Highly doped batio3:fe multiferroic thin film material and preparation method thereof

A multiferroic thin film and high doping technology, applied in the field of material science, can solve the problems of unfavorable large-scale production, complicated preparation process, expensive equipment, etc., and achieve the effect of high unidirectionality, uniform and dense surface, and good crystallization performance

Inactive Publication Date: 2017-10-10
HENAN UNIVERSITY
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Problems solved by technology

The equipment of the first three preparation methods is expensive, and the preparation process is complicated, which is not conducive to large-scale production; and in the preparation process of the existing sol-gel method, either expensive raw materials such as ferric alcohol [J Mater Chem 16,1626,2006], Iron isopropoxide [J Appl Phys 88, 1008, 2000] and methylferrocenemethanol [US Patent 7795663B2], or use a more toxic solvent such as diethanolamine [US Patent 7795663B2], or the iron doping amount does not exceed 1% [Mater Lett63, 2622, 2009]

Method used

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  • Highly doped batio3:fe multiferroic thin film material and preparation method thereof
  • Highly doped batio3:fe multiferroic thin film material and preparation method thereof
  • Highly doped batio3:fe multiferroic thin film material and preparation method thereof

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preparation example Construction

[0029] The invention provides a method for growing highly doped BaTiO on a suitable substrate 3 The preparation method of the film material of Fe comprises the following steps successively:

[0030] 1. Film preparation:

[0031] 1) Precursor solution. Fe source, Ba source and Ti source are dissolved in solvents such as acetylacetone, alcohol and organic acid and fully stirred to become clear; in addition, in order to enable the solution to be stored for a long time and improve the quality of film formation, add an appropriate amount of ethylene glycol or a suitable concentration of ethylene glycol and For the ethanol solution of polyvinylpyrrolidone (PVP), the content x of Fe in the precursor ranges from 0.01 to 0.4.

[0032] Below, Fe(NO 3 ) 3 9H 2 O is the source of Fe, barium acetate is the source of Ba, tetrabutyl titanate is the source of titanium, acetic acid and acetylacetone are solvents, ethylene glycol and PVP solution are additives, and BaTiO is doped with Fe w...

Embodiment 1

[0041] This example is in LaNiO 3 / Grow x=0.15 highly doped BaTiO on Si substrate 3 : The preparation process of Fe thin film material and its room temperature magnetic and ferroelectricity test.

[0042] 1. Film preparation

[0043] 1. Preparation of precursor solution. The Fe(NO 3 ) 3 9H 2 O, dissolving barium acetate powder in glacial acetic acid, stirring at 80°C for 90 minutes at a stirring rate of 500 rpm to completely dissolve ferric nitrate and barium acetate, then cooling to room temperature and adding acetylacetone and ethanol with a volume ratio of 10:1 ~1:1 mixed solution, continue to stir for 30 minutes, slowly add tetrabutyl titanate ethanol solution in the temperature range of room temperature to 80°C, and continue to stir for 2 hours. Then add ethylene glycol to adjust the viscosity of the solution so that the concentration of Ba ions in the solution is 0.3mol / L. Stirring was continued at room temperature for 60 minutes at a stirring rate of 600 rpm. A ...

Embodiment 2

[0057] This embodiment is to grow x=0.10 highly doped BaTiO on the quartz substrate 3 : The preparation process of Fe thin film material and its XRD and transmission spectrum test.

[0058] 1. Preparation of precursor solution. The Fe(NO 3 ) 3 9H 2 O, dissolving barium acetate powder in glacial acetic acid, stirring at 100°C for 60 minutes at a stirring rate of 600 rpm, completely dissolving ferric nitrate and barium acetate, then cooling to room temperature and adding acetylacetone and ethanol with a volume ratio of 10:1 ~1:1 mixed solution, continue to stir for 20 minutes, slowly add tetrabutyl titanate ethanol solution in the temperature range of room temperature to 80°C, and continue to stir for 2 hours. Then add ethylene glycol to adjust the viscosity of the solution so that the concentration of Ba ions in the solution is 0.25mol / L. Stirring was continued at room temperature for 60 minutes at a stirring rate of 600 rpm. A brown-red clear and transparent solution was...

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Abstract

The invention relates to a high-Fe-content doped BaTiO3 multiferroic thin-film material and a preparation method thereof. The molecular formula of the high-Fe-content doped BaTiO3 multiferroic thin-film material is BaTi<1-x>FexO3, wherein x is the atomic ratio of doped components and ranges from 0.01 to 0.4. The preparation method sequentially includes the steps that (1) a precursor is prepared; (2) a substrate is cleaned and pretreated; (3) a highly doped BaTiO3:Fe multiferroic thin film is prepared, specifically, the substrate obtained in the step (2) is spin-coated with the highly doped BaTiO3:Fe sol precursor prepared in the step (1), and then stepped annealing is conducted on the precursor; and (4) the sol coating and annealing processes of the step (3) are repeated, and a thin film sample of a needed thickness is obtained. A precursor solution is clear and transparent and can be stored for a long time; the grown thin film is uniform and compact in surface, good in crystallization property and free of impurity phases, and the grown thin film is good in thickness controllability and high in unipolarity; and the thin-film material has good ferroelectricity and ferromagnetism at the room temperature.

Description

technical field [0001] The invention relates to a high Fe content doped BaTiO 3 A multiferroic thin film material and a preparation method thereof belong to the field of material science. Background technique [0002] BaTiO 3 It is a material with photovoltaic, piezoelectric, ferroelectric, electro-optic and nonlinear optical properties, and has practical and potential applications in memory, photovoltaic and light detection. By doping, BaTiO 3 Certain properties of the can be improved and improved. Fe is an important doping element, Fe doped BaTiO 3 It is a potential new multiferroic material with both ferroelectricity and ferromagnetism. Currently, Fe-doped BaTiO 3 The preparation methods of thin films include pulsed laser deposition, magnetron sputtering, chemical vapor deposition and sol-gel method and so on. The equipment of the first three preparation methods is expensive, and the preparation process is complicated, which is not conducive to large-scale producti...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C23C18/16H01F41/22H01F41/24
CPCC23C18/1694H01F41/22H01F41/24
Inventor 田建军高惠平田军锋范素娟秦勉贾彩虹郑海务张伟风
Owner HENAN UNIVERSITY
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