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A kind of lanthanide rare earth ion-doped bismuth titanate single crystal flake and preparation method thereof

A lanthanide rare earth and ion doping technology is applied in the field of lanthanide rare earth ion doped bismuth titanate single crystal flakes and the preparation thereof, which can solve the problem that Bi salts are prone to hydrolysis side reactions, and it is difficult to obtain bismuth titanate series materials. and other problems to achieve the effect of avoiding hydrolysis reaction, large size, and avoiding the formation of impurity phase

Inactive Publication Date: 2016-06-08
XIANGTAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Bismuth titanate doped with lanthanide rare earth ions is a ferroelectric material with a complex bismuth layered perovskite structure. In the preparation of bismuth titanate or other ion-doped bismuth titanate and other titanium by liquid phase method, especially hydrothermal method Bismuth titanate series micro-nano materials, because the reaction medium contains a large amount of water, Bi salt is prone to hydrolysis side reactions, so that the product contains Bi2O3 or pyrochlore phase Bi2Ti2O7 and other impurities, it is difficult to obtain pure-phase bismuth titanate series materials
At present, some bismuth titanate series micro-nano materials have been prepared, but it needs to go through a cumbersome co-precipitation process to remove impurity ions, or add additives to obtain pure-phase bismuth titanate series materials

Method used

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  • A kind of lanthanide rare earth ion-doped bismuth titanate single crystal flake and preparation method thereof
  • A kind of lanthanide rare earth ion-doped bismuth titanate single crystal flake and preparation method thereof
  • A kind of lanthanide rare earth ion-doped bismuth titanate single crystal flake and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment example 1

[0021] The first step: Weigh bismuth nitrate pentahydrate, neodymium nitrate and butyl titanate according to the molar ratio of 3.15:0.85:3, first dissolve bismuth nitrate pentahydrate and neodymium nitrate in ethylene glycol methyl ether, and then pour them into Add butyl titanate to prepare 16ml, 0.02mol / L Bi3.15Nd0.85Ti3O12 precursor solution;

[0022] Step 2: Dissolve 2mol / L sodium hydroxide in deionized water to prepare 4ml aqueous sodium hydroxide solution;

[0023] The third step: Add the solution in the second step to the Bi3.15Nd0.85Ti3O12 precursor solution in the first step to obtain a precipitate. After stirring the precipitate evenly, put it into the reactor and heat it to 160°C for 30 hours. The reaction is complete After cooling down to room temperature naturally, the bottom black precipitate was washed with distilled water and ethanol several times, and dried in a vacuum oven at 80°C for 12 hours to obtain Nd-doped bismuth titanate single crystal flakes.

Embodiment example 2

[0025] The first step: according to the molar ratio of 3.54:0.46:3, weigh bismuth nitrate pentahydrate, neodymium nitrate and butyl titanate, first dissolve bismuth nitrate pentahydrate and neodymium nitrate in ethylene glycol methyl ether, and then add them Add butyl titanate to prepare 15ml, 0.05mol / L Bi3.54Nd0.46Ti3O12 precursor solution;

[0026] Step 2: Dissolve 3mol / L sodium hydroxide in deionized water to prepare 5ml aqueous sodium hydroxide solution;

[0027] The third step: Add the solution in the second step to the solution in the first step to obtain a precipitate. After stirring the precipitate evenly, put it into a reaction kettle and heat it to 180°C for 25 hours. After the reaction is completed, cool it down to room temperature naturally. The bottom black precipitate was washed with distilled water and ethanol several times, and dried in a vacuum drying oven at 80°C for 12 hours to obtain neodymium-doped bismuth titanate single crystal flakes.

Embodiment example 3

[0029] The first step: according to the molar ratio of 3.7:0.3:3, weigh bismuth nitrate pentahydrate, neodymium nitrate and butyl titanate, first dissolve bismuth nitrate pentahydrate and neodymium nitrate in ethylene glycol methyl ether, and then add Add butyl titanate to it to prepare 14ml, 0.1mol / L Bi3.7Nd0.3Ti3O12 precursor solution;

[0030] Step 2: Dissolve 4mol / L sodium hydroxide in deionized water to prepare 6ml aqueous sodium hydroxide solution;

[0031] The third step: Add the solution in the second step to the solution in the first step to obtain a precipitate. After stirring the precipitate evenly, put it into a reaction kettle and heat it to 200°C for 20 hours. After the reaction is completed, cool it naturally to room temperature, and take The bottom black precipitate was washed with distilled water and ethanol several times, and dried in a vacuum drying oven at 80°C for 12 hours to obtain neodymium-doped bismuth titanate single crystal flakes.

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Abstract

The invention discloses a lanthanide rare earth ion doped bismuth titanate monocrystal thin slice and a preparation method thereof. The lanthanide rare earth ion doped bismuth titanate monocrystal thin slice is 5-10 microns in length and 50-200nm in thickness. The preparation method comprises the following steps of: 1, preparing a lanthanide rare earth ion doped bismuth titanate precursor solution by adopting ethylene glycol monomethyl ether as a solvent according to an element molar ratio of Bi:R:Ti=(4-x):x:3 in a formula Bi4-xRxTi3O12 (R is a lanthanide rare earth element, and x is more than 0 and is less than or equal to 1.5); 2, adding an NaOH aqueous solution into the precursor solution, and then filtering to obtain a deposit; and 3, uniformly stirring the deposit, heating the deposit in a reaction kettle, and cleaning and drying a product after reaction to obtain the lanthanide rare earth ion doped bismuth titanate monocrystal thin slice. According to the preparation method, an organic solvent is used as a main reaction medium, and a hydrolysis reaction caused by a lot of water is effectively avoided, so that the generation of an impurity phase is avoided. The lanthanide rare earth ion doped bismuth titanate monocrystal thin slice prepared by the preparation method is large in size and high in purity without the generation of the impurity phase.

Description

technical field [0001] The invention belongs to the field of inorganic chemistry, and in particular relates to a bismuth titanate single crystal flake doped with lanthanide rare earth ions and a preparation method thereof. Background technique: [0002] With the advancement of science and technology and the miniaturization trend of electronic devices, ferroelectric micro-nano materials have been paid attention to. Micro-nanomaterials have physical and chemical properties different from their bulk materials, and these physical and chemical properties depend to a large extent on the size and morphology of the material. Lanthanide rare earth ions (such as La3+, Nd3+, Pr3+, Sm3+, Eu3+, etc.) doped bismuth titanate materials have large remnant polarization, good fatigue resistance, high Curie temperature and low heat treatment temperature. The most promising new lead-free ferroelectric materials to replace traditional lead-based ferroelectrics. At present, there are many method...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C30B7/14C30B29/32
Inventor 王金斌王芳钟向丽李波廖敏谭丛兵
Owner XIANGTAN UNIV
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