铁酸铋—钛酸铅系大功率压电陶瓷及器件的设计、研制与性能
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摘要
钙钛矿结构x(BiFeO_3)–(1-x)(PbTiO_3)（BF-PT）压电固溶体具有较高的居里温度和介电强度以及良好的压电性能，在高温大功率压电器件领域有广阔的应用前景。但是，BF-PT陶瓷矫顽场强场强大，难于极化，介电损耗大，机械品质因子低，限制了其在大功率压电器件中的应用。本文采用固相反应工艺制备了(1-x)Bi(Ga_(0.05)Fe_(0.95))O_3-xPbTiO_3(BGF-PT)陶瓷，研究BGF-PT陶瓷的MPB效应。此外，采用溶胶凝胶工艺制备出具有优异机电性能和温度稳定性的Mn掺杂的0.6(Bi_(0.9)La_(0.1))FeO_3-0.4Pb(Ti_(1-x)Mn_x)O_3（BLF-PTM)）陶瓷；测量了BLF-PTM陶瓷的室温、高温和大功率压电性能，讨论了BLF-PTM陶瓷介电、压电和弹性非线性特征。最后，用性能优化的BLF-PTM陶瓷制备了单向极化、圆片型大功率压电变压器，分析建立了变压器的等效电路模型，表征了变压器室温、高温下的升压比和功率密度。
BGF-PT陶瓷具有钙钛矿结构。当x=0.3和0.35，BGF-PT陶瓷中三方相和四方相共存，晶粒尺寸较小，具有较大的介电常数和剩余极化、较小的介电损耗，呈现MPB特征。XPS分析表明，MPB附近，BGF-PT中Fe~(2+)离子和氧化物杂质含量较少。阻抗分析结果表明，MPB附近，BGF-PT陶瓷的宏观电性能主要来自晶粒的贡献；远离相界，x=0.25和0.45，晶粒和晶界均对陶瓷的宏观电性能有贡献，但晶粒的贡献远大于晶界。高温时，BGF-PT陶瓷中导电载流子主要是氧空位，晶粒和晶界电导主要是氧空位的移动引起，MPB附近，氧空位的热激活能较大。
BLF-PTM陶瓷具有三方相和四方相共存的钙钛矿结构，Mn掺杂明显提高了陶瓷的晶粒尺寸。BLF-PTM陶瓷表现出硬性压电材料特征，具有较小的介电常数、介电损耗、机械内耗、弹性模量、剩余极化和回线面积以及较大的频率常数，极化后样品的电滞回线明显不对称。适量Mn掺杂BLF-PTM陶瓷具有理想的极化状态，表现出优异的室温、高温压电和机电耦合性能。Mn含量1at％的BLF-PTM陶瓷d33，g33，kp，Qm，Tc分别为124pC/N、37X10-3Vm/N、0.338、403和473oC；且d33和kp具有优异的温度稳定性，退极化温度达到370oC，250oC温度下的Qm大于200。在激励电场作用下，1at％Mn掺杂BLF-PTM陶瓷具有最大的振动速率和小的升温，最大振动速率可以达到1.1m/s，升温仅为6oC。
BLF-PTM在强电场下出现介电、压电和弹性非线性特征。Mn掺杂同时降低了BLF-PTM陶瓷的介电和压电非线性系数，以及三阶非线性弹性柔顺系数和机电耦合系数。未掺Mn的BLF-PT陶瓷介电和压电非线性符合瑞利定理；Mn掺杂BLF-PTM陶瓷的介电和压电非线性偏离瑞利定理。BLF-PTM陶瓷的弹性非线性是引起机械振动谐振频率频移和非线性机电耦合效应的主要原因。Mn掺杂BLF-PTM陶瓷的电畴比较稳定，在电场作用下不易翻转，而极化后电畴运动更加困难，抑制了BLF-PTM陶瓷的非线性。
BLF-PTM单向极化圆片型压电变压器的等效电路模型分析表明，压电变压器在谐振频率和三次谐振频率工作时的匹配电阻分别为8.1k和2.1k，效率分别为91.2%和84.3%。实际测量表明，匹配负载压电变压器具有最大的功率密度和效率，谐振频率和三次谐振频率功率密度分别为30.1W/cm~3和23.5W/cm~3，效率分别为83.4%和80.2%。温度升高，压电变压器空载谐振频率向低频移动，电压增益先增大后减小；200oC时，电压增益达到最大值35.6。工作温度低于300oC，压电变压器能保持较高的功率密度，250oC时，功率密度仍大于20W/cm~3。BLF-PTM压电变压器是一种可以在较高温工作的大功率压电变压器，目前文献中还未见相关报道。
BiFeO_3PbTiO_3based piezoelectric ceramics have drawn much attention owing to theirrelatively high Curie temperature, high dielectric strength, good ferroelectric and piezoelectricproperties, which have potential application in high-temperature piezoelectric field. However,development of BF–PT materials has been hampered due to their high coercive field, lowmechanical quality factor and high dielectric loss. In this work，(1-x)Bi(Ga_(0.05)Fe_(0.95))O_3-xPbTiO_3(BGF-PT) ceramics for x=0.25,0.3,0.35and0.45have been fabricated by the solid state reactionprocess. The MPB effects of BGF-PT have been studed. Piezoelectric ceramics of0.6(Bi_(0.9)La_(0.1))FeO_3-0.4Pb(Ti_(1-x)Mn)x)O_3(BLF-PTM) for x=0,0.01,0.02and0.03, with greatelectomechanical properties and temperature stability, were fabricated by sol-gel process combinedwith a solid state reaction method. The dielectric, piezoelectric and elastic nonlinearities forBLF-PTM ceramics have been discussed. Unipole radial high power piezoelectric transformer wasprepared using BLF-PTM ceramics, and the equavilent circuit model has been built，and itselectrical properties have been characterized at room and elevated temperature.
BGF-PT at MPB is coexistence of rhombohedral and tetragonal phases, exhibting enhanceddielectric constant, remanent polarization and decreased dielectric loss. XPS analysis indicates thatMPB components have less concentration of Fe~(2+)and oxide impurities. The impedance analysisshows that only grain contributed to the electrical properties of x=0.3and0.35, while both grain andgrain boundary contributed to that of x=0.25and0.45. The motion of oxygen vacancies contributeto the conductivity in the high temperature region, and MPB compositions shows high activationenergy.
BLF-PTM ceramics have perovskite structure, and are coexistence of rhombohedral andtetragonal. Mn modification promotes grain growth. Upon using Mn substituents, BLF-PTMceramics exhibites the characteristics of hard piezoelectrics, such as (1) low polarization,(2) lowdielectric constant and loss,(3) high mechanical quality factor Qm,(4) low internal friction,(5) lowelastic modulus,(6) asymmetrical P-E loops. The dielectric loss, piezoelectric constant d33,piezoelectric voltage coefficient g33, planar coupling coefficient kp, mechanical quality factor Qmand Curie temperature Tcof0.006,124pC/N,37×10-3Vm/N,0.338,418and473oC, respectively,are achieved for BLF-PTM of x=0.01. kp，d33and Qmof Mn modified BLF-PTM show greattemperature stability, the depoled temperature Tdis370oC, and Qmis still more than200at250oC.A large vibration velocity of1.1m/s is achieved for this composition, with only6oC temperaturerise.
Under higher applied fields, the nonlinear dielectric, elastic and piezoelectric effects areobserved in BLF-PTM. The dielectric and piezoelectric properties of BLF-PTM without Mnmodification obey the Rayleigh law under high electric field, whereas Mn modified BLF-PTM donot. The third order nonlinear elastic effect results in the shift of resonance frequency. However, thenonlinear dielectric constant, piezoelectric coefficient, nonlinear elastic compliance andelectromechanical coupling coefficient decrease by Mn substituents, attributed to its stable domainstructure, leading to low nonlinearities.
According to equivalent circuit model, the match load and efficiency of unipole radialpiezoelectric transformer is found to be8.1k and2.1k,91.2%and84.3%at resonancefrequency and third order resonance frequency. Under resonance frequency and third order resonance frequency, the power density and efficiency of piezoelectric is30.1W/cm~3and23.5W/cm~3,83.4%and80.2%. With temperature rising, the voltage gain increases initially and thendecreases; the maximum voltage gain is35.6at200oC. The power density of piezoelectrictransformer is20W/cm~3at250oC, and exhibits large power density ever at300oC. Our resutsshows that the transformer prepared by BLF-PTM is a kind of high temperature and high powerpiezoelectric transformer.
BGF-PT陶瓷具有钙钛矿结构。当x=0.3和0.35，BGF-PT陶瓷中三方相和四方相共存，晶粒尺寸较小，具有较大的介电常数和剩余极化、较小的介电损耗，呈现MPB特征。XPS分析表明，MPB附近，BGF-PT中Fe~(2+)离子和氧化物杂质含量较少。阻抗分析结果表明，MPB附近，BGF-PT陶瓷的宏观电性能主要来自晶粒的贡献；远离相界，x=0.25和0.45，晶粒和晶界均对陶瓷的宏观电性能有贡献，但晶粒的贡献远大于晶界。高温时，BGF-PT陶瓷中导电载流子主要是氧空位，晶粒和晶界电导主要是氧空位的移动引起，MPB附近，氧空位的热激活能较大。
BLF-PTM陶瓷具有三方相和四方相共存的钙钛矿结构，Mn掺杂明显提高了陶瓷的晶粒尺寸。BLF-PTM陶瓷表现出硬性压电材料特征，具有较小的介电常数、介电损耗、机械内耗、弹性模量、剩余极化和回线面积以及较大的频率常数，极化后样品的电滞回线明显不对称。适量Mn掺杂BLF-PTM陶瓷具有理想的极化状态，表现出优异的室温、高温压电和机电耦合性能。Mn含量1at％的BLF-PTM陶瓷d33，g33，kp，Qm，Tc分别为124pC/N、37X10-3Vm/N、0.338、403和473oC；且d33和kp具有优异的温度稳定性，退极化温度达到370oC，250oC温度下的Qm大于200。在激励电场作用下，1at％Mn掺杂BLF-PTM陶瓷具有最大的振动速率和小的升温，最大振动速率可以达到1.1m/s，升温仅为6oC。
BLF-PTM在强电场下出现介电、压电和弹性非线性特征。Mn掺杂同时降低了BLF-PTM陶瓷的介电和压电非线性系数，以及三阶非线性弹性柔顺系数和机电耦合系数。未掺Mn的BLF-PT陶瓷介电和压电非线性符合瑞利定理；Mn掺杂BLF-PTM陶瓷的介电和压电非线性偏离瑞利定理。BLF-PTM陶瓷的弹性非线性是引起机械振动谐振频率频移和非线性机电耦合效应的主要原因。Mn掺杂BLF-PTM陶瓷的电畴比较稳定，在电场作用下不易翻转，而极化后电畴运动更加困难，抑制了BLF-PTM陶瓷的非线性。
BLF-PTM单向极化圆片型压电变压器的等效电路模型分析表明，压电变压器在谐振频率和三次谐振频率工作时的匹配电阻分别为8.1k和2.1k，效率分别为91.2%和84.3%。实际测量表明，匹配负载压电变压器具有最大的功率密度和效率，谐振频率和三次谐振频率功率密度分别为30.1W/cm~3和23.5W/cm~3，效率分别为83.4%和80.2%。温度升高，压电变压器空载谐振频率向低频移动，电压增益先增大后减小；200oC时，电压增益达到最大值35.6。工作温度低于300oC，压电变压器能保持较高的功率密度，250oC时，功率密度仍大于20W/cm~3。BLF-PTM压电变压器是一种可以在较高温工作的大功率压电变压器，目前文献中还未见相关报道。
BiFeO_3PbTiO_3based piezoelectric ceramics have drawn much attention owing to theirrelatively high Curie temperature, high dielectric strength, good ferroelectric and piezoelectricproperties, which have potential application in high-temperature piezoelectric field. However,development of BF–PT materials has been hampered due to their high coercive field, lowmechanical quality factor and high dielectric loss. In this work，(1-x)Bi(Ga_(0.05)Fe_(0.95))O_3-xPbTiO_3(BGF-PT) ceramics for x=0.25,0.3,0.35and0.45have been fabricated by the solid state reactionprocess. The MPB effects of BGF-PT have been studed. Piezoelectric ceramics of0.6(Bi_(0.9)La_(0.1))FeO_3-0.4Pb(Ti_(1-x)Mn)x)O_3(BLF-PTM) for x=0,0.01,0.02and0.03, with greatelectomechanical properties and temperature stability, were fabricated by sol-gel process combinedwith a solid state reaction method. The dielectric, piezoelectric and elastic nonlinearities forBLF-PTM ceramics have been discussed. Unipole radial high power piezoelectric transformer wasprepared using BLF-PTM ceramics, and the equavilent circuit model has been built，and itselectrical properties have been characterized at room and elevated temperature.
BGF-PT at MPB is coexistence of rhombohedral and tetragonal phases, exhibting enhanceddielectric constant, remanent polarization and decreased dielectric loss. XPS analysis indicates thatMPB components have less concentration of Fe~(2+)and oxide impurities. The impedance analysisshows that only grain contributed to the electrical properties of x=0.3and0.35, while both grain andgrain boundary contributed to that of x=0.25and0.45. The motion of oxygen vacancies contributeto the conductivity in the high temperature region, and MPB compositions shows high activationenergy.
BLF-PTM ceramics have perovskite structure, and are coexistence of rhombohedral andtetragonal. Mn modification promotes grain growth. Upon using Mn substituents, BLF-PTMceramics exhibites the characteristics of hard piezoelectrics, such as (1) low polarization,(2) lowdielectric constant and loss,(3) high mechanical quality factor Qm,(4) low internal friction,(5) lowelastic modulus,(6) asymmetrical P-E loops. The dielectric loss, piezoelectric constant d33,piezoelectric voltage coefficient g33, planar coupling coefficient kp, mechanical quality factor Qmand Curie temperature Tcof0.006,124pC/N,37×10-3Vm/N,0.338,418and473oC, respectively,are achieved for BLF-PTM of x=0.01. kp，d33and Qmof Mn modified BLF-PTM show greattemperature stability, the depoled temperature Tdis370oC, and Qmis still more than200at250oC.A large vibration velocity of1.1m/s is achieved for this composition, with only6oC temperaturerise.
Under higher applied fields, the nonlinear dielectric, elastic and piezoelectric effects areobserved in BLF-PTM. The dielectric and piezoelectric properties of BLF-PTM without Mnmodification obey the Rayleigh law under high electric field, whereas Mn modified BLF-PTM donot. The third order nonlinear elastic effect results in the shift of resonance frequency. However, thenonlinear dielectric constant, piezoelectric coefficient, nonlinear elastic compliance andelectromechanical coupling coefficient decrease by Mn substituents, attributed to its stable domainstructure, leading to low nonlinearities.
According to equivalent circuit model, the match load and efficiency of unipole radialpiezoelectric transformer is found to be8.1k and2.1k,91.2%and84.3%at resonancefrequency and third order resonance frequency. Under resonance frequency and third order resonance frequency, the power density and efficiency of piezoelectric is30.1W/cm~3and23.5W/cm~3,83.4%and80.2%. With temperature rising, the voltage gain increases initially and thendecreases; the maximum voltage gain is35.6at200oC. The power density of piezoelectrictransformer is20W/cm~3at250oC, and exhibits large power density ever at300oC. Our resutsshows that the transformer prepared by BLF-PTM is a kind of high temperature and high powerpiezoelectric transformer.
引文
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