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1.
High-dense SiC-(TixZr1?x)B2 composite ceramics were fabricated by in-situ synthesis of (TixZr1?x)B2 solid solution using solid-state spark plasma sintering (SPS). 64 vol% SiC, 20 vol% ZrB2, 15 vol% TiB2, and 1 vol% graphite powders are chosen as raw materials. The composite ceramics has the relative density of 99.97 %, the Vickers hardness of 24.71 GPa, the flexure strength of 435 MPa and the fracture toughness of 8.05 MPa ? m1/2. Compared with the single-phase SiC ceramics and SiC-TiB2 composite ceramics, the fracture toughness of SiC-(TixZr1?x)B2 composite ceramics increased by 242.6 % and 53.6 %, respectively. A shell-core structure is found in the SiC-(TixZr1?x)B2 composite ceramics, in which (TixZr1?x)B2 solid solution is the core and fine SiC grain is the shell. The results show that the toughening effect of solid-state sintered SiC-(TixZr1?x)B2 composite ceramics is attributed to the shell-core structure.  相似文献   

2.
Hf0.95Nb0.05B2 ceramics and their composites containing 20 vol% SiC were prepared via high-pressure spark plasma sintering in the study. The densification, microstructures, and mechanical properties of the prepared materials were then investigated. It is challenging to achieve full densification of HfB2 ceramics, even with markedly refined Hf0.95Nb0.05B2 solid solution powder under the sintering conditions of 2000 °C/30 MPa. However, under the sintering conditions of 1700 °C/200 MPa, a dense microstructure of Hf0.95Nb0.05B2 ceramics was achieved. Moreover, the Hf0.95Nb0.05B2-20 vol% SiC composite was densified at a lower temperature (1500 °C) and exhibited ultrafine grains (300 nm) and high-density defects, including stacking faults, Lomer-Cottrell locks, and twins, thus resulting in exceptional comprehensive mechanical properties, such as ultra-high hardness (32 GPa) and significantly improved fracture toughness (5.2 MPa.m1/2).  相似文献   

3.
《Ceramics International》2022,48(1):199-204
MgNb2-xVx/2O6-1.25x (0.1≤x≤0.6) ceramics with orthorhombic columbite structures were prepared at low-temperature by a solid-phase process. The phase component, microscopic morphology, low-temperature sintering mechanism and microwave dielectric performance of MgNb2-xVx/2O6-1.25x ceramics were comprehensively investigated. Low-temperature sintering densification of dielectric ceramics was achieved via the nonstoichiometric substitution of vanadium (V) at the Nb-site. In contrast to pure MgNb2O6 ceramics, the sintering temperature of MgNb2-xVx/2O6-1.25x (x = 0.2) ceramics was reduced by nearly 300 °C owing to the liquid-phase assisted sintering mechanism. The liquid phase arises from the autogenous low-melting-point phase. Meanwhile, MgNb2-xVx/2O6-1.25x (x = 0.2) samples with nonstoichiometric substitution could achieve a more than 900% improvement in the Q × f value, compared with stoichiometrically MgNb2-xVxO6 (x = 0.1, 0.2) ceramics. Finally, MgNb2-xVx/2O6-1.25x dielectric ceramics possess outstanding microwave dielectric properties: εr = 20.5, Q × f = 91000, and τf = -65 ppm/°C when sintered at 1030 °C for x = 0.2, which provides an alternative material for LTCC technology and an effective approach for low-temperature sintering of Nb-based microwave dielectric ceramics.  相似文献   

4.
The effects of the starting SiC powder (α or β) with the addition of 5.67 wt% AlN–Y2O3–CeO2–MgO additives on the residual porosity and thermal conductivity of fully ceramic microencapsulated (FCM) fuels were investigated. FCM fuels containing ~41 vol% and ~37 vol% tristructural isotropic (TRISO) particles could be sintered at 1870 °C using α-SiC and β-SiC powders, respectively, via a pressureless sintering route. The residual porosities of the SiC matrices in the FCM fuels prepared using the α-SiC and β-SiC powders were 1.1% and 2.3%, respectively. The thermal conductivities of FCM pellets with ~41 vol% and ~37 vol% TRISO particles (prepared using the α-SiC and β-SiC powders, respectively) were 59 and 41 Wm?1K?1, respectively. The lower porosity and higher thermal conductivity of FCM fuels prepared using the α-SiC powder were attributed to the higher sinterability of the α-SiC powder than that of the β-SiC powder.  相似文献   

5.
Ultrafine HfB2 powders were synthesized by the combination of borothermal reduction of HfO2 and solid solution of 5 mol% TiB2 or 5 mol% TaB2, prototypically, (Hf0.95Ti0.05)B2 and (Hf0.95Ta0.05)B2. The influence of substitution on the particle growth, high-temperature stability, densification, microstructure, and mechanical properties of HfB2 was investigated. Results showed that the particle sizes of HfB2, (Hf0.95Ti0.05)B2 and (Hf0.95Ta0.05)B2 powders prepared by borothermal reduction at 1500°C were 1.73, 0.87, and 0.21 µm, respectively. The substitution of TaB2 led to a greater decrease in particles size than TiB2. After heat treatment at 1800°C, the particle sizes of HfB2, (Hf0.95Ti0.05)B2 and (Hf0.95Ta0.05)B2 powders increased to 2.60, 1.59, and 0.32 µm, respectively, indicative of the good high-temperature stability of TaB2-substituted HfB2. The relative densities of HfB2, (Hf0.95Ti0.05)B2 and (Hf0.95Ta0.05)B2 ceramics after spark plasma sintering at 2000°C were 76.1%, 85.2% and 99.8%, respectively. The fully dense (Hf0.95Ta0.05)B2 ceramics with fine microstructure showed comparably high Vickers hardness of 21.1 GPa combined with flexural strength of 521.2 MPa. It was proved that the solid solution of TaB2 could effectively inhibit the grain growth of HfB2 powders, and improve the densification, microstructure, and mechanical properties of HfB2 ceramics.  相似文献   

6.
《Ceramics International》2021,47(19):26898-26906
Ln2(Hf2-xLnx)O7-x/2 (Ln = Sm, Eu; x = 0.1) pyrochlores have been prepared via mechanical activation of oxide mixtures, followed by heat treatment for 4h at 1450 and 1600 °C, respectively. According to the ESR data, the Eu cations on the Hf site in the Hf1-xEuxO6 octahedra in pyrochlore Eu2(Hf2-xEux)O7-x/2 (x = 0.1) are most readily oxidized and reduced. Oxidation at 840 °C for 24h in air reduces the total conductivity of the Ln2(Hf2-xLnx)O7-x/2 (Ln = Sm, Eu; x = 0.1) by a factor of 2.5–6, due to the decrease in the concentrations of oxygen vacancies and Ln2+ ions as a result of the oxidation. The anomalous low-frequency behavior of the permittivity of the Eu2(Hf2-xEux)O7-x/2 (x = 0.1) at ~800 °C can be understood in terms of the changes in the oxygen sublattice of the pyrochlore structure as a result of the oxidation of divalent europium and partial filling of oxygen vacancies at this temperature.  相似文献   

7.
Mg(Ti1-xNbx)O3 (x = 0–0.09) ceramics were prepared by the conventional solid-state reaction method. The phase composition, sintering characteristics, microstructure and dielectric properties of Ti4+ replacement by Nb5+ in the formed solid solution Mg(Ti1-xNbx)O3 (x = 0–0.09) ceramics were systematically studied. The structural variations and influence of Nb5+ doping in Mg(Ti1-xNbx)O3 were also systematically investigated by X-ray diffraction and Raman spectroscopy, respectively. X-ray diffraction and its Rietveld refinement results confirmed that Mg(Ti1-xNbx)O3 (x = 0–0.09) ceramics crystallised into an ilmenite-type with R-3 (148) space group. The replacement of the low valence Ti4+ by the high valence Nb5+ can improve the dielectric properties of Mg(Ti1-xNbx)O3 (x = 0–0.09). This paper also studied the different sintering temperatures for Mg(Ti1-xNbx)O3 (x = 0–0.09) ceramics. The obtained results proved that 1350 °C is the best sintering temperature. The permittivity and Q × f initially increased and then decreased mainly due to the effects of porosity caused by the sintering temperature and the doping amount of Nb2O5, respectively. Furthermore, the increased Q × f is correlated to the increase in Ti–O bond strength as confirmed by Raman spectroscopy, and the electrons generated by the oxygen vacancies will be compensated by Nb5+ to a certain extent to suppress Ti4+ to Ti3+, which was confirmed by XPS. The increase in τf from ?47 ppm/°C to ?40.1 ppm/°C is due to the increment in cell polarisability. Another reason for the increased τf is the reduction in the distortion degree of the [TiO6] octahedral, which was also confirmed by Raman spectroscopy. Mg(Ti0.95Nb0.05)O3 ceramics sintered at 1350 °C for 2 h possessed excellent microwave dielectric properties of εr = 18.12, Q × f = 163618 GHz and τf = ?40.1 ppm/°C.  相似文献   

8.
《Ceramics International》2020,46(10):16119-16125
Ba1-xCaxMoO4 (0 ≤ x ≤ 0.20) ceramics were prepared from powders to form solid solutions by a solid-state reaction sintering process. The influence of the Ca2+ content on the microstructure, sintering, densification, microwave dielectric properties and chemical stability of BaMoO4-based ceramics with Ag metal was discussed in detail. The sintering temperatures of the Ba1-xCaxMoO4 ceramics were effectively reduced to less than 950 °C by the formation of the solid solutions. Structural analysis indicates that the Ba1-xCaxMoO4 ceramics belong to the class of tetragonal scheelites. The crystal grain size begins to decrease and become more regular as x increases from 0 to 0.12. However, as x continues to increase, a liquid phase begins to appear, and the grain boundaries are no longer clear. The εr value increases from approximately 8.6 to 9.8 as x increases from 0 to 0.2. The Ba0.92Ca0.08MoO4 sample possesses the best microwave dielectric performance, namely an εr = 9.3 and the maximum Q × f value of 33593 GHz. The addition of 15 wt% TiO2 or 10 wt% CaTiO3 can effectively change the τf values of the Ba1-xCaxMoO4 ceramics to approximately 0. The Ba1-xCaxMoO4 ceramic samples can coexist with silver during the LTCC cofiring process.  相似文献   

9.
ZrB2-MeC and ZrB2-19 vol% SiC-MexCy where Me=Cr, Mo, W were obtained by pressureless sintering. The capability to promote densification of ZrB2 and ZrB2-SiC matrices is the highest for WC and lowest for Cr3C2. The interaction between the components results in the formation of new phases, such as MeB (MoB, CrB, WB), a solid solution based on ZrC, and a solid solution based on ZrB2. The addition of Cr3C2 decreases the mechanical properties. On the other hand, the addition of Mo2C or WC to ZrB2-19 vol% SiC composite ceramics leads increased mechanical properties. Long-term oxidation of ceramics at 1500 °C for 50 h showed that, in binary ZrB2-MexCy, a protective oxide scale does not form on the surface thus leading to the destruction of the composite. On the contrary, triple composites showed high oxidation resistance, due to the formation of dense oxide scale on the surface, with ZrB2-SiC-Mo2C displaying the best performance.  相似文献   

10.
《Ceramics International》2017,43(6):5343-5346
A polycrystalline SiC ceramic prepared by pressureless sintering of α-SiC powders with 3 vol% Al2O3-AlN-Y2O3 additives in an argon atmosphere exhibited a high electrical resistivity of ~1013 Ω cm at room temperature. X-ray diffraction revealed that the SiC ceramics consisted mainly of 6H- and 4H-SiC polytypes. Scanning electron microscopy and high resolution transmission electron microscopy investigations showed that the SiC specimen contained micron-sized grains surrounded by an amorphous Al-Y-Si-O-C-N film with a thickness of ~4.85 nm. The thick boundary film between the grains contributed to the high resistivity of the SiC ceramic.  相似文献   

11.
《Ceramics International》2023,49(19):31517-31523
In this study, a dual charge-compensator formulation was developed for zirconolite with the nominal composition Ca1-xCexZrTi2-2xFexCrxO7 (x = 0–0.30). The design strategy here was such that trivalent Fe and Cr were both targeted to substitute across the Ti site(s) to charge balance an inventory of CeO2 included as a structural analogue for Pu. The targeted solid solution was prepared by sintering constituent oxides at 1400 °C for 10 h under an air atmosphere. By means of powder XRD refinement and selected area electron diffraction analysis, the dominant zirconolite polytype was confirmed to be 2M across the solid solution. The obtained product density was significantly increased when compared to the previously discussed Ca1-xCexZrTi2-2xCr2xO7 system, suggesting that the partial inclusion of Fe in a 1:1 molar ratio with Cr may improve sintering behaviour. The limit of solid solution was reached at approximately x = 0.30, for which the segregation of CeO2 and Cr2O3 phases was clearly evidenced. An evaluation of obtained chemical compositions and bulk oxidation states was performed to inform the solid solution mechanism of Ce, Cr and Fe within zirconolite.  相似文献   

12.
《Ceramics International》2022,48(22):33563-33570
Lanthanum hafnate (La2Hf2O7) with a pyrochlore structure has excellent high temperature stability and low thermal conductivity, which is promising for thermal/environmental barrier coatings (T/EBCs) applications. To reduce its thermal expansion coefficient (TEC) so as to better match SiCf/SiC composites, a smaller tetravalent dopant Ti4+ has been introduced in the Hf-sites to form La2(Hf1-xTix)2O7 (x ≤ 0.20). The phase composition and microstructure confirms that La2(Hf1-xTix)2O7 solid solutions possess a pure pyrochlore structure. With an increase of x, their TECs are decreasing consistently, whilst their thermal conductivities of La2(Hf1-xTix)2O7 are slightly increasing at high temperature but still much lower than those of meta-stable yttria partially stabilized zirconia, both of which are attributing to an increase of elastic modulus after Ti4+ doping on Hf-sites. The extremely excellent high temperature stability, relatively low thermal conductivities and low TECs suggest that La2(Hf1-xTix)2O7 is a prospective candidate material for T/EBC applications.  相似文献   

13.
Temperature above 2000°C and additional pressure is generally required to achieve the full densification of TaxHf1−xC-based ceramics. This work proposed a novel method to fabricate dense Ta0.2Hf0.8C ceramics at relatively low temperature. Using a small amount of Si as a sintering aid, Ta0.2Hf0.8C was densified at 1700°C by reactive hot-pressing (RHP), with SiC formed in situ. Microstructure evolution mechanisms of the ceramics during RHP were investigated. The effect of silicon content on the densification and mechanical properties of the ceramics was revealed. It is indicated that the apparent porosity of the Ta0.2Hf0.8C–SiC ceramics was as low as 0.5%, whereas bending strength and fracture toughness of the ceramics were as high as ∼637 MPa and 6.7 MPa m1/2, respectively, when the silicon content was 8 wt.%. This work provides a new idea for the low-temperature densification of TaxHf1−xC and other ultrahigh temperature ceramics with high performance.  相似文献   

14.
(Hf1-xZrx)B2 solid solution powders were synthesized by two methods. First, solution-based processing of HfCl4, ZrCl4, sucrose, and H3BO3 was conducted followed by heat treatment in Argon to carry out the carbothermal reduction (CTR) reaction to form the diboride powders. Alternatively, in the so-called borohydride reduction (BHR) method, HfCl4, ZrCl4 and NaBH4 were mixed in an Argon glove box followed by heat treatment in Argon at 700?1500 °C. The synthesized powders were characterized by XRD, SEM, TEM, EDS, and TGA, and the influence of different parameters such as starting composition, heat treatment temperature and time on products characteristics were revealed. Both CTR and BHR solid solution powders were then consolidated within ~5 min in a homemade flash sintering (FS) setup. The composition, microstructure, hardness, and thermal-oxidation properties of flash sintered ceramics were characterized, and the implication of this study and directions for future research were discussed.  相似文献   

15.
《Ceramics International》2022,48(18):26452-26459
To reduce the negative effects of the long-time and B2O3 phase on the traditional sintering process for B4C-based composite ceramics, nearly fully dense B4C–VB2 composite ceramics were prepared by reactive spark plasma sintering (SPS) technology at 2000 °C with B and V8C7 powders as raw materials in this paper. The effects of the degassing time during SPS on the microstructure and the mechanical properties of the final products were investigated in detail. The results revealed that the proper degassing time was beneficial for the vent of B2O3 during the sintering process, which refined the grain size, promoted densification and improved the mechanical properties of the composite ceramic. However, the redundant degassing time increased the holding time at high temperature, resulting in abnormal grain growth and mechanical performance deterioration. In the present work, the optimal degassing time was 6 min, and the final product prepared under the above conditions exhibited excellent comprehensive performance with a relative density of 99.2%, Vickers hardness of 31.2 GPa, bending strength of 654 MPa and fracture toughness of 5.7 MPa m1/2. In addition, the strengthening and toughening mechanisms of the products were mainly attributed to the residual thermal stresses and bridging structure caused by the fine B4C and VB2 grains distributed uniformly.  相似文献   

16.
《Ceramics International》2017,43(16):13047-13054
Zr-Al-C was in-situ synthesized as a toughening component in ZrB2-SiC ceramics by spark plasma sintering (SPS) ball-milled ZrB2-based composite powders with SiC and graphite powders. The phase composition of Zr-Al-C toughened ZrB2-SiC (ZSA) composite ceramics fabricated through the two-step process (ball milling and SPS) did not change dramatically with varying content of Zr-Al-C which shows a major phase of Zr3Al4C6. With increasing Zr-Al-C content, the fracture toughness of the ZSA ceramics initially increased and then decreased when the content reached 40 vol%. The ZSA ceramic with 30 vol% Zr-Al-C exhibited a maximum fracture toughness value of 5.96 ± 0.31 MPa m1/2, about 22% higher than that of the ZSA ceramic with 10 vol% Zr-Al-C. When the Zr-Al-C content goes beyond 30 vol%, the higher open porosity and component agglomeration led to the relatively lower fracture toughness. Crack deflection and bridging resulted from the weak interface bonding between Zr-Al-C and matrix phases and the weak internal layers of Zr-Al-C crystals, leading to longer crack paths and, hence, the toughened ZSA composite ceramics. Compared to the one-step in-situ synthesis process of Zr-Al-C and the direct incorporation process of synthesized Zr-Al-C grains, the two-step in-situ synthesis process not only led to the more uniform distribution of different components but also resulted in a much larger size of Zr-Al-C grains with a large aspect ratio causing longer crack propagation path as the result of crack deflection and bridging. The larger Zr-Al-C grains combined with the more homogeneous microstructure achieve the most substantial toughening of the ZSA composite ceramics. This work points out a promising approach to control and optimize the microstructure and improve the fracture toughness of ZrB2-SiC composite ceramics by selecting the incorporation process of compound reinforcement components.  相似文献   

17.
The Li1+xAlxTi2?x(PO4)3 (LATPx) series displays the highest “bulk” reported conductivity, but a much lower “overall” contribution, that changes with the powder preparation and sintering conditions. In this work, the preparation of LATPx ceramics is discussed, by using the sol-gel technique for powders synthesis and mild spark plasma (SPS) for ceramics sintering at 800 °C. An “overall” conductivity ~ 2.10?3 Ω?1 cm?1 was obtained for the x = 0.4 composition, that was the result of a high “bulk” conductivity, an optimized microstructure and almost full density, in absence of micro-cracks, with a small content of secondary phases and clean grain boundaries. Fast-ion ceramics prepared by SPS are good candidates for solid electrolytes in all solid state batteries (ASSB).  相似文献   

18.
《Ceramics International》2023,49(3):4290-4297
Li(Al1-xLix)SiO4-x (x = 0.005, 0.01, 0.015, and 0.02) ceramics were synthesized via a traditional solid phase reaction method with different sintering temperatures. To determine the positions occupied by Li+ in the lattice, the defect formation energies and total energies of various sites of LiAlSiO4 (LAS) occupied by Li+ were examined, and the energy of LAS systems were calculated using density functional theory of first-principle with the CASTEP module. The results demonstrated that the Al-sites occupied by Li+ had the lowest formation energies and total energy, so Li + should substitute Al3+. The impacts of replacing Al3+ with Li+ on the bulk density, sintering properties, phase composition, microstructure, and microwave dielectric properties of Li(Al1-xLix)SiO4-x (0 = x ≤ 0.02) ceramics were thoroughly studied. With Li+-doping, the sintering temperature decreased from 1300 °C (x = 0) to 1175 °C (x = 0.02), while the Q × f and τf values of LAS ceramics significantly increased. The Li(Al0.99Li0.01)SiO3.99 ceramic was fully sintered at 1250 °C for 10 h to obtain excellent microwave dielectric properties: εr = 3.49, Q × f = 51,358 GHz, and τf = ?51.48 × 10?6 °C?1.  相似文献   

19.
Perovskite solid solution ceramics of (1 ? x)BaTiO3xBi(Mg2/3Nb1/3)O3 (BT–BMN) (= 0.05–0.2) were synthesized by solid‐state reaction technique. The results show that the BMN addition could lower the sintering temperature of BT‐based ceramics. X‐ray diffraction results reveal a pure perovskite structure for all studied samples. Dielectric measurements exhibit a relaxor‐like characteristic for the BT–BMN ceramics, where broadened phase transition peaks change to a temperature‐stable permittivity plateau (from ?50°C to 300°C) with increasing the BMN content (= 0.2), and slim polarization–electric field hysteresis loops were observed in samples with ≥ 0.1. The dielectric breakdown strength and electrical resistivity of BT–BMN ceramics show their maxima of 287.7 kV/cm and 1.53 × 1013 Ω cm at = 0.15, and an energy density of about 1.13 J/cm3 is achieved in the sample of = 0.1.  相似文献   

20.
《Ceramics International》2022,48(16):22967-22974
A novel single-source precursor was synthesized to prepare HfCxN1-x/SiC multiphase ceramics by using hafnium chloride (HfCl4), diallylamine (DAA) and polycarbosilane (PCS). We conducted an investigation of the synthesis process, polymer-to-ceramic conversion, as well as the microstructure and phase evolution of HfCxN1-x/SiC multiphase ceramics with different levels of SiC content. The results showed that the core-shell particles of HfCxN1-x-carbon were embedded homogeneously in the β-SiC matrix which is beneficial for preventing grain growth and improving oxidation resistance. Based on data from oxidation tests, the ceramics improved the oxidation temperature and remained stable at a high temperature (1500 °C) with oxidation layer formation on the surface. Due to the highly cross-linked structure without oxygen, high ceramic yield, homogeneous composition and excellent oxidation resistance of the pyrolysis product, the as-prepared precursor is a promising material for making high-performance composite ceramics.  相似文献   

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