铌酸锶钡/钛酸锶钡复相陶瓷制备、结构和性能研究
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摘要
本文采用粉末-溶胶法制备铌酸锶钡(Sr_xBa_(1-x)Nb_2O_6, 0.25≤x≤0.75,SBN)和钛酸锶钡(Sr_xBa_(1-x)TiO_3,SBT)两相共存的复相陶瓷,简称SBN/SBT。系统研究了SBN/SBT复相陶瓷的制备方法及制备过程中的影响因素。利用TG-DTA、X射线衍射仪(X-Ray diffraction,XRD)、扫描电子显微镜(Scanning Electron Microscopy , SEM)、X射线光电子能谱(X-Ray Photoelectron Spectroscopy,XPS)、LCR数字电桥和静电计等研究了相组成、显微结构与介电性能和热释电性能之间的关系。
采用粉末-溶胶法,当预烧温度为800℃、烧结温度为1250℃、保温时间为3h时可获得SBN和SBT两相微观结构均匀、致密的复相陶瓷。提出了粉末-溶胶工艺制备复相陶瓷SBN/SBT的双相形成机理,研究了不同Nb/Ti比、Sr/Ba比以及La~(3+)掺杂量变化对体系的致密度、颗粒形貌和介电损耗等性能的影响。提出并利用公式Δ(O-Nb)= BE(O_(1s)) - BE(Nb _(3d5/2))和Δ(O-Ti)= BE(O_(1s)) - BE(Ti_(2p3/2)),研究复相陶瓷的Nb/Ti比、La~(3+)掺杂变化对[NbO_6]和[TiO_6]的结构影响,解释了与介电损耗之间的关系。利用公式Δ(O-Ba) = BE[O_(1s)(I)] - BE[Ba_(3d5/2)]和Δ(O-Sr) = BE[O_(1s)(II)]-BE[Sr_(2p3/2)],解释复相陶瓷中的Ba~(2+)和Sr~(2+)对复相陶瓷介电常数的影响。随着Nb/Ti比接近5:5,O-Nb键和O-Ti键的晶格振动回复力逐渐增加,降低了复相陶瓷的本征介电损耗,Δ(O-Ba)和Δ(O-Sr)则逐渐增加,即复相陶瓷的极化率提高,增加了复相陶瓷介电常数,而复相陶瓷0.7BaO·0.3SrO·0.5TiO_2·0.5Nb_2O_5热释电系数,相对于单相钙钛矿相(Ba_(0.7)Sr_(0.3))TiO_3和钨青铜相(Ba_(0.7)Sr_(0.3))Nb_2O_6温度响应范围明显提高。
采用公式Δ(O-Nb)=BE(O_(1s))-BE(Nb_(3d5/2))和Δ(O-Ti) = BE(O_(1s))-BE(Ti_(2p3/2))和Δ(O-Ba) = BE[O_(1s)(I)]-BE[Ba_(3d5/2)]和Δ(O-Sr) = BE[O_(1s)(II)] -BE[Sr_(2p3/2)],表征La~(3+)掺杂对复相陶瓷的[NbO_6]和[TiO_6]与Ba-O和Sr-O特性的影响。研究表明(0.7-z)BaO·(0.3-z)SrO·zLa_2O_3·0.5Nb_2O_5·0.5TiO_2中Nb元素价态不受La~(3+)掺杂的影响,Ti元素价态受La~(3+)掺杂的影响,0.25%mol的La~(3+)掺杂使体系的致密度、颗粒形貌和介电损耗得到明显的改善。通过La~(3+)掺杂使复相陶瓷优值因子的温度稳定性优于0.7BaO·0.3SrO·0.5TiO_2·0.5Nb_2O_5、钙钛矿相(Ba_(0.7)Sr_(0.3))TiO_3和钨青铜相(Ba_(0.7)Sr_(0.3))Nb_2O_6。
In this thesis, (1-x)BaO·xSrO·(1-y)TiO_2·yNb_2O_5 (SBN/SBT) with coexistence of Strontium barium niobate(Sr_xBa_(1-x)Nb_2O_6,0.25≤x≤0.75, SBN) and barium strontium titanate (Sr_xBa_(1-x)TiO_3, SBT) were successfully prepared by a powder-sol method, and the formation mechanism of the composite ceramics was investigated in details. By X-ray diffraction (XRD), Scanning electron microscope (SEM), X-Ray Photoelectron Spectroscopy (XPS), LCR digital bridge and electrometer, the phase structure, dielectric properties and the pyroelectric properties of SBN/SBT composite ceramics were also studied. Following results can be obtained from this thesis:
SBN/SBT composite ceramics have been prepared by powder-sol process. The powder-sol process parameters were: 800℃for presintering temperature, 1250℃for sintering temperature, 3h for sintering time. SBN/SBT composite ceramics with uniform SBT and SBN grains size and high density were obtained by powder-sol process parameters. The formation mechanism is put forward for the SBN/SBT composite ceramics by powder-sol process. The influence of Nb/Ti ratios, Sr/Ba ratios, La~(3+) doping on relative density, grain morphology and dielectric loss were studied.
The new formulasΔ(O-Nb) = BE[O_(1s)(III)]-BE[Nb_(3d5/2)] andΔ(O-Ti) = BE[O_(1s)(IV)]-BE[Ti_(2p3/2)] are put forward. By the above formula, the influences ofΔ(O-Nb) andΔ(O-Ti) on dielectric loss was studied. The relationship betweenΔ(O-Nb),Δ(O-Ti) and dielectric loss was explained. ByΔ(O-Ba) = BE[O_(1s)(I)] - BE[Ba3d5/2] andΔ(O-Sr) = BE[O_(1s)(II)]-BE[Sr_(2p3/2)] being put forward, the influences ofΔ(O-Ba) andΔ(O-Sr) on dielectric constants was explained. With Nb/Ti ratios nearing 5:5, the reversion force of lattice vibration for O-Nb and O-Ti bond are increased gradually. This decreases tanδfor composite ceramics. It helps to increase the FOM (figure of merit, FD) of composite ceramics. TheΔ(O-Ba) andΔ(O-Sr) for O-Ba and O-Sr bond are increased gradually. This help to increase dielectric constants for SBN/SBT composite ceramics. The pyroelectric coefficient have more wide pyroelectric coefficient reponse than those of (Ba_(0.7)Sr_(0.3))TiO_3 and (Ba_(0.7)Sr_(0.3))Nb_2O_6 for SBN/SBT composite ceramics.
The influence of La_2O_3 doping on structure and properties for the 0.7BaO·0.3SrO·0.5TiO_2·0.5Nb_2O_5 composite ceramics was studied. The relative density and dielectric loss were improved by La_2O_3 doping. This helps to improve the FOM for composite ceramics. The XPS for the (0.7-z)BaO·(0.3-z)SrO·zLa_2O_3·0.5TiO_2·0.5Nb_2O_5 were studied. It is shown that the binding energy of Nb3d5/2 was not influenced by La_2O_3 doping. The binding energies of Ti2p were strongly dependent on La_2O_3 doping. The influences of La_2O_3 doping on the O-Nb and O-Ti bond are put forward to byΔ(O-Nb)= BE(O_(1s))-BE(Nb_(3d5/2)) andΔ(O-Ti) = BE(O_(1s))-BE(Ti_(2p3/2)). The SBN/SBT with La~(3+) doping has higher FOM than those of (Ba_(0.7)Sr_(0.3))TiO_3 0.7BaO·0.3SrO·0.5TiO_2·0.5Nb_2O_5 and (Ba_(0.7)Sr_(0.3))Nb_2O_6.
采用粉末-溶胶法,当预烧温度为800℃、烧结温度为1250℃、保温时间为3h时可获得SBN和SBT两相微观结构均匀、致密的复相陶瓷。提出了粉末-溶胶工艺制备复相陶瓷SBN/SBT的双相形成机理,研究了不同Nb/Ti比、Sr/Ba比以及La~(3+)掺杂量变化对体系的致密度、颗粒形貌和介电损耗等性能的影响。提出并利用公式Δ(O-Nb)= BE(O_(1s)) - BE(Nb _(3d5/2))和Δ(O-Ti)= BE(O_(1s)) - BE(Ti_(2p3/2)),研究复相陶瓷的Nb/Ti比、La~(3+)掺杂变化对[NbO_6]和[TiO_6]的结构影响,解释了与介电损耗之间的关系。利用公式Δ(O-Ba) = BE[O_(1s)(I)] - BE[Ba_(3d5/2)]和Δ(O-Sr) = BE[O_(1s)(II)]-BE[Sr_(2p3/2)],解释复相陶瓷中的Ba~(2+)和Sr~(2+)对复相陶瓷介电常数的影响。随着Nb/Ti比接近5:5,O-Nb键和O-Ti键的晶格振动回复力逐渐增加,降低了复相陶瓷的本征介电损耗,Δ(O-Ba)和Δ(O-Sr)则逐渐增加,即复相陶瓷的极化率提高,增加了复相陶瓷介电常数,而复相陶瓷0.7BaO·0.3SrO·0.5TiO_2·0.5Nb_2O_5热释电系数,相对于单相钙钛矿相(Ba_(0.7)Sr_(0.3))TiO_3和钨青铜相(Ba_(0.7)Sr_(0.3))Nb_2O_6温度响应范围明显提高。
采用公式Δ(O-Nb)=BE(O_(1s))-BE(Nb_(3d5/2))和Δ(O-Ti) = BE(O_(1s))-BE(Ti_(2p3/2))和Δ(O-Ba) = BE[O_(1s)(I)]-BE[Ba_(3d5/2)]和Δ(O-Sr) = BE[O_(1s)(II)] -BE[Sr_(2p3/2)],表征La~(3+)掺杂对复相陶瓷的[NbO_6]和[TiO_6]与Ba-O和Sr-O特性的影响。研究表明(0.7-z)BaO·(0.3-z)SrO·zLa_2O_3·0.5Nb_2O_5·0.5TiO_2中Nb元素价态不受La~(3+)掺杂的影响,Ti元素价态受La~(3+)掺杂的影响,0.25%mol的La~(3+)掺杂使体系的致密度、颗粒形貌和介电损耗得到明显的改善。通过La~(3+)掺杂使复相陶瓷优值因子的温度稳定性优于0.7BaO·0.3SrO·0.5TiO_2·0.5Nb_2O_5、钙钛矿相(Ba_(0.7)Sr_(0.3))TiO_3和钨青铜相(Ba_(0.7)Sr_(0.3))Nb_2O_6。
In this thesis, (1-x)BaO·xSrO·(1-y)TiO_2·yNb_2O_5 (SBN/SBT) with coexistence of Strontium barium niobate(Sr_xBa_(1-x)Nb_2O_6,0.25≤x≤0.75, SBN) and barium strontium titanate (Sr_xBa_(1-x)TiO_3, SBT) were successfully prepared by a powder-sol method, and the formation mechanism of the composite ceramics was investigated in details. By X-ray diffraction (XRD), Scanning electron microscope (SEM), X-Ray Photoelectron Spectroscopy (XPS), LCR digital bridge and electrometer, the phase structure, dielectric properties and the pyroelectric properties of SBN/SBT composite ceramics were also studied. Following results can be obtained from this thesis:
SBN/SBT composite ceramics have been prepared by powder-sol process. The powder-sol process parameters were: 800℃for presintering temperature, 1250℃for sintering temperature, 3h for sintering time. SBN/SBT composite ceramics with uniform SBT and SBN grains size and high density were obtained by powder-sol process parameters. The formation mechanism is put forward for the SBN/SBT composite ceramics by powder-sol process. The influence of Nb/Ti ratios, Sr/Ba ratios, La~(3+) doping on relative density, grain morphology and dielectric loss were studied.
The new formulasΔ(O-Nb) = BE[O_(1s)(III)]-BE[Nb_(3d5/2)] andΔ(O-Ti) = BE[O_(1s)(IV)]-BE[Ti_(2p3/2)] are put forward. By the above formula, the influences ofΔ(O-Nb) andΔ(O-Ti) on dielectric loss was studied. The relationship betweenΔ(O-Nb),Δ(O-Ti) and dielectric loss was explained. ByΔ(O-Ba) = BE[O_(1s)(I)] - BE[Ba3d5/2] andΔ(O-Sr) = BE[O_(1s)(II)]-BE[Sr_(2p3/2)] being put forward, the influences ofΔ(O-Ba) andΔ(O-Sr) on dielectric constants was explained. With Nb/Ti ratios nearing 5:5, the reversion force of lattice vibration for O-Nb and O-Ti bond are increased gradually. This decreases tanδfor composite ceramics. It helps to increase the FOM (figure of merit, FD) of composite ceramics. TheΔ(O-Ba) andΔ(O-Sr) for O-Ba and O-Sr bond are increased gradually. This help to increase dielectric constants for SBN/SBT composite ceramics. The pyroelectric coefficient have more wide pyroelectric coefficient reponse than those of (Ba_(0.7)Sr_(0.3))TiO_3 and (Ba_(0.7)Sr_(0.3))Nb_2O_6 for SBN/SBT composite ceramics.
The influence of La_2O_3 doping on structure and properties for the 0.7BaO·0.3SrO·0.5TiO_2·0.5Nb_2O_5 composite ceramics was studied. The relative density and dielectric loss were improved by La_2O_3 doping. This helps to improve the FOM for composite ceramics. The XPS for the (0.7-z)BaO·(0.3-z)SrO·zLa_2O_3·0.5TiO_2·0.5Nb_2O_5 were studied. It is shown that the binding energy of Nb3d5/2 was not influenced by La_2O_3 doping. The binding energies of Ti2p were strongly dependent on La_2O_3 doping. The influences of La_2O_3 doping on the O-Nb and O-Ti bond are put forward to byΔ(O-Nb)= BE(O_(1s))-BE(Nb_(3d5/2)) andΔ(O-Ti) = BE(O_(1s))-BE(Ti_(2p3/2)). The SBN/SBT with La~(3+) doping has higher FOM than those of (Ba_(0.7)Sr_(0.3))TiO_3 0.7BaO·0.3SrO·0.5TiO_2·0.5Nb_2O_5 and (Ba_(0.7)Sr_(0.3))Nb_2O_6.
引文
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