Bi2O3及MnO2掺杂对[(Pb,Ca) La](Fe,Nb)O3介质陶瓷结构及微波性能的影响

研究了Bi2O3及MnO2掺杂量对[(Pb0.5Ca0.5)0.92La0.08](Fe0.5Nb0.5)O3陶瓷结构及介电性能的影响.结果表明Bi2O3及MnO2均是良好的烧结助剂,可降低体系的烧结温度60～100 ℃,同时提高陶瓷的密度.XRD图谱证明当MnO2的质量分数≤2%时,陶瓷为钙钛矿相及焦绿石相,表明Mn4+进入主相晶格,而Bi2O3的掺杂会使体系中出现未知第三相.随MnO2的增加,陶瓷的介电常数先增加后减小,同时使品质因数及谐振频率温度系数的单调下降.Bi2O3的掺杂则会使陶瓷介电常数及谐振频率温度系数升高,而品质因数下降.Bi2O3及MnO2的联合掺杂比单一掺杂更有效地降低了陶瓷的烧结温度,达100～140 ℃,且在低温烧结条件下有比单一掺杂时更好的微波介电性能.其中当Bi2O3和MnO2的质量比k=1,2种添加物总质量分数w=1%,烧结条件为1 050 ℃,保温4 h,陶瓷的相对介电常数εr,品质因数(Q)与谐振频率(f)的乘积Qf以及谐振频率温度系数分别为91.1, 4 870 GHz和18.5×10-6/℃.     

弛豫铁电陶瓷Ba(Mg,Nb)O_3的制备及性能研究

采用传统陶瓷烧结方法,在空气气氛下烧结制得Ba(Mg,Nb)O3(BMN)陶瓷,并分析了烧结温度对体系相组成及相结构的影响。X射线衍射(XRD)研究表明,随着烧结时间的增加,体系中钙钛矿相也相应增加。红外(FTIR)研究研究表明结构无序的BMN钙钛矿相中部分的区域出现了结构有序现象。通过X射线光电子能谱(XPS)可以发现,随着烧结温度的增加,体系中Nb2O5进入Ba(Mg1/3,Nb2/3)O3晶格。微波介电性能表明,随着烧结温度的增加,Ba(Mg,Nb)O3的rε和Qf值有逐渐增加的趋势。     

等轴晶ZrO2(Al2O3, Fe2O3)复相陶瓷的制备

讨论了以硝酸盐溶液为原料，经喷雾干燥、热解、成型、烧结或直接烧结制备等轴晶ZrO2(Al2O3, Fe2O3)复相陶瓷的过程. 研究了成型压力、烧结温度、恒温时间及Al3+, Fe3+的加入对ZrO2陶瓷的相组成、晶粒大小和形貌的影响. 结果表明：成型压力对相组成及晶粒尺寸无明显影响；无论是直接采用硝酸盐复合粉末还是采用氧化物粉末压坯作为前驱物，烧结产物的形貌、相组成不变；加入Fe2O3可克服微观结构层状堆垛，获得相对细小均匀的等轴晶粒，且随Fe2O3含量的增加，单位体积中a-(Al, Fe)2O3核心的数量增加，晶粒尺寸更加细小、均匀，Fe2O3含量相对于Al2O3在20%左右时效果最佳；各相晶粒在长时间高温烧结时生长速度较为缓慢，0.5 h为0.5 mm左右，烧结12 h才到2.0 mm左右.     

以MnO2-TiO2-MgO为添加剂注浆成型低温烧结Al2O3陶瓷

采用注浆成型方法,通过加入MnO2-TiO2-MgO复相添加剂,在1350℃空气气氛中常压烧结,获得了相对密度最大为95.7%的氧化铝陶瓷.研究了MnO2-TiO2-MgO复相添加剂对氧化铝陶瓷显微结构与力学性能的影响.在添加质量分数为3%MnO2,0.5%MgO的情况下,比较添加不同质量分数的TiO2(1.0～3.0%)对氧化铝陶瓷烧结性能的影响.通过对比发现,该复相添加剂能有效降低氧化铝陶瓷的烧结温度,在同一温度下,随着TiO2的增加,烧结体密度也随之增加,强度也有明显差别.结果表明,1350℃下Al2O3+0.5%MgO+3%MnO2+1.5%TiO2体系烧结效果最好,断口为沿晶断裂,无明显气孔,晶粒分布均匀,平均粒径为2μm,无晶粒异常长大现象.烧结体密度达到3.80g/cm3,抗弯强度为243MPa.     

锰掺杂对PNW-PMS-PZT压电陶瓷结构和性能的影响

采用传统陶瓷工艺制备了Pb(Ni1/2W1/2)O3-Pb(Mn1/3Sb2/3)O3-Pb(Ti，Zr)O3-xMnO2压电陶瓷，分析了经1150℃烧结2h制备的陶瓷样品的相结构组成。实验结果表明：所有陶瓷样品均为钙钛矿相，未发现其它晶相。随着锰掺杂量的增加，陶瓷晶粒逐渐长大。研究了不同剂量的锰掺杂对压电陶瓷介电和压电性能的影响。结果表明：随着锰掺杂量的增加，材料逐渐变“硬”，当MnO2掺杂量少于0．2％(按质量计，下同)时，相对介电常数εr、压电常数d33和机械品质因数Qm逐渐增加，介电损耗tanδ减小；当MnO2掺杂量多于0．2％时，εr、d33和Qm逐渐降低，tanδ增加。随着锰掺杂量的增加，机电耦合系数kp和Curie温度θc逐渐减小。MnO2掺杂量为0．2％的压电陶瓷适合制作大功率压电陶瓷变压器。其压电性能为：εr=2138，tanδ=0．0058，kp=0．613，Qm=1275，d33=380pC／N和θc=205℃。     

TiO_2添加量对Zn_(0.8)Mg_(0.2)ZrNb_2O_8微波介质陶瓷结构和性能的影响

采用传统固相合成工艺制备(1–x)Zn0.8Mg0.2Zr Nb2O8-x TiO_2(ZMZNT,x=0.00,0.20,0.40,0.50,0.60,0.65,0.70,0.80)微波介质陶瓷,研究了TiO_2添加量对Zn0.8Mg0.2Zr Nb2O8陶瓷烧结行为、相结构、微观结构以及微波介电性能的影响。结果表明:随着TiO_2添加量增加,ZMZNT陶瓷的烧结温度逐步下降。当x=0~0.5时,形成了Zn0.8Mg0.2(Zr,Ti)Nb2O8固溶体;而当x=0.6~0.8时,陶瓷体系发生了复杂物相变化,微观形貌也呈现对应的变化规律。随着TiO_2添加量的增加,ZMZNT陶瓷相对介电常数εr逐渐增大,品质因数Q×f呈下降趋势,谐振频率温度系数τf呈上升趋势。当x=0.65时,0.35Zn0.8Mg0.2Zr Nb2O8-0.65 TiO_2陶瓷在1 170℃烧结4 h,可以获得较佳的微波介电性能:εr=36.7,Q×f=37 432 GHz,τf=7.12×10–6/℃。     

添加剂对低温烧结95氧化铝陶瓷性能的影响

采用MnO2-TiO2-CaO-La2O3复相添加剂作为氧化铝陶瓷的烧结助剂,研究了MnO2添加量对95氧化铝陶瓷烧结性能、力学性能和微观结构的影响。结果表明:当配方中MnO2含量为3.0%时,在1550℃烧结温度下制得的氧化铝陶瓷的综合性能最佳,烧结试样的体积密度达到3.76g.cm-3,试样的抗弯强度和洛氏硬度(HRA)分别达到355.22MPa和84.3。     

Sn掺杂对锂铌钛体系微波介质陶瓷性能的影响

引入SnO2对Li2O-Nb2O5-TiO2体系陶瓷进行掺杂改性研究，考察了SnO2的添加量对LiNb0.6Ti0.5-xSn2O3陶瓷的烧结性能、显微结构和微波介电性能的影响。研究表明：对所考察的体系而言．随着SnO2添加量的增加．烧结样品体积密度和介电常数基本保持不变；而品质因数Qf值随SnO2的加入有所提高，而后随SnO2含量继续增加而快速下降；在1100℃的烧结温度下．当X=0．01时．获得微波介电性能优良的微波陶瓷，其ε=678．x1=＋4ppm／℃．Qf=6780GHz。     

Na_(0.5)Bi_(0.5)TiO_3:ZnO无铅复相陶瓷的显微结构与铁电性能

采用二步固相法制备了0.8Na_(0.5)Bi_(0.5)TiO_3:0.2ZnO无铅复相铁电陶瓷,研究了不同烧结温度制备的复相陶瓷的烧结性能、显微结构和铁电性能。结果表明:Na_(0.5)Bi_(0.5)TiO_3中引入20%(摩尔分数)ZnO后,复相陶瓷产生了第三相Zn_2TiO_4,并且随着烧结温度的升高,Zn_2TiO_4含量逐渐增加。1 000℃烧结的陶瓷样品的剩余极化强度在测试温度为135℃时仍然保留了室温下的81%,且随着烧结温度的升高,不同样品的剩余极化强度没有减小的趋势,证明了ZnO所形成的内建电场提高了Na_(0.5)Bi_(0.5)TiO_3铁电性的高温稳定性。     

铌酸锶钡/钛酸锶钡复相陶瓷形成过程研究

应用粉末-溶胶工艺合成出铌酸锶钡/钛酸锶钡复相陶瓷(SBN/SBT)。采用X射线衍射技术研究了不同预烧温度的原始粉料、不同烧结温度和不同保温时间得到的铌酸锶钡/钛酸锶钡复相陶瓷。研究表明:钨青铜相和钙钛矿相共存于体系之中。复相陶瓷形成过程中形成了TiO2、BaNb2O6(BN)、SrNb2O6(SN)等中间相,增加烧结温度至1250℃,形成了铌酸锶钡/钛酸锶钡复相陶瓷。     

ZnO和Na2O对CaO-B2O3-SiO2介电陶瓷结构与性能的影响

研究了烧结助剂ZnO和Na2 O对CaO -B2 O3 -SiO2 (CBS)系微波介质陶瓷介电性能、相组成及结构特性的影响。烧结助剂ZnO在烧结过程中与B2 O3 及SiO2 生成低熔点玻璃相 ,有效地降低了材料的致密化温度 ,烧结机理为液相烧结。碱金属氧化物Na2 O虽然能够有效降低材料的烧结温度 ,但会破坏硅灰石晶体结构 ,引起材料微波性能显著降低。通过实验 ,制备出了具有优良微波介电性能的陶瓷材料 ,适用于LTCC基板及滤波器等高频微波器件的生产     

Comparison of hydrothermal corrosion behavior of SiC with Al2O3 and Al2O3 + Y2O3 sintering additives

Fully dense SiC bulks with Al₂O₃ and Al₂O₃ + Y₂O₃ sintering additives were prepared by spark plasma sintering and the effect of sintering additives on the hydrothermal corrosion behavior of SiC bulks was investigated in the static autoclave at 400°C/10.3 MPa. The SiC specimen with Al₂O₃ sintering additive exhibited a higher weight loss and followed a linear law. However, the SiC specimen with Al₂O₃ + Y₂O₃ additive exhibited a lower weight loss and followed a parabolic law, indicating that the corrosion kinetic and mechanism were different for these two SiC bulks. Further examination revealed that, a deposited layer was formed on the surface of SiC specimen with Al₂O₃ + Y₂O₃ sintering additive after corrosion, which can effectively protect the SiC specimen from further corrosion, and thereby improved the corrosion resistance of the SiC specimen with Al₂O₃ + Y₂O₃ sintering additive.     

Pixelated sintering of α-Al2O3

The sintering of α-alumina by a brand new and innovative technique, called pixelated sintering (PS), is here studied. Densification and grain growth by PS of perfectly controlled granular compacts are analysed and compared to results obtained using Spark Plasma Sintering (SPS) and Pressure-Less SPS (PL-SPS). Materials are exposed to the same temperature profiles whatever the sintering technique used in order to assess the potential of PS in terms of microstructure control. It is shown that PS can be used as an alternative technique to SPS for fast sintering with the advantages of a much simpler and cost-effective set-up, as well as a better control of the localised heat input. PS also appears to be a very modular technology in the way it controls the temperature gradients allowing its implementation for multi-step sintering approaches, as well as for the fabrication of large and complex parts.     

Al2O3/Cr3C2/(W,Ti)C陶瓷材料的力学性能及微观结构

用热压烧结工艺在1 700℃,28 MPa保温保压30 min及N2气氛条件下,制备了添加不同含量Cr3C2和(W,Ti)C颗粒的Al2O3/CraC2/(W,Ti)C复合陶瓷材料.对复合陶瓷的力学性能进行测试.用环境扫描电镜、透射电镜和能谱分析仪对复合陶瓷的显微结构进行观察.结果表明与纯Al2O3相比,70Al2O3/10Cr3C2/20(W,Ti)C复合陶瓷材料的显微组织更均匀细化,具有良好的综合力学性能,其断裂韧性自纯Al2Oa陶瓷的4.0 MPa·m1/2提高到8.92 MPa·m1/2.分析发现其内部位错机制、纳米颗粒的淀析、裂纹扩展路径偏转、沿晶断裂、韧窝及解理撕裂等是材料断裂韧性提高的主要原因.     

Ultra-rapid microwave sintering of pure and Y2O3-doped MgAl2O4

MgAl₂O₄ samples were microwave sintered to near-full density in rapid processes with heating rates on the order of 100°C/min and zero isothermal hold. The experiments were carried out using a gyrotron system for microwave processing of materials operating at a frequency of 24 GHz with a maximum power of 6 kW. In the regimes with a preset heating rate sustained by the automatically regulated microwave power, the maximum achieved density was about 95% of the theoretical value in pristine MgAl₂O₄ samples (maximum sintering temperature 1650°C) and about 97% in 1 wt.% Y₂O₃-doped samples (1700°C). In the regimes with a fixed microwave power (about 3.5 kW), translucent spinel samples with a relative density above 99% were obtained at 1700°C. The duration of the high-temperature stage of sintering was 1.5-10 minutes. The suggested mechanism responsible for the enhanced densification involves development of a thermal instability and formation of transient liquid phases at grain boundaries. The estimated specific absorbed power in the samples during the high-temperature stage of ultra-rapid microwave sintering was 27-80 W/cm³, similar to the values observed in dc field-assisted flash sintering experiments.     

Highly resistive SiC ceramics sintered with Al2O3-AlN-Y2O3 additions

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.     

纳米Al2O3-ZrO2(3Y)复相陶瓷的微波烧结

采用纳米Ａｌ２Ｏ３粉和纳米ＺｒＯ２（３Ｙ）粉为原料,对不同成分配比的Ａｌ２Ｏ３－ＺｒＯ２（３Ｙ）复相陶瓷进行了微波为烧结的研究。实验结果表明微波烧结可获得委肮的致密度,并提高断裂韧性,但晶粒长大倾身大于其它烧结方式;在Ａｌ２Ｏ３－ｚｒ２（３Ｙ）二元系中,随ＺｒＯ２（３Ｙ）含量啬,烧结时的致密化过程加速,且晶粒长大倾向减小。     

BaCu（B2O5）助烧剂对CaO-Li2O-Sm2O3-TiO2微波介质陶瓷介电性能的影响

16CaO-9Li2O-12Sm2O3-63TiO2(CLST)陶瓷的烧结温度接近1 300℃,添加BaCu(B2O5)(BCB)陶瓷粉体使CLST陶瓷的烧结温度降至1050℃.随着烧结温度的升高,样品的体积密度先升高而后趋于稳定,添加质量分数为4?B的CLST陶瓷在1 050℃烧结后得到96%的相对密度.相对介电常数(εr)随着BCB添加量的增大先增大后略有减小.由于液相的存在,介电损耗(tanoδ随着BCB添加量的增大而增大.谐振频率温度系数(tf)与纯CLST陶瓷相比更加近零.添加质量分数为4?B的CLST陶瓷在1 050℃烧结2h后得到良好的介电性能:εr=81,tanδ=0.021,tf=0.5×10-6/℃(1MHz).     

CaO-SiO2-Al2O3-Fe2O3-SO3多元体系高温相变研究

实验采用石灰石、砂岩、粉煤灰和低品位铝矾土等工业原料,制备C3S相和C4A3S-相共存的水泥熟料;利用DSC-TG、高温XRD、岩相等方法对CaO-SiO2-Al2O3-Fe2O3-SO3多元体系烧制过程中高温相变进行分析,获得C4A3S-相和C3S相的变化规律,为利用废渣制备低碳排放的水泥熟料提供了理论支持.