Preparation method for lead zinc niobate-lead titanate monocrystal
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A technology of lead niobate zincate and lead titanate, which is applied in the growth field of single crystal materials, can solve the problems of environmental hazards, PbO is volatile, and has not been applied to PZN-PT single crystals, etc., and achieves accelerated growth speed and crystal integrity Good, the effect of shortening the crystal growth cycle
Inactive Publication Date: 2012-03-21
NANJING UNIV OF AERONAUTICS & ASTRONAUTICS
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However, because PbO is easy to volatilize at high temperature and has certain harm to
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Embodiment 1
[0033] Example 1 0.91Pb(Zn 1 / 3 Nb 2 / 3 )O 3 -0.09PbTiO 3 Single crystal preparation
[0034] Using high-purity PbO, ZnO, Nb 2 o 5 and TiO 2 As an initial raw material, the following processes are included:
[0035] 1. Raw material processing
[0036] (1), the ZnO, Nb 2 o 5 , TiO 2 Mix materials according to stoichiometric ratio, ball mill for 4 hours and pre-sinter at 850°C for about 4 hours to obtain ZnNb 2 o 6 and a small amount of zinc niobium titanium oxide;
[0037] (2) Add PbO according to the stoichiometric ratio, heat to 700°C after ball milling and hold for 3 hours to obtain 0.91PZN-0.09PT ceramic powder;
[0038] (3) According to the metering relationship of the molar ratio of PZN-PT ceramic powder to flux = 3:7, add flux to the 0.91PZN-0.09PT ceramic obtained in step (2), and the flux is pure PbO. The flux and the solute are ball milled and mixed, and pressed into blocks to obtain the starting material for single crystal growth, which is put into the pl...
Embodiment 2
[0047] Example 2 0.88Pb(Zn 1 / 3 Nb 2 / 3 )O 3 -0.12PbTiO 3 Single crystal preparation
[0048] Select high-purity chemical reagents PbO, ZnO, Nb 2 o 5 and TiO 2 Grow as starting material.
[0049] 1. Raw material processing
[0050] (1), the raw materials ZnO, Nb 2 o 5 , TiO 2 Mix materials according to stoichiometric ratio, ball mill for 8 hours and pre-sinter at 1150°C for 1 hour to obtain ZnNb 2 o 6 and a small amount of zinc niobium titanium oxide;
[0051] (2) Add PbO according to the stoichiometric ratio, heat to 800°C after ball milling and hold for 1 hour to obtain 0.88PZN-0.12PT ceramics;
[0052] (3) According to the metering relationship of the molar ratio of PZN-PT ceramic powder to flux = 5:5, add flux to the PZN ceramic powder obtained in step (2). Fluxes are PbO and B 2 o 3 mixture of PbO and B 2 o 3The mol ratio=48:2. The flux and the solute are mixed by ball milling and pressed into blocks to obtain the starting material for single crystal grow...
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Abstract
The invention relates to a preparation method for a lead zinc niobate-lead titanate monocrystal. The preparation method comprises the following steps of: mixing raw materials of PbO, ZnO, Nb2O5 and TiO2 according to chemical composition (1-x)Pb(Zn1/3Nb2/3)O3-xPbTiO3PZN-PT, wherein x is mole fraction of PT in a solid solution system and is 0-1; mixing the raw materials of ZnO, Nb2O5 and TiO2 in a stoichiometric ratio, and ball-milling and sintering to obtain ZnNb2O6 with a niobite structure and a small amount of zinc niobium titanium oxide with a rutile structure; mixing PbO and sintering to obtain PZN-PT ceramic powder with a perovskite structure; mixing the PZN-PT ceramic powder and a fluxing agent for the growth of the crystal; processing a seed crystal according to crystal orientation (111) and (011); and growing the monocrystal, namely raising the temperature to the saturated growth temperature and reducing the temperature at a speed of 0.5 to 2 DEG C per hour, wherein the pulling speed of the monocrystal is 0.1 to 0.5 mm/h and the rotating speed of the monocrystal is 10 to 25 rpm, when the temperature is reduced to be between 900 and 1,030 DEG C, the crystal is separated from a melt solution and the monocrystal is obtained by reducing the temperature to room temperature at a speed of 50 to 100 DEG C per hour. The monocrystal has large size, high uniformity and obvious crystal appearance and is easy for directional process. The crucible can be reused, and smelting cost is reduced.
Description
technical field [0001] The invention belongs to the field of material preparation and relates to the growth of a single crystal material. During the implementation process, the solid solution single crystal lead niobate zincate-lead titanate is grown by the pulling method. Background technique [0002] Lead titanate (PbTiO 3 ) is a typical perovskite ferroelectric, lead niobate zincate (Pb(Zg 1 / 3 Nb 2 / 3 )O 3 ) is a typical relaxor ferroelectric. In March 1997, the internationally renowned journal "SCIENCE" reported the pseudo-binary solid solution system formed by the two - the relaxor ferroelectric single crystal (1- x )Pb(Zn 1 / 3 Nb 2 / 3 )O 3 - x PbTiO 3 (PZN-PT, x is the mole fraction of PT in the solid solution system) piezoelectric properties. Compared with traditional PZT piezoelectric ceramics, its piezoelectric constant d 33 Increased from 600pC / N to 2500pC / N, electromechanical coupling factor k 33 Increased from 70% to 93-95%, the maximum electrostric...
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