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Method for preparing barium calcium columbate column-like monocrystal particles

A technology of single crystal particles and barium niobate, which is applied in the direction of single crystal growth, single crystal growth, chemical instruments and methods, etc., can solve the problems of high preparation temperature, complicated preparation process, and restrictions on the wide application of barium calcium niobate

Inactive Publication Date: 2007-11-14
NORTHWESTERN POLYTECHNICAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The prepared barium calcium niobate is a single crystal, and the preparation process is complicated, the preparation temperature is as high as 1150 ℃ ~ 1250 ℃, and the preparation cycle is as long as more than 15 hours, which still limits the wide application of barium calcium niobate

Method used

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  • Method for preparing barium calcium columbate column-like monocrystal particles

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Experimental program
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Effect test

Embodiment 1

[0014] Embodiment 1, get analytically pure CaCO 3 0.7778g, analytically pure BaCO 3 3.5781g, analytically pure Nb 2 o 5 6.8852g is put into the ball mill jar that agate ball is housed, with absolute ethanol as dispersion medium, dry after ball milling 10 hours. Take 22.4g of the dried powder and mix it with 22.4g of analytically pure KCl, use ethanol as the medium, put it into a ball mill jar equipped with agate balls and mix for 16 hours, mix evenly and then dry. Put the dried powder in a closed alumina crucible and calcinate it at 1150°C for 3h to synthesize it. The obtained powder was washed repeatedly with deionized water at 80°C until the filtrate could not detect Cl with silver nitrate reagent. - until. Barium calcium niobate columnar single crystal particles are obtained after drying. It can be clearly seen from Fig. 1 that a pure phase of barium calcium niobate was synthesized at 1050 °C. It can be clearly seen from the photomicrograph in Fig. 2 that the prepa...

Embodiment 2

[0015] Embodiment 2, get analytically pure CaCO 3 0.7778g, analytically pure BaCO 3 3.5781g, analytically pure Nb 2 o 5 6.8852g is put into the ball mill jar that agate ball is housed, with absolute ethanol as dispersion medium, dry after ball milling 8 hours. Take 22.4g of the dried powder and mix it with 44.8g of analytically pure KCl, use ethanol as the medium, put it into a ball mill jar equipped with agate balls and mix for 20h, mix evenly and then dry. Put the dried powder in a closed alumina crucible and calcinate it at 1150°C for 4h to synthesize it. The obtained powder was washed repeatedly with deionized water at 90°C until the filtrate could not detect Cl with silver nitrate reagent. - until. Barium calcium niobate columnar single crystal particles are obtained after drying.

Embodiment 3

[0016] Embodiment 3, get analytically pure CaCO 3 1.1667g, analytically pure BaCO 3 5.3672g, analytically pure Nb 2 o 5 10.3278g is put into the ball mill jar that agate ball is housed, with absolute ethanol as dispersion medium, dry after ball milling 11 hours. Take 33.72g of the dried powder and mix it with 33.72g of analytically pure KCl, use ethanol as the medium, put it into a ball mill jar equipped with agate balls and mix for 26 hours, mix evenly and then dry. Put the dried powder in a closed alumina crucible and calcinate at 950°C for 5h to synthesize. The obtained powder was repeatedly washed with deionized water at 95°C until the filtrate could not detect Cl with silver nitrate reagent. - until. Barium calcium niobate columnar single crystal particles are obtained after drying. It can be clearly seen from Figure 1 that a pure phase of barium calcium niobate has been synthesized at 950°C.

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Abstract

The present invention discloses a barium niobate crystal particles of calcium columnar preparation methods, its features include the following steps: from bansichun CaCO3, BaCO3, and Nb2O5, according to a chemical-Ca0.3Ba0.7Nb2O6 ingredients, and then release all equipped with agate ball milling in the tank with anhydrous ethanol as the dispersion medium, milling 8-12 hours after drying; to the powder after drying KCl which has a 1:1 or 1:2 ratio of mixing, ethanol for the media, with agate Add to pot the ball milling in mixed 16 to 26 hours after drying evenly mixed; to the powder after drying confined on the alumina crucible, in the 950 -1150 degree C calcinations temperature of 3 to 6 hours; to the calcite powders synthesis of 80 -100 degree C with the deionized water repeatedly washed until the filtrate with silver nitrate test for less than Cl-, the drying. Compared with the existing technology, the preparation temperature from 1150 to 1250degree C and lowed it to 950 degree C-1150 degree C, preparation cycle from more than 15 hours to 3 to 6 hours, and barium niobate prepared for the columnar crystal particles of calcium.

Description

technical field [0001] The invention relates to a preparation method of barium calcium niobate columnar single crystal particles. Background technique [0002] Literature "Growth, dielectric, ferroelectric and optical properties of Ca 0.28 Ba 0.72 Nb 2 o 6 singlecrystals", J.Crystal Growth, 2006, 290 (2): 431-435 " discloses a barium calcium niobate single crystal Ca x Ba 1-x Nb 2 o 6 (x=0.28 abbreviated CBN28) preparation method, and pointed out that the prepared barium calcium niobate has excellent optical properties similar to strontium barium niobate, and compared with the phase transition temperature of strontium barium niobate 79 ℃, its 265 ℃ The phase transition temperature makes barium calcium niobate have a wider application range. [0003] The prepared barium calcium niobate is a single crystal, and the preparation process is complex, the preparation temperature is as high as 1150°C-1250°C, and the preparation cycle is as long as 15 hours or more, which st...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C30B29/30
Inventor 樊慧庆王炜
Owner NORTHWESTERN POLYTECHNICAL UNIV