CN1059570A - The poling method of Potassium Iodate monocrystalline - Google Patents
The poling method of Potassium Iodate monocrystalline Download PDFInfo
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- CN1059570A CN1059570A CN 91109478 CN91109478A CN1059570A CN 1059570 A CN1059570 A CN 1059570A CN 91109478 CN91109478 CN 91109478 CN 91109478 A CN91109478 A CN 91109478A CN 1059570 A CN1059570 A CN 1059570A
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Abstract
The present invention has provided a kind of method of poling and detwinning of Potassium Iodate monocrystalline.Potassium iodate crystal is put into the silicone oil of polarization stove, to crystal heating, added electric field, or to crystal heating, added electric field and plus-pressure, near 72 ℃ or 212 ℃ of transformation temperatures, adopt " temperature oscillation " to eliminate crystalline twin and multidomain structure (the temperature oscillation scope is 65 ℃-85 ℃ or 200 ℃-235 ℃), thereby it is good to obtain optical homogeneity, satisfies optics and makes the single domain potassium iodate crystal that requires.The inventive method is easy, easy handling.
Description
The present invention relates to poling method as the multidomain Potassium Iodate monocrystalline of device for non-linear optical material.
Potassium Iodate (KIO
3) monocrystalline is a kind of multi-functional ferroelectric material, its nonlinear optical coefficients are higher than present widely used non-linear optic crystal.Its thermostability is fabulous, is suitable for using under different temperature condition.Therefore it all has important use value in laser technology and other photoelectron technology field.The Potassium Iodate monocrystalline is the water solution growth, and this crystal contains twin and complicated many domain structures, therefore makes its optical homogeneity matter can not reach the requirement of making optics, thereby has influenced the performance of its premium properties.The Potassium Iodate monocrystalline is the same with other ferroelectric crystal, needed to carry out poling (or polarization) and handle before making device.
Ferroelectric common poling method mainly is simultaneously to crystal heating, added electric field, or simultaneously to crystal heating, added electric field and plus-pressure.For the Potassium Iodate monocrystalline,, make that its condition of poling is comparatively harsh because its domain structure is complicated and contain factor such as twin.G.R.Crane in 1972 (J.Appl.Cryst., 5(1972), 350) once reported millimetre-sized potassium iodate crystal was heated the method for removing twin with plus-pressure simultaneously, heat to more than 212 ℃ plus-pressure 180kg/cm
2The KIO that above-mentioned condition is with practical value to bulk
3Crystal is inapplicable, because bulky crystal is difficult to make it stressed even especially, so at 180kg/cm
2Under the pressure, high temperature more than 212 ℃ nearly all bulk potassium iodate crystal all want broken.
The objective of the invention is to provide a kind of novel method-" temperature oscillation " of realizing the Potassium Iodate single crystal domainsization.This method can make operating voltage and institute's plus-pressure reduce, thereby sample is difficult for bursting.This method is easy, easy handling.
Main points of the present invention are:
(1) the Potassium Iodate monocrystalline is put into the polarization stove silicone oil, heat for crystal simultaneously, added electric field, moving towards applied field along prevailing intrinsic domain boundary in the crystal is 7-10kv/cm, near 72 ℃ of transformation temperatures, adopt the temperature oscillation scope be 65 ℃-85 ℃ temperature oscillation by the crystalline temperature in this scope back and forth by transformation temperature, reach and eliminate twin and realize poling.
(2) heat for crystal simultaneously, added electric field also applies certain pressure, carries out temperature oscillation near 212 ℃ of transformation temperatures, and the temperature oscillation scope is 200 ℃-235 ℃, applies the electric field of 4-5kv/cm along crystal x direction, applies 6-10kg/cm along crystalline y direction again
2Pressure, reach and eliminate twin and realize complete poling.
Poling embodiment below in conjunction with the Potassium Iodate monocrystalline further describes implementation process of the present invention.
For the convenience of narrating below provides the sign of Potassium Iodate monocrystalline direction now, Potassium Iodate crystalline structure at room temperature belongs to triclinic(crystalline)system, but its three axial lengths and the value of three angles all be close respectively, therefore can press experimentally
The three parts treats, and then available hexagonal system represents that the crystalline profile is a hexagonal prism, and the selection of its profile and coordinate as shown in Figure 1.Fig. 1 has represented the relation between crystal boundary, example interface and the coordinate axis.
(1) near 72 ℃ of transformation temperatures, adopt temperature oscillation to eliminate twin and multidomain.Simultaneously to crystal heating and added electric field.
Potassium Iodate more than 72 ℃ and below be ferroelectric phase, and the transformation mutually from a ferroelectric phase to another ferroelectric phase is a reversible.
Apply the selection of direction of an electric field, Potassium Iodate has complicated domain structure, but prevailing be 120 ° of farmlands, its polarization components that is mutually 120 ° of distributions is always in the Z face, but the intensity of these three components generally all is unequal.Our experimental result shows that the main domain boundary trend of Potassium Iodate often only appears on a certain specific direction, and forms the close quarters of parallel domain boundary, is easy to find the trend of these parallel domain boundaries under polarizing microscope.Along these domain boundary direction added electric fields, 120 ° of the polarization vector rotations of domain boundary both sides are overlapped with direction of an electric field.It is best to make the poling effect like this.And this direction is normally near perpendicular with one of six prismatic sides of crystalline.
The Potassium Iodate sample is the hexagonal prism body, put into the silicone oil of polarization stove, be heated to more than 72 ℃ to crystal, when temperature reaches about 85 ℃, add the electric field of 7-10kv/cm in the y of sample direction (being that the intrinsic domain boundary of sample is orientated dominant direction), lower the temperature with 1 ℃/minute V-bar again, when temperature during by 72 ℃ of transformation temperatures, begin to disappear along the electricdomain that the crystalline Z-direction can be observed with telemicroscope on twin and the non-electric field direction at viewing window, when temperature is reduced to 65 ℃, can be repeatedly reciprocal with temperature oscillation between 65 ℃-85 ℃, whenever once by transformation temperature, electricdomain on twin and the non-electric field direction just disappears, and till the macroscopical electricdomain completely dissolve on twin and the non-electric field direction, cools to room temperature with the speed less than 1 ℃/minute again.Experimental result as shown in Figure 2.Fig. 2 has provided the comparison of poling front and back potassium iodate crystal optical homogeneities.The advantage of this method is that working temperature is lower in the poling process, and sample is difficult for bursting, and the most close room temperature of transformation temperature by a transformation temperature, just can directly obtain the room temperature single domain crystal.From Fig. 2 in (a) and the comparison (b) as can be seen after treatment the crystalline optical homogeneity be improved significantly.
(2) near 212 ℃ of transformation temperatures, adopt temperature oscillation to eliminate twin and many electricdomains.Simultaneously to crystal heating, added electric field and pressure.
Potassium iodate crystal more than 212 ℃ and following be respectively paraelectric phase and ferroelectric phase, this phase transformation from the paraelectric phase to the ferroelectric phase also is a reversible.
The Potassium Iodate monocrystalline is processed into parallelepiped, its three class boundary faces are respectively x, y, z face, x, y, z face are respectively perpendicular to x, y, z axle (referring to Fig. 1), sample is put into the silicone oil of polarization stove, sample is slowly heated to more than 212 ℃, at this moment sample is in paraelectric phase, and its domain structure disappears.Add along crystalline x direction and the electric field of 4-5kv/cm to add 6-10kg/cm in the y direction
2Pressure, as shown in Figure 3.Fig. 3 has provided added electric field and stressed direction.Polarization pulse electric current behind the added electric field is 1.5mA/cm
2About.The polar working current is generally 15-20 μ A/cm
2Warming and cooling rate is 1 ℃/minute, between 200 ℃-235 ℃, adopts temperature oscillation to handle, until twin and electricdomain completely dissolve.And then reduce to room temperature with cooling rate slowly.Can obtain single domain crystal, as shown in Figure 4.Fig. 4 has provided poling and has handled the inhomogeneity contrast of crystal optics of front and back.
When near 212 ℃, implementing poling, to note following two problems in the operating process:
(1) working temperature must not surpass 250 ℃, and at high temperature Potassium Iodate has the possibility of decomposition, because separating out of iodine makes crystal become opaque garnet, and this process is irreversible.
(2) voltage can not be too high, preferably is no more than 6kv/cm, otherwise sample has breakdown and possibility that pulverize.
Sample behind poling, optical homogeneity be improved significantly, can reach the requirement of making optics.Scattered light in its transmitted light of potassium iodate crystal behind the poling all disappears as can be seen from Figure 5.
The explanation of Figure of description drawing
Fig. 1. crystalline coordinate and profile.X, y, z are coordinate axis, and 1 is the x face, and 2 is the y face, and 3 is the z face.
Fig. 2 .(a) Photomicrograph of potassium iodate crystal under cross-polarized light before the poling amplifies 80 times.
(b) Photomicrograph of potassium iodate crystal under cross-polarized light behind the poling amplifies 80 times.
Fig. 3. the poling device, 4 is silicone oil, and 5 is electrode, and 6 is the plus-pressure system, and 7 is the potassium iodate crystal sample.
Fig. 4 .(c) Photomicrograph of potassium iodate crystal under cross-polarized light before the poling amplifies 160 times.
(d) Photomicrograph of potassium iodate crystal under cross-polarized light behind the poling amplifies 160 times.
Fig. 5 .(e) the preceding potassium iodate crystal of poling is to scattering of light.
(f) behind the poling potassium iodate crystal to scattering of light.
Claims (4)
1, the poling method of Potassium Iodate monocrystalline is put into the silicone oil of polarization stove with the Potassium Iodate sample, adopt crystal heating, added electric field, or heating, added electric field and stressed method removes twin and realize poling, it is characterized in that:
(1) adopted " temperature oscillation " near 72 ℃ of transformation temperatures, and applied electric field along prevailing intrinsic domain boundary trend in the crystal.
(2) adopted " temperature oscillation " near 212 ℃ of transformation temperatures, and applied electric field and exert pressure along the y direction along crystalline x direction.
2, according to the said method of claim 1, it is characterized in that the hunting range when the temperature that adopts is 65 ℃-85 ℃, when transformation temperature is 72 ℃, move towards to apply the electric field of 7-10kv/cm to crystal along the intrinsic domain boundary in the crystal, allow temperature near transformation temperature back and forth, to reach twin and the multidomain structure of eliminating one by one in the crystal.
3, according to the said method of claim 1, it is characterized in that the hunting range when the temperature that adopts is 200 ℃-235 ℃, when transformation temperature is 212 ℃, apply the electric field of 4-5kv/cm to crystal, apply 6-10kg/cm along crystalline y direction to crystal again along crystalline x direction
2Pressure, allow temperature near 212 ℃ of transformation temperatures back and forth, just can obtain room temperature single domain potassium iodate crystal.
4,, it is characterized in that the electric field that institute adds 7-10kv/cm is to move towards its best results along 120 ° of parallel domain boundaries by claim 1 or 2 said methods.
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| Application Number | Priority Date | Filing Date | Title |
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| CN 91109478 CN1059570A (en) | 1991-10-10 | 1991-10-10 | The poling method of Potassium Iodate monocrystalline |
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| CN 91109478 CN1059570A (en) | 1991-10-10 | 1991-10-10 | The poling method of Potassium Iodate monocrystalline |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101587278B (en) * | 2008-05-22 | 2013-01-02 | 中国科学院福建物质结构研究所 | Nonlinear optical crystal plumbum-lanthanum iodate |
| CN106757343A (en) * | 2016-12-08 | 2017-05-31 | 中国科学院福建物质结构研究所 | A kind of novel nonlinear optical crystal Bi (IO3)F2Preparation and purposes |
| CN107326443A (en) * | 2017-06-05 | 2017-11-07 | 西安交通大学 | A kind of method of nonlinear optical material relaxor ferroelectric monocrystal poling |
-
1991
- 1991-10-10 CN CN 91109478 patent/CN1059570A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101587278B (en) * | 2008-05-22 | 2013-01-02 | 中国科学院福建物质结构研究所 | Nonlinear optical crystal plumbum-lanthanum iodate |
| CN106757343A (en) * | 2016-12-08 | 2017-05-31 | 中国科学院福建物质结构研究所 | A kind of novel nonlinear optical crystal Bi (IO3)F2Preparation and purposes |
| CN106757343B (en) * | 2016-12-08 | 2019-05-28 | 中国科学院福建物质结构研究所 | A kind of novel nonlinear optical crystal Bi (IO3)F2Preparation and purposes |
| CN107326443A (en) * | 2017-06-05 | 2017-11-07 | 西安交通大学 | A kind of method of nonlinear optical material relaxor ferroelectric monocrystal poling |
| CN107326443B (en) * | 2017-06-05 | 2019-10-11 | 西安交通大学 | A kind of method of nonlinear optical material relaxor ferroelectric monocrystal poling |
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