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Magnesium tantalate series crystals and preparation method thereof

A technology of crystal and orthorhombic crystal system, applied in the chemical industry, can solve the problems of poor quality and performance of magnesium tantalate crystals, and achieve the effect of solving the problem of easy cracking

Active Publication Date: 2021-03-19
SHANGHAI INST OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Aiming at the above-mentioned technical problems in the prior art, the present invention provides magnesium tantalate series crystals and a preparation method thereof. The magnesium tantalate series crystals and the preparation method thereof will solve the problems of preparing magnesium tantalate crystals in the prior art. Technical issues with poor quality and performance

Method used

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  • Magnesium tantalate series crystals and preparation method thereof
  • Magnesium tantalate series crystals and preparation method thereof
  • Magnesium tantalate series crystals and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Example 1 Growth of Mg by micro-pull down method 4 Ta 2 O 9 crystal

[0042] (1) Synthesis of high-purity Mg by solid-phase reaction 4 Ta 2 O 9 powder

[0043] 1) 5.2Mg(OH) 2 :1Ta 2 O 5 Synthetic pure phase Mg 4 Ta 2 O 9 powder

[0044] According to the molar ratio of 5.2:1, weigh out Mg(OH) with purities of 99.999% and 99.99%, respectively 2 and Ta 2 O 5 A total of 5g of raw materials were put into a mortar and mixed, sieved with 220 meshes, and put into ZrO 2 The balls were milled on a ball mill for 1 h in a ball milling jar. Under the action of a pressure of 350MPa, a cylindrical sheet with a size of Φ13mm×5mm was prepared, which was placed in a muffle furnace for pre-sintering at 1300°C for 16h, and the heating and cooling rate was 100°C / h. The phase purity of the obtained ceramic cylindrical sheet was obtained by powder XRD ( figure 2 (a)) Characterization.

[0045] 2) 5.6Mg(OH) 2 :1Ta 2 O 5 Synthetic pure phase Mg 4 Ta 2 O 9 powder

[00...

Embodiment 2

[0057] Example 2 Micro-pull-down method for growing Mg 3 Ta 2 O 8 crystal

[0058] The high-purity powder raw material Mg(OH) 2 (99.999%) and Ta 2 O 5 (99.99%) ingredients in a molar ratio of 4:1, put a total of 5g into a mortar and mix well, sieve with 220 mesh, and put it into a ZrO 2 In the ball-milling tank of the ball, the ball is milled on a ball mill for 1 hour, and the ball-milled material is ground again in a mortar, sieved with 220 mesh, and pressed into a cylindrical sheet with a size of Φ13mm×5mm at 350MPa, which is placed in a high-temperature muffle furnace. , set the pre-burning temperature to 1300°C, the holding time to 16h, and the temperature to rise and fall at a rate of 100°C / h. The phase purity of the obtained ceramic cylindrical sheet is characterized by powder XRD, and its spectral characteristics are as follows: Figure 7 (a). found no Mg 3 Ta 2 O 8 phase, is 0.62Mg 4 Ta 2 O 9 +0.38MgTa 2 O 6 Mixed phase, the composition of which is roug...

Embodiment 3

[0062] Example 3 Growth of MgTa by micro-pull-down method 2 O 6 crystal

[0063] The raw material Mg(OH) 2 (Noah chemical, 99.999%) and Ta 2 O 5 (Aldrich, 99.99%), weighed in a molar ratio of 1.15:1, mixed in a total of 5g mortar, sieved with 220 mesh, ball milled for 1h, under 350MPa to prepare a cylindrical sheet of Φ13mm×5mm, put it in a muffle furnace for 1400 ℃ pre-burning for 8h, 100℃ / h heating and cooling. Powder XRD, such as Figure 10 (a) shows that the obtained ceramic sheet is pure phase MgTa 2 O 6 . The synthesized pure phase MgTa 2 O 6 Powder and Mg(OH) 2 The powder is ball-milled and mixed at a molar ratio of 100:1, and a total of 5g is dry-pressed into a column with a diameter of 13mm. figure 1 The Ir crucible shown, with Y 3 Al 5 O 12 (referred to as YAG) single crystal rod as the seed crystal, the upper end of the seed crystal is cut flat and polished, and kept clean and dry, fixed in the hollow Al 2 O 3 on the seed rod. Adjust various compon...

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Abstract

The invention discloses magnesium niobate series crystals, namely a MgO-Ta2O5 pseudo binary system. The magnesium niobate series crystals are Mg4Ta2O9, Mg3Ta2O8 and MgTa2O6, respectively. A method forpreparing the magnesium niobate series crystals is also provided. High-purity MgTa2O6 and Mg4Ta2O9 powders are synthesized by solid phase reaction using excess MgO or Mg(OH)2 component compensation,and the centimeter-scale rod-shaped MgTa2O6 and Mg4Ta2O9 single crystal is grown by a micro-downdraw method. Using Mg4Ta2O9 and MgTa2O6 as melting starting materials, a centimeter-scale rod-shaped Mg3Ta2O8 single crystal is grown on a MgTa2O6 ceramic seed rod by a spontaneous nucleation technique. According to the magnesium niobate series crystals, the micro-downdraw method is adopted, and the high temperature gradient near a growth interface is effectively utilized, to achieve rapid and high uniform crystallization; and a post-heater is effectively utilized to solve the cracking problem caused by excessive thermal stress.

Description

technical field [0001] The invention belongs to the field of chemical industry, and relates to a microwave dielectric material, in particular to magnesium tantalate series crystals and a preparation method thereof. Background technique [0002] With the rapid development of microwave communication, modern mobile phones and electronic communication, microwave dielectric materials, which play an important role in the communication system, have received great attention from scientific researchers and technology industry manufacturers. Mg 4 Ta 2 O 9 , Mg 3 Ta 2 O 8 , MgTa 2 O 6 and its doped materials, which have excellent microwave dielectric properties and luminescence properties, have been widely studied in the form of ceramics and powders, respectively. In order to explore MgO-Ta in depth 2 O 5 The microwave dielectric, optical and other intrinsic properties of the system materials and their changing laws with the composition, structure and crystal orientation have...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C30B29/30C30B15/08
CPCC30B15/08C30B29/30
Inventor 马云峰徐家跃蒋毅坚
Owner SHANGHAI INST OF TECH
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