CN101628810B - High transparent and high electro-optical property doped PMN-PT electro-optic ceramic material and preparation method thereof - Google Patents

High transparent and high electro-optical property doped PMN-PT electro-optic ceramic material and preparation method thereof Download PDF

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CN101628810B
CN101628810B CN2009100563000A CN200910056300A CN101628810B CN 101628810 B CN101628810 B CN 101628810B CN 2009100563000 A CN2009100563000 A CN 2009100563000A CN 200910056300 A CN200910056300 A CN 200910056300A CN 101628810 B CN101628810 B CN 101628810B
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CN101628810A (en
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李国荣
阮伟
曾江涛
郑嘹赢
丁爱丽
殷庆瑞
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Jiangsu Institute of advanced inorganic materials
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Shanghai Institute of Ceramics of CAS
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Abstract

The invention relates to a doped PMN-PT electro-optic ceramic material with a high transparent and high electro-optical property and a preparation method thereof; the ceramic material is characterized in that the general formula of the electro-optic ceramic material is (1-x)Pb(MgyNbz)O3-xPbTi(5-3y)/4O3+(3y-1)A, wherein, (3y-1)A represents that (3y-1)mol of A is doped in 1mol of PMN-PT, x is more than 0 and not more than 0.55; y is more than 0.334 and not more than 0.5; y+z=1; and A is one or two or three of Y, Bi and La. The transmittance of the transparent electro-optic ceramic series provided by the invention can vary between 60% to 66% with x, y and z without considering that when surface reflected light is lost, the transmittance is up to 90% to 95% and the secondary electro-optical coefficient is up to 20-60*10<-16>m<2>/V<2>. Therefore, the doped Pb(Mg1/3Nb2/3)O3-PbTiO3 provided by the invention is a transparent electro-optic ceramic with application value.

Description

High transparent and high electro-optical property doped PMN-PT electro-optic ceramic material and preparation method
Technical field
The present invention relates to doped P MN-PT electro-optic ceramics material and preparation method, relate to the doped P b (Mg of one type of high-clarity, low Tc, high electro-optic coefficient or rather 1/ 3Nb 2/ 3) O 3-PbTiO 3The transparent electro-optic ceramics material of system belongs to the PMN-PT system.
Background technology
Electrooptical material field, lithium niobate crystals are actual industrial standardss always.As the lithium niobate crystals non-linear optic crystal of perovskite-like structure, it has a stronger electrooptic effect and higher Curie temperature and very high response speed, is used widely at optical communication field.Except not being used as the light source detector, lithium niobate crystals is fit to make the various control couplings and the transmission apparatus of light, like devices such as light isolation, amplification, waveguide, modulation.But because growing technology can not get breaking through for a long time, also be difficult to produce the lithium niobate crystals that meets stoichiometric ratio at present, make its performance be difficult to satisfy objective requirement; Secondly the processing of lithium niobate crystals will be considered the problem of optical axis alignment, and difficulty of processing is big, and cost value is higher relatively; The electro-optic coefficient of lithium niobate crystals is lower and receive light injury easily in addition, simultaneously temperature is had bigger dependency [Wang Zhongmin, " Study on Development of Lithium Niobate Crystal, " artificial lens journal, vol.31, pp.173-175,2002.].
PLZT Pb-based lanthanumdoped zirconate titanates base transparent ceramic is a kind of transparent relaxation ferroelectric ceramic of lanthanum modification of mixing, and compares with crystalline material Lithium niobium trioxide etc., and PLZT has higher electro-optic coefficient and light transmission; Lower optical loss, wideer transmission wavelength scope, higher quadratic electro-optical effect; Response speed is fast, WV is low, driving voltage is with characteristics [K.Uchino such as temperature variation are stable; " Electro-optic ceramics and their displayapplications, " Ceramics International, vol.21; Pp.309-315,1995.].Research to transparent electro-optic ceramics at present mainly concentrates on the PLZT material.Have the research and the application report of a large amount of PLZT crystalline ceramics in the past, and also obtained the stupalith of high-clarity and higher electro-optic coefficient.But the significant electric field inductive effect of PLZT, polarization rely on scattering loss and high electricity returns stagnant phenomenon, makes such transparent electro-optic ceramics in optical tech is used, be restricted [J.Lappalainen; J.Hiltunen, and V.Lantto, " Characterization of optical properties of nanocrystalline doped PZT thinfilms; " Journal of the European Ceramic Society; Vol.25, pp.2273-2276,2005.].
Lead magnoniobate lead titanate (1-x) Pb (Mg 1/3Nb 2/3) O 3-xPbTiO 3(PMN-PT) be a kind of relaxor ferroelectric material with high tension performance.As transparent electro-optic ceramics material lead magnoniobate lead titanate (1-x) Pb (Mg that it is found that modification 1/3Nb 2/3) O 3-xPbTiO 3After having better electro-optical properties; Obtain high-clarity PMN-PT electro-optic ceramics and caused people's attention [K.Uchino; " Electro-opticceramics and their display applications, " Ceramics International, vol.21; Pp.309-315,1995.; K.Zou, Q.Chen, K.Li, R.Zhang, H.Jiang, B.Inc, and M.Woburn, " Characterization of new electro-optic ceramics, " 2004.].
A small amount of report [J.Giniewicz, D.McHenry, T.Shrout that obtains the PMN-PT crystalline ceramics through hot-pressing sintering technique only arranged in the past; S.Jang, A.Bhalla, and F.ainger; " Characterization of (1-x) Pb (Mg1/3Nb2/3) O3-(x) PbTiO3 and Pb (Sc1/2Ta1/2) O3 transparent ceramics prepared by uniaxial hot-pressing, " Ferroelectrics, vol.109; Pp.167-172,1990.; D.McHenry, J.Giniewicz, S.Jang, T.Shrout; And A.Bhalla, " Optical and electro-optical properties of lead magnesium niobate-leadtitanate, " Ferroelectrics; Vol.107, pp.45-46,1990.]; Kong L.B [L.Kong, J.Ma, W.Zhu; And O.Tan, " Translucent PMN and PMN-PT ceramics from high-energy ballmilling derived powders, " Materials Research Bulletin; Vol.37; Pp.23-32,2002.] etc. processed PMN-PT powder, through adding excessive 10% PbO with uhligite phase with high energy ball mill method; Adopt two step atmosphere sintering technologies to process the PMN-PT transparent electro-optic ceramics, but transmittance very low (21%600nm).Domestic also only have Wuhan University of Technology that transparent technology and the influence factor of PMN-PT pottery was certain discussion [Jiang Sheng; Liu Zhongming etc., " material behavior and the technology of preparing [J] of PMN-PT transparent photoelectric pottery, " material Leader vol.21; Pp.289-292,2006.].
The present invention intends the adulterating method with multicomponent, and above-mentioned PMN-PT crystalline ceramics is done further modification, and transmitance and secondary electro-optic coefficient are further improved, and is expected to develop more valuable transparent electro-optic ceramics material, thereby is built into design of the present invention.
Summary of the invention
As stated; The objective of the invention is in order to provide one type to have electro-optic ceramics material of high-clarity high electro-optical property and preparation method thereof; The electro-optic ceramics material that is expected to provide can be used for preparation of devices such as variable optical attenuator, Polarization Controller, sinusoidal filter, dynamic flat filter, tunable optical filter, photoswitch and grating, has a wide range of applications at key areas such as optical communication and light sensings.
Specifically, the composition general formula of described doping PMN-PT stupalith of the present invention is:
(1-x)Pb(Mg yNb Z)O 3-xPbTi (5-3y)/4O 3+(3y-1)A。Wherein (3y-1) A representes the A of doping (3y-1) mol among the 1molPMN-PT, wherein, and 0＜x≤0.55; 0.334＜y≤0.5; Y+z=1; A be among Y, Bi and the La a kind of, two kinds or three kinds.Electro-optic ceramics provided by the present invention is actually the doping vario-property of PMN-PT electro-optic ceramics material, and it is a kind of pure ABO that does not contain the Jiao Lvshi phase 3The type calcium titanium ore structure.
The preparation method of stupalith of the present invention is the synthesis technique and the two-step sintering method of conventional oxide pottery.Detailed process comprises:
(1) batching: the PbO, the MgCO that adopt CP level or AR level 3, TiO 2, Nb 2O 5, Bi 2O 3, Y 2O 3, La 2O 3Be raw material, by (1-x) Pb (Mg yNb Z) O 3-xPbTi (5-3y)/4O 3+ (3y-1) the accurate weighing of the stoichiometric ratio of A.
(2) ball mill mixing: do medium with deionized water, planetary ball mill 3-10 hour.Discharging is dry behind the mixing.
(3) synthetic: powder is contained in the corundum crucible, synthesizes in 1-4 hour 700-1000 ℃ of insulation.
(4) synthetic material ball milling: synthetic material was pulverized, and crosses 40 mesh sieves, does medium with deionized water, with planetary ball mill ball milling 4-6 hour.Discharging is dry.The powder adding additives, 1-2T/cm is used in manual granulation 2Pressure be pressed into the disk of diameter 20mm.
(5) two step method sintering: the first step: at 1000-1250 ℃, in the Ar or the N of logical oxygen atmosphere 2The ceramic body densification was come out of the stove in pressureless sintering 2-4 hour in the mixed atmosphere and be cooled to room temperature, second step: under 1100-1300 ℃, in hot pressing furnace, apply pressure sintering 2-10 hour of 20-100MPa then.Oxygen level in the mixed atmosphere of logical oxygen atmosphere is 30-95vol%.
Through adopting new compositing formula to obtain not containing the pure perovskite phase of Jiao Lvshi phase; Secondly through changing the preparation technology of ceramic transparence; Be the first step pressureless sintering under oxygen containing mixed atmosphere condition; Be cooled to room temperature, second step is pressurized heat processing again in hot pressing furnace, thereby obtains the preferable doping PMN-PT crystalline ceramics of over-all properties; Has higher transmittance 60%-66% (transmitance was up to 90%-95% when the Considering Surface reflected light did not lose), higher secondary electro-optic coefficient R:20-45x10 -16m 2/ V 2Therefore be an of great value transparent electro-optic ceramics material system.
Doped PMN-PT electro-optic ceramic provided by the invention can be used for preparation of devices such as variable optical attenuator, Polarization Controller, sinusoidal filter, dynamic flat filter, tunable optical filter, photoswitch and grating, has a wide range of applications at key areas such as optical communication and light sensings.
Description of drawings
Fig. 1 is the XRD figure that embodiment 1 forms;
Fig. 2 is the SEM figure that embodiment 1 forms;
Fig. 3 composes for the back dielectric temperature of burning till that embodiment 1 forms;
The transmittance curve that Fig. 4 forms after burning till for embodiment 1;
The crystalline ceramics sample 0.5mm of Fig. 5 the present invention preparation;
Fig. 6 is refringence-electric field curve that embodiment 1 forms.
Embodiment
Through concrete embodiment embodiment of the present invention is described below
Embodiment 1:
Get x=0.3, y=0.34, z=0.66, A is Bi, by the batching of doping PMN-PT composition general formula, adopts the chemical reagent Bi of CP or AR level 2O 3, PbO, MgCO 3, Nb 2O 5, TiO 2Be raw material, after the thorough drying, form the general formula weighing by doping PMN-PT.
Do medium with deionized water, ball mill mixing 3 hours.Drying is sieved, and powder synthesized under 850 ℃ of conditions in corundum crucible in 2 hours.Crushing screening then, ball milling 3 hours, drying; Adding additives, dry-pressing formed, behind the plastic removal; At first at 1160 ℃, oxygen level is that pressureless sintering made the ceramic body densification in 2 hours in the logical oxygen gas mixture atmosphere of 90vol%, under 1200 ℃, in hot pressing furnace, applies 80MPa sintering 8 hours then.This ceramic transmitance reaches 64% (transmitance was up to 93% when the Considering Surface reflected light did not lose), and pottery has higher secondary electro-optic coefficient R:45x10 simultaneously -16m 2/ V 2The XRD of the doped P MN-PT electro-optic ceramics of present embodiment preparation is as shown in Figure 1, by finding out that pottery is pure phase ABO among the figure 3Structure does not contain the Jiao Lvshi phase; Its SEM photo is as shown in Figure 2, and pottery has high density; Its dielectric temperature spectrum is as shown in Figure 3, and its Tc is approximately 60 ℃; Its transmittance curve is as shown in Figure 4, and its transmitance reaches as high as 64%; Ceramics sample behind the sintering is as shown in Figure 5 through polishing, and it is faint yellow that pottery is, can clear demonstration under the literal of paper.This ceramic specific refractory power-electric field curve is as shown in Figure 6, can reach 45x10 through calculating its electro-optic coefficient -16m 2/ V 2
Embodiment 2:
Get x=0.2, y=0.34, z=0.66 forms the general formula batching by doped P MN-PT, and A is La and Bi, and the two ratio is 8: 2.Adopt the chemical reagent La of CP or AR level 2O 3, PbO, MgCO 3, Nb 2O 5, TiO 2Be raw material, after the thorough drying, press the weighing of following formula stoichiometry.
Do medium with deionized water, ball mill mixing 5 hours.Drying is sieved, and powder synthesized under 800 ℃ of conditions in corundum crucible in 3 hours.Crushing screening then, ball milling 5 hours, drying; Adding additives, dry-pressing formed, behind the plastic removal; At first at 1180 ℃, oxygen level is that pressureless sintering made the ceramic body densification in 4 hours in the logical oxygen gas mixture atmosphere of 45vol%, under 1220 ℃, in hot pressing furnace, applies 80MPa sintering 8 hours then.This ceramic transmitance transmitance reaches 62% (transmitance was up to 91% when the Considering Surface reflected light did not lose), has higher secondary electro-optic coefficient R:35x10 simultaneously -16m 2/ V 2All the other are with embodiment 1.
Embodiment 3:
Get x=0.3, y=0.34, z=0.66, A is 50wt%La and 50wt%Bi, presses general formula (1-x) Pb (Mg yNb Z) O 3-xPbTi (5-3y)/4O 3+ (3y-1) A adopts the chemical reagent La of CP or AR level 2O 3, Bi2O3, PbO, MgCO 3, Nb 2O 5, TiO 2Be raw material, after the thorough drying, press the weighing of following formula stoichiometry.
Do medium with deionized water, ball mill mixing 5 hours.Drying is sieved, and powder is in corundum crucible, and is synthetic at 800 ℃/3 hours.Crushing screening then, ball milling 5 hours, drying; Adding additives, dry-pressing formed, behind the plastic removal; At first at 1180 ℃, oxygen level is that pressureless sintering made the ceramic body densification in 2 hours in the logical oxygen gas mixture atmosphere of 30vol%, pressure sintering 8 hours in hot pressing furnace under 1200 ℃ then.Its transmitance 60% (transmitance was up to 89% when the Considering Surface reflected light did not lose), secondary electro-optic coefficient R is: 24x10 -16m 2/ V 2All the other are with embodiment 1.

Claims (5)

1. a doped P MN-PT electro-optic ceramics material is characterized in that the composition general formula of described doping PMN-PT stupalith is (1-x) Pb (Mg yNb z) O 3-xPbTi ( 5-3y)/4O 3+ (3y-1) A, (3y-1) A A of (3y-1) mol that representes to mix among every 1mol PMN-PT wherein, 0＜x in the formula≤0.55,0.334＜y≤0.5, y+z=1, A be among Y, Bi and the La a kind of, two kinds or three kinds.
2. by the described doped PMN-PT electro-optic ceramic material of claim 1, it is characterized in that described doping PMN-PT stupalith is not for containing the pure ABO of Jiao Lvshi phase 3The type perovskite structure.
3. the preparation method of doped PMN-PT electro-optic ceramic material according to claim 1 or claim 2 is characterized in that adopting conventional oxide and the two-step sintering technology that combines, and concrete steps are:
(a) batching: the PbO, the MgCO that adopt CP level or AR level 3, TiO 2, Nb 2O 5, Bi 2O 3, Y 2O 3, La 2O 3Be raw material, by claim 1 described (1-x) Pb (MgyNbz) O 3-xPbTi (5-3y)/4O 3+ (3y-1) the accurate weighing of the stoichiometric ratio of A;
(b) ball mill mixing: do medium with deionized water, planetary ball mill, discharging is dry behind the mixing;
(c) synthetic: powder is contained in the corundum crucible, and is synthetic at 700-1000 ℃;
(d) synthetic material ball milling: synthetic material is pulverized, and sieves, and does medium with deionized water, uses the planetary ball mill ball milling, powder adding additives granulation and dry-pressing formed after the discharging drying;
(e) two step method sintering: the first step: at 1000-1250 ℃; Pressureless sintering in Ar that leads to oxygen atmosphere or N2 mixed atmosphere; The ceramic body densification is come out of the stove be cooled to room temperature, second step: the pressure sintering that under 1100-1300 ℃, in hot pressing furnace, applies 20-100MPa then.
4. by the preparation method of the described doped PMN-PT electro-optic ceramic material of claim 3, it is characterized in that:
(1) the planetary ball mill time is 3-10 hour among the step b;
Insulation is 1-4 hour when (2) synthesizing among the step c;
(3) synthetic material is pulverized the back and is crossed 40 mesh sieves in the steps d;
(4) in the steps d after the synthetic granulation pressure of dry-pressing be 1-2T/cm 2
5. by the preparation method of the described doped PMN-PT electro-optic ceramic material of claim 3, it is characterized in that:
(1) oxygen level in the first step sintering is 30-95vol%; The first step pressureless sintering soaking time is 2-4 hour;
(2) second step hot pressed sintering soaking times are 2-10 hour.
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CN103496980B (en) * 2013-09-23 2016-05-18 青岛大学 The pressureless sintering preparation method of high transparent PMN-PT base electro-optic ceramics
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