Method for improving homogeneity of potassium tantalate niobate crystal through double-crucible real-time material-feeding technology

A technology of potassium tantalum niobate and double crucibles is applied in the research field of preparation technology of functional crystal materials, which can solve the problems of difficulty in taking into account crystal size and uniformity, difficulty in obtaining modulation effect, fluctuation in crystal composition, etc., and simplify the ratio of raw materials. Design, avoid fluctuations in growth temperature and melt composition, reduce the effect of fluctuations in crystal composition

Inactive Publication Date: 2015-01-21
NEW MATERIAL INST OF SHANDONG ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, a prominent problem that limits the application of KTN crystal electro-optical components is that it is difficult to balance the size and uniformity of the crystal. In order to obtain a large-size KTN crystal, it is necessary to increase the cooling range of the crystal growth process. In the case of constant melt quality, The larger the crystal, the greater the change of the melt composition, both of which will in turn affect the fluctuation of the crystal composition, forming stripe defects, resulting in the scattering of the laser spot during light modulation, especially in the case of long optical path and large beam diameter. In some cases, it is difficult to obtain a satisfactory modulation effect

Method used

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  • Method for improving homogeneity of potassium tantalate niobate crystal through double-crucible real-time material-feeding technology
  • Method for improving homogeneity of potassium tantalate niobate crystal through double-crucible real-time material-feeding technology

Examples

Experimental program
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Effect test

Embodiment 1

[0029] Example 1: KTa 0.63 Nb 0.37 o 3 Crystal Growth Preparation

[0030] Since KTN crystal has significantly superior electro-optical and other physical properties near the phase transition point, while KTa 0.63 Nb 0.37 o 3 The Curie phase transition point of the crystal is near room temperature, which is beneficial to the development and design of KTN electro-optic components that can be applied at room temperature. The crystal preparation process is as follows: take high-purity K 2 CO 3 (purity 99.99%), high-purity Ta 2 o 5 (purity 99.99%), high-purity Nb 2 o 5 (Purity 99.99%) The raw materials are weighed according to the molar ratio of 1.25:0.3:0.7, mixed evenly and in 10 8 Compacted into blocks under Pa, sintered at 1050°C for 24 hours to obtain KTa 0.63 Nb 0.37 o 3 Base material, at this time the base material is block. K 2 CO 3 : Ta 2 o 5 :Nb 2 o 5 Weigh according to the molar ratio 1:0.63:0.37, mix well and 8 Compacted into blocks under Pa, sint...

Embodiment 2

[0033] Example 2: KTa 0.9 Nb 0.1 o 3 Crystal Growth Preparation

[0034] The process of this embodiment is the same as that of Embodiment 1, but the specific parameters need to be adjusted as follows, the ratio of base material and supplementary material is adjusted to K 2 CO 3 : Ta 2 o 5 :Nb 2 o 5 =1.25:0.72:0.28 and 1:0.9:0.1; the sintering temperature of the base material and the supplementary material is adjusted to 1090°C and 1100°C respectively, the full melting point of the crystal growth stage is 1275°C, overheating, planting, shouldering and so on The diameter growth temperature is adjusted to 1375°C, 1275°C, 1265°C, 1270°C, and the cooling rate at the end of crystal growth can be increased to 45°C / h to room temperature.

Embodiment 3

[0035] Example 3: KTa 0.75 Nb 0.25 o 3 Crystal Growth Preparation

[0036] The process of this embodiment is basically the same as that of Embodiment 1. The specific parameters are adjusted as follows, and the ratio of base material and supplementary material is adjusted to K 2 CO 3 : Ta 2 o 5 :Nb 2 o 5 =1.25:0.43:0.57 and 1:0.75:0.25; the sintering temperature of the base material and the supplementary material is adjusted to 1050°C and 1080°C respectively, the full melting point of the crystal growth stage is 1225°C, overheating, planting, shouldering and so on The diameter growth temperature was adjusted to 1325°C, 1225°C, 1215°C, 1220°C, and the cooling rate at the end of crystal growth was adjusted to 35°C / h to room temperature.

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Abstract

The invention discloses a method for improving homogeneity of a potassium tantalate niobate crystal through a double-crucible real-time material-feeding technology. In the method, high-purity K2CO3, Ta2O5, Nb2O5 are employed as raw materials. A KTN polycrystal basic material and a KTN polycrystal supplying material are respectively weighted and prepared according to required crystal components. The polycrystal materials are prepared through a grinding process, a uniformly blending process, a pressing moulding process and a sintering process. According to requirements of the double-crucible real-time material-feeding technology, an internal-external double-crucible temperature field system is designed and corresponding transformation of a lifting furnace is carried out for satisfying a real-time material-supplying requirement. A crystal growing process includes following steps: a seed adding process, a necking process, a shoulder-releasing process, an equal-neck turning process and an equal-neck growing process. During the crystal growing process, a crystal growing speed and a material-supplying speed are maintained to be equal for ensuring melt components to be stable. When the crystal growth is finished, the crystal is lifted from a liquid surface and is cooled slowly to room temperature to obtain a KTN monocrystal. By means of the technical scheme, crystal component fluctuation caused by fluctuations of the melt components and a growth temperature during the KTN monocrystal growing process through a conventional melt lifting method is greatly reduced, thereby greatly improving the homogeneity of the KTN crystal. The method has an important significance on practical application of the KTN crystal.

Description

technical field [0001] The invention belongs to the research field of preparation technology of functional crystal materials, and relates to a method for improving the compositional uniformity of potassium tantalum niobate crystals by introducing double-crucible real-time feeding technology on the basis of pulling method, thereby improving the optical quality of potassium tantalum niobate crystals . Background technique [0002] The electro-optic effect is a phenomenon in which the refractive index of the medium changes under the action of an external electric field. The phase, intensity and propagation direction of light can be modulated by using the electro-optic effect of crystal materials. Electro-optic modulation is due to high efficiency, fast response and non-mechanical (no Inertia) and other advantages, usually used to make laser modulators, scanners and optical switches and other devices, widely used in laser radar, laser ranging, biomedical microscopic imaging and...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C30B15/12C30B15/20C30B29/30
Inventor 王旭平刘冰张园园
Owner NEW MATERIAL INST OF SHANDONG ACADEMY OF SCI
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