低温烧结BSCT-MgO复合铁电材料及其介电性能研究
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摘要
为了实现钛酸锶钡钙(BSCT)基调谐性材料LTCC应用化,本文的目标是低温烧结下制备适中介电常数、低介电损耗、高可调性和介电温度稳定性好的陶瓷材料。本课题研究MgO在BSCT-MgO复相材料的作用和机理,Mn掺杂和B_2O_3-ZnO玻璃的掺杂对BSCTM材料的介电性能改善和低温烧结的影响。纳米MgO粉体和共沉淀的BSCT粉体具有精细结构,采用B_2O_3-Li_2CO_3烧结助剂,发现单一相材料在1000℃下未达到致密烧结,且含有较多的气孔。MgO的加入使复合材料气孔消失,结构变得致密。MgO增加,BSCT晶粒逐渐减小,介电常数也随之降低,居里温度向低温移动,MgO添加量为60wt%时,晶粒减小为0.7-1.5μm,介电常数为90,损耗维持在1×10~(-3)数量级,居里温度为-27℃。950℃烧结时,BSCT-1wt%MgO在室温、1kV/mm直流偏场条件下的可调性高达18%,介电温度曲线较为平坦,这一优异性能可以与1200℃制备的纯BSCT材料的可调性20%相媲美。实现了低温烧结制备高调谐性、介温性能稳定的BSCT基铁电材料。MgO的加入,改善了高温下B_2O_3-Li_2O液相的粘度,提高了液相的流动性,便于扩散与传质。MgO的加入,提高了B_2O_3-Li_2O液相对BSCT晶粒的润湿性,良好的润湿环境促使“小颗粒粉体—MgO-B_2O_3-Li_2O液相—BSCT晶粒”模式进行顺畅,晶粒更好地吸收液相传质,从而促进晶粒发育,材料致密化程度增加。
BSCTM复相材料的居里温度随着Mn离子掺杂量增大向负温度移动,可调性呈先增大后减小趋势。当Mn=0.50mol%时,950℃烧结的BSCT-45wt%MgO复相材料在0.71kV/mm下的可调性高达4.8%,实现了低温烧结制备高可调性材料的目的。BSCT-45wt%MgO材料,添加10wt% B_2O_3-ZnO玻璃时,1000℃烧结形成大量的玻璃相,破坏了BSCT中Ti离子非谐运动的连续性,导致可调性丧失。为了改善这一材料,采用提高铁电相和降低玻璃量,BSCT-22wt%MgO复相材料添加2.5wt%和5.0wt% B_2O_3-ZnO玻璃后,1000℃烧结,在1MHz下的介电常数ε、介电损耗tanδ和可调性(直流偏场)依次为235.7, 1.52×10~(-3), 5.29%(0.66kV/mm)和299.8, 1.43×10~(-3), 4.17%(0.75kV/mm);其介电常数温度稳定性得到极大改善;在20Hz~2MHz的频率范围内,介电常数基本稳定不变。
In order to achieve the application of LTCC on barium strontium calcium titanate(BSCT)-based tuning materials,this article aims to prepare moderate dielectric constant, low dielectric loss, high tunability and good dielectric temperature stability of BSCT based ceramics at low sintering temperature. In this thesis, we have had more focus on role mechanism of MgO and Mn-doping and B_2O_3-ZnO glass doping on low-temperature sinterability and dielectric properties of Ba_(0.55)Sr_(0.4)Ca_(0.05)TiO_3–MgO composite ferroelectric ceramics. Nano-MgO powder and Ba_(0.55)Sr_(0.4)Ca_(0.05)TiO_3 powder prepared by co-precipitation both had superfine structure. Using B_2O_3-Li_2CO_3 as sintering additives, we found that a single phase material (pure BSCT or MgO) sintered at 1000℃contain more pores and non-dense structure. After doping MgO low-dielectric, non-ferroelectric phase, BSCT-MgO composite material become less pores and more densely. When increasing the content of MgO in composite material, the size of BSCT grains and dielectric constant gradually reduced, curie temperature also shifted to lower temperature. When w(MgO)=60wt%, the size of BSCT grains reduced to 0.7-1.5μm, whose dielectric constant, dielectric loss and curie temperature were about 90, 1×10~(-3) and -27℃, respectively. BSCT-1wt%MgO composite material sintered at 950℃had more relatively flat dielectric-temperature curve and higher tunability 18% (room temperature, 1kV/mm), these excellent performance are compatible with the tunability 20% of pure BSCT sintered at 1200℃, this technology can have realized low-temperature sintering of BSCT based ferroelectric materials with high tunability, stable dielectric-temperature properties. MgO doping did not only improve the viscosity of B_2O_3-Li_2O liquid to increase the flow of liquid and mass diffusion, but also increased wettability of B_2O_3-Li_2O liquid at high temperature for BSCT grains, thus "Small particles—MgO-B_2O_3-Li_2O liquid—BSCT grains "pattern was carried out more smoothly by good wetting environment, Grains growth were accelerated by mass transfer in liquid phase, therefore densification of BSCTM material also increased.
With the increasing of the amount of Mn ions, the curie temperature of BSCTM composite material shifted to lower temperature and tunability first increased and then decreased. When sintering temperature lower to 950℃and Mn= 0.50mol%, the tunability of BSCT-45wt%MgO composite material under a DC field of 0.71 kV/mm achieves 4.8%. It had realized preparation technology of high tunability of ferroelectric material at lower sintering temperatures. After doping 10wt% B_2O_3-ZnO glass, BSCT-45wt% MgO material sintered at 1000℃had very small tunability because a large number of glass phase destroyed the continuity of the non-harmonic movement of Ti ions in BSCT. In order to improve this poor performance, we can increase the ferroelectric phase and reduce the amount of B_2O_3-ZnO glass. Adding 2.5wt% and 5.0wt% B_2O_3-ZnO glass to BSCT-22wt%MgO composite material can be sintered at 1000℃with excellent dielectric properties, when measure at 1MHz, theirε, tanδand tunability (under a DC field) were 235.7, 1.52×10~(-3), 5.29% (0.66kV/mm) and 299.8, 1.43×10~(-3), 4.17% (0.75kV/mm), respectively, the temperature stability of dielectric constant is improved, dielectric constant remains stable between 20Hz and 2MHz.
BSCTM复相材料的居里温度随着Mn离子掺杂量增大向负温度移动,可调性呈先增大后减小趋势。当Mn=0.50mol%时,950℃烧结的BSCT-45wt%MgO复相材料在0.71kV/mm下的可调性高达4.8%,实现了低温烧结制备高可调性材料的目的。BSCT-45wt%MgO材料,添加10wt% B_2O_3-ZnO玻璃时,1000℃烧结形成大量的玻璃相,破坏了BSCT中Ti离子非谐运动的连续性,导致可调性丧失。为了改善这一材料,采用提高铁电相和降低玻璃量,BSCT-22wt%MgO复相材料添加2.5wt%和5.0wt% B_2O_3-ZnO玻璃后,1000℃烧结,在1MHz下的介电常数ε、介电损耗tanδ和可调性(直流偏场)依次为235.7, 1.52×10~(-3), 5.29%(0.66kV/mm)和299.8, 1.43×10~(-3), 4.17%(0.75kV/mm);其介电常数温度稳定性得到极大改善;在20Hz~2MHz的频率范围内,介电常数基本稳定不变。
In order to achieve the application of LTCC on barium strontium calcium titanate(BSCT)-based tuning materials,this article aims to prepare moderate dielectric constant, low dielectric loss, high tunability and good dielectric temperature stability of BSCT based ceramics at low sintering temperature. In this thesis, we have had more focus on role mechanism of MgO and Mn-doping and B_2O_3-ZnO glass doping on low-temperature sinterability and dielectric properties of Ba_(0.55)Sr_(0.4)Ca_(0.05)TiO_3–MgO composite ferroelectric ceramics. Nano-MgO powder and Ba_(0.55)Sr_(0.4)Ca_(0.05)TiO_3 powder prepared by co-precipitation both had superfine structure. Using B_2O_3-Li_2CO_3 as sintering additives, we found that a single phase material (pure BSCT or MgO) sintered at 1000℃contain more pores and non-dense structure. After doping MgO low-dielectric, non-ferroelectric phase, BSCT-MgO composite material become less pores and more densely. When increasing the content of MgO in composite material, the size of BSCT grains and dielectric constant gradually reduced, curie temperature also shifted to lower temperature. When w(MgO)=60wt%, the size of BSCT grains reduced to 0.7-1.5μm, whose dielectric constant, dielectric loss and curie temperature were about 90, 1×10~(-3) and -27℃, respectively. BSCT-1wt%MgO composite material sintered at 950℃had more relatively flat dielectric-temperature curve and higher tunability 18% (room temperature, 1kV/mm), these excellent performance are compatible with the tunability 20% of pure BSCT sintered at 1200℃, this technology can have realized low-temperature sintering of BSCT based ferroelectric materials with high tunability, stable dielectric-temperature properties. MgO doping did not only improve the viscosity of B_2O_3-Li_2O liquid to increase the flow of liquid and mass diffusion, but also increased wettability of B_2O_3-Li_2O liquid at high temperature for BSCT grains, thus "Small particles—MgO-B_2O_3-Li_2O liquid—BSCT grains "pattern was carried out more smoothly by good wetting environment, Grains growth were accelerated by mass transfer in liquid phase, therefore densification of BSCTM material also increased.
With the increasing of the amount of Mn ions, the curie temperature of BSCTM composite material shifted to lower temperature and tunability first increased and then decreased. When sintering temperature lower to 950℃and Mn= 0.50mol%, the tunability of BSCT-45wt%MgO composite material under a DC field of 0.71 kV/mm achieves 4.8%. It had realized preparation technology of high tunability of ferroelectric material at lower sintering temperatures. After doping 10wt% B_2O_3-ZnO glass, BSCT-45wt% MgO material sintered at 1000℃had very small tunability because a large number of glass phase destroyed the continuity of the non-harmonic movement of Ti ions in BSCT. In order to improve this poor performance, we can increase the ferroelectric phase and reduce the amount of B_2O_3-ZnO glass. Adding 2.5wt% and 5.0wt% B_2O_3-ZnO glass to BSCT-22wt%MgO composite material can be sintered at 1000℃with excellent dielectric properties, when measure at 1MHz, theirε, tanδand tunability (under a DC field) were 235.7, 1.52×10~(-3), 5.29% (0.66kV/mm) and 299.8, 1.43×10~(-3), 4.17% (0.75kV/mm), respectively, the temperature stability of dielectric constant is improved, dielectric constant remains stable between 20Hz and 2MHz.
引文
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