CN101628810A - 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 PDFInfo
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Abstract
The invention relates to a high transparent and high electro-optical property doped PMN-PT electro-optic ceramic material 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
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 a class high-clarity, low Curie temperature, 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 can 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, as 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 be subjected to 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, compare with crystalline material Lithium niobium trioxide etc., 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, operating voltage is low, driving voltage varies with temperature characteristics [K.Uchino such as 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, make 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.].
Report [the J.Giniewicz that obtains the PMN-PT crystalline ceramics on a small quantity by hot-pressing sintering technique was only arranged in the past, D.McHenry, T.Shrout, 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. made PMN-PT powder with high energy ball mill method with uhligite phase, by adding excessive 10% PbO, two step of employing atmosphere sintering technologies have been made 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 of PMN-PT transparent photoelectric pottery and technology of preparing [J], " 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 mentioned above, the objective of the invention is for electro-optic ceramics material that a class has the high-clarity high electro-optical property and preparation method thereof is provided, 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 represents 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 perovskite 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 milling mixes: do medium with deionized water, planetary ball mill 3-10 hour.Discharging drying 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 is pulverized, and crosses 40 mesh sieves, does medium with deionized water, uses planetary ball mill ball milling 4-6 hour.The discharging drying.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%.
By adopting new compositing formula to obtain not containing the pure perovskite phase of Jiao Lvshi phase, secondly by 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 obtain the preferable doping PMN-PT crystalline ceramics of over-all properties, has higher transmittance 60%-66% (transmitance is not up to 90%-95% when not considering the surface reflection light loss), 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
Below by specific embodiment explanation the specific embodiment of the present invention
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 milling mixed 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%, applies 80MPa sintering 8 hours then under 1200 ℃ in hot pressing furnace.This ceramic transmitance reaches 64% (transmitance is not up to 93% when not considering the surface reflection light loss), 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 as shown in Figure 1, as can be seen from Figure, pottery is pure phase ABO
3Structure does not contain the Jiao Lvshi phase; Its SEM photo as shown in Figure 2, pottery has high density; Its dielectric temperature is composed as shown in Figure 3, and its Curie temperature is approximately 60 ℃; Its transmittance curve as shown in Figure 4, its transmitance reaches as high as 64%; Ceramics sample behind the sintering through polishing as shown in Figure 5, it is faint yellow that pottery is, can clear demonstration under the literal of paper.This ceramic specific refractory power-electric field curve as shown in Figure 6, its electro-optic coefficient can reach 45x10 as calculated
-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 milling mixed 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%, applies 80MPa sintering 8 hours then under 1220 ℃ in hot pressing furnace.This ceramic transmitance transmitance reaches 62% (transmitance is not up to 91% when not considering the surface reflection light loss), 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 milling mixed 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 is not up to 89% when not considering the surface reflection light loss), secondary electro-optic coefficient R is: 24x10
-16m
2/ V
2All the other are with embodiment 1.
Claims (5)
1, a kind of 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 represents 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 La, Bi and the La a kind of, two kinds or three kinds.
2,, it is characterized in that described doping PMN-PT stupalith is not for containing the pure ABO of Jiao Lvshi phase by the described doped PMN-PT electro-optic ceramic material of claim 1
3The type perovskite structure.
3, the method for preparation doped PMN-PT electro-optic ceramic material as claimed in claim 1 or 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 (MgyNb
Z) O
3-xPbTi
(5-3y)/4O
3+ (3y-1) the accurate weighing of the stoichiometric ratio of A;
(b) ball milling mixes: do medium with deionized water, planetary ball mill, discharging drying 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 ℃, in the Ar or the N of logical oxygen atmosphere
2Pressureless sintering in the mixed atmosphere is come out of the stove the ceramic body densification and is cooled to room temperature, second step: the pressure sintering that applies 20-100MPa then under 1100-1300 ℃ in hot pressing furnace.
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/em
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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