Effect of milling process on the core-shell structures and dielectric properties of fine-grained BaTiO3-based X7R ceramic materials

Fine-grained BaTiO₃-based X7R ceramic materials were prepared and the effects of milling process on the core-shell structures and dielectric properties were investigated using scanning electron microscope, transmission electron microscope, and energy dispersive spectroscopy (EDS). As the milling time extends, the dielectric constant of the ceramics increases, whereas the temperature coefficient of capacitance at 125℃ drops quickly. The changes in dielectric properties are considered relevant to the microstructure evolution caused by the milling process. Defects on the surface of BaTiO₃ particles increase because of the effects of milling process, which will make it easier for additives to diffuse into the interior grains. As the milling time increases, the shell region gets thicker and the core region gets smaller; however, EDS results show that the chemical inhomogeneity between grain core and grain shell becomes weaker.     

超重力反应沉淀法制备的纳米钛酸钡粉体的烧结与介电性能研究

将超重力法制备的纳米钛酸钡粉体在不同温度(700～900℃ )下煅烧,以提高粉体的结晶度,粉体的粒径从40nm增大到80nm。煅烧后的粉体经过干压成型后,在1100℃下保温2h烧结得到的钛酸钡最高室温介电常数为2880,相对密度为90%,晶粒尺寸达到0.70 μm左右。讨论了煅烧温度对粉体的烧结性能、陶瓷的介电性能及微观结构的影响。     

Dielectric properties of spark plasma sintered AlN/SiC composite ceramics

In this study, we have investigated how the dielectric loss tangent and permittivity of AlN ceramics are affected by factors such as powder mixing methods, milling time, sintering temperature, and the addition of a second conductive phase. All ceramic samples were prepared by spark plasma sintering (SPS) under a pressure of 30 MPa. AlN composite ceramics sintered with 30wt%–40wt% SiC at 1600℃ for 5 min exhibited the best dielectric loss tangent, which is greater than 0.3. In addition to AlN and β-SiC, the samples also contained 2H-SiC and Fe₅Si₃, as detected by X-ray difraction (XRD). The relative densities of the sintered ceramics were higher than 93%. Experimental results indicate that nano-SiC has a strong capability of absorbing electromagnetic waves. The dielectric constant and dielectric loss of AlN-SiC ceramics with the same content of SiC decreased as the frequency of electromagnetic waves increased from 1 kHz to 1 MHz.     

金属氧化物在Si3N4陶瓷烧结中的使用现状

Si₃N₄陶瓷具有较高的热导率、良好的耐磨性和耐腐蚀性,高温强度高,且高温稳定性和抗热冲击性好,作为结构材料在机械工业,电子工业和化学工业中广泛应用。由于Si₃N₄陶瓷烧结温度过高,无法在工业生产中大量使用,为了降低其烧结温度、改善烧结致密度和强度等性能,在烧结过程中经常使用烧结助剂。综述了国内外金属氧化物作为烧结助剂在Si₃N₄陶瓷烧结中的研究现状,提出了其烧结过程中存在的问题。     

Preparation and photocatalytic activity of Cu-doped TiO2/SiO2

Cu²⁺-doped nanostructured TiO₂-coated SiO₂ (TiO₂/SiO₂) particles were prepared by the layer-by-layer assembly technique and their photocatalytic property was studied. TiO₂ colloids were synthesized by the sol-gel method using TiOSO₄ as a precursor. The experimental results showed that TiO₂ nanopowders on the surface of SiO₂ particles were well distributed and compact. The amount of TiO₂ increased with the increase in coating layers. The shell structure appeared to be composed of anatase titania nanocrystals at 550°C. The 2-layer coated TiO₂ particles on the surface showed a higher degradation rate compared with all the different-layer samples. The photocatalytic activity of Cu²⁺-doped TiO₂/SiO₂ was higher than that of undoped TiO₂/SiO₂. The optimum dopant content was about 0.10wt%.     

高能球磨法制备MgNb2O6粉体及其陶瓷性能

 采用高能球磨法在800℃保温2h预烧合成MgNb₂O₆粉体,研究了MgNb₂O₆陶瓷的相结构、显微结构和微波介电性能随烧结温度的变化关系。实验结果表明,高能球磨法有效促进MgNb₂O₆粉体的低温合成,降低MgNb₂O₆陶瓷的烧结温度。1220℃保温2h烧结MgNb₂O₆陶瓷,密度为4.80g/cm³,平均粒径为3.5μm,介电常数ε_r为19.7,品质因数(Q·f)为29444GHz的优良微波介电性能,MgNb₂O₆粉体有望成为新一代中温烧结高频微波介质基板材料。     

球磨时间对Mo_2FeB_2基金属陶瓷组织和力学性能的影响

以Mo、FeB、Cr、Ni、Fe粉末以及少量的C粉为原料,采用行星球磨法对其球磨后烧结制备Mo2FeB2基金属陶瓷,利用扫描电镜观察球磨粉及其烧结试样的组织形貌,并测定烧结试样的孔隙度、硬度和抗弯强度,研究原料粉末球磨时间对Mo2FeB2基金属陶瓷组织和力学性能的影响。结果表明,随着球磨时间的增加,粉末粒度逐渐变小,Mo2FeB2基金属陶瓷的孔隙度明显降低,其硬度和抗弯强度明显增大,晶粒也随之细化;球磨30h原料粉末所制Mo2FeB2基金属陶瓷的综合性能最优,其硬度(HRA)达到90.2,抗弯强度达到1850MPa。     

SLS工艺参数对Al2O3/SiO2/ZrO2复合陶瓷烧结质量的影响

针对复合陶瓷材料Al2O3/SiO2/ZrO2脆性大难加工等问题,结合选择性激光烧结(SLS)工艺成形复合陶瓷粉末,采用Nd:YAG激光器及其送粉装置进行激光烧结试验.利用扫描电镜(SEM)、能量色散X射线光谱仪(EDX)和X射线衍射分析仪(XRD)观察了成形件的微观组织并分析了微观组织成分.探讨了激光烧结的主要工艺参数对单层烧结质量的影响及扫描速度对显微结构的影响.结果表明:采用正交试验方法系统地分析了工艺过程,获得最佳工艺参数为扫描速度15mm/s、激光功率40W、搭接量04mm,得到了气孔较少、密度372g/cm3的烧结表面,能够烧结出致密并具有枝状组织的陶瓷.     

二次烧成对CaO-B2O3-SiO2系微晶玻璃结构和性能的影响

研究一次和二次烧成对CaO-B2O3-SiO2(CBS)微晶玻璃的烧结性能与介电性能的影响。用X线衍射(XRD)、扫描电镜(SEM)等分析探讨二次烧成对CBS微晶玻璃的微观结构与介电性能的关系。结果表明:与一次烧成相比,二次烧成能够促进玻璃体中的小晶粒生长,试样的收缩率和体积密度有所增加,有利于介电常数提高和介质损耗的降低,且体系中没有出现新的晶相;875℃烧结的试样,X/Y轴收缩率均为14.33%,体积密度达到2.46 g/cm3,10MHz介电常数和损耗相应为6.21和3.5×10-3,热膨胀系数为11.86×10-6/℃,抗折强度为157.36MPa。     

Microwave sintering of Ca<Subscript>0.6</Subscript>La<Subscript>0.2667</Subscript>TiO<Subscript>3</Subscript> microwave dielectric ceramics

Ca_0.6La_0.2667TiO₃ ceramics were prepared by conventional and microwave sintering techniques and their sinterability, microstructure, and microwave dielectric properties were investigated in detail for comparison. Densified Ca_0.6La_0.2667TiO₃ ceramics were obtained by microwave sintering at 1350°C for 30 min and by conventional sintering at 1450°C for 4 h. An unusual phenomenon was found that some larger grains (grain size range: 8–10 μm) inclined to assemble in one area but some smaller ones (grain size range: 2–4 μm) inclined to gather in another area in the microwave sintered ceramics. The microwave dielectric properties of Ca_0.6La_0.2667TiO₃ ceramics prepared by microwave sintering at 1350°C were as follows: dielectric constant (ɛ _r) = 119.6, quality factor (Qf) = 17858.5 GHz, and temperature coefficient of resonant frequency (τ _f) = 155.5 ppm/°C. In contrast, the microwave dielectric properties of the ceramics prepared by conventional sintering at 1450°C were ɛ _r = 117.4, Qf = 13375 GHz, and τ _f = 217.2 ppm/°C.     

Effect of B2O3 on the aqueous tape casting and microwave properties of Li2O–Nb2O5–TiO2 ceramics

The effect of B2O3 addition on the aqueous tape casting, sintering, microstructure and microwave dielectric properties of Li2O-Nb2O5-TiO2 ceramics has been investigated. The tape casting slurries exhibit a typical shear-thinning behavior without thixotropy, but the addition of B2O3 increases the viscosity of the slurries significantly. It was found that doping of B2O3 can decrease the tensile strength, strain to failure and density of the green tapes. The sintering temperature could be lowed down to 900℃ with the addition of 2 wt% B2O3 due to the liquid phase effect. No secondary phase is observed. The addition of B2O3 does not induce much degradation on the microwave dielectric properties. Optimum microwave dielectric properties of εr 67, Q×f 6560 GHz are obtained for Li2O-Nb2O5-TiO2 ceramics containing 2 wt% B2O3 sintered at 900 1C. It represents that the ceramics could be promising for multilayer low-temperature co-fired ceramics (LTCC) application.     

Ca(Sm0.5Nb0.5)O3介质陶瓷的微波烧结

通过改变微波烧结温度和保温时间,优化Ca( Sm0.5 Nb0.5) O3 (CSN)陶瓷的微波烧结工艺,用X线衍射仪(XRD)、扫描电镜(SEM)和微波网络分析仪等对试样进行表征.从相组成、显微结构及微波介电性能等方面对微波烧结试样与常规烧结试样进行对比分析.结果表明:微波烧结可大幅降低CSN的烧结温度,促进试样的致密化,其物相组成和传统烧结试样无明显差别;微波烧结还可以改善CSN陶瓷的微波介电性能,在1 375℃微波烧结30 min可获得优异的微波介电性能,介电常数(εr)=20.08,品质因数(Q×f)=37.03 THz,谐振频率温度系数(Tf)=-10.2×10-6℃-1.     

真空烧结SrTiO3系多功能瓷涂覆的研究

The influence of oxide(Na₂O) and composite oxides(PbO-Bi₂O₃-B₂O₃,MnO-Bi₂O₃) as diffusants on the microstructure and voltage-sensitive characteristics of SrTiO₃-based semi-conductor ceramics which is sintered in vacuum was studied.     

Dielectric properties of low dielectric constant Ba0.60Sr0.40Mg0.15Ti0.85O3-Mg2TiO4 composite thin films for tunable applications

Ba0.60Sr0.40Mg0.15Ti0.85O3-xmol%Mg2TiO4 （x = 0-40 mol%） （BSTM-MT） composite thin films were fabricated by sol-gel method. The precursor solution of these composite thin films was prepared through mixing the Ba0.80Sr0.40Mg0.15Ti0.85O3 and Mg2TiO4 solution. The microstructures and dielectric tunability of composite thin films were investigated. The dielectric constant of composite thin films can be tailored from 155 to 55 by changing the concentration of Mg2TiO4. The dielectric loss of these composite thin films were still kept below 0.01 and the tunability was above 20% at a dc-applied electric field of 500 kV/cm. Suitable dielectric constant, low dielectric loss, and high tunability of this kind of composite thin films can be useful for potential microwave tunable applications.     

CaBi4Ti4O15基陶瓷制备与镧掺杂的性能优化

两步法烧结制备一系列CaBi4-xLaxTi4O15（x=0,0．1,0．2,0．3,0．4）（CBLT—X）：以氧化物为前驱体用熔盐法合成片状粉体,然后通过晶体定向技术制备后烧结成陶瓷．通过SEM微观结构表征来确定增加镧掺杂和温度对晶粒生长和织构形成的影响．当镧掺杂（z=0．4）烧结温度在1150℃时,CBLT—X陶瓷在垂直于流延方向上介电常数可提高到570．CBLT—X系列陶瓷的介电常数和介电损耗在垂直于流延的方向的数值都高于平行方向上．控制CBLT—X陶瓷结构化和晶粒生长的机理首次用3D模式进行了讨论．     

Effect of KNbO3 content on the crystal structure and electrical properties of (1 − x)PbZr0.54Ti0.46O3-xKNbO3 piezoelectric ceramics

(1 ? x)PbZr_0.54Ti_0.46O₃-xKNbO₃ (0 ≤ x ≤ 25mol%) (abbreviated as PZT-xKN) piezoelectric ceramics were successfully fabricated by a traditional sintering technique at 1225°C for 30 min. The influence of KNbO₃ content on the crystal structure and electrical properties of the PZT-xKN piezoelectric ceramics was studied. Samples with 0 ≤ x ≤ 0.20 show a pure perovskite structure, indicating that all KNbO₃ diffused into the crystal lattice of PZT to form a single solid solution in this compositional range. A second Pb₃Nb₄O₁₃ phase is observed in the PZT-0.25KN sample, showing that the maximum solid solubility of KNbO₃ in PZT matrix ceramic is less than 25mol%. Compared with pure PZT piezoelectric ceramics, samples containing KNbO₃ have smaller crystal grains. PZT-0.15KN exhibits excellent piezoelectric properties with d ₃₃ = 209 pC/N.     

Effect of CuO addition on the sintering temperature and microwave dielectric properties of CaSiO3– Al2O3 ceramics

CuO-doped CaSiO3–1 wt% Al2O3 ceramics were synthesized via a traditional solid-state reaction method, and their sintering behavior,microstructure and microwave dielectric properties were investigated. The results showed that appropriate CuO addition could accelerate the sintering process and assist the densification of CaSiO3–1 wt% Al2O3 ceramics, which could effectively lower the densification temperature from1250 1C to 1050 1C. However, the addition of CuO undermined the microwave dielectric properties. The optimal amount of CuO addition was found to be 0.8 wt%, and the derived CaSiO3–Al2O3ceramic sintered at 1100 1C presented good microwave dielectric properties of εr?7.27,Q f?16,850 GHz and τf? 39.53 ppm/1C, which is much better than those of pure CaSiO3 ceramic sintered at 1340oC(Q f?13,109 GHz).The chemical compatibility of the above ceramic with 30 Pd/70 Ag during the cofiring process has also been investigated, and the result showed that there was no chemical reaction between palladium–silver alloys and ceramics.& 2014 Chinese Materials Research Society. Production and hosting by Elsevier B.V. All rights reserved.     

Preparation of Ln3-xEuxS4 （Ln=Ce,Pr, and Nd） ceramics by pressureless sintering

The preparation of ternary rare earth sulfides of Ln3-xEuxS4 （Ln = Ce, Pr, and Nd） ceramics was investigated, and the effect of Eu substitution on Ln3-xEuxS4 ceramics was also studied. Ln3-xEuxS4 powders were synthesized by the sulfurization of their oxide powders using carbon disulfide gas. Ln3-xEuxS4 ceramics were sintered by pressure-less sintering method. All pressureless sintered Ln3-xEuxS4 ceramics crystallized in y-phase. It was found that Eu substitution could improve the density of Ln3-xEuxS4 ceramics. Furthermore, Eu substitution might narrow the optical band gaps of Ln3-xEuxS4 ceramics.     

Ferroelectricity of nanocrystalline BaTiO<Subscript>3</Subscript> ceramics by first principle calculation

The vibrational modes of BaTiO₃ in different crystalline phases have been investigated by means of density functional theory pseudo potential method. The evidence of tetragonal to orthorhombic and orthorhombic to rhombohedral phase transitions present for 8 nm BaTiO₃ ceramics further demonstrates that the similar successive transitions in 8 nm BaTiO₃ ceramics from rhombohedral to orthorhombic, tetragonal and cubic transitions are as those in coarse BaTiO₃ ceramics.     

Phase modification and dielectric properties of a cullet-paper ash-kaolin clay-based ceramic

Novel ceramics from waste material made of (x) paper ash-(80-x) cullet-20 kaolin clay (10wt% ≤ x ≤ 30wt%) were successfully synthesized using a conventional solid-state reaction technique. Energy-dispersive X-ray analysis confirmed the presence of Si, Ca, Al, and Fe in the waste material for preparing these ceramics. The influence of the cullet content on the phase structures and the dielectric properties of these ceramics were systematically investigated. The impedance spectra were verified in the range from 1 Hz to 10 MHz at room temperature. The phase of the ceramics was found to primarily consist of wollastonite (CaSiO₃), along with minor phases of γ-dicalcium silicate (Ca₂SiO₄) and quartz (SiO₂). The sample with a cullet content of 55wt% possessed the optimum wollastonite structure and exhibited good dielectric properties. An increase of the cullet content beyond 55wt% resulted in a structural change from wollastonite to dicalcium silicate, a decrease in dielectric constant, and an increase in dielectric loss. All experimental results suggested that these novel ceramics from waste are applicable for electronic devices.>