Manufacturing of ceramic matrix composite using a hybrid process combining TiSi2 active filler infiltration and preceramic impregnation and pyrolysis

The manufacturing of silicon carbide reinforced ceramic matrix composites by a hybrid process is explored. Fibre preforms are infiltrated with TiSi₂ powders using the slurry method. Using TiSi₂ active filler leads to reduce the porosity by the subsequent formation of nitride phases after treatment under N₂ atmosphere at low temperatures (≤1100 °C). Taking into account the influence of the specific surface area of the powder on the nitridation rate, it is shown that it is possible to produce nitrides TiN and Si₃N₄ at 1100 °C with an interesting volume expansion inside the composite. To complete the densification of the composite, a polymer impregnation and pyrolysis (PIP) process are performed with a liquid polymeric precursor. Characterizations of the composites show that mechanical properties are improved with the presence of the TiN and Si₃N₄ phases, and the number of PIP cycles.     

Characterization and transport properties of ceramic filler incorporated natural rubber composites

Crystalline glass–ceramic fillers were prepared from calcium carbonate, silica, alumina, and calcium fluoride by heating and subsequent quenching in cold water. The fillers were incorporated into natural rubber (1,4-cis-polyisoprene) and the filled rubber composites were crosslinked with sulfur in the presence of different rubber additives. The unfilled and filled rubber composites were characterized. The transport properties of benzene, toluene, and p-xylene (BTX) through the rubber composites were studied in terms of sorption, diffusion, permeation, and mass transfer coefficients. The effect of the ceramic fillers on the mechanical, thermal and transport properties were studied. The sorption data at different temperatures were used for calculating activation energy of diffusion, permeation, free energy, and enthalpy of sorption. The BTX remained in the liquid state within the composite matrix as evident from negative ΔS. The diffusion coefficient (D) and mass transfer coefficient (k_mtc) of BTX decreased with the increase in filler loading. Accordingly, for the transport of BTX the unfilled rubber showed a D (D × 10⁷ cm²/s) and mass transfer coefficient (k_mtc × 10⁴ cm/s) of 5.67/3.97/2.96 and 7.71/7.08/7.04, respectively which decreased to 5.06/2.95/2.57 and 7.53/6.95/6.90, respectively for the composite containing 50 wt.% ceramic filler.     

Interaction of fiber matrix bonding in SiC/SiC ceramic matrix composites

Non-oxide ceramic matrix composites (CMC) based on SiC fibers with SiC matrix were fabricated by polymer infiltration and pyrolysis (PIP) and characterized regarding their microstructural features and their mechanical properties. The fiber preform was made using winding technology. During the winding process, the SiC fiber roving was impregnated by a slurry containing SiC powder and sintering additives (Y₂O_3, Al₂O₃ and SiO₂). This already helped to achieve a partial matrix formation during the preform fabrication. In this way, the number of PIP cycles to achieve composites with less than 10% open porosity could be reduced significantly. Additionally, damage-tolerant properties of the composites were obtained by an optimal design of the matrix properties although only uncoated fibers were used. Finally, composites with a strength level of about 500 MPa and a damage-tolerant fracture behavior with about 0.4% strain to failure were obtained.     

Laser-supported joining of SiC-fiber/SiCN ceramic matrix composites fabricated by precursor infiltration

SiC-fiber/SiCN ceramic matrix composites were manufactured by means of polymer infiltration and pyrolysis. The fiber preform was made by slurry infiltration and winding using a computer-controlled winding module. Multiple infiltration steps using a Si–C–N precursor were included to increase the density. The influence of the sintering conditions on the microstructure of the CMC was demonstrated.Pipe sections made of the CMC materials were joined using a laser-supported heating technology with an Y–Al–Si–O glass–ceramic filler. The thermal response of the CMC components was controlled by the anisotropic thermal conductivity. Fast heating by laser beam was achieved for elements rotating in the direction of the fiber winding. SEM micrographs of the joints showed the good wettability of the CMC by the glass–ceramic filler. Nearly defect-free joints were obtained using a nitrogen process atmosphere. The laser-supported technology was shown to be promising for the joining of CMC components.     

Fabrication of carbon fiber reinforced ceramic matrix composites with improved oxidation resistance using boron as active filler

Boron was introduced into C_f/SiC composites as active filler to shorten the processing time of PIP process and improve the oxidation resistance of composites. When heat-treated at 1800 °C in N₂ for 1 h, the density of composites with boron (C_f/SiC-BN) increased from 1.71 to 1.78 g/cm³, while that of composites without boron (C_f/SiC) decreased from 1.92 to 1.77 g/cm³. So when boron was used, two cycles of polymer impregnation and pyrolysis (PIP) could be reduced. Meanwhile, the oxidation resistance of composites was greatly improved with the incorporation of boron-bearing species. Most carbon fiber reinforcements in C_f/SiC composite were burnt off when they were oxidized at 800 °C for 10 h. By contrast, only a small amount of carbon fibers in C_f/SiC-BN composite were burnt off. Weight losses for C_f/SiC composite and C_f/SiC-BN composite were about 36 and 16 wt%, respectively.     

高温熔烧法制备金属基陶瓷涂层的研究

以玻璃熔块、氧化铬粉、粘土粉和硅酸锆微粉为原料制成的涂料,用滚涂法将其均匀涂覆在不锈钢管上,经高温(1000~1050℃保温20min)熔烧制备出了耐磨、抗高温氧化的陶瓷涂层。对陶瓷涂层的耐磨性、抗高温氧化性、抗热震性等性能进行了测试,并对影响涂层性能的因素进行了研究。结果表明:引入具有较大热膨胀系数的玻璃熔块料有利于提高涂层结合性;加涂层的试样均能明显改善基体的耐磨性和抗高温氧化性。涂层的耐磨性随硅酸锆微粉加入量的增加而提高,加入量为15%时耐磨性和抗热震性最好,其热震循环(1000℃空冷)可达22次。     

复合固体推进剂填料/基体脱湿研究进展

概述了复合固体推进剂脱湿的表征方法,分析了各表征方法的优缺点,以及各表征方法适合研究脱湿的范畴,提出了可能的改进方向.概述了各因素对脱湿的影响:内因包括黏合剂基体模量,固体大颗粒含量、粒度、形貌等;外因包括测试温度、拉伸速率、应变率、湿热老化、环境压强等.提出对应的减少各因素影响脱湿发生的方法.     

Reactive wetting behavior and mechanism of AlN ceramic by CuNi-Xwt%Ti active filler metal

In order to propel the application of the developed CuNi-Xwt%Ti active filler metal in AlN brazing and get the universal reactive wetting mechanism between liquid metal and solid ceramic, the reactive wetting behavior and mechanism of AlN ceramic by CuNi-Xwt%Ti active filler metal were investigated. The results indicate that, with the increasing Ti content, surface tension for liquid CuNi-Xwt%Ti filler metal increases at low-temperature interval, but very similar at high-temperature interval, which influence the wetting behavior on AlN ceramic obviously. CuNi/AlN is the typical non-reactive wetting system, the wetting process including rapid wetting stage and stable stage. The wettability is depended on surface tension of the liquid CuNi filler metal completely. However, the wetting process of CuNi-8wt.%Ti/AlN and CuNi-16 wt%Ti/AlN reactive wetting system is composed by three stages, which are rapid wetting stage decided by surface tension, slow wetting stage caused by interfacial reaction and stable stage. For CuNi-8wt.%Ti/AlN and CuNi-16 wt%Ti/AlN reactive wetting system, although the surface tension of liquid filler metal is the only factor to influence the instant wetting angle θ₀ at rapid wetting stage, the reduced free energy caused by interfacial reaction at slow wetting stage plays the decisive role in influencing the final wettability.     

活性污泥法污水处理应用亲水性填料实验研究

亲水性填料比普通填料可提高好氧处理工艺的效率2％～10％,在活性污泥法污水处理曝气池中通过添加亲水性填料,最佳污泥回流比从70％降为40％,并可以提高污水处理效率,增加处理装置的容积负荷,从而可以增加现有污水处理厂的处理能力。     

Interfacial microstructure and mechanical properties of zirconia ceramic and niobium joints vacuum brazed with two Ag-based active filler metals

Reliable brazing of a zirconia ceramic and pure niobium was achieved by using two Ag-based active filler metals, Ag-Cu-Ti and Ag-Cu-Ti+Mo. The effects of brazing temperature, holding time, and Mo content on the interfacial microstructure and mechanical properties of ZrO₂/Nb joints were investigated. Double reaction layers of TiO and Ti₃Cu₃O formed adjacent to the ZrO₂ ceramic, whereas TiCu₄+Ti₂Cu₃+TiCu compounds appeared in the brazing interlayer. With increasing brazing temperature and time, the thickness of the Ti₃Cu₃O layer increased with consumption of the TiO layer, and the total thickness of the reaction layers increased slightly. Meanwhile, the blocky Ti-Cu compounds in the brazing interlayer tended to accumulate and grow. This microstructural evolution and its formation mechanism are discussed. The maximum shear strength was 157 MPa when the joints were brazed with Ag-Cu-Ti at 900 °C for 10 min. The microstructure and bonding properties of the brazed joints were significantly improved when Mo particles were added into the Ag-Cu-Ti. The shear strength reached 310 MPa for joints brazed with 8.0 wt% Mo additive, which was 97% higher than that of joints brazed with single Ag-Cu-Ti filler metal.     

Brazing ZrO2 ceramic and TC4 alloy by novel WB reinforced Ag-Cu composite filler: Microstructure and properties

Residual stresses in ceramic-metal joints is the important factor for their reliable implementation in cutting-edge industries. Composite fillers is reported to be a promising approach to reduce the residual stresses. Until now, few experimental researches on the brazing of ZrO₂ ceramic and TC4 alloy using composite fillers have been reported. In this study, to release the residual stresses and improve the joints strength, novel WB reinforced Ag-Cu composite filler was fabricated to braze ZrO₂ ceramic and TC4 alloy. Scanning electron microscope (SEM), energy dispersive spectroscopy (EDS) and transmission electron microscopy (TEM) were applied for the analysis of microstructure and phases structure in the joints. The TiB whiskers and W particles were in situ synthesized via the reaction between active Ti and WB particles, and randomly distributed in the brazing seam. The effect of brazing temperature and WB content on interfacial microstructure and mechanical strength in the brazed joints were investigated. When brazed at 870 °C for 10 min, favorable microstructure reinforced by TiB whiskers and W particles in the brazing seam was achieved with 7.5 wt% WB addition in composite filler. The maximum average shear strength of the joints was 83.2 MPa, which about 59.4% increase over the joints without WB addition.     

Microstructural evolution and mechanical property of a SiCf/SiC composite/Ni-based superalloy joint brazed with an Au-Cu-Ti filler

A new Au-Cu-Ti filler featuring superior mechanical properties was developed to enable the brazing of a SiC_f/SiC composite (CMCs) to itself and a Ni-based superalloy (GH536). The progression of the interfacial reactions was studied using a combination of thermodynamic calculations and experimental observations. It was found that the interfacial reaction was Ti-dominant at the early brazing stage and then gradually transformed to Ni-dominant with the continuous dissolution of the GH536 substrate. Thus, the typical microstructure of GH536/Ti-Ni-Cr-Fe+(Au, Cu)ss + MoNiSi/Ni-Cr-Fe-Si-C (Ni₂Si + Fe₂Si + Cr₃C₂)+(Au, Cu)ss/Ni₂Si + TiC+(Au, Cu)ss/ Cr₃C₂+Ni₂Si + TiC + Fe₂Si/CMCs could be described by the following three stages: a Ti-dominated stage, full interdiffusion stage, and Ni-dominated stage. A maximum shear strength of 36 MPa was obtained for joints brazed at 1050℃ for 10 min, at which a failure occurred at the CMCs/brazing seam interface. The control of the interfacial reactions and the stress relaxation of (Au, Cu)ss contributed to the superior mechanical performance of the composite.     

Fabrication and mechanical properties of metal matrix composite with homogeneously dispersed ceramic particles

Titanium carbide (TiC) particles were coated with nickel (Ni) to increase their compatibility with a metal matrix, leading to an improvement in the dispersibility of TiC particles in the molten matrix. TiC particles were dispersed into a basic aqueous solution of pH 12, and then nickel nitrate (Ni(NO₃)₂), as a Ni precursor, was added to the TiC suspension. The interaction between the TiC particles and the Ni precursor is driven by the attractive force between the Ni cations and the TiC particles with negative charge. An inoculant (ferrosilicon), which has been used in the foundry industry to improve crystal growth of graphite, was used as a core particle. The Ni-treated TiC particles were coated onto the surface of the inoculant using an inorganic binder converted into its glass phase by sol–gel reactions. The reinforcement particles prepared through the dual-coating process were then injected into the molten matrix based on iron at 1500 °C. The crystal phase of the graphite is more finely and shortly grown in the reinforced metal matrix than in that without the reinforcement particles. This means that the reinforcement particles are homogeneously and uniformly dispersed into the matrix without any aggregation of particles, implying that the mechanical properties of the reinforced matrix would be greater than those of a non-reinforced matrix. Consequently, metal matrix composites with reasonable properties can be fabricated successfully using the reinforcement particles prepared by the dual-coating process.     

白云岩钙镁填料的制备及其应用

简要介绍了白云岩钙镁填料制备工艺,对其在橡胶、塑料及燃煤脱硫中的应用也一一作了介绍、说明白云岩钙镁填料是一种可以代替轻质碳酸钙的新型填料。     

Fabrication of unidirectional continuous fiber-reinforced mullite matrix composite with excellent mechanical property

This article reports the fabrication of continuous fiber reinforced mullite matrix composite via layer-by-layer assembly method, involving the coating of mullite fiber with BN coating, followed by compositing the coated fibers with mullite matrix and hot pressing. The influences of the fiber coating, fiber content and sintering temperature on the microstructure and mechanical properties of the composite are investigated. By optimizing the sintering temperature and fiber content, the damage of fiber could be avoided and the microstructure and mechanical properties could be improved. The composite containing 30?vol% fibers coated by BN layer sintered at 1300?°C exhibits 90.9% theoretical density with flexural strength value of 203.2?MPa and fracture toughness value of 4.74?MPa?m^1/2. Fracture behavior is investigated to explain the toughening mechanisms. The layer-by-layer assembly method realizes the achievement of an individual architecture featuring fibers distribution and weak interfaces.     

Oxidation behavior and high-temperature flexural property of CVD-SiC-coated PIP-C/SiC composites

Polymer infiltration pyrolysis (PIP) was used to prepare carbon fiber-reinforced silicon carbide (C/SiC) composites, and chemical vapor deposition (CVD) was employed to fabricate SiC coating. The oxidation behavior at 1700?°C and the flexural property at 1200?°C were tested. SiC coating exerted remarkable oxidation effects on PIP-C/SiC composites. In the absence of coating, PIP-C/SiC composites lost 29.2% of its mass, with merely 6.74% of the original flexural strength retained. In contrast, CVD-SiC coated PIP-C/SiC composites had the mass loss of 10.2% and the flexural strength retention ratio of 23.4%. In high-temperature tests, SiC coating played an important role in the flexural strength of PIP-C/SiC composites. The flexural strength of uncoated composites became 330.7?MPa, and that of coated ones reduced from 655.3 to 531.2?MPa.     

AKD-淀粉-碳酸钙复合填料的制备及应用

利用玉米淀粉、烷基烯酮二聚体(AKD)和重质碳酸钙(GCC)制备造纸用复合填料,并比较了复合填料与GCC填料的基本性能(如微观形貌、溶解性、溶胀度和接触角等)以及对纸张力学性能的影响。结果表明:随着AKD用量的增加,复合填料的溶胀度和溶解性略有下降,接触角明显增大;与GCC填料相比,复合填料能明显提高纸张的拉伸强度(99.1%)和耐破强度(98.9%),但纸张的光学性能略有降低;纸张的耐水性随着AKD用量的增加而明显提高;当w(AKD)=15%时,复合填料的应用效果最佳。     

Preparation and properties of a novel precursor-derived Zr-C-B-N composite ceramic via zirconocene and borazine

A novel preceramic polymer polyzirconocenyborazane (PZCBN) was synthesized by the polymerization of Bis(cyclopentadienyl)zirconium divinyl and borazine, introducing Zr, B, C, N together. The formation and concentration of elements Zr, C, B, N in the precursor and ceramic were detected through FTIR NMR, XRD, SEM and TEM. From the analysis, the Cp₂Zr(CH?CH₂)₂ and borazine linked together via the addition reaction between C?C and B-H. And after pyrolysis at 1200 °C, the precursor turned to ZrC/ZrB₂/BN composite ceramics, with a yield of 52 wt%. EDX resulted showed that the elements were well dispersed in the ceramics. According to SEM and TEM, the ceramic had a relatively dense structure with nano crystalline areas of ZrC embedded in the amorphous Zr-C-B-N matrix. TGA in air demonstrated that the ceramic had a favorable property on oxidation resistance.     

Microstructure and oxidation resistance of a multiphase Mo-Si-B ceramic coating on Mo substrates deposited by a plasma transferred arc process

To improve the oxidation resistance of a Mo substrate, a multiphase Mo-Si-B ceramic coating was deposited using a plasma transferred arc (PTA) process. The phase constituents, microstructure, and oxidation resistance of the coating were investigated. The results show that the microstructure of the Mo-Si-B coating is characterised by rod-like Mo₅SiB₂ dendrites, a lamellar structure of Mo₃Si/Mo₅SiB₂ binary eutectics, and cellular Mo₅Si₃ dendrites. Compared with the Mo substrate, the Mo-Si-B coating exhibits a significant improvement in the oxidation resistance at 1300?°C in an air atmosphere. This is mainly owing to a dense and continuous borosilicate layer formed on the surface of the Mo-Si-B coating, which acts as an oxygen diffusion barrier. Moreover, it is observed that the Mo₅SiB₂ dendrites exhibit a higher oxidation resistance compared to Mo₃Si/Mo₅SiB₂ eutectics during high-temperature oxidation exposure. The oxidation behaviour is discussed based on the oxidation kinetics and a cross-sectional microstructure analysis of the oxidised Mo-Si-B specimen.     

Microstructure observation and analysis of 3D carbon fiber reinforced SiC-based composites fabricated through filler enhanced polymer infiltration and pyrolysis

3D C/SiC-BN composites were fabricated by filler enhanced polymer infiltration and pyrolysis (FE-PIP) through in situ conversion of active filler boron into h-BN in the high temperature treatment process. The bending strengths and microstructures of composites were studied here. Interphase layers deposited on the fiber surfaces can prevent the strong bonding between fiber reinforcements and composite matrix and repair the defects on the fiber surface, which can improve the bending strength and toughness of composites. The bending stress of C/SiC-BN composites without interphase layer is about 170 MPa while those of composites with PyC or PyC/SiC interphase layers are higher than 300 MPa. Some large pores were left in the interwoven zones while intra-bundle zones were relatively dense, only a small amount of micro-pores could be observed. It could also be concluded that the length of pulled-out fibers was much longer and the pulled-out fiber surface was smoother when interphase layers were deposited. Because the matrix derived from the pyrolysis of slurries adheres to the fiber bundles, some phases with layered structures could be observed in the matrix near the reinforcements. The microstructure evolution of 3D fiber reinforced ceramic matrix composites were also analyzed in this work based on the observation of both 3D C/SiC-BN composites and 3D C/SiC composites fabricated by FE-PIP, where boron and SiC particles were applied as active fillers and inert fillers respectively.