MRAlO_4（M=Sr，Ca；R=La，Nd，Sm，Y）微波介质陶瓷的基础问题及其改性
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摘要
系统地研究了属于14/mmm空间群的MRAlO_4(M=Sr,Ca;R=La,Nd,Sm,Y)基微波介质陶瓷的制备、结构、微波介电性能及其随成分与结构变化的规律,并基于上述规律对CaSmAlO_4基陶瓷进行了改性,取得如下主要结论与成果:
建立了一套包括开腔法和闭腔法的微波介电性能的测量评价系统。对复介电常数的数值计算的算法进行了改进,大幅度提高了计算效率,从而间接地提高了计算精度,并利用改进算法拓展了闭腔法的应用范围。
通过XRD全谱拟合对MRAlO_4(M=Sr,Ca;R=La,Nd,Sm,Y)陶瓷的晶体结构进行精修。AlO_6八面体和(M,R)P_9十二面体在c轴方向分别受到强烈拉伸和强烈压缩,而在ab平面内的情况则正好相反。层间尺寸失配和层间极化是造成多面体畸变的两个主要原因,它们可以分别用结构许容因子和氧八面体畸变程度(或者(M,R)O_9中心阳离子与O(2a)原子面的距离)来衡量。随着结构许容因子的减小,(M,R)O。的畸变加剧,而AlO_6的畸变基本保持不变。根据键价理论的分析,SrYAlO_4的不稳定性和CaLaAlO_4的亚稳定性分别是由共同占据A位的两种阳离子的离子半径相差太大和离子价态相差太大造成的。
为了从极性声子模的角度理解MRAlO_4(M=Sr,Ca;R=La,Nd,Sm,Y)陶瓷的微波介电响应的本质,测量了MRAlO_4陶瓷50～4000cm~(-1)范围内的红外反射光谱,利用K-K关系、经典谐振子模型对红外数据进行分析,并将红外数据外推到微波频段以估计本征微波介电损耗。(M,R)-AlO_6沿着ab平面的弯曲振动模和沿着c轴的伸缩振动模是对微波介电常数和介电损耗起主要贡献的两个模式。(M,R)O_9十二面体的畸变极大地影响了这两个模式的色散参数,从而决定了极化率和本证损耗,这就是MRAlO_4实测的极化率大幅度偏离氧化物加和法则得到的预测值以及MRAlO_4的Qf计算值随着结构许容因子的减小而减小的原因。减小本征介电损耗的关键是减小(M,R)O_9十二面体的畸变。Qf计算值大大高于实测值,表明通过优化微结构还能大幅度减小非本征损耗。
通过改变CaO、Sm_2O_3和Al_2O_3的配比,研究了CaSmAlO_4基陶瓷的相组成及其对微结构和微波介电性能的影响。在(2+2x)CaO～(1-x)Sm_2O_3～Al_2O_3(x=-0.10,-0.05,0,0.05,0.10,0.20)陶瓷中,当x＞0时检测到Ca_3Al_2O_6和CaO第二相,而当x≤0时则是SmAlO_3和Sm_2O_3第二相。在(2+2x)CaO·Sm_2O_3·Al_2O_3(x=-0.02,-0.01,0,0.02,0.04)陶瓷中,当x＞0时检测到CaSmAl_3O_7、CaO和Sm_2O_3第二相,而当x≤0时,检测到SmAlO_3第二相。Ca_3Al_2O_6和SmAlO_3第二相会大幅度降低体系的Qf值,而CaSmAl_3O_7、CaO和Sm_2O_3第二相对体系的Qf值的不利影响很小甚至有利于Qf值的提高。在(2+2x)CaO·Sm_2O_3·Al_2O_3(x=0.02,0.03,0.04)陶瓷中获得了优异的微波介电性能:ε_r=19,Qf=120,000～125,300GHz,τ_f=-10～-9ppm/℃。
通过Ca/Ti协同置换对CaSmAlO_4进行改性,得到了Ca_(1+x)Sm_(1-x)Al_(1-x)Ti_xO_4(0≤x≤0.4)陶瓷。对于Ca_(1+x)Sm_(1-x)Al_(1-x)Ti_xO_4主相而言,随着x的增大,晶胞参数a和c分别线性地增大和减小;(Al,Ti)O_6八面体的畸变略有减小,而(M,R)O_9十二面体的畸变逐渐加大,后者是晶胞参数c减小的原因。Ca_(1+x)Sm_(1-x)Al_(1-x)Ti_xO_4陶瓷具有良好的微波介电性能,尤其是当0.06≤x≤0.2时(ε_r≈20,Qf=96,500～118,700GHz,τ_f=-8～2ppm/℃)。当x=0时检测到了少量的SmAlO_3第二相,而当x≥0.15时检测到了微量的CaTiO_3第二相;在x=0和0.02成分点1500℃烧结的样品中观察到晶粒的异常长大。抑制这些微结构的产生有助于改善体系的微波介电性能。适当加入过量的CaO,Ca_(1+x)Sm_(1-x)Al_(1-x)Ti_xO_4基陶瓷的微波介电性能得到进一步改善,当x=0.15时,实现了极其优异的微波介电性能(ε_r=20.2,Qf=100,000GHz和τ_f=0.5 ppm/℃)。
Synthesis,structures,and microwave dielectric properties of MRAlO_4-based(M=Ca, Sr;R=La,Nd,Sm,Y) ceramics with I4/mmm space group were systermatically investigated together with their property-structure relationship,and based on these findings,the modification of microwave dielectric properties was carried out for CaSmAlO_4 ceramics through structure tailoring and microstructure control.The following primary findings and/or achiements were obtained:
An evaluation system involving the open cavity method and the closed cavity method was built up to characterize the microwave dielectric properties with high accurately.An innovative algorithm for numerical calculation of complex permittivity was developed,and the computational efficiency was improved greatly.With the algorithm,the application scope of the close cavity method was significantly extended.
Crystal structure refinements were carried out for MRAlO_4 ceramics by Rietveld method.Along the c axis,AlO_6 octahedra and(M,R)O_9 dodecahedra were heavily stretched and compressed,respectively,while within the ab plane,the situation was reversed.The interlayer size mismatch and the interlayer electric polarization were the primary reasons for these distortions,and they could be evaluated with the tolerance factor and the deformation degree of octahedron(or the distance from(M,R) cation to O(2a) atomic plane),respectively.As the tolerance factor decreased,the distortion of AlO_6 octahedra kept nearly unchanged,while that of(M,R)O_9 increased.Based on the analysis by the bond valence method,the instability of SrYAlO_4 and the metastability of CaLaAlO_4 were attributed to large differences of ionic radius and of apparent bond valence between M and R cations,respectively.
To understand the dielectric nature of MRAlO_4 ceramics in terms of phonon modes,Fourier transform infrared reflectivity spectra in the range of 50-4000 cm~(-1) were measured and evaluated by means of K-K ananlysis and classical oscillator fit.The data were extrapolated below the measured frequency range to estimate the intrinsic microwave losses.The bending and stretching vibration modes of(M,R)-AlO_6 gave primary contributions to the microwave complex permittivity,therefore the distortion of (M,R)O_9 dodecahedra greatly affected the dispersion parameters of these two modes and consequently dominated polarizabilities and intrinsic dielectric losses of MRAlO_4. This could explain the great deviation of measured polarizabilities from those predicted by the oxide additivity law and the variation of calculated Qf values with the tolerance factor.To minimize the intrinsic dielectric loss,it was the keypoint to reduce the distortion of(M,R)O_9 dodecahedra.Moreover,the fact that the calculated Qf values were much higher than the measured ones suggested a great opportunity to improve Qf through optimizing the microstructures.
By changing molar ratios among CaO,Sm_2O_3,and Al_2O_3,the effects of secondary phases on mcirostructures and microwave dielectric properties were investigated for CaSmAlO_4-based ceramics.In(2+2x)CaO·(1-x)Sm_2O_3·Al_2O_3(x=-0.10,-0.05,0,0.05, 0.10,0.20)ceramics,Ca_3Al_2O_6 and CaO secondary phases were observed at x＞0,while SmAlO_3 and Sm_2O_3 secondary phases were observed at x≤0.In (2+2x)CaO·Sm_2O_3·Al_2O_3(x=-0.02,-0.01,0,0.02,0.04) ceramics,CaSmAl_3O_7,CaO, and Sm_2O_3 secondary phases were observed at x＞0,while SmAlO_3 secondary phase was observed at x≤0.The secondary phases Ca_3Al_2O_6 and SmAlO_3 decreased the Qf values greatly,whereas CaSmAl_3O_7,CaO and Sm_2O_3 had much weaker minus effects on Qf values.Good microwave dielectric properties were achieved in (2+2x)CaO·Sm_2O_3·Al_2O_3(x=0.02,0.03,0.04) ceramics:ε_r≈19,Qf =120,000～125,300 GHz,τ_f=-10～-9ppm/℃.
Modification of CaSmAlO_4 was performed by cosubstitution of Ca on A site and Ti on B site,and Ca_(1+x)Sm_(1-x)Al_(1-x)Ti_xO_4(0≤x≤0.4) ceramics were prepared and characterized.For Ca_(1+x)Sm_(1-x)Al_(1-x)Ti_xO_4 phases,as x increased,lattice parameter a increased linearly whereas lattice parameter c decreased linearly;the distortion of (Al,Ti)O_6 octahedra reduced slightly,whereas(M,R)O_9 dodecahedra were further compressed along the c axis,and this was responsible for the decrease in lattice parameter c.Ca_(1+x)Sm_(1-x)Al_(1-x)Ti_xO_4 ceramics showed very good microwave dielectric properties,especially when 0.06≤x≤0.2(ε_r≈20,Qf=96,500～118,700GHz,andτ_f=-8～2 ppm/℃).SmAlO_3 secondary phase was detected at x=0,and trace amount of CaTiO_3 secondary phase was detected at x≥0.15;abnormal grain growth was observed in samples with x=0,0.02 and sintering temperature of 1500℃. Suppression of these microstructures would help Ca_(1+x)Sm_(1+x)Al_(1-x)Ti_xO_4 ceramics maintain high Qf values.With certain amount of excessive CaO in composition, microwave dielectric properties of Ca_(1+x)Sm_(1-x)Al_(1-x)Ti_xO_4-based ceramics were further improved and excellent microwave dielectric properties(ε_r=20.2,Qf=100,000GH,τ_f=0.5 ppm/℃) were achieved at x=0.15.
建立了一套包括开腔法和闭腔法的微波介电性能的测量评价系统。对复介电常数的数值计算的算法进行了改进,大幅度提高了计算效率,从而间接地提高了计算精度,并利用改进算法拓展了闭腔法的应用范围。
通过XRD全谱拟合对MRAlO_4(M=Sr,Ca;R=La,Nd,Sm,Y)陶瓷的晶体结构进行精修。AlO_6八面体和(M,R)P_9十二面体在c轴方向分别受到强烈拉伸和强烈压缩,而在ab平面内的情况则正好相反。层间尺寸失配和层间极化是造成多面体畸变的两个主要原因,它们可以分别用结构许容因子和氧八面体畸变程度(或者(M,R)O_9中心阳离子与O(2a)原子面的距离)来衡量。随着结构许容因子的减小,(M,R)O。的畸变加剧,而AlO_6的畸变基本保持不变。根据键价理论的分析,SrYAlO_4的不稳定性和CaLaAlO_4的亚稳定性分别是由共同占据A位的两种阳离子的离子半径相差太大和离子价态相差太大造成的。
为了从极性声子模的角度理解MRAlO_4(M=Sr,Ca;R=La,Nd,Sm,Y)陶瓷的微波介电响应的本质,测量了MRAlO_4陶瓷50～4000cm~(-1)范围内的红外反射光谱,利用K-K关系、经典谐振子模型对红外数据进行分析,并将红外数据外推到微波频段以估计本征微波介电损耗。(M,R)-AlO_6沿着ab平面的弯曲振动模和沿着c轴的伸缩振动模是对微波介电常数和介电损耗起主要贡献的两个模式。(M,R)O_9十二面体的畸变极大地影响了这两个模式的色散参数,从而决定了极化率和本证损耗,这就是MRAlO_4实测的极化率大幅度偏离氧化物加和法则得到的预测值以及MRAlO_4的Qf计算值随着结构许容因子的减小而减小的原因。减小本征介电损耗的关键是减小(M,R)O_9十二面体的畸变。Qf计算值大大高于实测值,表明通过优化微结构还能大幅度减小非本征损耗。
通过改变CaO、Sm_2O_3和Al_2O_3的配比,研究了CaSmAlO_4基陶瓷的相组成及其对微结构和微波介电性能的影响。在(2+2x)CaO～(1-x)Sm_2O_3～Al_2O_3(x=-0.10,-0.05,0,0.05,0.10,0.20)陶瓷中,当x＞0时检测到Ca_3Al_2O_6和CaO第二相,而当x≤0时则是SmAlO_3和Sm_2O_3第二相。在(2+2x)CaO·Sm_2O_3·Al_2O_3(x=-0.02,-0.01,0,0.02,0.04)陶瓷中,当x＞0时检测到CaSmAl_3O_7、CaO和Sm_2O_3第二相,而当x≤0时,检测到SmAlO_3第二相。Ca_3Al_2O_6和SmAlO_3第二相会大幅度降低体系的Qf值,而CaSmAl_3O_7、CaO和Sm_2O_3第二相对体系的Qf值的不利影响很小甚至有利于Qf值的提高。在(2+2x)CaO·Sm_2O_3·Al_2O_3(x=0.02,0.03,0.04)陶瓷中获得了优异的微波介电性能:ε_r=19,Qf=120,000～125,300GHz,τ_f=-10～-9ppm/℃。
通过Ca/Ti协同置换对CaSmAlO_4进行改性,得到了Ca_(1+x)Sm_(1-x)Al_(1-x)Ti_xO_4(0≤x≤0.4)陶瓷。对于Ca_(1+x)Sm_(1-x)Al_(1-x)Ti_xO_4主相而言,随着x的增大,晶胞参数a和c分别线性地增大和减小;(Al,Ti)O_6八面体的畸变略有减小,而(M,R)O_9十二面体的畸变逐渐加大,后者是晶胞参数c减小的原因。Ca_(1+x)Sm_(1-x)Al_(1-x)Ti_xO_4陶瓷具有良好的微波介电性能,尤其是当0.06≤x≤0.2时(ε_r≈20,Qf=96,500～118,700GHz,τ_f=-8～2ppm/℃)。当x=0时检测到了少量的SmAlO_3第二相,而当x≥0.15时检测到了微量的CaTiO_3第二相;在x=0和0.02成分点1500℃烧结的样品中观察到晶粒的异常长大。抑制这些微结构的产生有助于改善体系的微波介电性能。适当加入过量的CaO,Ca_(1+x)Sm_(1-x)Al_(1-x)Ti_xO_4基陶瓷的微波介电性能得到进一步改善,当x=0.15时,实现了极其优异的微波介电性能(ε_r=20.2,Qf=100,000GHz和τ_f=0.5 ppm/℃)。
Synthesis,structures,and microwave dielectric properties of MRAlO_4-based(M=Ca, Sr;R=La,Nd,Sm,Y) ceramics with I4/mmm space group were systermatically investigated together with their property-structure relationship,and based on these findings,the modification of microwave dielectric properties was carried out for CaSmAlO_4 ceramics through structure tailoring and microstructure control.The following primary findings and/or achiements were obtained:
An evaluation system involving the open cavity method and the closed cavity method was built up to characterize the microwave dielectric properties with high accurately.An innovative algorithm for numerical calculation of complex permittivity was developed,and the computational efficiency was improved greatly.With the algorithm,the application scope of the close cavity method was significantly extended.
Crystal structure refinements were carried out for MRAlO_4 ceramics by Rietveld method.Along the c axis,AlO_6 octahedra and(M,R)O_9 dodecahedra were heavily stretched and compressed,respectively,while within the ab plane,the situation was reversed.The interlayer size mismatch and the interlayer electric polarization were the primary reasons for these distortions,and they could be evaluated with the tolerance factor and the deformation degree of octahedron(or the distance from(M,R) cation to O(2a) atomic plane),respectively.As the tolerance factor decreased,the distortion of AlO_6 octahedra kept nearly unchanged,while that of(M,R)O_9 increased.Based on the analysis by the bond valence method,the instability of SrYAlO_4 and the metastability of CaLaAlO_4 were attributed to large differences of ionic radius and of apparent bond valence between M and R cations,respectively.
To understand the dielectric nature of MRAlO_4 ceramics in terms of phonon modes,Fourier transform infrared reflectivity spectra in the range of 50-4000 cm~(-1) were measured and evaluated by means of K-K ananlysis and classical oscillator fit.The data were extrapolated below the measured frequency range to estimate the intrinsic microwave losses.The bending and stretching vibration modes of(M,R)-AlO_6 gave primary contributions to the microwave complex permittivity,therefore the distortion of (M,R)O_9 dodecahedra greatly affected the dispersion parameters of these two modes and consequently dominated polarizabilities and intrinsic dielectric losses of MRAlO_4. This could explain the great deviation of measured polarizabilities from those predicted by the oxide additivity law and the variation of calculated Qf values with the tolerance factor.To minimize the intrinsic dielectric loss,it was the keypoint to reduce the distortion of(M,R)O_9 dodecahedra.Moreover,the fact that the calculated Qf values were much higher than the measured ones suggested a great opportunity to improve Qf through optimizing the microstructures.
By changing molar ratios among CaO,Sm_2O_3,and Al_2O_3,the effects of secondary phases on mcirostructures and microwave dielectric properties were investigated for CaSmAlO_4-based ceramics.In(2+2x)CaO·(1-x)Sm_2O_3·Al_2O_3(x=-0.10,-0.05,0,0.05, 0.10,0.20)ceramics,Ca_3Al_2O_6 and CaO secondary phases were observed at x＞0,while SmAlO_3 and Sm_2O_3 secondary phases were observed at x≤0.In (2+2x)CaO·Sm_2O_3·Al_2O_3(x=-0.02,-0.01,0,0.02,0.04) ceramics,CaSmAl_3O_7,CaO, and Sm_2O_3 secondary phases were observed at x＞0,while SmAlO_3 secondary phase was observed at x≤0.The secondary phases Ca_3Al_2O_6 and SmAlO_3 decreased the Qf values greatly,whereas CaSmAl_3O_7,CaO and Sm_2O_3 had much weaker minus effects on Qf values.Good microwave dielectric properties were achieved in (2+2x)CaO·Sm_2O_3·Al_2O_3(x=0.02,0.03,0.04) ceramics:ε_r≈19,Qf =120,000～125,300 GHz,τ_f=-10～-9ppm/℃.
Modification of CaSmAlO_4 was performed by cosubstitution of Ca on A site and Ti on B site,and Ca_(1+x)Sm_(1-x)Al_(1-x)Ti_xO_4(0≤x≤0.4) ceramics were prepared and characterized.For Ca_(1+x)Sm_(1-x)Al_(1-x)Ti_xO_4 phases,as x increased,lattice parameter a increased linearly whereas lattice parameter c decreased linearly;the distortion of (Al,Ti)O_6 octahedra reduced slightly,whereas(M,R)O_9 dodecahedra were further compressed along the c axis,and this was responsible for the decrease in lattice parameter c.Ca_(1+x)Sm_(1-x)Al_(1-x)Ti_xO_4 ceramics showed very good microwave dielectric properties,especially when 0.06≤x≤0.2(ε_r≈20,Qf=96,500～118,700GHz,andτ_f=-8～2 ppm/℃).SmAlO_3 secondary phase was detected at x=0,and trace amount of CaTiO_3 secondary phase was detected at x≥0.15;abnormal grain growth was observed in samples with x=0,0.02 and sintering temperature of 1500℃. Suppression of these microstructures would help Ca_(1+x)Sm_(1+x)Al_(1-x)Ti_xO_4 ceramics maintain high Qf values.With certain amount of excessive CaO in composition, microwave dielectric properties of Ca_(1+x)Sm_(1-x)Al_(1-x)Ti_xO_4-based ceramics were further improved and excellent microwave dielectric properties(ε_r=20.2,Qf=100,000GH,τ_f=0.5 ppm/℃) were achieved at x=0.15.
引文
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