C/C-SiC component for metallic phase change materials

Thanks to their high energy density and thermal conductivity, metallic Phase Change Materials (mPCM) have shown great potential to improve the performance of thermal energy storage systems. However, the commercial application of mPCM is still limited due to their corrosion behavior with conventional container materials. This work first addresses on a fundamental level, whether carbon-based composite-ceramics are suitable for corrosion critical components in a thermal storage system. The compatibility between the mPCM AlSi₁₂ and the Liquid Silicon Infiltration (LSI)-based carbon fiber reinforced silicon carbide (C/C-SiC) composite is then investigated via contact angle measurements, microstructure analysis, and mechanical testing after exposure. The results reveal that the C/C-SiC composite maintains its mechanical properties and microstructure after exposure in the strongly corrosive mPCM. Based on these results, efforts were made to design and manufacture a container out of C/C-SiC for the housing of mPCM in vehicle application. The stability of the component filled with mPCM was proven nondestructively via computer tomography (CT). Successful thermal input- and output as well as thermal storage ability were demonstrated using a system calorimeter under conditions similar to the application. The investigated C/C-SiC composite has significant application potential as a structural material for thermal energy storage systems with mPCM.     

Electrical properties of C/C and C/C-SiC ceramic fibre composites

The electrical properties of carbon/carbon (C/C) and carbon/carbon-silicon carbide (C/C-SiC) ceramic composites were measured. The results show that the capacitance decreases rapidly with an increase in frequency and it becomes constant above a frequency of 500 kHz, whereas the dissipation factor increases with increasing frequency. C/C-SiC composites give higher value than C/C composites due to the presence of microcracks.     

Experimental evaluation and theoretical prediction of elastic properties and failure of C/C-SiC composite

The paper presents experimental characterization and theoretical predictions of elastic and failure properties of continuous carbon fiber reinforced silicon carbide (C/C-SiC) composite fabricated by Liquid Silicon Infiltration (LSI). Its mechanical properties were determined under uniaxial tensile, compression, and pure shear loads in two sets of principal coordinate systems, 0°–90° and ±45°, respectively. The properties measured in the 0°–90° coordinate system were employed as the input data to predict their counterparts in the ±45° coordinate system. Through coordinate transformations of stress and strain tensors, the elastic constants and stress-strain behaviors were predicted and found to be in good agreement with the experimental results. In the same way, three different failure criteria, maximum stress, Tsai-Wu, and maximum strain, have been selected for the evaluation of the failure of C/C-SiC as a type of genuinely orthotropic material. Based on the comparisons with experimental results, supported by necessary practical justifications, the Tsai-Wu criterion was found to offer a reasonable prediction of the strengths, which can be assisted by the maximum stress criterion to obtain an indicative prediction of the respective failure modes.     

Fabrication process and mechanical properties of C/SiC corrugated core sandwich panel

Carbon fiber reinforced SiC composite is a kind of promising high-temperature thermal protection structural material owing to the excellent oxidative resistance and superior mechanical properties at high temperatures. In this work, a novel design and fabrication process of lightweight C/SiC corrugated core sandwich panel will be proposed. The compressive and three-point bending of the C/SiC corrugated sandwich panels are conducted by experiment and numerical simulation. The relative density of as-prepared C/SiC sandwich panel and the density composite material are 1.1 and 2.1 g/cm³, respectively. As the density of the C/SiC sandwich panel is only 52.3% of the bulk C/SiC, suggesting that lightweight characteristic is realized. Moreover, the C/SiC sandwich panel manifests itself as linear-elastic behavior before failure in compression and the strength is as high as 15.1 MPa. The failure mode is governed by the core shear failure and panel interlayer cracking. The load capacity under the three-point bending C/SiC composite sandwich panel is 1947.0 N. The main failure behavior is core shear failure. The stress distribution under the compression and three-point bend was simulated by FE analysis, and the results of numerical simulations are in accordance with the experimental results.     

Fabrication of C/C-SiC composites using high-char-yield resin

Carbon fiber reinforced ceramic matrix composites (C/C-SiC composites) were fabricated using a type of high-char-yield phenolic resin with the char yield of 81.17 wt.%. Firstly, the fabric prepreg was prepared by spreading the phenolic resin solution onto the two dimensional carbon fiber plain weave fabric and dried consequently. Afterward, the resin was cured and then the carbon fiber reinforced polymer (CFRP) was pyrolyzed to get amorphous carbon. Finally, C/C-SiC composites were obtained through liquid silicon infiltration (LSI) process. SEM micrographs showed that the Si/SiC area was homogeneously dispersed in the matrix, and during the siliconization process, a layer of SiC was formed along the surface of carbon fibers or carbon matrix. The fiber volume of CFRP was about 40 vol.%, which was much lower than other studies. XRD result indicated that only β-SiC type was formed. The result of X-ray computed tomography clearly showed the structure changes before and after the melt infiltration process. Mechanical property test showed that the composites had fracture strength of 186 ± 23 MPa, and a flexural modulus of 106 ± 8 GPa.     

Thermoset IM-LSI-based C/C-SiC: Influence of flow direction and weld lines on microstructure and mechanical properties

The production of ceramic matrix composites (CMC) based on C/C-SiC is still very cost-intensive and therefore only economical for a few applications. The fabrication of the preforms involves many costs that need to be reduced. In this work, the shaping of the CFRP-preforms is realized by thermoset injection molding, which enables large-scale production. The polymeric matrix used is a multi-component matrix consisting of novolak resin, curing agent and lubricant. Six millimeter chopped carbon fiber with a proportion of 50 wt.% were used as a reinforcement. These ingredients are processed by an industrial equipment for compounding and injection molding in order to manufacture a CFRP demonstrator representing a brake disc. Test specimens are cut out of the demonstrator in different directions in order to investigate influences of flow direction and weld lines on microstructural and mechanical properties. Afterward, the CFRP samples were converted to C/C-SiC composites by the liquid silicon infiltration process. The article addresses the flow behavior of the compound during the injection molding and the building of the weld lines in the demonstrator. In addition, results of the directional dependence of the microstructural and mechanical properties within the fabricated disc in the different production steps are presented.     

Effects of Preform Shear on Tensile Properties of a Woven C/SiC Composite

This article addresses effects of weave defects in an angle‐interlock C‐fiber preform on the tensile properties of the resulting fully processed C‐fiber/SiC‐matrix composite. For this purpose, a preform was intentionally sheared in a controlled manner after weaving. The resulting distortions were quantified by analyzing high‐resolution images of the preform surface after the first step of matrix processing, while the tows were still clearly visible. Comparisons are made of tensile test results on specimens cut from this composite panel and from a pristine panel in select loading orientations. Strain maps obtained by digital image correlation are used to identify local strain variations that are attributable to weave defects. The results are discussed in terms of: (i) the shear‐normal coupling that arises in loading orientations of present interest, and (ii) the geometric effects of tow misalignment on tow continuity along the specimen gauge length. The composite is found to perform in a robust manner, in the sense that the tensile properties are not sensitive to the presence of the defects.     

Properties of C/C-SiC composites produced via transfer moulding and inner siliconization

Short carbon fiber reinforced polymers (CFRP) are successfully prepared by transfer moulding technology. For this purpose, compounds on the basis of novolac/urotropin with different 6 mm chopped carbon fibers and silicon powder contents are produced utilizing a laboratory tempered sigma-blade kneader. These compounds are then shaped into 46 × 8 × 3 mm³ CFRP specimens using a transfer moulding machine. Depending on the material composition, the conversion to C/C-SiC composites is performed through liquid silicon infiltration (LSI) process or inner siliconization. First, the short fiber content is varied between 30 and 50 wt% and its influence on the process and properties of the composites is studied. Second, an investigation of the inner siliconization through the co-mixing of silicon powder (1-23 wt% in CFRPs) during the compound production as well as a comparison with the external silicon infiltration process are presented and discussed. According to the results, the best mechanical properties are achieved at a fiber content of 40 wt% in the case of the external silicon infiltration and at silicon content below 14 wt% for composites produced by the inner siliconization process.     

Joining oxide ceramic matrix composites by ionotropic gelation

The production of complex-shaped all-oxide ceramic matrix composites (Ox-CMC) is somewhat restricted by their current processing methods, as well as by the lack of applicable joining techniques. Thus, we present a new method for joining Ox-CMCs based on the gelation of slurries with the polysaccharide polymer alginate. For this investigation, Nextel 610/alumina-zirconia composites were produced using alginate as binder and aluminum acetate as gelling agent. The joining capabilities of this technique were investigated with microstructural analyses and single-lap compression shear tests. For that, a slurry-containing alginate was used to join two composite plates at different stages of the processing: gel state, dried green body and after sintering. Joining composites plates in their gel or green state was successful as the joints showed shear strength values similar to the interlaminar shear strength of the composites plates. The quality of the joints was attributed to the interactions between the alginate chains of the composite plates and the joint. We also show that even the joining of already sintered Ox-CMCs is feasible. However, densification cracks and lower shear strength are observed for such cases.     

Surface engineering of SiCf/SiC composites by selective thermal removal

Surface engineering based on the Selective Thermal Removal (STR) of SiC fibers from SiC_f/SiC composites was used to obtain a brush‐like surface in view of joining processes. As observed through 3D confocal microscopy, the thermal treatment led to a selective removal of the surface fibers so that the specific surface increased. Wetting tests were performed using a Ag–Cu–Ti brazing alloy. The STR led to a negligible increase in the contact angles, which ranged from 16° to 21° for as‐received composites and increased to 28° for composites after STR. Microstructural observations showed that the brazing alloy perfectly adhered to the brush‐like surfaces were giving a mechanical interlocking expected to enhance the strength of the joint.     

C/C-SiC梯度基复合材料氧化行为研究

研究比较了Ｃ／Ｃ－ＳｉＣ梯度基复合材料和Ｃ／Ｃ复合材料的氧化行为．实验结果表明：ＳｉＣ通过占据表面活性点提高了共沉积基体的氧化起始温度;由于减少了碳与氧的接触面积,阻挡氧化凹坑的扩展,降低了材料的氧化质量损失速率．利用ＳＥＭ观察了梯度基复合材料微观氧化过程     

Evaluation of dynamic modulus measurement for C/C-SiC composites at different temperatures

The determination of elastic properties at application temperature is fundamental for the design of fibre reinforced ceramic composite components. An attractive method to characterize the flexural modulus at room and high temperature under specific atmosphere is the nondestructive Resonant Frequency Damping Analysis (RFDA). The objective of this paper was to evaluate and validate the modulus measurement via RFDA for orthotropic C/C-SiC composites at the application temperature. At room temperature flexural moduli of C/C-SiC with 0/90° reinforcement were measured under quasi-static 4-point bending loads and compared with dynamic moduli measured via RFDA longitudinally to fibre direction. The dynamic modulus of C/C-SiC was then measured via RFDA up to 1250°C under flowing inert gas and showed an increase with temperature which fitted with literature values. The measured fundamental frequencies were finally compared to those resulting from numerical modal analyses. Dynamic and quasi-static flexural moduli are comparable and the numerical analyses proved that bending modes are correctly modeled by means of dynamic modulus measured via RFDA. The nondestructive RFDA as well as the numerical modeling approach are suitable for evaluation of C/C-SiC and may be transferred to other fibre reinforced ceramic composite materials.     

C/C多孔体对C/C-SiC复合材料微观结构和弯曲性能的影响

以4种纤维含量相同(32%,体积分数,下同),用化学气相渗透(chemical vapor infiltration,CVI)法制备了4种密度的碳纤维增强碳(carbon fiber reinforced carbon,C/C)多孔体,基体炭含量约20%～50%.利用液相渗硅法(liquid silicon infiltration,LSI)制备了C/C-SiC复合材料,研究了C/C多孔体对所制备的C/C-SiC复合材料微观结构和弯曲性能的影响.结果表明:不同密度的C/C多孔体反应渗硅后,复合材料的物相组成均为SiC,C及单质Si;随着C/C多孔体中基体炭含量的增加,C/C-SiC复合材料中SiC含量逐渐减少而热解炭含量逐渐增加.C/C-SiC复合材料弯曲强度随着材料中残留热解炭含量增加而逐渐增加,热解炭含量为约42%的C/C多孔体所制备的C/C-SiC复合材料的弯曲强度最大,达到320 MPa.     

Fabrication and properties of CNT/Ni/Y/ZrB2 nanocomposites reinforced in situ

Carbon nanotubes (CNTs) were synthesized in situ by chemical vapor deposition of methane over nano‐ZrB₂ matrix using Ni/Y catalysts. Well‐grown CNTs with tangled and long bodies and mainly composed of well‐crystallized graphite were obtained when the Ni content reaches 10 wt%. The CNT/ZrB₂ nanocomposites obtained by spark plasma sintering at 1400°C exhibited full density and optimal mechanical properties. The flexural strength and fracture toughness of the nanocomposites were 1184 ± 52 MPa and 10.8 ± 0.3 MPa·m^1/2, respectively. Results indicated that the dispersion of CNTs in situ can improve composite performance, rendering the mechanical properties of the CNT/ZrB₂ nanocomposites synthesized in situ considerably superior to those of monolithic ZrB₂ nanoceramics and CNT/ZrB₂ nanocomposites synthesized using the traditional method. The toughening mechanisms included crack deflection, crack bridging, CNT debonding, pull‐out, and fracture.     

Effect of carbon nanotubes on the strength of adhesive lap joints of C/C and C/C-SiC ceramic fibre composites

Similar substrates of carbon/carbon (C/C) and carbon/carbon-silicon carbide (C/CSiC) composites were bonded with pure epoxy resin and the one containing 3% multiwall carbon nanotubes (MWCNTs). The results show that MWCNT/filled epoxy resin bonded C/CC/C and C/CSiCC/CSiC substrates have a higher adhesive joint strength than those bonded with epoxy resin alone. MWCNTs increase the toughness and strength of the epoxy resin, which increases the interface bond strength between two similar matching surfaces.     

Core–shell NTC materials with low thermal constant and high resistivity for wide-temperature thermistor ceramics

Core–shell structures have been proposed to improve the electrical properties of negative-temperature coefficient (NTC) thermistor ceramics. In this work, Al₂O₃-modified Co_1.5Mn_1.2Ni_0.3O₄ NTC thermistor ceramics with adjustable electrical properties were prepared through citrate-chelation followed by conventional sintering. Co_1.5Mn_1.2Ni_0.3O₄ powder was coated with a thin Al₂O₃ shell layer to form a core–shell structure. Resistivity (ρ) increased rapidly with increasing thickness of the Al₂O₃ layer, and the thermal constant (B) varied moderately between 3706 and 3846 K. In particular, Co_1.5Mn_1.2Ni_0.3O₄@Al₂O₃ ceramic with 0.08 wt% Al₂O₃ showed the increase of ρ double, and the change in its B was less than 140 K. The Co_1.5Mn_1.2Ni_0.3O₄@Al₂O₃ NTC ceramics showed high stability, and their grain size was relatively uniform due to the protection offered by the shell. The aging coefficient of the ceramic was less than 0.2% after aging for 500 hours at 125°C. Taken together, the results indicate that as-prepared Co_1.5Mn_1.2Ni_0.3O₄@Al₂O₃ NTC ceramics with a core–shell structure may be promising candidates for application as wide-temperature NTC thermistor ceramics.     

Fabrication and properties of Cf/(Ti0.2Zr0.2Hf0.2Nb0.2Ta0.2)C-SiC high-entropy ceramic matrix composites via precursor infiltration and pyrolysis

In this work, C_f/(Ti_0.2Zr_0.2Hf_0.2Nb_0.2Ta_0.2)C-SiC high-entropy ceramic matrix composites were reported for the first time. Based on the systematic study of the pyrolysis and solid-solution mechanisms of (Ti_0.2Zr_0.2Hf_0.2Nb_0.2Ta_0.2)C precursor by Fourier transform infrared spectroscopy, TG-MS and XRD, C_f/(Ti_0.2Zr_0.2Hf_0.2Nb_0.2Ta_0.2)C-SiC with uniform phase and element distribution were successfully fabricated by precursor infiltration and pyrolysis. The as-fabricated composites have a density and open porosity of 2.40 g/cm³ and 13.32 vol% respectively, with outstanding bending strength (322 MPa) and fracture toughness (8.24 MPa m^1/2). The C_f/(Ti_0.2Zr_0.2Hf_0.2Nb_0.2Ta_0.2)C-SiC composites also present excellent ablation resistant property at a heat flux density of 5 MW/m², with linear and mass recession rates of 2.89 μm/s and 2.60 mg/s respectively. The excellent combinations of mechanical and ablation resistant properties make the C_f/(Ti_0.2Zr_0.2Hf_0.2Nb_0.2Ta_0.2)C-SiC composites a new generation of reliable ultra-high temperature materials.     

Effects of preform structures on the mechanical and ablation properties of C/ZrC-SiC composites

In order to investigate the effects of preform structures on the mechanical and ablation properties of C/ZrC-SiC composites, 3D4X, 3D5X and 3DZC C/ZrC-SiC composites were fabricated with the same process. The mechanical and ablation properties of 3D4X, 3D5X, and 3DZC C/ZrC-SiC composites were investigated. Results showed that the tensile strength (122.26 MPa) and bending strength (233.29 MPa) of 3D5X C/ZrC-SiC composites were the largest, followed by the tensile strength (112.79 MPa) and bending strength (203.03 MPa) of 3DZC composites and the tensile strength (86.22 MPa) and bending strength (137.59 MPa) of 3D4X composites. The mechanical properties of C/ZrC-SiC composites were mainly related to the fiber content in the axis direction and matrix compactness. In terms of ablation properties, 3DZC C/ZrC-SiC composites acted out the worst performance (the linear ablation rates of 0.0293 mm/s and the mass ablation rates 0.00766 g/s), followed by 3D4X composites (the linear ablation rates of 0.0276 mm/s and the mass ablation rates 0.00683 g/s) and 3D5X composites (the linear ablation rates of 0.0175 mm/s and the mass ablation rates 0.00653 g/s), respectively, which were mainly due to the specific ablation angles, thermal conductivities, and ablation oxides contents caused by fiber volume fraction, braided angles, and other forming parameters.     

Photoluminescence mechanism of annealed ZnO/Zn/Al2O3 sandwich structures deposited on glass substrates

ZnO/Zn/Al₂O₃ sandwich structures are grown on glass substrates by magnetron sputtering. The effect of Al₂O₃ layers on optical properties of ZnO/Zn/Al₂O₃ sandwich structures is investigated. Results indicated that as the deposition time of Al₂O₃ increases, violet peak centered at 402 nm gradually shifted to 412 nm and the intensity firstly decreases and then increases. We discuss the intensity change and shift of violet peak relating to V_Zn defects and the band alignment of ZnO/Zn/Al₂O₃ sandwich structures, respectively. We proposed that ZnO/Zn/Al₂O₃ sandwich structures can be approximately regarded as a quasiquantum-well-like structure. So the electron tunneling from Zn to Al₂O₃ layer is suppressed and the photogenerated carriers can be confined in the Zn Fermi level. In order to further understand the effect of posttreatment on optical properties of samples, samples are annealed in vacuum at 350 °C for 1 h. PL emissions are weakened with the increase of Al₂O₃ deposition time. Interestingly, at a same deposition condition, PL emissions are still improved after posttreatment. Combined Al₂O₃ layer modulation with annealing treatment, steady PL properties can be effectively improved.     

Evaluation of the moulding process for production of short-fibre-reinforced C/C-SiC composites

For the production of C/C-SiC brake discs via the liquid silicon infiltration method (LSI), the hot pressing process is the state of art technique for the moulding of the CFRP composites. This technique consists of several manual steps which increase production cost. The overall cost can be reduced by implementing injection moulding process.In this paper the influence of the moulding process (hot pressing, injection moulding) on the properties of semi-finished and final products during the production of short-fibre-reinforced C/C-SiC composites by means of the LSI process are examined. The starting polymer is chemically characterised. Carbon-fibre-reinforced plastic (CFRP) composites are fabricated by hot pressing, as well as injection moulding process. The CFRP composites are converted into porous C/C composites by pyrolysis. Liquid silicon is infiltrated to form dense C/C-SiC composites, which are further investigated during the course of this paper. Significant differences in properties of the composites are discussed.