不同烧结法对3Y-TZP陶瓷力学性能的影响

本文研究了低温烧结含3mol%氧化钇的四方多晶氧化锆(3Y-TZP)的烧结性能和力学性能,以及进行热等静压(HIP)后其力学性能的变化。成形后的3Y-TZP在常压、1300～1450℃温度下进行烧结。由于该粉料有很高的烧结活性,在1300℃低温烧成下就可获得相对密度大于94%的烧结体;在1350℃烧成温度下3Y-TZP获得了最佳的力学性能。其断裂韧性(KIC)和维氏硬度(HV)分别达到18.7MPa.m1/2和13.7GPa,其中应力诱导相变是其主要的增韧机理。对低温烧成的3Y-TZP陶瓷进行热等静压烧结后发现,HIP增大3Y-TZP陶瓷HV的作用显著,可使其增至14.3GPa。     

Sintering behavior,phase structure and microwave dielectric properties of CeO2 added CaTiO3-SmAlO3 ceramics prepared by reaction sintering method

Novel 0.695CaTiO₃-0.305SmAlO₃+xwt% CeO₂ (x = 0, 0.5, 1.0, 1.5) ceramics were fabricated using a reaction-sintering (RS) approach. The crystal structure, morphology, and microwave dielectric properties of ceramics were systematically studied. The addition of CeO₂ could effectively improve the sintering behavior of 0.695CaTiO₃-0.305SmAlO₃ (CTSA) ceramics. When x = 0.5 wt%, the ceramics exhibited optimal microwave dielectric properties, with ε_r = 43.9, Q×f = 48 779 GHz, and τ_? = ?0.24 ppm/°C, thereby indicating that the samples prepared via the RS route possess superior dielectric properties compared to those prepared by the conventional solid phase reaction. The results demonstrate that CaTiO₃-SmAlO₃ ceramics can be prepared simply and efficiently through a reaction-sintering process.     

Tuning of electrocaloric performance in (Ba0.85Ca0.15)(Zr0.1Ti0.9)O3 by induced relaxor-like behavior

Induced relaxor-like behavior is reported by addition of a sintering additive to the (Ba_0.85Ca_0.15)(Zr_0.1Ti_0.9)O₃ solid solution. The effect of Bi₂O₃ sinter additive on microstructure is determined. The phase transition behavior is highlighted by dielectric permittivity measurements. The electrocaloric temperature change is directly measured and comparison with literature data is provided on basis of the material related cooling power. Addition of Bi₂O₃ drastically increases the temperature stability and an ultra-wide temperature range of over 100?K is achieved. The findings path a way to tune electrocaloric materials for optimization of properties for solid-state coolers based on the electrocaloric effect.     

Effect of synthesis process on the densification,microstructure, and electrical properties of Ca0.9Yb0.1MnO3 ceramics

Ca_0.9Yb_0.1MnO₃ thermoelectric materials have been prepared, through a classical solid‐state sintering method, from attrition‐ and ball‐milled precursors. After calcination step, microstructural observations have shown that attrition‐milled precursors possess much smaller particle sizes than the obtained by ball milling. Smaller precursors sizes lead to higher reactivity, producing higher density, hardness, and thermoelectric phase content in the sintered materials. The thermoelectric properties reflect the microstructural features, decreasing electrical resistivity in the attrition milling prepared samples without a drastic decrease in the Seebeck coefficient. As a consequence, power factor values are higher than the obtained in the classical solid‐state method samples. Moreover, the highest power factor values at 800°C are much higher than the best results obtained in this CaMnO₃ family. As a result, it has been found that it is possible to tailor the thermoelectric properties of Ca_0.9Yb_0.1MnO₃ ceramics by designing the appropriate preparation procedure while keeping in mind its industrial scalability.     

Effect of Gd doping on electrical transport properties of La0.8Sr0.2MnO3 polycrystalline ceramics

Gd doped La_0.8Sr_0.2MnO₃ (La_0.8-xGd_xSr_0.2MnO₃, LGSMO) ceramics were prepared by a sol-gel method. X-ray diffraction (XRD) patterns showed that all samples exhibited distorted perovskite structures, R_3c. When the Gd³⁺ content x > 0.03, the crystal structure changed to orthorhombic, Pnma. Scanning electron microscopy (SEM) images showed that the ceramics characterize high density and grain boundary connectivity, and higher Gd³⁺ doping decreased the grain size from 26.72 μm to 7.42 μm. The temperature dependence of resistivity showed a transition from a low-temperature metal to a high-temperature insulator. The resistivity increased with Gd doping content, and the metal-insulator transition temperature, T_P, increased first and then decreased, while the temperature coefficient of resistance (TCR) of the samples first decreased and then increased with Gd³⁺, and the magnetoresistance (MR) increased first and then decreased. The peak TCR at x = 0.06 was 5.18%·K^?1, and MR at 0.04 was 34.57%. The electrical transport properties of the ceramics were explained based on the double exchange (DE) interaction mechanism. The obtained material may have application prospects in magnetic devices and infrared detectors.     

Core-shell structure strategy and oxygen vacancy engineering of 0.1LaMnO3@0.9(Ba0.5Sr0.5)TiO3 ceramics towards tuning electrical properties

In recent years, core-shell structures have attracted much attention for their potential in tuning the functional properties of materials and have become an effective method for preparing high-performance materials. In this work, core-shell structured 0.1LaMnO₃@0.9(Ba_0.5Sr_0.5)TiO₃ nanoparticles were fabricated by sol-gel method and dense ceramics were prepared at different sintering temperatures. The phase composition, morphology, chemical state and electrical properties were systematically investigated. Structural analysis confirmed the formation of 0.1LaMnO₃@0.9(Ba_0.5Sr_0.5)TiO₃ core-shell nanostructures. The results show that the prepared samples exhibit typical negative temperature coefficient characteristics in the range of 50–1000 °C, which is derived from the effect of carrier pairs and oxygen vacancies on the electrical properties. This study provides new insights from structure to material into guiding the development and design of advanced thermistor materials for temperature sensing applications.     

Effect of Sintering Atmosphere on the Densification and Electrical Properties of Alumina

The effect of sintering atmosphere on the final density and electrical properties of alumina compacts has been investigated using two different oxygen pressures: air and CO/CO₂. Measuring of electrical behavior has been considered a tool for determining the mechanism responsible for densification. Finally, the importance of a reducing atmoshphere on the electrical behavior of polycrystalline alumina is pointed out.     

Structural,ferroelectric, magnetic and magnetoelectric properties of (1-x) Ba0.85Ca0.15Zr0.1Ti0.9O3 -x La0.67Sr0.33MnO3 lead-free magnetoelectric composites

The influence of an additional La_0.67Sr_0.33MnO₃ (LSMO) magnetic phase on the structural, ferromagnetic, ferroelectric, and magnetoelectric properties of Ba_0.85Ca_0.15Zr_0.1Ti_0.9O₃ (BCZT) ferroelectric phase was studied for composites of (1-x)BCZT -xLSMO (x = 0, 25, 50, 75 and 100%). The ferroelectric BCZT sample showed a perovskite single phase formation with a tetragonal crystal structure of the P4mm space group, and the magnetic phase of LSMO presented a rhombohedral crystal structure of R3c space group as shown by XRD. The composite sample with 25% LSMO exhibited large ferroelectric and piezoelectric properties with remnant, saturation polarization, and coercive electric field P_r ~7.74 μC/cm², P_s ~11.69 μC/cm² and E_C ~12.22 kV/cm with a piezoelectric coefficient d₃₃ ~ 231 pC/N. The magnetic characterization for the composites showed that the sample containing 75% of LSMO revealed the highest remnant, saturation magnetization, and coercive field of M_r ~1.358 emu/g, M_s ~19.17 emu/g, and H_C ~33.19 Oe, respectively. Moreover, it revealed the largest magnetoelectric coupling coefficient α_ME ~2.51 mV/cm.Oe with high coupling quality at a lower applied magnetic field. The results highlight the value of these composites as lead-free room temperature magnetoelectric sensors and actuators.     

Sintering behaviour and properties of manganese-doped alumina

The effect of manganese (0.1, 0.5 and 1.0?wt%) on the sintering and mechanical properties of alumina was studied. Sintering was carried out by the conventional heating method in a box furnace and in a hybrid multimode microwave furnace. XRD analysis revealed the precipitation of a spinel second phase (MnAl₂O₄) in manganese-doped samples as a result of manganese limited solubility in the corundum lattice. The addition of 0.1?wt% manganese was most beneficial in enhancing the densification of alumina (97.5% relative density when compared to 94.2% for the undoped sample), hindered grain growth, and improved the hardness of the ceramic when sintered at 1500?°C. The study also revealed that microwave sintering was effective in suppressing grain growth of alumina. In addition, the hardness was dependent on the sintered bulk density and that grain coarsening ensued as the density of the sintered alumina exceeded 95% of theoretical.     

Enhanced high temperature microwave absorption of La0.9Sr0.1MnO3/MgAl2O4 composite ceramics based on controllable electrical conductivity

The high temperature microwave absorbing efficiency (HTMAE) of xLa_0.9Sr_0.1MnO₃/(1 − x)MgAl₂O₄ composite ceramics was investigated by studying the crystal structure, electrical conductivity, and permittivity. The crystal structure of La_0.9Sr_0.1MnO₃ and MgAl₂O₄ were maintained, but the Mn³⁺ and Al³⁺ ions were exchanged with each other through doping. The conductivity and permittivity of the composite ceramics increased with the increase of La_0.9Sr_0.1MnO₃ content and test temperature. When x = 0.36, the electrical conductivity in La_0.9Sr_0.1MnO₃ significantly enhanced the microwave polarization of the composite ceramics at high temperature. According to transmission/reflection modelling, the composite ceramics with x = 0.24 showed excellent HTMAE near the optimal thickness of 1.8 mm. Although the optimal thickness of the composite with x = 0.36 was reduced to 1.1 mm, the HTMAE was seriously lessened due to an impedance mismatch. xLa_0.9Sr_0.1MnO₃/(1 − x)MgAl₂O₄ are promising as thin and efficient microwave absorbing materials at high temperatures and the microwave permittivity can be further enhanced by adjusting the conductivity of La_0.9Sr_0.1MnO₃.     

Influence of Eu and Sr co-substitution on multiferroic properties of BiFeO3

Pure BiFeO₃ (BFO), and Eu-Sr co-substituted BFO samples were prepared by a sol–gel method. The effects of Eu and Sr codoped on the structural, morphological, magnetic and ferroelectric properties were systematically investigated. The X-ray diffraction and Fourier transform infrared spectroscopy reveal that substitution of Eu and Sr at the Bi site results in structural change and single phase formation. The maximum remnant magnetization of 0.287 emu/g and coercive field of 10.305 kOe are observed in the Bi_0.85Eu_0.05Sr_0.10FeO₃ sample. The suppression of spin cycloid caused from the structural distortion can play an important role in the improvement of magnetic properties. The Eu and Sr co-doped samples also exhibit good ferroelectric properties, which may be attributed to suppressing the formation of oxygen vacancies by Eu substitution.     

烧结温度对La22/27Sr1/27K4/27MnO3的电输运性质及磁电阻的影响

采用固相反应法在不同烧结温度制备出La22/27Sr1/27K4/27MnO3多晶样品,研究了烧结温度对La22/27Sr1/27K4/27MnO3电输运性质及磁电阻的影响。结果表明:1 523、1 573K烧结样品的电输运性质出现反常;磁电阻-温度(RM-T)曲线中,低温区RM随温度降低持续增大,是界面引起的自旋相关隧穿磁电阻;高温区出现的磁电阻峰是颗粒相本征磁电阻;中间温区RM-T曲线出现一个平台。在314～274K、0.8T磁场下,1 373℃烧结的样品磁电阻(7.96±0.08)%保持不变,这有利于庞磁电阻的实际应用。钙钛矿颗粒分为体相和界面相,RM温度稳定性的机制为:高温区体相产生的本征磁电阻占优势;低温区界面产生的隧穿磁电阻占优势;中间温区二者叠加,产生不随温度变化的磁电阻。     

Fabrication and high-temperature thermoelectric properties of Ti-doped Sr0.9La0.1TiO3 ceramics

Ti-doped Sr_0.9La_0.1TiO₃ ceramics with high density were successfully prepared in argon atmosphere by conventional solid state reaction. The influences of titanium doping content on the microstructure and thermoelectric properties were investigated. The results showed that titanium was oxidized during the calcination procedure. TiO₂ phase survived and coexisted with Sr_0.9La_0.1TiO₃ phase in the sintered ceramics. The Seebeck coefficients were increased from −163 to −259 μV/K as the temperature increased from 350 K to 1073 K. The thermal conductivity can be significantly reduced by doping Ti. Thermoelectric figure of merit (ZT) first decreased and then increased with increasing Ti doping content. Ceramics showed the best thermoelectric properties when Ti doping amount was 5 wt%, the maximum PF was 7.13 μW/K²/cm, and ZT value was 0.144 at 1073 K.     

SUS430合金La0.75Sr0.25MnO3涂层烧成气氛研究

采用溶胶-凝胶法分别在空气和N2气气氛中不同烧成时间下制备了均匀致密度的SUS430合金LSM涂层.观察了不同气氛下烧结3h的涂层样品的SEM表面形貌;采用四点法测量了不同气氛和不同烧成时间下制备的各涂层样品的ASR值,测量分析了各涂层样品在800℃下空气中热处理120h过程中的氧化增重量变化.结果表明,N2气气氛下烧成的涂层比空气气氛下烧结的涂层烧结程度更好、ASR值更低,并具有更好的抗氧化保护作用;空气气氛下烧成时间对涂层的烧结程度、导电性能和抗氧化性能影响显著,N2气气氛下烧成时间对涂层的烧结程度、导电性能和抗氧化性能影响不大.     

Effects of structural transition on microwave dielectric properties of Sr3(Ti1-xSnx)2O7 ceramics

Sr₃(Ti_1-xSn_x)₂O₇ (x = 0–1.0) ceramics were prepared via a standard solid-state reaction method. X-ray diffraction patterns and Rietveld refinement results indicated a composition induced onset of octahedral tilting when x > 0.2, and the crystal structure transformed in sequence: tetragonal (I4/mmm) → coexistence of tetragonal and orthorhombic (I4/mmm + Amam) → orthorhombic (Amam). The τ_f value could be successfully tuned towards zero and the effects of octahedral tilting on the evolution of τ_f value were emphasized. Meanwhile, the role of tolerance factor in tailoring the resultant τ_ε of the present ceramics was revealed and compared with the empirical rule for complex perovskites. Qf value decreased monotonously with increasing x, which could be elucidated by the variations of extrinsic parameters and intrinsic dielectric loss extrapolated from the infrared reflectivity spectra. The optimum microwave dielectric properties were achieved at x = 0.8 (ε_r = 18.6, Qf = 45,250 GHz, τ_f =–14 ppm/^oC).     

Optimization of room-temperature TCR of polycrystalline La0.9-xSrxK0.1MnO3 ceramics by Sr adjustment

High-density La_0.9-xSr_xK_0.1MnO₃ ceramics (LSKMO, A-site = La, Sr and K, 0 ≤ x ≤ 0.25) are successfully fabricated by using facile sol-gel method. Electrical properties are performed by using combination of phenomenological percolation (PP) model, double exchange (DE) mechanism, and Jahn-Teller (JT) effect. Moreover, X-ray diffraction and scanning electron microscopy are employed to analyze the structure and morphology of LSKMO ceramics. Valence states and ionic stoichiometry are assessed by using X-ray photoemission spectrometry. Results reveal that Sr²⁺ ions, substituting La³⁺ ions, significantly influenced DE mechanism and JT effect. In addition, Sr-doping plays essential role in improving electrical properties of LSKMO ceramics. At optimal doping content of x = 0.09, peak temperature coefficient of resistance (TCR) of the resistivity is found to be 11.56% K^?1 at 297.15 K, which is optimal TCR for A-site K-occupied perovskite manganese oxides. These results confirm that polycrystalline LSKMO ceramics render high room-temperature TCR values due to Sr-doping.     

不同烧结气氛下制备的AlN陶瓷结构和电性能的差异

以AlN粉末为原料、Y2O3粉末为烧结助剂,分别在氮气气氛下和真空气氛下,采用放电等离子烧结方法在1700℃、25MPa条件下保温10min制备AIN陶瓷。X-射线衍射、扫描电镜和X-射线光电子能谱分析表明：不同烧结气氛下制备的AlN陶瓷的结构和体积电阻率各有不同。真空气氛AlN陶瓷与氮气气氛AlN陶瓷相比较,除舍有主晶相AlN和第二相Y3Al5O12外,还含有微量Al2Y相。正是由于微量Al2Y相的存在,使得真空气氛下得到的AlN陶瓷比氮气气氛下得到的A1N陶瓷的体积电阻率低约2个数量级。     

Comparison between microwave and conventional sintering on the properties and microstructural evolution of tetragonal zirconia

In this research, the comparison between microwave sintering and conventional sintering on the mechanical properties and microstructural evolution of 3?mol% yttria-stabilised zirconia were studied. Green bodies were compacted and sintered at various temperatures ranging from 1200?°C to 1500?°C. The results showed that microwave assisted sintering was beneficial in enhancing the densification and mechanical properties of zirconia, particularly when sintered at 1200?°C. It was revealed that as the sintering temperature was increased to 1400?°C and beyond, the grain size and mechanical properties for both microwave- and conventional-sintered ceramics were comparable thus suggesting that the sintering temperature where densification mechanism was activated, grain size was strongly influenced by the sintering temperature and not the sintering mode.     

Dielectric properties of conventional and microwave sintered Lanthanum doped CaCu3Ti4O12 ceramics for high-frequency applications

The colossal dielectric response of La-doped CaCu₃Ti₄O₁₂ ceramics has been probed at room temperature for a frequency of 1Hz–20 MHz. In this work, the La-doped (CaCu₃Ti₄O₁₂)_x samples for x = 0.1, 0.2, and 0.3 have been sintered at 1100 °C using two different heating modes. SEM and EDS analysis investigated the microstructural chrysalis, grain size distribution, and the inhibitions of Cu-rich phase segregation into grain boundaries by the effect of La³⁺. The presence of main cubic single-phase of CCTO and the diminutive Bragg peak shift due to ion size effect of La³⁺ and Ca²⁺ have been identified by XRD for both conventional (CS) and microwave sintered (MWS) samples. XPS study revealed the effect of La³⁺ on the binding energies of Cu and Ti in CCTO. The dielectric properties namely dielectric constant (?), tan δ, and dielectric relaxation peaks were measured using BDS in which CS and MWS La-doped samples demonstrated (?) ～ >10⁴ and ～ >10³ along with low tan δ for x ≥ 0.1 at medium and high frequency (10⁴–10⁷Hz) than pure CCTO.