CN101691655A - Method of preparing BiFeO3 thin film - Google Patents
Method of preparing BiFeO3 thin film Download PDFInfo
- Publication number
- CN101691655A CN101691655A CN200910072848A CN200910072848A CN101691655A CN 101691655 A CN101691655 A CN 101691655A CN 200910072848 A CN200910072848 A CN 200910072848A CN 200910072848 A CN200910072848 A CN 200910072848A CN 101691655 A CN101691655 A CN 101691655A
- Authority
- CN
- China
- Prior art keywords
- film
- bifeo
- target
- sio
- thin film
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Landscapes
- Physical Vapour Deposition (AREA)
Abstract
The invention relates to a method of preparing a BiFeO3 thin film, aiming at solving the problem that the BiFeO3 thin film prepared with the prior magnetron sputtering technology has insufficient Fe. The method of preparing the BiFeO3 thin film comprises the following steps: (1) Bi1.1 FeO3 and Fe are sputtered on a Pt/Ti/SiO2/Si substrate with a Bi1.1 FeO3 target and a Fe target. (2) The Pt/Ti/SiO2/Si substrate is placed in oxygen to be subjected to heat preservation for 5 min, and the Pt/Ti/SiO2/Si substrate is cooled to room temperature to obtain the BiFeO3 thin film. The method can accurately control the components of the BiFeO3 thin film, and the BiFeO3 thin film prepared with the method has excellent ferroelectric and ferromagnetic properties.
Description
Technical field
The present invention relates to a kind of preparation BiFeO
3The method of film.
Background technology
The material that has at least two specific characters in ferroelectric, ferromagnetic, the iron bullet simultaneously is multi-ferroic material, in recent years, ferroic material causes that people more and more pay close attention to, and the iron electromagnet thin-film material has a series of important properties such as the electricity similar to ferroelectric material, light, heat, sound, have again simultaneously that volume is little, operating voltage is low, be convenient to develop miniature device and with advantages such as semiconductor technology is mutually integrated, be with a wide range of applications in microelectronics, photoelectronics, integrated optics, micro mechanics and the contour technical field of microcomputer electricity.Along with the important breakthrough of modern film preparing technology, the research of ferroelectric membranc becomes one of focus of modern material scientific research.As a kind of typical single-phase ferromagnetic electric material, BiFeO
3(BFO) has triangle distortion perovskite structure, be to have one of ferroelectricity and ferromagnetic material simultaneously under the room temperature few in number, also have ferroelectric preface parameter and antiferromagnetic preface parameter simultaneously, epitaxially grown BFO film is compared with the BFO block, caused investigator's extensive concern because of having the excellent performance of uniqueness, but monocrystalline BFO film preparation cost is quite high, therefore prepare excellent performance and the cheap polycrystalline BFO film of cost is the ferroelectric worker target of unremitting pursue always, therefore magnetron sputtering technique is the film preparing technology that is widely used in the semi-conductor industry, explores magnetron sputtering technique and prepares polycrystalline BFO film and have great importance.The sputter productivity (sputtering yield) that it is the Fe element that yet magnetron sputtering technique prepares an important difficult problem that the BFO film faces is relatively low, this just causes the content of Fe in the film often on the low side, in addition because the volatility of Bi, make the composition be difficult to accurately control the BFO film, thereby influenced the multi-ferrum property of BFO.
Summary of the invention
The present invention is in order to solve the problem that existing magnetron sputtering technique is difficult to accurately to control the composition of BFO film, and a kind of preparation BiFeO is provided
3The method of film.The inventive method is controlled BiFeO accurately
3The content of Fe in the film has obtained high-quality BiFeO
3Film.
The present invention prepares BiFeO
3The method of film is carried out according to following steps: one, Bi
1.1FeO
3Target and Fe target are simultaneously with Bi
1.1FeO
3Be splashed to Pt/Ti/SiO with Fe
2On/Si the matrix, control Bi
1.1FeO
3The sputtering power density of target is 1.8～2.2W/cm
2, the sputtering power density of control Fe is 0.66～1.1W/cm
2, the mixture of feeding argon gas and oxygen in the sputter procedure, wherein the volume ratio of argon gas and oxygen is 1: 1～4: 1, air pressure is 1.5Pa, Pt/Ti/SiO
2/ Si substrate temperature is 200～500 ℃; Two, with the Pt/Ti/SiO after the step 1 sputter end
2/ Si matrix places under the oxygen atmosphere, is heated to 400～700 ℃ of insulation 5min with the speed of 50 ℃/s, and control air pressure is 1.013 * 10
5Pa is cooled to room temperature then, promptly prepares BiFeO
3Film.
The inventive method is passed through Bi
1.1FeO
3The method of target and Fe target cosputtering prepares BiFeO
3Film is controlled BiFeO accurately
3The content of Fe in the film, the BiFeO that the inventive method prepares
3The molar ratio of Bi and Fe is 0.999～1.002 in the film, has overcome the content of Fe problem on the low side in the film, and method of the present invention is controlled the composition of BFO film accurately, the BiFeO for preparing
3Film has excellent ferroelectric properties and good ferromagnetic property, and the present invention prepares BiFeO
3The leakage current density of film under the current field condition of 120kV/cm is 0.9 * 10
-31.1 * 10
-3A/cm
2, remnant polarization has reached 30 μ C/cm
2More than, saturation magnetization has reached 20emu/cm
3More than.The inventive method prepares BiFeO
3Film performance is superior, has a good application prospect.
Description of drawings
The BiFeO that Fig. 1 prepares for embodiment
3The ferroelectric hysteresis loop figure of film; The BiFeO that Fig. 2 prepares for embodiment
3The magnetic hysteresis loop figure of film.
Embodiment
Technical solution of the present invention is not limited to following cited embodiment, also comprises the arbitrary combination between each embodiment.
Embodiment one: present embodiment prepares BiFeO
3The method of film is carried out according to following steps: Bi
1.1FeO
3Target and Fe target are simultaneously with Bi
1.1FeO
3(purity is 99.9%) and Fe (purity is 99.9%) are splashed to Pt/Ti/SiO
2On/Si the matrix, control Bi
1.1FeO
3The sputtering power density of target is 1.8～2.2W/cm
2, the sputtering power density of control Fe is 0.66～1.1W/cm
2, the mixture of feeding argon gas and oxygen in the sputter procedure, wherein the volume ratio of argon gas and oxygen is 1: 1～4: 1, air pressure is 1.5Pa, Pt/Ti/SiO
2/ Si substrate temperature is 200～500 ℃; Two, with the Pt/Ti/SiO after the step 1 sputter end
2/ Si matrix places under the oxygen atmosphere, is heated to 400～700 ℃ of insulation 5min with the speed of 50 ℃/s, and control air pressure is 1.013 * 10
5Pa is cooled to room temperature then, promptly prepares BiFeO
3Film.
The BiFeO that present embodiment prepares
3The molar ratio of Bi and Fe is 0.999～1.002 in the film.
That the present embodiment making obtains is polycrystalline BiFeO
3Film.
The BiFeO that present embodiment prepares
3The leakage current density of film under the current field condition of 120kV/cm is 0.9 * 1
-3～1.1 * 10
-3A/cm
2, remnant polarization has reached 30C/cm
2More than, saturation magnetization has reached 20emu/cm
3More than.
Embodiment two: what present embodiment and embodiment one were different is to control Bi in the step 1 in the step 1
1.1FeO
3The sputtering power density of target is 1.8W/cm
2Other steps and parameter are identical with embodiment one.
Embodiment three: what present embodiment and embodiment one were different is to control Bi in the step 1 in the step 1
1.1FeO
3The sputtering power density of target is 1.9W/cm
2Other steps and parameter are identical with embodiment one.
Embodiment four: present embodiment is different with embodiment one or two is that the sputtering power density of control Fe target in the step 1 is 1.06W/cm
2Other steps and parameter are identical with embodiment one or two.
Embodiment five: present embodiment is different with embodiment one or two is that the sputtering power density of control Fe target in the step 1 is 1.1W/cm
2Other steps and parameter are identical with embodiment one or two.
Embodiment six: that present embodiment and embodiment four are different is Pt/Ti/SiO in the step 1
2The sputter pressure of/Si matrix is 1.5Pa, Pt/Ti/SiO
2The sputter temperature of/Si matrix is 450 ℃.。Other steps and parameter are identical with embodiment four.
Embodiment seven: that present embodiment and embodiment four are different is Pt/Ti/SiO in the step 1
2The sputter pressure of/Si matrix is 1.6Pa, Pt/Ti/SiO
2The sputter temperature of/Si matrix is 430 ℃.Other steps and parameter are identical with embodiment four.
Embodiment eight: what present embodiment and embodiment one, two or six were different is that annealing time is 5min in the step 2, and temperature is 600 ℃.Other steps and parameter are identical with embodiment one, two or six.
Embodiment nine: what present embodiment and embodiment one, two or six were different is that annealing time is 6min in the step 2, and temperature is 610 ℃.Other steps and parameter are identical with embodiment one, two or six.
Embodiment ten: present embodiment prepares BiFeO
3The method of film is carried out according to following steps: Bi
1.1FeO
3Target and Fe target are simultaneously with Bi
1.1FeO
3(purity is 99.9%) and Fe (purity is 99.9%) are splashed to Pt/Ti/SiO
2On/Si the matrix, control Bi
1.1FeO
3The sputtering power density of target is 1.8W/cm
2, the sputtering power density of control Fe is 1.06W/cm
2, the mixture of feeding argon gas and oxygen in the sputter procedure, wherein the volume ratio of argon gas and oxygen is 4: 1, air pressure is 1.5Pa, Pt/Ti/SiO
2/ Si substrate temperature is 450 ℃; Two, with the Pt/Ti/SiO after the step 1 sputter end
2/ Si matrix places under the oxygen atmosphere, is heated to 600 ℃ of insulation 5min with the speed of 50 ℃/s, and control air pressure is 1.013 * 10
5Pa is cooled to room temperature then, promptly prepares BiFeO
3Film.
That the present embodiment making obtains is polycrystalline BiFeO
3Film.
The BiFeO that present embodiment prepares
3The leakage current density of film under the current field condition of 120kV/cm only is 1 * 10
-3A/cm
2, remnant polarization has reached 37 μ C/cm
2, saturation magnetization has reached 21emu/cm
3
The BiFeO that present embodiment prepares
3The ferroelectric hysteresis loop of film as shown in Figure 1, magnetic hysteresis loop as shown in Figure 2, from Fig. 1 and Fig. 2 BiFeO of preparing of present embodiment as can be seen
3The ferroelectric properties of film and ferromagnetic property are good.
Claims (5)
1. one kind prepares BiFeO
3The method of film is characterized in that preparing BiFeO
3The method of film is carried out according to following steps: one, Bi
1.1FeO
3Target and Fe target are simultaneously with Bi
1.1FeO
3Be splashed to Pt/Ti/SiO with Fe
2On/Si the matrix, control Bi
1.1FeO
3The sputtering power density of target is 1.8～2.2W/cm
2, the sputtering power density of control Fe is 0.66～1.1W/cm
2, the mixture of feeding argon gas and oxygen in the sputter procedure, wherein the volume ratio of argon gas and oxygen is 1: 1～4: 1, air pressure is 1.5Pa, Pt/Ti/SiO
2/ Si substrate temperature is 200～500 ℃; Two, with the Pt/Ti/SiO after the step 1 sputter end
2/ Si matrix places under the oxygen atmosphere, is heated to 400～700 ℃ of insulation 5min with the speed of 50 ℃/s, and control air pressure is 1.013 * 10
5Pa is cooled to room temperature then, promptly prepares BiFeO
3Film.
2. a kind of preparation BiFeO according to claim 1
3The method of film is characterized in that controlling in the step 1 Bi
1.1FeO
3The sputtering power density of target is 1.8W/cm
2
3. a kind of preparation BiFeO according to claim 1 according to claim 1 and 2
3The method of film is characterized in that the sputtering power density of control Fe target in the step 1 is 1.06W/cm
2
4. a kind of preparation BiFeO according to claim 3
3The method of film is characterized in that Pt/Ti/SiO in the step 1
2The sputter pressure of/Si matrix is 1.5Pa, Pt/Ti/SiO
2The sputter temperature of/Si matrix is 450 ℃.
5. according to claim 1,2 or 4 described a kind of preparation BiFeO
3The method of film is characterized in that annealing time is 5min in the step 2, and temperature is 600 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910072848A CN101691655A (en) | 2009-09-10 | 2009-09-10 | Method of preparing BiFeO3 thin film |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910072848A CN101691655A (en) | 2009-09-10 | 2009-09-10 | Method of preparing BiFeO3 thin film |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101691655A true CN101691655A (en) | 2010-04-07 |
Family
ID=42080367
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN200910072848A Pending CN101691655A (en) | 2009-09-10 | 2009-09-10 | Method of preparing BiFeO3 thin film |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101691655A (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102051582A (en) * | 2010-11-12 | 2011-05-11 | 北京工业大学 | Method for preparing highly (100) oriented BiFeO3 films on Si substrate |
| CN102603360A (en) * | 2012-03-18 | 2012-07-25 | 西北工业大学 | Method for preparing bismuth ferric thin film material |
| CN103540904A (en) * | 2013-10-15 | 2014-01-29 | 中国科学院半导体研究所 | Method used for preparation of T-phase BiFeO3 thin film |
| CN108559962A (en) * | 2018-05-16 | 2018-09-21 | 深圳万佳互动科技有限公司 | A kind of iron-based optical electro-chemistry film |
| CN110029308A (en) * | 2019-04-18 | 2019-07-19 | 武汉理工大学 | A kind of preparation method of bismuth ferrite photovoltaic film and its bismuth ferrite photovoltaic film of preparation |
| CN111525024A (en) * | 2020-04-13 | 2020-08-11 | 欧阳俊 | Bismuth ferrite film material, method for integrally preparing bismuth ferrite film on silicon substrate at low temperature and application |
-
2009
- 2009-09-10 CN CN200910072848A patent/CN101691655A/en active Pending
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102051582A (en) * | 2010-11-12 | 2011-05-11 | 北京工业大学 | Method for preparing highly (100) oriented BiFeO3 films on Si substrate |
| CN102051582B (en) * | 2010-11-12 | 2012-11-07 | 北京工业大学 | Method for preparing highly (100) oriented BiFeO3 films on Si substrate |
| CN102603360A (en) * | 2012-03-18 | 2012-07-25 | 西北工业大学 | Method for preparing bismuth ferric thin film material |
| CN102603360B (en) * | 2012-03-18 | 2013-08-28 | 西北工业大学 | Method for preparing bismuth ferric thin film material |
| CN103540904A (en) * | 2013-10-15 | 2014-01-29 | 中国科学院半导体研究所 | Method used for preparation of T-phase BiFeO3 thin film |
| CN103540904B (en) * | 2013-10-15 | 2015-11-18 | 中国科学院半导体研究所 | Preparation T-phase BiFeO 3the method of film |
| CN108559962A (en) * | 2018-05-16 | 2018-09-21 | 深圳万佳互动科技有限公司 | A kind of iron-based optical electro-chemistry film |
| CN110029308A (en) * | 2019-04-18 | 2019-07-19 | 武汉理工大学 | A kind of preparation method of bismuth ferrite photovoltaic film and its bismuth ferrite photovoltaic film of preparation |
| CN110029308B (en) * | 2019-04-18 | 2020-09-08 | 武汉理工大学 | Preparation method of bismuth ferrite photovoltaic film and bismuth ferrite photovoltaic film prepared by same |
| CN111525024A (en) * | 2020-04-13 | 2020-08-11 | 欧阳俊 | Bismuth ferrite film material, method for integrally preparing bismuth ferrite film on silicon substrate at low temperature and application |
| CN111525024B (en) * | 2020-04-13 | 2022-04-05 | 欧阳俊 | Bismuth ferrite film material, method for integrally preparing bismuth ferrite film on silicon substrate at low temperature and application |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101691655A (en) | Method of preparing BiFeO3 thin film | |
| CN103250263B (en) | Method for producing tunneling magnetoresistance element | |
| CN105989983A (en) | Permanent magnet | |
| CN107043914A (en) | A kind of batch (-type) magnetically controlled DC sputtering preparation method of amorphous cobalt based magnetic thin film | |
| JP5503714B2 (en) | Metal substrate for thin film superconducting wire, method for producing the same, and method for producing thin film superconducting wire | |
| WO2016157764A1 (en) | Thin film magnet and method for manufacturing thin film magnet | |
| WO2014073388A1 (en) | Ceramic material and sputtering-target member | |
| JP6353901B2 (en) | Magnetic material | |
| JP5765721B2 (en) | Ultra-thin perpendicular magnetization film exhibiting high perpendicular magnetic anisotropy, its production method and use | |
| WO2014038022A1 (en) | Nd-Fe-B THIN FILM MAGNET, AND METHOD FOR PRODUCING SAME | |
| JP2016186990A (en) | R-t-b-based thin film permanent magnet | |
| Huang et al. | Low transition-temperature characteristic in VOx films grown on Si3N4/Glass substrates | |
| Roy Dakua et al. | Effect of quenching on the magnetic properties of Mg-ferrite thin films | |
| CN100369200C (en) | Method for preparing ferromagnetic manganese silicon film on silicon substrate by magnetic control sputtering | |
| CN103714942B (en) | A kind of automatic biasing heterogeneous body microwave ferromagnetic thin film material and preparation method thereof | |
| CN104419895B (en) | The method that under low temperature, preparation has the ruthenic acid strontium thin film of height (001) preferred orientation | |
| CN104513963A (en) | Method for preparing ferromanganese film on silicon through magnetron sputtering | |
| CN107059119B (en) | Method for preparing polycrystalline SiC film through sapphire substrate | |
| JP4483166B2 (en) | Permanent magnet thin film | |
| CN102965633B (en) | Preparation method of M-type barium ferrite film with c-axis vertical film surface orientation | |
| CN105198406B (en) | Nanocrystalline complex phase film of barium titanate/nickel-zinc ferrite that magnetic is mutually orientated and preparation method thereof | |
| CN112011773B (en) | Yttrium silicate coating and preparation method and application thereof | |
| JP2005286152A (en) | Manufacturing method of anisotropic rare earth/iron -based magnet film and micro motor | |
| JP2004307310A (en) | METHOD FOR MANUFACTURING Fe-Si-BASED THIN FILM, AND Fe-Si-BASED THIN FILM | |
| CN114783768B (en) | SrFeO for improving interface mismatch strain 2.0 Method for film magnetic performance and application |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Open date: 20100407 |