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Method for preparing high-remanent-polarization BiFeO3 film with preferentially growing (110) crystal face by sol-gel process

A technology of sol-gel method and polarization strength, which is applied in the direction of single crystal growth, crystal growth, single crystal growth, etc., can solve the problem that ferroelectricity cannot be correctly measured for saturation polarization, it is difficult to observe hysteresis loops, and low Dielectric constant and other issues, to achieve the effect of aggravated structural distortion, easy control, and improved ferroelectric performance

Active Publication Date: 2013-04-24
SHAANXI UNIV OF SCI & TECH
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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 hysteresis loop
These characteristics greatly limit its application

Method used

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  • Method for preparing high-remanent-polarization BiFeO3 film with preferentially growing (110) crystal face by sol-gel process
  • Method for preparing high-remanent-polarization BiFeO3 film with preferentially growing (110) crystal face by sol-gel process

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Step 1: Bi(NO 3 ) 3 ·5H 2 O, Fe(NO 3 ) 3 9H 2 O, Nd(NO 3 ) 3 ·6H 2 O and Co(NO 3 ) 2 ·6H 2 O was dissolved in a mixture of ethylene glycol methyl ether and acetic anhydride at a molar ratio of 0.90:0.99:0.15:0.01, and magnetically stirred for 2 hours to obtain a stable metal ion concentration of 0.3mol / L BiFeO 3 Precursor solution, wherein the volume ratio of ethylene glycol methyl ether and acetic anhydride is 3:1.

[0016] Step 2: Spin-coat BiFeO on FTO / glass substrate by spin-coating method 3 Precursor solution to prepare film, uniform glue at 4000r / min for 15s, after the glue is finished, bake at 200°C for 10~15min to get a dry film, then quickly anneal at 550°C for 6~8min, cool down naturally, repeat the above process to get the desired thickness film.

[0017] In crystalline BiFeO 3 Preparation of 0.502mm thin film surface by ion sputtering 2 The Au electrode is kept at 300°C for 20 minutes to make the electrode and the substrate fully contact. Det...

Embodiment 2

[0019] Step 1: Bi(NO 3 ) 3 ·5H 2 O, Fe(NO 3 ) 3 9H 2 O, Nd(NO 3 ) 3 ·6H 2 O and Co(NO 3 ) 2 ·6H 2 O is dissolved in a mixture of ethylene glycol methyl ether and acetic anhydride at a molar ratio of 0.90:0.98:0.15:0.02, and magnetically stirred for 2 hours to obtain a stable metal ion concentration of 0.3mol / L BiFeO 3 Precursor solution, wherein the volume ratio of ethylene glycol methyl ether and acetic anhydride is 3:1.

[0020] Step 2: Spin-coat BiFeO on FTO / glass substrate by spin-coating method 3 Precursor solution to prepare film, uniform glue at 4000r / min for 15s, after the glue is finished, bake at 200°C for 10~15min to get a dry film, then quickly anneal at 550°C for 6~8min, cool down naturally, repeat the above process to get the desired thickness film.

[0021] In crystalline BiFeO 3 Preparation of 0.502mm thin film surface by ion sputtering 2 The Au electrode is kept at 300°C for 20 minutes to make the electrode and the substrate fully contact. Dete...

Embodiment 3

[0023] Step 1: Bi(NO 3 ) 3 ·5H 2 O, Fe(NO 3 ) 3 9H 2 O, Nd(NO 3 ) 3 ·6H 2 O and Co(NO 3 ) 2 ·6H 2 O is dissolved in a mixture of ethylene glycol methyl ether and acetic anhydride at a molar ratio of 0.90:0.97:0.15:0.03, and magnetically stirred for 2 hours to obtain a stable metal ion concentration of 0.3mol / L BiFeO 3Precursor solution, wherein the volume ratio of ethylene glycol methyl ether and acetic anhydride is 3:1.

[0024] Step 2: Spin-coat BiFeO on FTO / glass substrate by spin-coating method 3 Precursor solution to prepare film, uniform glue at 4000r / min for 15s, after the glue is finished, bake at 200°C for 10~15min to get a dry film, then quickly anneal at 550°C for 6~8min, cool down naturally, repeat the above process to get the desired thickness film.

[0025] In crystalline BiFeO 3 Preparation of 0.502mm thin film surface by ion sputtering 2 The Au electrode is kept at 300°C for 20 minutes to make the electrode and the substrate fully contact. Deter...

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Abstract

The invention provides a method for preparing a high-remanent-polarization BiFeO3 film with preferentially growing (110) crystal face by a sol-gel process, which comprises the following steps: dissolving bismuth nitrate, ferric nitrate, neodymium nitrate and cobalt nitrate used as raw materials in a mol ratio of 0.90:(1-x):0.15:x (x=0.01-0.03) in mixed ethylene glycol monomethyl ether and acetic anhydride (in a volume ratio of 3:1) to obtain a stable BiFeO3 precursor solution with the metal ion concentration of 0.3 mol / L, wherein bismuth ions are 5% excessive to compensate the volatilization in the film annealing process; and evenly coating the BiFeO3 precursor solution on an FTO (fluorine-doped tin oxide) substrate, drying to obtain a dry film, and carrying out layer-by-layer quick annealing at 550 DEG C to obtain the crystalline BiFeO3 film with expected thickness. The facility requests are simple, the experimental conditions can be easily achieved, and the BiFeO3 film with preferentially growing (110) crystal face, of which the remanent polarization is higher than 130 mu C / cm<2>, can be prepared by accurately controlling the solvent ratio of the precursor solution and the codoping of the A-B position.

Description

technical field [0001] The invention belongs to the field of functional materials, in particular to a method for preparing BiFeO 3 method for ferroelectric thin films. Background technique [0002] BiFeO 3 As the representative multiferroic compound system, a worldwide research boom of single-phase multiferroic magnetoelectric materials has been formed. With the development of microelectronics technology, optoelectronics and sensors, the requirements for material properties are getting higher and higher. Ferroelectric thin films have become widely used in microelectronics, Important functional materials in fields such as optoelectronics, integrated optics, and microelectromechanical systems. [0003] However, BiFeO 3 Its nature determines that it is difficult to prepare a pure phase, and a saturated hysteresis loop is observed. On the one hand, the presence of Bi and Fe affects the preparation of pure phase BiFeO 3 Material. Preparation of BiFeO by traditional slow an...

Claims

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Application Information

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IPC IPC(8): C30B5/02C30B29/22
Inventor 谈国强薛旭
Owner SHAANXI UNIV OF SCI & TECH
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