Si₂N₂O Formed by Reaction of Si with SiO₂ under High Nitrogen Pressure. Part 2: Materials Properties

by Brice Taillet, René Pailler and Francis Teyssandier

J. Compos. Sci. 2021, 5(7), 179; https://doi.org/10.3390/jcs5070179 - 8 Jul 2021

Cited by 1 | Viewed by 1598

Abstract

Ceramic matrix composites (CMCs) have been prepared and optimized as already described in part I of this paper. The fibrous preform made of Hi-Nicalon S fibers was densified by a matrix composed of Si₂N₂O prepared inside the CMC by reacting a mixture of Si and SiO₂ under high nitrogen pressure. This part describes the oxidation resistance and mechanical properties of the optimized CMC. The CMC submitted to oxidation in wet oxygen at 1400 °C for 170 h exhibited an oxidation gradient from the surface to almost the center of the sample. In the outer part of the sample, Si₂N₂O, Si₃N₄ and SiC were oxidized into silica in the cristobalite-crystallized form. The matrix microstructure looks similar to the original one at the center of the sample, while at the surface large pores are observed and the fiber/matrix interphase is consumed by oxidation. The elastic modulus and the hardness measured at room temperature by nano-indentation are, respectively, 100 and 8 GPa. The elastic modulus measured at room temperature by tensile tests ranges from 150 to 160 GPa and the ultimate yield strength from 320 to 390 MPa, which corresponds to a yield strain of about 0.6%. The yield strength identified by acoustic emission is about 40 MPa. Full article

(This article belongs to the Special Issue Ceramic-Matrix Composites)

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36 pages, 7125 KiB

Open AccessArticle

Densification of Ceramic Matrix Composite Preforms by Si₂N₂O Formed by Reaction of Si with SiO₂ under High Nitrogen Pressure. Part 1: Materials Synthesis

by Brice Taillet, René Pailler and Francis Teyssandier

J. Compos. Sci. 2021, 5(7), 178; https://doi.org/10.3390/jcs5070178 - 7 Jul 2021

Cited by 2 | Viewed by 1926

Abstract

Ceramic matrix composites (CMCs) have been designed and developed for extreme operating environments. The aim of the present study is to look for a rapid densification process providing a high level of material performance. The fibrous preform was made of Hi-Nicalon S fibers woven in a 3D interlock weave. The matrix was composed of Si₂N₂O prepared inside the CMCs by reacting a mixture of Si and SiO₂ under high nitrogen pressure (1 to 3 MPa). Silica was either impregnated by slurry or obtained by oxidation of silicon grains inside the preform. The synthesis reaction was initiated by heating the impregnated preform by means of a carbon resistor submitted to Joule effect. Composition, homogeneity and porosity of the formed matrix were studied and interpreted as a function of the experimental parameters (nitrogen pressure, heating rate of the preform) as well as the recorded thermal history of the process. The present results show that the matrix formation is almost completed in less than one minute. Melting of silicon has a major influence on the process. Competition was observed between the formation of Si₃N₄ and Si₂N₂O, which could be mainly controlled by the heating rate of the preform and the nitrogen partial pressure. Full article

(This article belongs to the Special Issue Ceramic-Matrix Composites)

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20 pages, 5375 KiB

Open AccessArticle

Prediction of Failure in Ceramic Matrix Composites Using Damage-Based Failure Criterion

by Neraj Jain and Dietmar Koch

J. Compos. Sci. 2020, 4(4), 183; https://doi.org/10.3390/jcs4040183 - 7 Dec 2020

Cited by 4 | Viewed by 2960

Abstract

This paper presents a damage-based failure criterion and its implementation in order to predict failure in ceramic matrix composites (CMC) manufactured via filament winding. The material behavior of CMCs is anisotropic and strongly depends on the angle between fiber orientation and loading direction. The inelastic behavior of laminates with different fiber orientations under tension and shear is modeled with the help of continuum damage mechanics. The parameters required for the damage model are obtained from a standard tensile and shear test. An isotropic damage law determines the evolution of damage in thermodynamic space and considers the interaction of damage parameters in different principal material directions. A quadratic damage-based failure criterion inspired by the Tsai-Wu failure criterion is proposed. Failure stress and strain can be predicted with higher accuracy compared to the Tsai-Wu failure criterion in stress- or strain-space. The use of the proposed damage limits allows designing a CMC component based on the microstructural phenomenon of stiffness loss. With the help of results obtained from modeling and experiments, fracture mechanics during the Iosipescu-shear test of CMCs and its capability to determine the shear strength of the material is discussed. Full article

(This article belongs to the Special Issue Ceramic-Matrix Composites)

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