掺Li_2O–B_2O_3–SiO_2玻璃低温烧结MgTiO_3–CaTiO_3陶瓷及其微波介电性能

研究了Li_2O–B_2O_3–SiO_2玻璃(LBS)对MgTiO_3–CaTiO_3(MCT)介质陶瓷烧结特性、相组成和介电性能的影响,分析了MCT陶瓷与银电极的共烧行为。结果表明通过液相烧结,LBS能有效降低MCT烧结温度至890℃。X射线衍射结果显示有Li_2MgTi_3O_8、硼钛镁石以及Li_2TiSiO_5等新相生成。随着LBS添加量的增大,陶瓷致密化温度和饱和体积密度降低,介电常数εr、品质因数与谐振频率乘积Q×f也呈现下降趋势,频率温度系数τf向负值方向移动。添加质量分数为20%的LBS的0.97MgTiO3–0.03CaTiO3陶瓷在890℃烧结4h,获得最佳性能εr=16.4,Q×f=11640GHz,τf=–1.5×10–6/℃。陶瓷与银电极共烧界面结合状况良好,无明显扩散。该材料可用于制造片式多层微波器件。     

(Mg1-xCox)TiO3基微波陶瓷介电性能研究

以MgO,Co2O3和TiO2为原料,用固相反应法制备了(Mg1-xCox)TiO3(MCT)系陶瓷.研究了CoTiO3含量对其微观结构和微波介电性能的影响.结果表明:添加适量的CoTiO3,可以适当降低烧结温度,调整烧结温度范围.当掺入量为10 mol%,烧结温度为1350 ℃时,MCT陶瓷具有优良微波介电性能:εr=18.99;Q×f=154000 GHz,τf=-45 ppm/℃.     

Zn2+掺杂对0.965MgTiO3-0.035SrTiO3微波介质陶瓷结构与性能影响研究

采用固相反应法制备了0.965 MgTiO3-0.035SrTiO3 (MST)微波介质陶瓷,选用Zn2+对MST陶瓷进行了A位离子掺杂,研究了不同Zn2+掺杂量对陶瓷烧结性能、晶相组成、显微结构及微波介电性能的影响.结果表明,Zn2的掺入促进了陶瓷的烧结,显著提高了陶瓷的致密度,且没有改变陶瓷的主晶相.在掺杂量小于0.04mol％范围内,随着Zn2+掺杂量的增加,陶瓷的介电常数增加,品质因素和频率温度系数略有降低.中间相MgTi2 O5的衍射峰强度随着Zn2+掺杂量的增加逐渐减弱直至完全消失.当Zn2掺杂量为x=0.03时,陶瓷的烧结温度由1380℃降低至1290℃,并呈现优异的微波介电性能:εr=22.51,Q×f=16689 GHz,τf=-4.52×10-6/℃.     

水热法制备Ba6-3xNd8+2xTi18O54微波介质陶瓷

利用水热法合成了Ba6-3xNd8 2xTi18O54微波介质陶瓷,并对合成的微波介质陶瓷进行了X射线衍射分析和性能测试.结果表明:选择活性较大的前驱物[如Nd(OH)3,TiCl4],用水热法在360℃保温12h,能合成纯的Ba6-3xNd8 2xTi18O54粉体,极大地降低了粉体的合成温度.用水热法合成的Ba6-3xNd8 2xTi18O54粉体制备陶瓷,其烧结温度为1 250℃,比传统固相法要低100℃左右,陶瓷的介电常数(εr)稍大于用固相法制备的陶瓷,品质因数(Q)也有较大的提高,谐振频率温度系数(τf)也有所改善,当x=2/3时,水热法制备的Ba6-3xNd9 2xTi18O54陶瓷具有最佳微波介电性能:εr=88,Q与谐振频率(f)的乘积Q×f=8 890 GHz,τf=24x10-6/℃.     

添加剂对0.95MgTiO3-0.05CaTiO3陶瓷性能的影响

采用同相反应法分别制备了V2O5,Co2O3和ZnO氧化物掺杂的0.95MgTiO3-0.05CaTiO3(95MCT)介质陶瓷.研究了V2O5,Co2O3和ZnO氧化物掺杂对95MCT陶瓷烧结特性和介电性能的影响.结果表明:V2O5.Co2O3和ZnO氧化物掺杂的95MCT陶瓷的主晶相为MgTiO3和CaTiO3两相结构,无中间相MgTi2O5出现.V2O5,Co2O3和ZnO氧化物掺杂可以有效地降低95MCT陶瓷的烧结温度,提高致密化程度,降低介电损耗,调节温度系数.ZnO掺杂的95MCT陶瓷性能最好:烧结温度降低至1 250℃,介电常数为21.7,烧结密度可达3.8g、cm3(理论密度的98.4%),介电损耗降低至10-5,温度系数为0.12×10-5/℃.     

B2O3-CuO掺杂CSLST微波介质陶瓷介电性能研究

选用B2O3-CuO(BC)低熔点复合氧化物作为烧结助剂,采用固相法制备(Ca0.9375Sr0.0625)0.25(Li0.5Sm0.5)0.75TiO3(CSLST)陶瓷,研究了不同含量的BC对CSLST陶瓷的晶相组成、烧结性能及微波介电性能的影响.研究结果表明:随BC添加量的增多,CSLST陶瓷的烧结温度降低,陶瓷的微波介电常数εr和谐振频率温度系数(Τ)f下降,品质因素Qf明显降低.当BC添加量为5wt％时,在1000℃保温5h可烧结,此时陶瓷具有较佳的微波介电性能:εr=80.4,Q×f=1380 GHz,(Τ)f=- 32.89×10-6/℃.     

H3BO3对Li2Zn3Ti4O12微波介质陶瓷低温烧结与微波介电性能的影响

采用传统固相反应法制备了添加H3BO3助烧剂的Li2Zn3Ti4O12 (LZT)陶瓷,分别通过XRD、SEM、排水法及网络分析仪等方法研究了不同H3BO3添加量对所得陶瓷的物相、微观形貌、烧结特性与微波介电性能的影响.结果表明在LZT陶瓷中添加3wt% H3BO3可有效降低烧结温度,在900 ℃/2 h烧结条件下可以获得高致密性及优异的微波介电性:ρ=4.15 g/cm3,εr=17.916,Q×f=61200 GHz,Tf=-52.87×10-6/℃.     

低温烧结Mg_4Nb_2O_9-0.75wt%V_2O_5-1.5wt%Li_2CO_3微波介质陶瓷及其性能研究

采用高能球磨法制备陶瓷,研究了0.75wt%V2O5和1.5wt%Li2CO3共掺杂对Mg4Nb2O9陶瓷的烧结性能和微波介电性能的影响。实验结果表明0.75wt%V2O5和1.5wt%Li2CO3共掺杂有助于Mg4Nb2O9陶瓷在烧结过程中形成液相,促进低温致密化烧结,进而降低陶瓷的烧结温度。900℃烧结Mg4Nb2O9陶瓷,结构致密、组织均匀,平均粒径0.75μm,εr=12.58,Q×f=5539 GHz。随烧结温度升高,晶粒长大,密度升高,εr和Q×f值增大。微波介电性能表征表明Mg4Nb2O9-0.75wt%V2O5-1.5wt%Li2CO3陶瓷在950℃下低温烧结,获得εr=13.07,Q×f=10858GHz的亚微米级陶瓷,其优良的微波介电性能使其有望成为新一代低温烧结低介高频微波介质基板材料。     

Bi_4B_2O_9对(Ca_(0.2)Sr_(0.05)Li_(0.375)Sm_(0.375_)TiO_3陶瓷烧结和微波介电性能的影响

采用传统固相法制备(Ca0.2Sr0.05Li0.375Sm0.375)TiO3钙钛矿微波介质陶瓷,研究了Bi4B2O9对(Ca0.2Sr0.05Li0.375Sm0.375)TiO3陶瓷微波介电性能的影响,利用X射线衍射仪、扫瞄电子显微镜和矢量网络分析仪对其晶体结构、显微组织和微波介电性能进行了研究。结果表明:掺10%Bi4B2O9的(Ca0.2Sr0.05Li0.375Sm0.375)TiO3陶瓷,其烧结温度由1 300℃降至1 080℃。当添加3.5%Bi4B2O9时,其最佳烧结温度为1 150℃,陶瓷的微波介电性能最佳(相对介电常数εr=116.9;品质因数Q×f=3 500GHz;频率温度系数τf=1.2×10-6/℃)。     

Bi4B2O9对(Ca0.2Sr0.05Li0.375Sm0.375</sub>TiO3陶瓷烧结和微波介电性能的影响

采用传统固相法制备(Ca0.2Sr0.05Li0.375Sm0.375)TiO3钙钛矿微波介质陶瓷,研究了Bi4B2O9对(Ca0.2Sr0.05Li0.375Sm0.375)TiO3陶瓷微波介电性能的影响,利用X射线衍射仪、扫瞄电子显微镜和矢量网络分析仪对其晶体结构、显微组织和微波介电性能进行了研究。结果表明:掺10%Bi4B2O9的(Ca0.2Sr0.05Li0.375Sm0.375)TiO3陶瓷,其烧结温度由1 300℃降至1 080℃。当添加3.5%Bi4B2O9时,其最佳烧结温度为1 150℃,陶瓷的微波介电性能最佳(相对介电常数εr=116.9;品质因数Q×f=3 500GHz;频率温度系数τf=1.2×10-6/℃)。     

Abnormal Grain Growth of Pb(Mg1/3Nb2/3)O3-35 mol% PbTiO3 Ceramics Induced by the Penetration Twin

Pb(Mg_1/3Nb_2/3)O₃-35 mol% PbTiO₃ (PMN-35PT) specimens with a 5 mol% excess PbO were prepared by excessive heat treatment at 1150°C to induce abnormal grain growth. Through electron backscatter diffraction analysis and the observation of a three-dimensional morphology, the abnormally grown PMN-35PT grains were found to be twinned crystals with penetration characteristics. The morphology of the PMN-35PT twinned crystal was crystallographically analyzed. The abnormal grain growth of PMN-35PT is suggested to be due to preferential growth at the reentrant angles formed by twins.     

Effect of Grain Coalescence on the Abnormal Grain Growth of Pb(Mg1/3Nb2/3)O3-35 mol% PbTiO3 Ceramics

Abnormal grain growth (AGG), which occurred during the heat treatment of Pb(Mg_1/3Nb_2/3)O₃-35 mol% PbTiO₃ (PMN-35PT) with excess PbO, was investigated. AGG has been suggested to be the consequence of grain coalescence that results in the formation of Σ3 coincidence site lattice and low angle grain boundaries. Because of reentrant edges appearing at the ends of these boundaries, the coarsening rate of grains was significantly enhanced and AGG occurred.     

Preparation of Dense Lead Magnesium Niobate–Lead Titanate (Pb(Mg1/3Nb2/3)O3–PbTiO3) Ceramics by Spark Plasma Sintering

The effect of spark plasma sintering (SPS) on the densification behavior of Pb(Mg_1/3Nb_2/3)O₃–PbTiO₃ ceramics has been investigated. Specimens with a density of >99% of the theoretical density (TD) were obtained using SPS treatment at 900°C. Through normal sintering at 1200°C, however, the density of the specimen was only ∼92% of TD.     

Processing and properties of Pb(Mg1/3Nb2/3)O3–PbTiO3-based ceramics

Ceramic compositions of a combination between lead magnesium niobate, Pb(Mg_1/3Nb_2/3)O₃, and lead titanate, PbTiO₃, were fabricated using the Mg₄Nb₂O₉ precursor technique. Their electrical properties with respect to temperature and frequency were examined and the effect of sintering conditions on phase formation, densification, microstructure and electrical properties of the ceramics were examined. It has been found that optimisation of sintering conditions can lead to a highly dense and pyrochlore-free PMN–PT ceramics. The gradual decrease of the physical properties of the sintered ceramics was related to the gradual decrease of density and inhomogeneous microstructure. The results also revealed that for the lower concentration of lead titanate, a relaxor behaviour is noticed with a high electrostrictive effect, which was almost hysteretic free. However, higher amount of lead titanate led to a normal ferroelectric behaviour.     

Crystal Structure and Dielectric Properites of Bao.6Sr0.4TiO3/MgO Ceramics Doped with ZrO2 and MnO2

通过固相反应法制备Mn、Zr共掺杂钛酸锶钡／氧化镁陶瓷粉体,经干压成型后在空气气氛中于l450℃烧结4h,通过扫描电子显微镜和X射线衍射研究了ZrO2和MnO2共掺杂的Bao6Sro4TiO3／MgO复合陶瓷材料的微结构和介电性能。结果表明：Zr02可以显著降低材料的介电常数和介电损耗,有效提高了陶瓷材料的温度稳定性;随ZrO2添加量的增加,体系的晶胞参数略有增加,MgO在钛酸锶钡中以独立相的形式存在：制备出的BST铁电陶瓷材料的25℃相对介电常数较低（＆〈110）,介质损耗小于1．0×10^-3（在频率为10kHz时）,温度系数小于6．012×10^-3,可调性大于20％（8．0kV／mm）,适用于制作移相器。     

添加Co2O3对微波低介电常数陶瓷机械品质因数的影响

研究了添加不同质量分数的Co2O3对Mg3TiO4-Mg2SiO3基微波低介瓷料微观结构及介电性能的影响，通过XRD，SEM分析，发现Co2O3在瓷料中起助溶作用，有效降低了瓷料的烧结温度，使瓷体致密化，同时降低了损耗即提高了机械品质因数Q。加入的Co2O3分解生成的Co2^ 置换主晶相Mg2TiO3中的Mg^2 形成了固溶体(Mg，Co)2TiO3。当添加质量分数为2．4％的Co2O3时获得介电性能较好的瓷料。     

Formation of the Perovskite Phase in the PbMg1/3Nb2/3O3─PbTiO3 System

The reaction sequences during calcination of oxide mixtures were studied for the PbMg_1/3Nb_2/3O₃─PbTiO₃ (PMN-PT) system. The effect of reactivity and composition of the starting mixtures was investigated. In the present study, a B-site-deficient, cubic pyrochlore phase in the PbO-Nb₂O₅ system was formed at 500°C. The perovskite phase of PMN was formed at 7007deg;C through the diffusion of MgO into the pyrochlore phase. The lattice parameter of the pyrochlore phase decreased as this transformation to perovskite progressed.     

Effect of MgO Doping on the Phase Transformations of BaTiO3

The successive phase transformations in MgO-doped BaTiO₃ were studied. Upon MgO doping, dielectric anomalies corresponding to lower phase transformations were broadened and depressed, while an anomaly for a cubic–tetragonal transformation remained and shifted to a lower temperature. XRD peak splitting upon tetragonality of BaTiO₃ was decreased, and the peaks exhibited abnormally broadened profiles which are different from the one for cubic BaTiO₃ above T _c. Raman spectroscopy revealed the existence of orthorhombic phase at room temperature for the solid solution with 0.5 mol% or more MgO. The temperature dependence of the Raman spectrum showed that orthorhombic and rhombohedral phases in MgO-doped BaTiO₃ were stabilized at higher temperatures than pure BaTiO₃.     

Al2(1-x)MgxTi1+xO5体系固溶体的合成及其热性能研究

通过固相法以MgO*2TiO2为稳定剂合成了Al2(1-x)MgxTi1+x O5 (简称AMT) (x=0, 0.01, 0.05,0.1, 0.3)体系固溶体粉末.研究了该固溶体粉末的物相组成、以及热分解性能与x值变化的关系.采用无压烧结法对制备的固溶体AMT粉末进行烧结,用热膨胀仪测试了烧结体热膨胀性能.粉末X射线衍射结果表明随着x 值的增大, 固溶体AMT晶格常数线性增大、热稳定性越高.当x=0.05时,将该固溶体在1 100 ℃保温10个 h, 仅有9%的分解率.通过热膨胀仪测试烧结体, 其结果表明在室温至550 ℃范围内AMT体系的热膨胀率均小于零.当x=0.1时, 固溶体AMT有相对较低的热膨胀率, 并对其原因进行了分析.