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Synthesis of constituent-homogeneous spherical lithium tantalite doping polycrystal raw material

A synthesis method, a technology of lithium tantalate, applied in the growth of polycrystalline materials, chemical instruments and methods, single crystal growth, etc., can solve the problems of difficult control, strong irritation, and difficult to remove ions, and achieve automation, improve Mobility, anti-floating effect

Inactive Publication Date: 2010-11-03
CETC DEQING HUAYING ELECTRONICS +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In 1999, KHSO was adopted by Judit Szanics and Masato Kakihana of Japan 4 -Oxalic acid method will Ta 2 o 5 Dissolved in the solution, however, this process is complex and easily introduces potassium impurities; in 2006, H.Muthurajan and H.H.Kumar of India et al. 2 o 5 Dissolved in HF (40%) after hot water bath for 10h, and HF has strong irritation, corrosion and toxicity, F - Ions are also easy to remain in the product and difficult to remove
In addition, the heating and evaporation rate of the solution is slow, and it is not easy to control, and it is difficult to realize the mass production of raw materials
And because this method cannot realize the control of the particle shape and particle size of the synthetic polycrystalline powder, the obtained powder is not suitable for crystal growth with continuous feeding

Method used

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  • Synthesis of constituent-homogeneous spherical lithium tantalite doping polycrystal raw material
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  • Synthesis of constituent-homogeneous spherical lithium tantalite doping polycrystal raw material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Synthesis of Lithium Tantalate Polycrystalline Material Doped with Mg(3mol%) Near Stoichiometric Ratio

[0036] (1) Weigh Ta(OH) 5 Ta 2 o 5 ·nH 2 O, add DL-malic acid (C 4 h 6 o 5 , DL-MA) 0.152g, adjust the pH to 7-8 with ammonia water (30%), and filter to remove impurities to obtain a clear and transparent Ta-MA complex solution.

[0037] (2) Use thermogravimetric analysis to test the true concentration of the solution: take 1.875g of Ta-MA solution and calcinate at 750°C for 2h, and calculate the actual concentration of the solution by weighing: 0.0655gTa 2 o 5 / g solution, X-ray diffraction results show that the powder obtained by calcination is Ta 2 o 5 single phase (eg figure 1 shown).

[0038] (3) Ta obtained according to thermogravimetric 5+ The exact amount, according to the equation: 0.97LiOH·H 2 O+0.03MgO+0.485Ta 2 o 5 →M:LiTaO 3 Calculate Li + , The exact amount of MgO.

[0039] (4) Add 0.0682g LiOH·H to the Ta-MA solution 2 O, 0.0020g Mg...

Embodiment 2

[0042] Example 2: Synthesis of Mg (3mol%) doped near-stoichiometric lithium tantalate polycrystalline material

[0043] (1) Weigh Ta(OH) 5 0.750g was heated and dissolved with 15ml of 36% concentrated hydrochloric acid to prepare highly active Ta 2 o 5 ·nH 2 O, add DL-malic acid (C 4 h 6 o 5 , DL-MA) 0.152g, adjust the pH to 7-8 with ammonia water (30%), and filter to remove impurities to obtain a clear and transparent Ta-CA complex solution.

[0044] (2) Use thermogravimetric analysis to test the true concentration of the solution: Take 2.036g of Ta-MA solution and calcinate at 750°C for 2h, and calculate the actual concentration of the solution by weighing: 0.0681g Ta 2 o 5 / g solution, X-ray diffraction results show that the powder obtained by calcination is Ta 2 o 5 Simplex.

[0045] (3) Ta obtained according to thermogravimetric 5+ The exact amount, according to the equation: 0.97LiOH·H 2 O+0.03MgO+0.485Ta 2 o 5 →M:LiTaO 3 Calculate Li + , The exact amoun...

Embodiment 3

[0048] Example 3: Synthesis of Mg (3mol%) doped near-stoichiometric lithium tantalate polycrystalline material

[0049] (1) Weigh the compound Ta(OH) of tantalum 5 The active Ta 2 o 5 ·nH 2 O, add DL-malic acid (C 4 h 6 o 5 , DL-MA) 0.152g, adjust the pH to 7-8 with ammonia water (30%), and filter to remove impurities to obtain a clear and transparent Ta-MA complex solution.

[0050] (2) Use thermogravimetric analysis to test the true concentration of the solution: take 2.126g of Ta-MA solution and calcinate at 750°C for 2h, and calculate the actual concentration of the solution by weighing: 0.0701g Ta 2 o 5 / g solution, X-ray diffraction results show that the powder obtained by calcination is Ta 2 o 5 Simplex.

[0051] (3) Ta obtained according to thermogravimetric 5+ The exact amount, according to the equation: 0.97LiOH·H 2 O+0.03MgO+0.485Ta 2 o 5 →Mg:LiTaO 3 Calculate Li + , The exact amount of MgO.

[0052] (4) Add 0.0707g LiOH·H to the Ta-MA solution 2 ...

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Abstract

The invention discloses a method for synthesizing a spherical lithium tantalate doped polycrystal raw material with even compositions. The method comprises the following steps that: tantalum source raw material is evenly mixed in an organic solvent containing a carboxylic group to form a coordination compound containing tantalum , the accurate content of the tantalum is calculated by a thermogravimetric analysis method, Li<+>, MgO or ZnO is added, the even mixing of the doped elements and the substrate material in the atom grade is realized by the magnetic stirring, the sprayer drying granulation technique is adopted to realize the control of the grain diameter of the polycrystal material, and the material is synthesized by the sintering process at a temperature lower than the solid phase reaction temperature. The polycrystal material synthesized by the method has the primary particle size in the nano scale, and the melting point which is evidently lower than the solid phase reactionpolycrystal material, thereby not only saving energy, but also realizing the automation of the lithium tantalate crystal growth by dopting the stoichiometry ratio as for the continuous feeding growthtechnology.

Description

technical field [0001] The invention relates to a synthesis method of doped lithium tantalate polycrystalline raw material, in particular to a synthesis method of spherical doped lithium tantalate polycrystalline raw material with uniform composition, belonging to the field of inorganic material preparation. Background technique [0002] Lithium tantalate is an excellent multifunctional crystal with excellent piezoelectric, photoelectric, pyroelectric and nonlinear optical properties. It can be used to make various functional devices. It is used as a Q-switching switch in laser technology, as a pyroelectric detector in infrared technology, and as a filter and resonator in the electronics industry. Since the near-stoichiometric lithium tantalate crystal is a natural single-domain single crystal with fewer defects, it has many advantages and wider uses, so it has become the focus of crystal growth research and development in the world. [0003] The near-stoichiometric lithium...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C30B29/30C30B29/60
Inventor 吴剑波夏宗仁郑斐斐秦晓勇朱怀列王继扬姚淑华颜涛刘宏
Owner CETC DEQING HUAYING ELECTRONICS
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