高度透明PMN-PT基电光陶瓷的制备与性能研究
发布时间：2018-11-24 14:37
【摘要】：弛豫铁电体(1-x)Pb(Mg1/3Nb2/3)O3-xPbTiO3【简称PMN-PT(1-x)/x】具有优异的电学与光学性能,PMN-PT基透明陶瓷适合研制电光开关等调制器件,在光通信领域应用前景诱人。本论文先用铌铁矿法合成PMN-PT(1-x)/x粉体,接着成功烧结了高度透明的PMN-PT基透明陶瓷,总结了粉体合成工艺、烧结工艺、La掺杂量等因素对透明陶瓷的结构与性能影响,研究了La掺杂量对PMN-PT75/25透明陶瓷的回线动力学标度的影响。主要结果和结论如下:1、用铌铁矿法合成了PMN-PT粉体,球磨转速提高,粉体的平均二次粒径明显减小,用转速2000 r/min球磨合成的粉体烧结的陶瓷透光率最高。分别用单轴热压、氧气氛和两步烧结工艺成功制备了纯钙钛矿相PMN-PT基透明陶瓷,其中两步烧结法制备的陶瓷透光率最高。在6 MPa热压烧结的PMN-PT基透明陶瓷在近红外波段透光率高达70.2%。2、用两步烧结工艺制备了不同La掺杂量的PMN-PT75/25透明陶瓷,掺La3.0 mol%的PMN-PT75/25陶瓷非常致密,气孔率很低,在近红外波段透光率约70%,接近其透光率的理论极限值71%。随着La掺杂量增加,PMN-PT75/25透明陶瓷XRD图谱中(200)峰向大角度方向移动,平均晶粒尺寸呈增大的趋势,介电温谱中的峰值温度逐渐降低,剩余极化与矫顽场也呈降低的趋势,铁电性能变弱。3、室温下不同掺La量PMN-PT75/25透明陶瓷的回线动力学标度结果表明,对低掺杂La陶瓷(La=0、1、2.5 mol%),在低电场幅值回线面积A急剧增大,在高电场幅值回线面积A逐渐趋于稳定;对高掺杂La陶瓷(La=3、4 mol%),回线面积A无明显的稳定阶段。在测试频率范围内,随外场频率f上升,所有PMNPT75/25陶瓷样品的回线面积A逐渐呈线性增大。除掺La 2.5 mol%陶瓷外,随掺La量增加,PMN-PT75/25陶瓷中铁电畴极化翻转对f和E0的依赖性逐渐增强。
[Abstract]:The relaxor ferroelectrics (1-x) Pb (Mg1/3Nb2/3) O3-xPbTiO3 [PMN-PT (1-x) / x] have excellent electrical and optical properties. PMN-PT based transparent ceramics are suitable for the development of modulating devices such as electro-optic switches. The application prospect in the field of optical communication is attractive. In this paper, PMN-PT _ (1-x) / x powders were synthesized by niobium ore method, and then highly transparent PMN-PT based transparent ceramics were successfully sintered, and the powder synthesis process and sintering process were summarized. The influence of La doping amount on the structure and properties of transparent ceramics was studied. The effect of La doping content on the loop kinetic scaling of PMN-PT75/25 transparent ceramics was studied. The main results and conclusions are as follows: 1. PMN-PT powders were synthesized by niobium iron ore method. The average secondary particle size of the powders decreased obviously with the increase of ball milling speed, and the transmittance of ceramics sintered by 2000 r/min ball milling was the highest. Pure perovskite PMN-PT based transparent ceramics were successfully prepared by uniaxial hot pressing, oxygen atmosphere and two-step sintering process respectively. The highest transmittance was obtained by two-step sintering method. The transmittance of PMN-PT based transparent ceramics sintered in 6 MPa hot pressing was as high as 70.2% in near infrared band. Different La doped PMN-PT75/25 transparent ceramics were prepared by two-step sintering process. The PMN-PT75/25 ceramics doped with La3.0 mol% are very compact and have very low porosity. The transmittance is about 70 in the near infrared band, which is close to the theoretical limit of the transmittance of the PMN-PT75/25 ceramics. With the increase of La doping, the peak of (200) in the XRD spectrum of PMN-PT75/25 transparent ceramics moves in a large angle, the average grain size increases, and the peak temperature in dielectric temperature spectrum decreases gradually. The remanent polarization and coercive field also showed a decreasing trend, and the ferroelectric properties became weaker. 3. The results of loop kinetic scaling of PMN-PT75/25 transparent ceramics with different La content at room temperature showed that, for low doped La ceramics (La=0,1,2.5 mol%), At the low electric field amplitude, the loop area A increases sharply, and at the high electric field amplitude, the loop area A tends to be stable. For highly doped La ceramics (La=3,4 mol%), the loop area A has no obvious stable phase. In the range of measurement frequency, the loop area A of all PMNPT75/25 ceramics samples increases linearly with the increase of external field frequency f. In addition to La 2.5 mol% ceramics, the dependence of ferroelectric domain polarization flip on f and E0 in PMN-PT75/25 ceramics increases with the increase of La content.
【学位授予单位】：青岛大学
【学位级别】：硕士
【学位授予年份】：2017
【分类号】：TQ174.6
本文编号：2354099
[Abstract]:The relaxor ferroelectrics (1-x) Pb (Mg1/3Nb2/3) O3-xPbTiO3 [PMN-PT (1-x) / x] have excellent electrical and optical properties. PMN-PT based transparent ceramics are suitable for the development of modulating devices such as electro-optic switches. The application prospect in the field of optical communication is attractive. In this paper, PMN-PT _ (1-x) / x powders were synthesized by niobium ore method, and then highly transparent PMN-PT based transparent ceramics were successfully sintered, and the powder synthesis process and sintering process were summarized. The influence of La doping amount on the structure and properties of transparent ceramics was studied. The effect of La doping content on the loop kinetic scaling of PMN-PT75/25 transparent ceramics was studied. The main results and conclusions are as follows: 1. PMN-PT powders were synthesized by niobium iron ore method. The average secondary particle size of the powders decreased obviously with the increase of ball milling speed, and the transmittance of ceramics sintered by 2000 r/min ball milling was the highest. Pure perovskite PMN-PT based transparent ceramics were successfully prepared by uniaxial hot pressing, oxygen atmosphere and two-step sintering process respectively. The highest transmittance was obtained by two-step sintering method. The transmittance of PMN-PT based transparent ceramics sintered in 6 MPa hot pressing was as high as 70.2% in near infrared band. Different La doped PMN-PT75/25 transparent ceramics were prepared by two-step sintering process. The PMN-PT75/25 ceramics doped with La3.0 mol% are very compact and have very low porosity. The transmittance is about 70 in the near infrared band, which is close to the theoretical limit of the transmittance of the PMN-PT75/25 ceramics. With the increase of La doping, the peak of (200) in the XRD spectrum of PMN-PT75/25 transparent ceramics moves in a large angle, the average grain size increases, and the peak temperature in dielectric temperature spectrum decreases gradually. The remanent polarization and coercive field also showed a decreasing trend, and the ferroelectric properties became weaker. 3. The results of loop kinetic scaling of PMN-PT75/25 transparent ceramics with different La content at room temperature showed that, for low doped La ceramics (La=0,1,2.5 mol%), At the low electric field amplitude, the loop area A increases sharply, and at the high electric field amplitude, the loop area A tends to be stable. For highly doped La ceramics (La=3,4 mol%), the loop area A has no obvious stable phase. In the range of measurement frequency, the loop area A of all PMNPT75/25 ceramics samples increases linearly with the increase of external field frequency f. In addition to La 2.5 mol% ceramics, the dependence of ferroelectric domain polarization flip on f and E0 in PMN-PT75/25 ceramics increases with the increase of La content.
【学位授予单位】：青岛大学
【学位级别】：硕士
【学位授予年份】：2017
【分类号】：TQ174.6
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