高度透明PMN-PT基電光陶瓷的制備與性能研究
發(fā)布時間:2018-11-24 14:37
【摘要】:弛豫鐵電體(1-x)Pb(Mg1/3Nb2/3)O3-xPbTiO3【簡稱PMN-PT(1-x)/x】具有優(yōu)異的電學與光學性能,PMN-PT基透明陶瓷適合研制電光開關(guān)等調(diào)制器件,在光通信領(lǐng)域應用前景誘人。本論文先用鈮鐵礦法合成PMN-PT(1-x)/x粉體,接著成功燒結(jié)了高度透明的PMN-PT基透明陶瓷,總結(jié)了粉體合成工藝、燒結(jié)工藝、La摻雜量等因素對透明陶瓷的結(jié)構(gòu)與性能影響,研究了La摻雜量對PMN-PT75/25透明陶瓷的回線動力學標度的影響。主要結(jié)果和結(jié)論如下:1、用鈮鐵礦法合成了PMN-PT粉體,球磨轉(zhuǎn)速提高,粉體的平均二次粒徑明顯減小,用轉(zhuǎn)速2000 r/min球磨合成的粉體燒結(jié)的陶瓷透光率最高。分別用單軸熱壓、氧氣氛和兩步燒結(jié)工藝成功制備了純鈣鈦礦相PMN-PT基透明陶瓷,其中兩步燒結(jié)法制備的陶瓷透光率最高。在6 MPa熱壓燒結(jié)的PMN-PT基透明陶瓷在近紅外波段透光率高達70.2%。2、用兩步燒結(jié)工藝制備了不同La摻雜量的PMN-PT75/25透明陶瓷,摻La3.0 mol%的PMN-PT75/25陶瓷非常致密,氣孔率很低,在近紅外波段透光率約70%,接近其透光率的理論極限值71%。隨著La摻雜量增加,PMN-PT75/25透明陶瓷XRD圖譜中(200)峰向大角度方向移動,平均晶粒尺寸呈增大的趨勢,介電溫譜中的峰值溫度逐漸降低,剩余極化與矯頑場也呈降低的趨勢,鐵電性能變?nèi)酢?、室溫下不同摻La量PMN-PT75/25透明陶瓷的回線動力學標度結(jié)果表明,對低摻雜La陶瓷(La=0、1、2.5 mol%),在低電場幅值回線面積A急劇增大,在高電場幅值回線面積A逐漸趨于穩(wěn)定;對高摻雜La陶瓷(La=3、4 mol%),回線面積A無明顯的穩(wěn)定階段。在測試頻率范圍內(nèi),隨外場頻率f上升,所有PMNPT75/25陶瓷樣品的回線面積A逐漸呈線性增大。除摻La 2.5 mol%陶瓷外,隨摻La量增加,PMN-PT75/25陶瓷中鐵電疇極化翻轉(zhuǎn)對f和E0的依賴性逐漸增強。
[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.
【學位授予單位】:青島大學
【學位級別】:碩士
【學位授予年份】:2017
【分類號】:TQ174.6
本文編號: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.
【學位授予單位】:青島大學
【學位級別】:碩士
【學位授予年份】:2017
【分類號】:TQ174.6
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