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Process of synthesizing spherical doped polycrystalline lithium niobate material with homogeneous component

A synthesis method, technology of lithium niobate, applied in the direction of polycrystalline material growth, lithium compounds, chemical instruments and methods, etc., can solve the problems that are not easy to control, impossible to realize, and powder is not suitable, so as to prevent floating crystals and realize Automated and energy-saving effects

Inactive Publication Date: 2009-12-02
SHANDONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This method cannot achieve the doping of high melting point raw materials such as magnesium oxide or zinc oxide.
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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  • Process of synthesizing spherical doped polycrystalline lithium niobate material with homogeneous component
  • Process of synthesizing spherical doped polycrystalline lithium niobate material with homogeneous component

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Synthesis of MgO(5mol%) Stoichiometric Lithium Niobate Polycrystalline Materials

[0035] 1. Weigh Nb(OH) 5 2.460g was heated and dissolved with concentrated hydrochloric acid 12ml to obtain highly active Nb 2 o 5 ·nH 2 O, add DL-malic acid (C 4 h 6 o 5 , DL-MA) 2.674g, adjusted to pH=7 with ammonia water (30%), and filtered to obtain a clear and transparent Nb-MA solution.

[0036] 2. Use thermogravimetric analysis to test the true concentration of the solution: take 10.856g of Nb-MA solution and calcinate at 700°C for 2h, and weigh the actual concentration of the solution to obtain: 0.01566gNb 2 o 5 / g solution, X-ray diffraction results show that the powder obtained by calcination is Nb 2 o 5 Simplex( figure 1 ).

[0037] 3. According to the equation:

[0038] LiOH·H 2 O+0.05MgO+0.49Nb 2 o 5 →LiNb 0.98 Mg 0.05 o 3 +1.5H 2 O Add 0.131g LiOH·H to the Nb-MA solution according to the data calculated by thermogravimetry 2 O, 0.006gMgO, stirred until co...

Embodiment 2

[0041] Embodiment 2: the synthesis of MgO (5mol%) doped near-stoichiometric lithium niobate polycrystalline material

[0042] 1. From the compound Nb(OH) of niobium 5 3.776g was heated and dissolved with concentrated hydrochloric acid 18ml to obtain highly active Nb 2 o 5 ·nH 2 O, add citric acid (C 6 h 8 o 7 , citric acid) 1.117g in ammonia water (30%) to adjust the pH value to 8, and filter to obtain a clear and transparent Nb-CA solution.

[0043] 2. Take a small amount of Nb-CA solution 9.361g for thermogravimetric analysis calculation: 0.01517gNb 2 o 5 / g solution, X-ray diffraction results show that the obtained powder is Nb 2 o 5 Simplex.

[0044] 3. According to the equation:

[0045] LiOH·H 2 O+0.05MgO+0.49Nb 2 o 5 →LiNb 0.98 Mg 0.05 o 3 +1.5H 2 O add 0.478g LiOH·H to the Nb-CA solution according to the data calculated by thermogravimetry 2 O, 0.047gMgO, stirred until completely dissolved in the solution.

[0046] 4. The solution is granulated by s...

Embodiment 3

[0047] Embodiment 3: the synthesis of MgO (5mol%) doped near-stoichiometric lithium niobate polycrystalline material

[0048] 1. Put niobium chloride NbCl 5 2.994g was dissolved in 25ml water and stirred for 12 hours to obtain highly active Nb 2 o 5 ·nH 2 O, and DL-malic acid (C 4 h 6 o 5 , DL-MA) 3.674g was adjusted in ammonia water (30%) to pH=7, and filtered to obtain a clear and transparent Nb-MA solution.

[0049] 2. Take a small amount of Nb-MA solution 12.245g for thermogravimetric analysis calculation: 0.0236gNb 2 o 5 / g solution, X-ray diffraction results show that the obtained powder is Nb 2 o 5 Simplex.

[0050] 3. According to the equation:

[0051] LiOH·H 2 O+0.05MgO+0.49Nb 2 o 5 →LiNb 0.98 Mg 0.05 o 3 +1.5H 2 O add 0.384g LiOH·H to the Nb-MA solution according to the thermogravimetric calculation data 2 O, 0.018gMgO, stirred until completely dissolved in the solution.

[0052] 4. Granulate the solution through spray drying equipment;

[0053]...

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Abstract

The invention relates to a method for synthesizing spherical doped lithium niobate polycrystalline raw materials with uniform composition, belonging to the field of inorganic material preparation. In this method, the niobium source raw materials are uniformly mixed in an organic solvent containing carboxylic acid groups to form a niobium-containing complex, and the accurate amount of niobium is calculated by thermogravimetric analysis, and then Li+, MgO, ZnO or HfO2 is added, and magnetic stirring is realized. Doping elements and matrix materials are uniformly mixed at the atomic level, and the solution is spray-dried and granulated to control the particle size of the polycrystalline material, and the polycrystalline material with a certain particle size is synthesized by calcining at a temperature lower than the solid-state reaction. The raw materials used in the invention are conventional materials, and the mixing in the solution can help improve the uniformity of the crystal, control the particle size, and broaden the application range of the crystal growth.

Description

(1) Technical field [0001] The invention relates to a method for synthesizing spherical doped lithium niobate polycrystalline raw materials with uniform composition, belonging to the field of inorganic material preparation. (2) Background technology [0002] Lithium niobate is an excellent multifunctional crystal with good piezoelectric properties, nonlinear optical properties, electro-optic and photorefractive properties, etc. It can be used to make various functional devices, such as: infrared detectors, laser modulators, optical switches, optical parametric oscillators, integrated optical components, high-frequency broadband filters, high-frequency high-temperature transducers, micro-acoustic devices, laser multipliers Frequency converters, self-frequency doubling lasers, photorefractive devices (such as high-resolution holographic storage), etc. Due to the wide range of applications and large dosage of lithium niobate crystals, the production of lithium niobate crystals...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B33/00C01D15/00C30B29/30
Inventor 王继扬姚淑华刘宏郑斐斐颜涛
Owner SHANDONG UNIV