Al2TiO5添加量对MgO-Al2TiO5复合陶瓷烧结及抗热震性的影响

以纳米MgO粉为原料,选用以纳米Al2O3粉和纳米TiO2粉经1500℃保温3 h烧结制备的Al2TiO5为添加剂,采用固相烧结法经1500℃保温3 h制备了Al2TiO5质量分数分别为0、5%、10%和20%的MgO-Al2TiO5复合陶瓷,并采用XRD、SEM和EDS等研究了Al2TiO5添加量对MgO-Al2TiO5复合陶瓷烧结性能及抗热震性能的影响。结果表明:添加Al2TiO5有利于促进复合陶瓷的烧结,其体积密度和线收缩率随Al2TiO5添加量的增加而增大,当Al2TiO5添加量为20%(w)时,其体积密度和线收缩率分别为3.68 g·cm-3和22.07%;当Al2TiO5添加量为10%(w)时,其抗热震性能最佳。Al2TiO5位于方镁石晶粒交界处,抑制方镁石晶粒生长,阻碍裂纹扩展,使MgO-Al2TiO5复合陶瓷的抗热震性能得到改善。     

Low-temperature reactive sintering of carbon vacant high-entropy carbide ceramics with in-situ formed silicon carbide

It is thought that the sintering of high-entropy (HE) ceramics is generally more difficult when compared to that of the corresponding single-component ceramics. In this paper, we report a novel approach to densify the HE carbide ceramics at relatively low temperatures with a small amount of silicon. Reactive spark plasma sintering (SPS) was used to densify the ceramics using powders of HE carbide and silicon as starting materials. Dense ceramics can be obtained at 1600 -1700°C. X-ray diffraction analysis reveals that only non-stoichiometric HE carbide phase with carbon vacancy and SiC phase exist in the obtained ceramics. The in-situ formed SiC phase inherits the morphology of the starting silicon powder owing to the slower diffusion of silicon atoms compared to that of the carbon atoms in HE carbide phase. The mechanical properties of the prepared ceramics were preliminarily studied.     

One-step cold sintering process towards translucent BaF2 ceramics

BaF₂ ceramics were prepared using a one-step cold sintering process with an ultra-low sintering temperature of 150 °C and uniaxial pressures ranging from 450 to 900 MPa. The relative density and microstructure improved steadily with the increasing pressure, and a fully densified microstructure with a relative density of 97.2% was achieved at 900 MPa. For BaF₂ ceramics with a thickness of 1 mm, the optimum in-line transmittance in the visible light region (58.5%) was achieved at a wavelength of 720 nm, and the maximum value (65.3%) was obtained at 1864 nm. The permittivity of the ceramics increased gradually from 6.18 to 7.09 with increasing pressure, and the dielectric loss was optimized from 0.01 to 0.003. Additionally, the mechanical properties improved continuously with the increasing pressure, and the optimal compressive strength (257 MPa), hardness (2.01 GPa), and Young's modulus (54.8 GPa) were achieved when cold sintered at 900 MPa.     

Middle-low temperature sintering and piezoelectric properties of CuO and Bi2O3 doped PMS-PZT based ceramics for ultrasonic motors

A ternary solid-solution piezoelectric ceramic of rare-earth oxides modified 0.03 Pb(Mn_1/3Sb_2/3)O₃-0.97 Pb(Zr_0.505Ti_0.495)O₃ + x wt.% CuO + y wt.% Bi₂O₃ (PMS-PZT + x wt.% CuO + y wt. % Bi₂O₃) (x, y = 0–0.2) was successfully prepared via a transient-liquid-phase sintering. Both Cu²⁺ and Bi³⁺ were believed to replace the A-site Pb ions and to evidently induce the lattice shrinkage and the distortion decrease. However, the addition of only a small amount of CuO was found to effectively reduce the sintering temperature, sustain good piezoelectric properties and predominant transgranular fracture modes, but obviously increase the average grain size and high-field dielectric loss. Further experimental results indicate that the grain growth of the ceramics was inhibited effectively and the high-field dielectric loss was reduced through CuO and Bi₂O₃ co-doping. The 0.05 wt% CuO and 0.15 wt% Bi₂O₃ co-doped PMS-PZT ceramics sintered at 1050 °C exhibit excellent dielectric and piezoelectric properties of d₃₃ = 410 pC/N, k_p = 0.62, Q_m = 1478, ε_r = 1550, tan δ = 0.8% (400 V/mm) and T_c = 330 °C. The experimental results can provide a solid fundament for multilayer piezoelectric actuating devices.     

Transparent polycrystalline MgO ceramic fabricated by low-temperature vacuum sintering with MgF2 additive

This study introduces transparent MgO ceramics produced via simply vacuum sintering at 1200–1500 °C by optimal incorporation of MgF₂ as a sintering additive. The effect of MgF₂ content and sintering temperature on the densification process, optical, and thermal properties of MgO ceramics is presented with emphasis on its function as a sintering aid and adverse effect of MgF₂ evaporation in the condition of high MgF₂ content or high sintering temperature. MgO ceramic with 1.0 mol% MgF₂ sintered at 1300 °C exhibits the highest relative density of 99.95% with average grain size of 17.46 μm. The in-line transmittance attains 60% at 1000 nm and >80% in the infrared range (3.8–6.8 μm), without absorption bands originated from the carbon contamination. The corresponding room-temperature thermal conductivity reaches 47.25 W/(m∙K). These results demonstrate that MgF₂ is an outstanding sintering additive for the preparation transparent MgO ceramics.     

Preparation of multicomponent A2Zr2O7 transparent ceramics by vacuum sintering

Recently, high-entropy oxide ceramics have become a hot topic in the field of high entropy materials. In this paper, multicomponent pyrochlore A₂Zr₂O₇ transparent ceramics were prepared via vacuum sintering using combustion synthesized nanopowders. The phase analysis results indicate that the powders exhibit defective fluorite structure and the ceramics are in pyrochlore structure. The structural order degree of ceramics varies with the increase of incorporated components. It is found that the grain size of A₂Zr₂O₇ ceramics is related with the component of A-site. The main fracture mode of final ceramics exhibit typical transgranular fracture. The multicomponent A₂Zr₂O₇ ceramics exhibit excellent optical transmittance, and the highest in-line transmittance reaches to 80% for #A2ZO ceramic at 1880 nm.     

氧化铝陶瓷低温烧结的研究现状和发展前景

本文综述了氧化铝陶瓷低温烧结的研究现状,包括粉体的制备,处理,成型及烧结工艺,并对此领域做了相应的设想和展望。     

Ultrafast high-temperature sintering of lanthanum-chromite-based ceramics

Conventional sintering of lanthanum-chromite-based ceramics typically requires a long isothermal duration, which leads to severe loss of volatile components. In this study, we prepared dense LaCrO₃ (LCO), La_0.8Ca_0.2CrO₃ (LCCO), and La_0.8(Mg_0.05Ca_0.05Sr_0.05Ba_0.05)CrO₃ (4LCO) ceramics with stable single-phase structures through ultrafast high-temperature sintering (UHS), and the total sintering period was shorter than 8 min. An investigation of the effects of sintering parameters and alkaline earth (AE) metal dopants on the density showed that doping with AE metal promoted the densification of LaCrO₃ through the liquid-phase-assisted sintering mechanism. The hardness and conductivity of the ceramics were in the order of LCCO>4LCO>LCO because of the effect of lattice distortion and the relative densities of the pellets. This work presents a compositional-design-based method to obtain high-performance perovskite-type oxides, and it is expected to broaden the use of UHS for the densification of novel ceramics.     

Low temperature sintering and microwave dielectric properties of TiO2 ceramics

The TiO₂ ceramics were prepared by a solid-state reaction in the temperature range of 920–1100 °C for 2 h and 5 h using TiO₂ nano-particles (Degussa-P25 TiO₂) as the starting materials. The sinterability and microwave properties of the TiO₂ ceramics as a function of the sintering temperature were studied. It was demonstrated that the rutile phase TiO₂ ceramics with good compactness could be readily synthesized from the Degussa-P25 TiO₂ powder in the temperature range of 920–1100 °C without the addition of any glasses. Moreover, the TiO₂ ceramics sintered at 1100 °C/2 h and 920 °C/5 h demonstrated excellent microwave dielectric properties, such as permittivity (Ɛ_r) value >100, Q × f  > 23,000 GHz and τ_f ≅ 200 ppm/°C.     

Cold sintering assisted CaF2 microwave dielectric ceramics for C-band antenna applications

A cold sintering process is adopted to pre-densify CaF₂ ceramics from 85.7% at 300 MPa to 91.7% at 750 MPa. Subsequent post-annealings at 1000–1150 °C lead to further improvements in densification, where great enhancements of grain size and crystallinity are also observed from the scanning and transmission electron micrographs. Significant advances in Qf values are achieved in the post-annealed CaF₂ ceramics. The optimum Qf value (80,522 GHz) is achieved after cold sintering at 750 MPa and post-annealing at 1000 °C, which is three times higher than the conventional sintered one at 1000 °C (26,448 GHz). Moreover, the obtained low-ε_r (5.9–6.5) of CaF₂ ceramics suggests broad application prospects in the high-band microwave communications. A microstrip patch antenna is fabricated using the CaF₂ ceramics as the substrate, which operates at 7.89 GHz in the C-band, with an S₁₁ of ?13.4 dB, simulated high gain and efficiency of 6.41 dBi and ?0.56 dB, respectively.     

Rutile TiO2 microwave dielectric ceramics prepared via cold sintering assisted two step sintering

In this work, a sintering route named cold sintering assisted two step sintering process (CSP-TS) is presented to prepare rutile TiO₂ ceramics with submicron grain sizes. Cold sintering process at 300 °C with tetrabutyl titanate and water as the liquid phase yields a ‘green body’ with a relatively high density of ～80 %, and finally dense (98.5–99.8 %) rutile TiO₂ ceramics with grain sizes of ～600 nm can be obtained in the second sintering process at 950?1000 °C. The microstructural analysis with SEM and TEM indicates that the CSP-TS samples sintered at 950 °C have an obvious phenomenon of recrystallization, accompanying by a decrease of amorphous phases and a formation of clear grain boundaries. Besides, the rutile TiO₂ ceramics prepared by CSP-TS possess excellent microwave dielectric properties with relative permittivity of 92.0–98.4 and Q × f values of 27,800?31,900 GHz. Therefore, it is feasible to utilize CSP-TS to prepare ceramics with small grain sizes at low sintering temperatures.     

Laser sintering of Al2O3-based green ceramics prepared by different pre-sintering temperatures

Al₂O₃-based green ceramics are prepared by isostatic cold pressing technology. The prepared green ceramics are pre-sintered at the temperature from room temperature to 1100°C, and then Al₂O₃ ceramics are prepared by laser sintering. The effects of pre-sintering temperatures and laser parameters on mechanical properties and the sintering quality are analyzed. The results show that good crystallinity of Al₂O₃ particles is obtained at a higher pre-sintering temperature. The flexural strength and density of green ceramics increase with the temperature of heat treatment. The flexural strength decreases slightly at ∼200°C due to the paraffin binder disintegration. The pre-sintering temperature and laser processing parameters have a significant influence on the sintering quality. With the increase of laser power and laser frequency, dynamic grain growth occurs, and then grains are refined. The majority of plate-like grains are transformed into long cylindrical-like grains in the severe densification process. However, porous flocculation microstructures are generated on the samples pre-sintered at 1100°C after laser sintering, which is due to the material gasification in atmospheric environment during sintering by infrared laser. More uniform microstructure and better sintering quality of samples pre-sintered at 500°C can be achieved after laser sintering with a relatively narrower grain size distribution.     

Influence of sintering conditions on piezoelectric properties of KNbO3 ceramics

A homogeneous KNbO₃ (KN) phase was formed in specimens that were sintered at 1020 °C and 1040 °C, without formation of the K₂O-deficient secondary phase, indicating that the amount of evaporation of K₂O during sintering was very small. However, the KN liquid phase was formed during sintering and assisted the densification of the KN ceramics. A dense microstructure was developed in the specimen sintered at 1020 °C for 6 h and abnormal grain growth occurred in this specimen. A similar microstructure was observed in the specimens sintered at 1040 °C for 1.0 h. The dielectric and piezoelectric properties of the KN ceramics were considerably influenced by the relative density. The KN ceramics sintered at 1020 °C for 6 h, which showed a large relative density that was 95% of the theoretical density, exhibited promising electrical properties: ɛ^T₃₃/ɛ_o of 540, d₃₃ of 109 pC/N, k_p of 0.29, and Q_m of 197.     

Spark plasma sintering of SiAlON ceramics

Investigated was the spark plasma sintering (SPS) of sialon ceramics from SHS-produced powders. Experimentally established were (a) sintering temperatures that ensure a required density, phase composition, and microstructure of sintered multicomponent sialon ceramics, (b) individual stages of the SPS process, and (c) the effect of starting powder composition on the phase composition and microstructure of sintered sialon ceramics.      

Stress-induced anisotropy during sintering of hierarchical porosity ceramics

There is significant interest in the design and processing of porous ceramics due to their use in a variety of applications including energy storage, catalysis, adsorption, separation, and life science applications. For many of these applications, it is desirable to have a hierarchical porous structure in which there is a distinct difference between sizes of pores. Our previous study has shown that microstructure and properties of porous materials become anisotropic after sinter-forging. In particular, the small interparticle pores (intrinsic pores) orient parallel to the applied compressive stress, in contrast to large pores from pore formers (extrinsic), which orient perpendicular to the applied stress. However, the pore size, for transition from extrinsic to intrinsic behavior, (transient pore size) has not been quantified. In this study, we report on the effect of applied stresses during sinter-forging on the morphology (shape and size) of pores of different size. Based on these results, we propose a two-step approach to predict transient pore size for hierarchically porous ceramics. We use this approach to quantify the effect of applied stresses on the transient pore size. Finally, we postulate that the stress dependence of the transient pore size may be related to sintering stress—a fundamental quantity in continuum models of sintering. In addition, it can be used to calculate the effective surface energy of complex sintering systems.     

Vacuum sintering of transparent Cr:Y2O3 ceramics

0–0.7 at% Cr:Y₂O₃ transparent ceramics were prepared by vacuum sintering. The optimum in-line transmittance in the visible and near infrared region is 78%, and the Vickers hardness of the sintered 0.1 at% Cr:Y₂O₃ is 10.1 GPa, respectively. The mechanism of Cr-doped and the optical properties has been discussed. The results indicated that the Cr:Y₂O₃ transparent ceramic is a promising laser material with enhanced mechanical property.     

Enhanced dielectric breakdown strength in TiO2-SiO2-Al2O3 based ceramics prepared through hot-press assisted liquid phase sintering

Linear dielectric ceramics have received much attention due to high power density, fast discharge speed and ultralow dielectric loss, which are expected as promising candidates for the pulsed power system applications. However, their relatively low dielectric breakdown strength usually cannot meet the requirements of practical application. In this work, we adopt hot-press sintering method to enhance the dielectric breakdown strength of the TiO₂-SiO₂-Al₂O₃ based ceramics, and the dielectric breakdown strength reaches 77.5 kV/mm, which is 1.8 times as large as samples prepared by conventional sintering method. The effect of different sintering methods on microstructure, dielectric properties and dielectric breakdown strength is investigated. The improvement of dielectric breakdown strength can be ascribed to improved bulk density, smaller grain size, and reduced reduction of Ti⁴⁺ to Ti³⁺, associated with the applied external pressure and lower sintering temperature. Eventually, large power density (18.20 MW/cm³) is obtained in pulse overdamped discharge circuit. Meanwhile, the stored energy is also released in a short time (about 11.3 ns to release 90% of saturated energy density value).     

Fabrication of translucent AlN ceramics with MgF2 additive by spark plasma sintering

Translucent AlN ceramics with 0‐2 wt.% MgF₂ additive were prepared by spark plasma sintering. AlN powder was heated temporarily up to 2000°C, before holding at 1850°C for 20 minutes in N₂ gas. The sintered ceramics consisted of a single phase of hexagonal AlN, and showed a transgranular fracture mode. The total transmittance was improved remarkably by the additive, to reach 74% at a wavelength of 800 nm for 1 wt.% MgF₂. For 2 wt.% MgF₂, the transmittance was slightly lower than that for 1 wt.% MgF₂, and an absorption band was observed apparently at around 400 nm. The addition of MgF₂ along with the temporary heating at higher temperatures than the sintering temperature contributed to improve the transmittance remarkably.     

High-pressure sintering of ultrafine-grained high-entropy diboride ceramics

Herein the ultrafine-grained (Hf_0.2Zr_0.2Ta_0.2Nb_0.2Ti_0.2)B₂ high-entropy diboride ceramics were successfully fabricated by high-pressure sintering technology for the first time. The results showed that the grain size, relative density, and Vickers hardness of the as-fabricated samples all increased gradually with increasing sintering temperatures from 1373 K to 1973 K. The relative density and mean grain size of the as-sintered samples at 1973 K were 97.2% and 684 nm, respectively, and simultaneously they exhibited excellent comprehensive mechanical properties, combining a Vickers hardness of 26.2 GPa and a fracture toughness of 5.3 MPa·m^1/2, which were primary attributed to the fine grain strengthening mechanism and microcrack deflection toughening mechanism.     

TiO2和CaO-Al2O3-SiO2复合烧结助剂对刚玉陶瓷烧结的影响

在以α-Al2O3为原料的刚玉陶瓷配料中,分别添加0、0.15%、0.30%、0.45%、0.60%的TiO2和0、0.5%、1.0%、2.0%、4.0%的CaO-Al2O3-SiO2(CAS)玻璃,共组合出25组试验配方,以150MPa压力干压成型为45mm×5mm×4mm的试样,烘干后以5℃.min-1的升温速率升至1550℃保温2h烧成,然后检测烧后试样的相对密度、常温抗折强度和断裂韧性,并用扫描电镜观察烧后试样的显微结构。结果表明:引入TiO2能显著提高刚玉陶瓷的烧结致密化速率,但是引起晶粒的异向生长和异常长大,并使其断裂方式以沿晶断裂为主,试样力学性能也普遍较低;引入少量的CaO-Al2O3-SiO2易引起样品反致密化,只有CaO-Al2O3-SiO2的引入量大于1.3%才能有效地促进刚玉陶瓷的烧结,并抑制由0.6%的TiO2引起的严重的晶粒异向生长和异常长大,使材料的断裂方式向穿晶断裂转变,并使其力学性能逐渐回升。