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Tb, Mn and Ni ternary co-doped low leakage current BiFeO3 film and preparation method thereof

A technology of leakage current and co-doping, applied in chemical instruments and methods, inorganic chemistry, iron compounds, etc., can solve the problems of low dielectric constant, low resistivity, large leakage current, etc., to improve the performance of multiferroics, improve Effect of magnetic properties and enhanced insulation

Active Publication Date: 2015-06-24
盐城市鹤业实业投资有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Fluctuations in the valence state of Fe lead to a large leakage conductance, making BiFeO 3 The leakage current is large, and due to the large leakage conduction, the ferroelectricity cannot be measured correctly and saturation polarization is obtained
On the other hand, BiFeO 3 The properties of low dielectric constant and low resistivity make it difficult to observe the electric hysteresis loop. These characteristics greatly limit the performance of BiFeO. 3 Film application

Method used

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  • Tb, Mn and Ni ternary co-doped low leakage current BiFeO3 film and preparation method thereof
  • Tb, Mn and Ni ternary co-doped low leakage current BiFeO3 film and preparation method thereof
  • Tb, Mn and Ni ternary co-doped low leakage current BiFeO3 film and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] 1) Bi(NO 3 ) 3 ·5H 2 O, Fe(NO 3 )3 9H 2 O, Tb(NO 3 ) 3 ·6H 2 O, C 4 h 6 MnO 4 4H 2 O and C 4 h 6 NiO 4 4H 2 O is dissolved in the mixed solution formed by mixing ethylene glycol methyl ether and acetic anhydride at a molar ratio of 0.94:0.95:0.11:0.04:0.01, and then stirred for 2 hours to make it uniform to obtain BiFeO 3 Precursor; Among them, BiFeO 3 The total metal ion concentration in the precursor solution is 0.3mol / L; the volume ratio of ethylene glycol methyl ether and acetic anhydride in the mixed solution is 3:1;

[0025] 2) BiFeO 3 The precursor solution was left to stand for 24h, and then spin-coated BiFeO on the FTO / glass substrate 3 The wet film was prepared from the precursor solution, and the wet film was baked at 200°C for 6 minutes to obtain a dry film, and then rapidly annealed at 550°C for 8 minutes to obtain crystalline BiFeO 3 film.

[0026] 3) To be crystalline BiFeO 3 After film cooling, repeat step 2) to make crystalline BiFeO...

Embodiment 2

[0028] 1) Bi(NO 3 ) 3 ·5H 2 O, Fe(NO 3 ) 3 9H 2 O, Tb(NO 3 ) 3 ·6H 2 O, C 4 h 6 MnO 4 4H 2 O and C 4 h 6 NiO 4 4H 2 O was dissolved in the mixed solution of ethylene glycol methyl ether and acetic anhydride at a molar ratio of 0.94:0.94:0.11:0.04:0.02, and stirred for 2 hours to make it uniform, to obtain BiFeO 3 Precursor; Among them, BiFeO 3 The total metal ion concentration in the precursor solution is 0.3mol / L; the volume ratio of ethylene glycol methyl ether and acetic anhydride in the mixed solution is 3:1;

[0029] 2) BiFeO 3 The precursor solution was left to stand for 32h, and then spin-coated BiFeO on the FTO / glass substrate 3 The wet film was prepared from the precursor solution, and the wet film was baked at 200°C for 12 minutes to obtain a dry film, and then rapidly annealed at 550°C for 10 minutes to obtain crystalline BiFeO 3 film;

[0030] 3) To be crystalline BiFeO 3 After film cooling, repeat step 2) again until crystalline BiFeO 3 The f...

Embodiment 3

[0037] 1) Bi(NO 3 ) 3 ·5H 2 O, Fe(NO 3 ) 3 9H 2 O, Tb(NO 3 ) 3 ·6H 2 O, C 4 h 6 MnO 4 4H 2 O and C 4 h 6 NiO 4 4H 2 O was dissolved in the mixed solution of ethylene glycol methyl ether and acetic anhydride in a molar ratio of 0.97:0.94:0.08:0.04:0.02, and stirred for 2 hours to make it uniform, to obtain BiFeO 3 Precursor; Among them, BiFeO 3 The total metal ion concentration in the precursor solution is 0.1mol / L; the volume ratio of ethylene glycol methyl ether and acetic anhydride in the mixed solution is 4:1;

[0038] 2) BiFeO 3 The precursor solution was left to stand for 28h, and then spin-coated BiFeO on the FTO / glass substrate 3 The wet film was prepared from the precursor solution, and the wet film was baked at 180°C for 8 minutes to obtain a dry film, and then rapidly annealed at 550°C for 13 minutes to obtain crystalline BiFeO 3 film;

[0039] 3) To be crystalline BiFeO 3 After film cooling, repeat step 2) again until crystalline BiFeO 3 The fi...

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Abstract

The invention discloses a Tb, Mn and Ni ternary co-doped low leakage current BiFeO3 film and a preparation method thereof. The preparation method of the Tb, Mn and Ni ternary co-doped low leakage current BiFeO3 film comprises the following steps: dissolving bismuth nitrate, ferric nitrate, terbium nitrate, manganese acetate and nickel acetate in a molar ratio of (0.91-0.97): (0.96-x): (0.08-0.14): 0.04:x in mixed liquor formed by mixing ethylene glycol methyl ether and acetic anhydride, then uniformly stirring to obtain BiFeO3 precursor liquor, wherein x is equal to 0.01-0.02; coating the BiFeO3 precursor liquor on an FTO (Fluorine-doped Tin Oxide) / glass substrate in a rotary manner to prepare a wet film, roasting the wet film to obtain a dry film, then, annealing for 8 minutes-13 minutes at 550 DEG C to obtain a crystalline-state BiFeO3 film; after the crystalline-state BiFeO3 film is cooled, repeating the annealing, so that the crystalline-state BiFeO3 film reaches needed thickness to obtain the Tb, Mn and Ni ternary co-doped low leakage current BiFeO3 film. The preparation method disclosed by the invention is simple in device requirement, suitable for preparing the film on a large surface and the surface with an irregular shape; moreover, chemical components are precise and controllable, electrical performance of the film can be improved, leakage current density of the BiFeO3 under 350 kV / cm test electric fields is kept below 10<-5>A / cm<2>, and dielectric constant under test frequency of 100 kHz is 240-270.

Description

technical field [0001] The invention belongs to the field of functional materials, in particular to a low leakage current BiFeO ternary co-doped with Tb, Mn and Ni 3 Thin films and methods for their preparation. Background technique [0002] In recent years, BiFeO 3 As the representative multiferroic compound system, a worldwide research boom of single-phase multiferroic magnetoelectric materials has been formed. It has both ferroelectric order and antiferromagnetic order at room temperature, due to its high ferroelectric phase transition temperature (T C =1103K) and magnetic phase transition temperature (T N =643K). Therefore BiFeO 3 It has become an important functional material that can be widely used in the fields of microelectronics, optoelectronics, integrated optics and microelectromechanical systems. [0003] BiFeO 3 The biggest problem with thin films is their low resistivity, which makes it impossible to measure their ferroelectric properties at room tempera...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G49/00
Inventor 谈国强董国华罗洋洋
Owner 盐城市鹤业实业投资有限公司
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