CN108004592A - A kind of Bi6Ti3Fe2O18More epitaxial ferroelectric films of stratiform and preparation method thereof - Google Patents
A kind of Bi6Ti3Fe2O18More epitaxial ferroelectric films of stratiform and preparation method thereof Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 144
- 229910052742 iron Inorganic materials 0.000 claims abstract description 40
- 238000004549 pulsed laser deposition Methods 0.000 claims abstract description 17
- 239000000203 mixture Substances 0.000 claims abstract description 9
- 239000000126 substance Substances 0.000 claims abstract description 4
- 239000010936 titanium Substances 0.000 claims description 84
- 239000000758 substrate Substances 0.000 claims description 33
- 238000000034 method Methods 0.000 claims description 23
- 238000010438 heat treatment Methods 0.000 claims description 19
- 229910052797 bismuth Inorganic materials 0.000 claims description 15
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims description 15
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 14
- 239000001301 oxygen Substances 0.000 claims description 14
- 229910052760 oxygen Inorganic materials 0.000 claims description 14
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 13
- 229910052709 silver Inorganic materials 0.000 claims description 13
- 239000004332 silver Substances 0.000 claims description 13
- 238000000151 deposition Methods 0.000 claims description 12
- 230000008021 deposition Effects 0.000 claims description 12
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 11
- 229910052719 titanium Inorganic materials 0.000 claims description 11
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims description 10
- 230000005415 magnetization Effects 0.000 claims description 10
- 239000002253 acid Substances 0.000 claims description 8
- 229910052746 lanthanum Inorganic materials 0.000 claims description 8
- 230000010287 polarization Effects 0.000 claims description 7
- 229910052706 scandium Inorganic materials 0.000 claims description 7
- SIXSYDAISGFNSX-UHFFFAOYSA-N scandium atom Chemical compound [Sc] SIXSYDAISGFNSX-UHFFFAOYSA-N 0.000 claims description 7
- 238000004062 sedimentation Methods 0.000 claims description 6
- 239000005084 Strontium aluminate Substances 0.000 claims description 5
- FNWBQFMGIFLWII-UHFFFAOYSA-N strontium aluminate Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Al+3].[Al+3].[Sr+2].[Sr+2] FNWBQFMGIFLWII-UHFFFAOYSA-N 0.000 claims description 5
- 229910052692 Dysprosium Inorganic materials 0.000 claims description 4
- KBQHZAAAGSGFKK-UHFFFAOYSA-N dysprosium atom Chemical compound [Dy] KBQHZAAAGSGFKK-UHFFFAOYSA-N 0.000 claims description 4
- -1 lanthanum aluminate Chemical class 0.000 claims description 4
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 claims description 4
- 229910052712 strontium Inorganic materials 0.000 claims description 4
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 claims description 4
- KPOOQKVTBKSXMC-UHFFFAOYSA-N [Ta].[Nd] Chemical compound [Ta].[Nd] KPOOQKVTBKSXMC-UHFFFAOYSA-N 0.000 claims description 3
- 150000001875 compounds Chemical class 0.000 claims description 3
- LNTHITQWFMADLM-UHFFFAOYSA-N gallic acid Chemical compound OC(=O)C1=CC(O)=C(O)C(O)=C1 LNTHITQWFMADLM-UHFFFAOYSA-N 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 229910052727 yttrium Inorganic materials 0.000 claims description 3
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 claims description 3
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 claims description 2
- 230000003068 static effect Effects 0.000 claims 1
- 229910052715 tantalum Inorganic materials 0.000 claims 1
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 claims 1
- 239000010408 film Substances 0.000 abstract description 90
- 239000010409 thin film Substances 0.000 abstract description 22
- 239000000463 material Substances 0.000 abstract description 21
- 230000009286 beneficial effect Effects 0.000 abstract description 3
- 230000005307 ferromagnetism Effects 0.000 abstract description 3
- 238000012512 characterization method Methods 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 description 12
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 10
- 229910000416 bismuth oxide Inorganic materials 0.000 description 9
- TYIXMATWDRGMPF-UHFFFAOYSA-N dibismuth;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Bi+3].[Bi+3] TYIXMATWDRGMPF-UHFFFAOYSA-N 0.000 description 9
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 8
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 8
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 7
- 230000005621 ferroelectricity Effects 0.000 description 7
- 230000005294 ferromagnetic effect Effects 0.000 description 7
- 239000000843 powder Substances 0.000 description 7
- 229910001882 dioxygen Inorganic materials 0.000 description 6
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 5
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 5
- 229910052757 nitrogen Inorganic materials 0.000 description 5
- 238000003825 pressing Methods 0.000 description 5
- 238000004140 cleaning Methods 0.000 description 4
- 239000004570 mortar (masonry) Substances 0.000 description 4
- 238000000465 moulding Methods 0.000 description 4
- 230000003287 optical effect Effects 0.000 description 4
- 230000002000 scavenging effect Effects 0.000 description 4
- 238000010792 warming Methods 0.000 description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- 238000002017 high-resolution X-ray diffraction Methods 0.000 description 3
- 230000005291 magnetic effect Effects 0.000 description 3
- 239000003960 organic solvent Substances 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- 229910002902 BiFeO3 Inorganic materials 0.000 description 2
- 244000137852 Petrea volubilis Species 0.000 description 2
- 229910002367 SrTiO Inorganic materials 0.000 description 2
- 238000000137 annealing Methods 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000011065 in-situ storage Methods 0.000 description 2
- 238000004377 microelectronic Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000012827 research and development Methods 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 238000007704 wet chemistry method Methods 0.000 description 2
- 229910002534 DyScO3 Inorganic materials 0.000 description 1
- 229910002244 LaAlO3 Inorganic materials 0.000 description 1
- 229910002331 LaGaO3 Inorganic materials 0.000 description 1
- AGDGPIPRLIPOPB-UHFFFAOYSA-N [La].[Ta] Chemical compound [La].[Ta] AGDGPIPRLIPOPB-UHFFFAOYSA-N 0.000 description 1
- ZDCBIXWPYFBYTO-UHFFFAOYSA-N [Ta].[La].[Sr] Chemical compound [Ta].[La].[Sr] ZDCBIXWPYFBYTO-UHFFFAOYSA-N 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000010668 complexation reaction Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000002173 high-resolution transmission electron microscopy Methods 0.000 description 1
- FAHBNUUHRFUEAI-UHFFFAOYSA-M hydroxidooxidoaluminium Chemical compound O[Al]=O FAHBNUUHRFUEAI-UHFFFAOYSA-M 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 238000001755 magnetron sputter deposition Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000001451 molecular beam epitaxy Methods 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/16—Oxides
- C30B29/22—Complex oxides
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
- C30B25/02—Epitaxial-layer growth
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B33/00—After-treatment of single crystals or homogeneous polycrystalline material with defined structure
- C30B33/02—Heat treatment
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- Chemical & Material Sciences (AREA)
- Metallurgy (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Thermal Sciences (AREA)
- Physics & Mathematics (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Physical Vapour Deposition (AREA)
- Inorganic Insulating Materials (AREA)
- Semiconductor Memories (AREA)
Abstract
The present invention relates to a kind of Bi6Ti3Fe2O18More epitaxial ferroelectric films of stratiform and preparation method thereof, the film is made using pulsed laser deposition, chemical composition Bi6Ti3Fe2O18.The Bi of the present invention6Ti3Fe2O18The more iron thin film thing phase purity of stratiform are high, XRD characterization result is without dephasign, and TEM, the result shows that film has good epitaxial nature, ferroelectric properties is good and is provided simultaneously with considerable ferromagnetism, it is the more ferroelectric material films of excellent room temperature, is very beneficial for the R＆D and promotion of new more iron thin films.
Description
Technical field
The invention belongs to technical field of new material preparation, is related to a kind of Bi6Ti3Fe2O18The more epitaxial ferroelectric films of stratiform and its system
Preparation Method.
Background technology
Multi-iron material can show ferroelectricity and ferromagnetism at the same time, and there are magneto-electric coupled effect between them, so that
It can realize mutual regulation and control (J.Wang the and R.Ramesh, Science 299,1719 (2003) of electricity and magnetic；
W.Eerenstein and J.F.Scott,Nature 442,759(2006)；).Therefore, multi-iron material is as a kind of new more
Functional material, has broad application prospects in spintronics and other various fields.Wherein multiferroic film material can be with
Microelectronic technique is compatible so that more iron thin films can be widely applied to the fields such as microsensor and multiple-state storage.For example, magnetic recording
Reading speed is fast and writes slowly, and ferroelectricity record reads complicated and writes soon, if using more ferroelectric material films as recording medium,
It can realize the read-write process of high speed.
Realize that multiple-state storage just needs to obtain the good more iron thin films of ferroelectric properties, the physics of the current generally use of this target
Method deposits epitaxial film to realize, such as pulsed laser deposition, molecular beam epitaxy, (Y Chu, the and R.Ramesh such as magnetron sputtering
et al,Nature Material 7,478(2008)；), wherein pulsed laser deposition has repeatability high, prepares film more
Meet stoichiometric ratio, epitaxial film quality is high, the advantages such as process is simple, is more suitable for the multivariant oxide of prepared composition complexity
Film.
In recent years, combined using different excitation units (ferroelectric cell and magnetoelectricity unit) on atomic scale, to realize room
The research of the single-phase more iron characteristics of temperature gets more and more people's extensive concerning, its typical structure is multilayer laminar perovskite multi-iron material Bim+ 1Fem-3Ti3O3m+3(m=4,5,6,7,8), which can regard BiFeO as3Magnet unit is inserted into three layers of laminated perovskite
Ferroelectric Bi4Ti3O12In (N.A.Lomanova, M.I.Morozov, V.L.Ugolkov, and V.V.Gusarov,
Inorganic Materials,42,189(2006)).This kind of more ferroelectric material film chemical compositions are relative complex, and the overwhelming majority is logical
Easily controllable thin film composition wet chemistry method is crossed to be prepared, it is general although wet chemistry method easily prepares more iron thin films of pure phase
Store-through poor ferroelectric property, leakage current is big the problems such as.For the Bi of m=56Ti3Fe2O18For material, have been reported that at present pair
Its Thin Films performance studied (W.Bai, J.H.Chu, Thin Solid Films, 525,195 (2012),
Z.Liu,Y.P.Sun,Applied Physics Letters,101,122402(2012),Y.Yun,Yalin Lu,Applied
Physics Express, 8,054001 (2015)), it is found that it has very big development potentiality in terms of more iron characteristics, but
Bi6Ti3Fe2O18More iron thin film chemical compositions are relative complex, and preparation process is also easy to produce dephasign, there are no article pair at present
Bi6Ti3Fe2O18Pure phase film room temperature ferroelectricity, ferromagnetic property are reported, and film is the main of the final application of multi-iron material
Channel, thus how to obtain with good ferroelectric properties and magnetic Bi6Ti3Fe2O18The more iron thin films of high quality, be it is current urgently
The problem of solution, it is following to the material to have great significance applied to popularization.
The content of the invention
For the problem above of the prior art, it is an object of the invention to provide a kind of Bi6Ti3Fe2O18The more iron extensions of stratiform
Film and preparation method thereof, layered more epitaxial ferroelectric film crystalline qualities are high, entirely without dephasign, and have excellent room temperature iron
Electrical property, while also obtain considerable ferromagnetic property in room temperature, it is expected to be applied as new multi-iron material.
Here, the present invention provides a kind of more epitaxial ferroelectric films of stratiform, the film is made using pulsed laser deposition, is changed
It is Bi to learn composition6Ti3Fe2O18。
It is preferred that the thickness of layered more epitaxial ferroelectric films is 10~200nm.
In the present invention, the film is the monocrystal thin films for having good epitaxial relationship with substrate, has excellent room temperature iron
Electrical property, remanent polarization during room temperature can reach 23.2 μ C/cm2, saturation magnetization can reach 21.5emu/cm3,
Null field remanent magnetization can reach 7.03emu/cm3。
Also, the coercive field during film room temperature of the present invention only has 239.3KV/cm.
The Bi of the present invention6Ti3Fe2O18The more iron thin film thing phase purity of stratiform are high, and XRD characterization result is without dephasign, and TEM results
Show that film has good epitaxial nature, ferroelectric properties is good and is provided simultaneously with considerable ferromagnetism, is the more iron of excellent room temperature
Thin-film material, is very beneficial for the R＆D and promotion of new more iron thin films.
The present invention also provides a kind of preparation method of layered more epitaxial ferroelectric films, including：
Bismuth source, titanium source, source of iron are mixed, it is compressing to obtain Bi6Ti3Fe2O18Target；
Pulsed laser deposition grows Bi6Ti3Fe2O18Film：Vacuum is evacuated to 1x10-5Below Torr (preferred deposition vacuums<
1x10-5Torr), 20~100mTorr of partial pressure of oxygen, 650~710 DEG C of underlayer temperature, laser output energy is 80~200mJ, bombardment
Target energy density is 0.7~2.0J/cm2, 1~5Hz of laser pulse frequency, sedimentation time 10~200 minutes are kept during deposition；
To Bi6Ti3Fe2O18Film carries out situ heat treatment, obtains Bi6Ti3Fe2O18The more epitaxial ferroelectric films of stratiform.
The present invention uses Bi6Ti3Fe2O18Target, carries out original position using pulsed laser deposition plated film, after the completion of deposition and moves back
Fire processing, the final Bi for obtaining good quality6Ti3Fe2O18The more epitaxial ferroelectric films of stratiform.Had using pulsed laser deposition and repeated
Property it is high, prepare film and be more in line with stoichiometric ratio, epitaxial film quality is high, the advantages such as process is simple.By adjusting laser energy
Metric density, grows frequency, silicon heating rate, oxygen partial pressure, and the key parameter such as rate of temperature fall, finally obtains high-quality
The Bi of amount6Ti3Fe2O18More epitaxial ferroelectric films.Prepared Bi6Ti3Fe2O18The more epitaxial ferroelectric film crystalline qualities of stratiform are high, completely
Without dephasign, and there is excellent room temperature ferroelectric properties, while also obtain considerable ferromagnetic property in room temperature.The present invention is research
Develop new more iron thin films and provide robust techniques route.In addition, the present invention method needed for equipment it is simple, directly once into
Film, can be adapted to past device to integrate direction and develops with microelectric technique process compatible.
It is preferred that according to molar ratio 6.2~6.7:3:2 mix bismuth source, titanium source, source of iron.In the present invention, by making bismuth source
It is excessive, so as to make up the volatilization of the Bi elements in high temperature preparation process.
It is preferred that the bismuth source is bismuthous oxide, the titanium source is tetravalence titanyl compound, and the source of iron is three
The oxide of valency iron.Such as with bismuth oxide (Bi2O3), titanium dioxide (TiO2), iron oxide (Fe2O3) it is used as raw material.
It is preferred that the bismuth source, titanium source, the purity of source of iron is more than 99.9%, for example with analytically pure raw material.
Compressing isostatic cool pressing, 150~260MPa of load pressure, 5~20 points of dwell time are used it is preferred that described
Clock.
It is preferred that the substrate is perovskite structure single crystalline substrate of the lattice constant between 3.8~4.0, preferably metatitanic acid
One kind in strontium, lanthanum aluminate, strontium aluminate tantalum neodymium, scandium acid dysprosium, strontium aluminate tantalum lanthanum, scandium acid yttrium, lanthanum gallate.
It is preferred that fix substrate with silver paste.Substrate is fixed using silver paste to has the following advantages：1st, heated more under hot conditions
Add uniformly；2nd, silver paste does not in itself pollute film.
In the preparation method of the present invention, the situ heat treatment includes：After growth, be filled with oxygen to 600Torr~
1atm, room temperature is down to 5~10 DEG C/min of speed.
Brief description of the drawings
Fig. 1：Bi prepared by embodiment 16Ti3Fe2O18The high-resolution X-ray diffraction spectrogram of epitaxial film；
Fig. 2：Bi prepared by embodiment 16Ti3Fe2O18High-resolution-ration transmission electric-lens (HRTEM) figure of epitaxial film；
Fig. 3：Bi prepared by embodiment 16Ti3Fe2O18Atomic force microscope (AFM) figure of epitaxial film；
Fig. 4：Bi prepared by embodiment 16Ti3Fe2O18The ferroelectricity loop line figure (P-E loops) of epitaxial thin-film layer；
Fig. 5：Bi prepared by embodiment 16Ti3Fe2O18The hysteresis curve figure (M-H loops) of epitaxial thin-film layer；
Fig. 6：Bi prepared by embodiment 26Ti3Fe2O18The high-resolution X-ray diffraction spectrogram of epitaxial film；
Fig. 7：Bi prepared by embodiment 26Ti3Fe2O18The ferroelectricity loop line figure (P-E loops) of epitaxial thin-film layer；
Fig. 8：Bi prepared by embodiment 36Ti3Fe2O18The high-resolution X-ray diffraction spectrogram of epitaxial film；
Fig. 9：Bi prepared by embodiment 36Ti3Fe2O18The ferroelectricity loop line figure (M-H loops) of epitaxial thin-film layer.
Embodiment
The present invention is further illustrated below in conjunction with attached drawing and following embodiments, it should be appreciated that following embodiments are only used for
Illustrate the present invention, be not intended to limit the present invention.
The present invention relates to a kind of Bi6Ti3Fe2O18More epitaxial ferroelectric films and preparation method thereof.The method is by two layers of octahedral
Body group BiFeO3It is inserted into three shape Ferroelectrics Bi layer by layer4Ti3O12It is middle to form new eight shape Ca-Ti ore types layer by layer
Bi6Ti3Fe2O18More epitaxial ferroelectric films.The present invention utilizes pulsed laser deposition plated film in single crystalline substrate, after the completion of deposition
O2Annealing in situ, obtains the Bi with room temperature ferroelectricity, ferromagnetic characteristic and good quality first in atmosphere6Ti3Fe2O18Stratiform
More epitaxial ferroelectric films.Equipment is simple needed for the method, can be with microelectric technique process compatible.The Bi prepared6Ti3Fe2O18Layer
The more iron thin film thing phase purity of shape are high, are the more ferroelectric material films of excellent room temperature, be very beneficial for the research and development of new more iron thin films with
Promote.
(Bi6Ti3Fe2O18The compacting of target)
In the present invention, Bi6Ti3Fe2O18Target as the bismuth source of raw material, titanium source, source of iron by mixing compressing obtain.
Bismuth source can use bismuthous oxide, and the purity in bismuth source is more than 99.9%.For example with analytically pure oxygen
Change bismuth (Bi2O3)。
Titanium source can use tetravalence titanyl compound, and the purity of titanium source is more than 99.9%.For example with analytically pure two
Titanium oxide (TiO2)。
Source of iron can use ferric oxide, and the purity of source of iron is more than 99.9%.For example with analytically pure oxygen
Change iron (Fe2O3)。
Raw material proportioning can be elemental mole ratios Bi:Ti:Fe=6.2~6.7:3:2.Wherein, in order to make up in high temperature system
The volatilization of Bi elements during standby, suitably makes bismuth source excessive.It is not particularly limited, can be used for the hybrid mode of raw material
The method mixing known.Such as powder material is put into automatic mortar and is sufficiently mixed and grinds more than 24h.
After raw material is sufficiently mixed fine grinding, will mix complete powder load mould pre-molding, shape can be it is cylindric, directly
Footpath is usually 2~2.5cm, thickness 0.5-1cm.
Then, it is compressing to obtain Bi6Ti3Fe2O18Target.It is compressing to use isostatic cool pressing mode, load pressure
150~260MPa, 5~20min of dwell time.
The present invention uses Bi6Ti3Fe2O18Target, can ensure the change of film growth with pulsed laser deposition process
Learn metering ratio.
(preparation and cleaning of substrate)
In the present invention, growth substrate can be used as using perovskite structure single crystalline substrate of the lattice constant between 3.8~4.0.Example
Such as, strontium titanates (SrTiO can be used3), lanthanum aluminate (LaAlO3), strontium aluminate tantalum neodymium (NSAT), scandium acid dysprosium (DyScO3), aluminic acid
Strontium tantalum lanthanum (LAST), scandium acid yttrium (YScO3), lanthanum gallate (LaGaO3) etc..Perovskite structure of the lattice constant between 3.8~4.0
Single crystalline substrate has the advantages that lattice mismatch is low.The orientation of substrate can be (001) (110) (111), be preferably (001)
(110).By selecting the orientation of substrate, the film for the orientation that matches can be grown.
Before use, substrate is cleaned.Specifically, as an example, such as had successively using acetone, isopropanol etc.
Solvent is cleaned by ultrasonic, and scavenging period is more than 5 minutes, is finally dried up with nitrogen gun.
In the present invention, substrate can be fixed on by heating plate by silver paste.Specifically, the step of fixed substrate, can wrap
Include：One layer of silver paste is first brushed at room temperature, and substrate is positioned in silver paste and is compacted with tweezers, is warming up to 60~80 DEG C, heating rate
It is maintained at 20 DEG C/below min, it is therefore an objective to prevent silver paste from producing bubble because of steep temperature rise.Use silver paste fix substrate have with
Lower advantage：1st, heated under hot conditions more uniform；2nd, silver paste does not in itself pollute film.
(Bi6Ti3Fe2O18The growth of film)
In the present invention, using pulsed laser deposition deposition film, this method has repeatability high, prepares being more in line with of film
Metering ratio is learned, epitaxial film quality is high, the advantages such as process is simple.In addition chemical synthesis, Physical plated film and semiconductor are compared
Integrated technique good compatibility, is conducive to application.Specifically, pulsed laser deposition deposition film can include：Vacuum is taken out
To 1x10-5Below Torr, is filled with oxygen, 20~100mTorr of partial pressure of oxygen；Laser optical path is adjusted, it is 80 to keep laser output energy
~200mJ, bombardment target energy density is 0.7~2.0J/cm2, 1~5Hz of laser pulse frequency, sedimentation time are kept during deposition
10~200min.By adjusting laser energy density, frequency, silicon heating rate, oxygen partial pressure, and cooling speed are grown
The key parameters such as rate, can finally obtain the Bi of high quality6Ti3Fe2O18More epitaxial ferroelectric films.
Wherein, oxygen purity can be more than 99.99.In addition, underlayer temperature can be risen to 650~710 DEG C before deposition,
It is preferred that 650~700 DEG C, heating rate can be in 5~20 DEG C/min.
(Bi6Ti3Fe2O18Film situ heat treatment)
After growth, to Bi6Ti3Fe2O18Film carries out situ heat treatment.Specifically, situ heat treatment includes：Grown junction
Shu Hou, closes slide valve, is filled with oxygen to 600Torr~1atm, is cooled to room temperature and takes out film, obtain Bi6Ti3Fe2O18It is more
Epitaxial ferroelectric film.Wherein, rate of temperature fall can be in 5~10 DEG C/min.By situ heat treatment, it is preferable can make it that film obtains
Crystallinity.In addition, annealing in situ can further improve the crystallization property of film in oxygen atmosphere.
In the present invention, the film thickness is in 10~200nm.Film thickness has and is suitable at present in 10~200nm
The advantages of microelectronic component.
It is also, as described above, of the invention by two layers of octahedra group BiFeO3It is inserted into three shape Ferroelectrics layer by layer
Bi4Ti3O12It is middle to form new eight shape Ca-Ti ore type Bi layer by layer6Ti3Fe2O18More epitaxial ferroelectric films, have the advantages that the more iron of room temperature.
The more epitaxial ferroelectric films of stratiform of the present invention are (001) direction orientation preferably along c-axis, can so cause the film surface of growth
Flatness higher, laminated crystalline orientation are more preferable.
, can be with sand paper by silicon to ensure the repeatability and stability of experiment in addition, every time before sample preparation
Platform polishing is clean, and is cleaned out settling chamber with isopropanol, and target is polished flat with sand paper before installation target every time
And purged with nitrogen gun clean.
Advantages of the present invention：
Have repeatability high using pulsed laser deposition, prepare film and be more in line with stoichiometric ratio, epitaxial film quality is high, mistake
The advantages such as journey is simple.In the present invention, by making bismuth source excessive, so as to make up the volatilization of the Bi elements in high temperature preparation process.This
Equipment needed for the method for invention is simple, direct one-pass film-forming, can be adapted to integrate direction toward device with microelectric technique process compatible
Development.Prepared Bi6Ti3Fe2O18The more epitaxial ferroelectric films of stratiform are the monocrystal thin films for having good epitaxial relationship with substrate.And
And the thin film crystallization quality is high, entirely without dephasign, and has excellent room temperature ferroelectric properties, remanent polarization is up to 23.2 μ
C/cm2, coercive field only has 239.3KV/cm, while also obtain considerable ferromagnetic property in room temperature, and saturation magnetization is reachable
21.5emu/cm3, null field remanent magnetization 7.03emu/cm3, it is expected to be applied as new multi-iron material.
Embodiment is enumerated further below so that the present invention will be described in detail.It will similarly be understood that following embodiments are served only for this
Invention is further described, it is impossible to is interpreted as limiting the scope of the invention, those skilled in the art is according to this hair
Some nonessential modifications and adaptations that bright the above is made belong to protection scope of the present invention.Following examples are specific
Technological parameter etc. is also only an example in OK range, i.e. those skilled in the art can be done properly by the explanation of this paper
In the range of select, and do not really want to be defined in hereafter exemplary concrete numerical value.
Embodiment 1
(a)Bi6Ti3Fe2O18The compacting of target：With analytically pure bismuth oxide (Bi2O3), titanium dioxide (TiO2), iron oxide
(Fe2O3) it is primary raw material, raw material proportioning Bi:Ti:Fe=6.48:3:2；Powder material is mixed, automatic mortar is put into and carries out
It is sufficiently mixed and grinds more than 24h；The powder completed will be mixed and load mould pre-molding, shape is a diameter of to be cylindric
2cm, thickness 0.5cm；Bi is pressed into using isostatic cool pressing mode6Ti3Fe2O18Target, load pressure 260MPa, dwell time
8min。
(b) preparation and cleaning of substrate：Strontium titanates (the SrTiO being orientated using (001)3) single crystalline substrate conduct growth base
Bottom, is cleaned by ultrasonic using organic solvents such as acetone, isopropanols successively, and scavenging period is 5 minutes, is finally blown with nitrogen gun
It is dry.
(c)Bi6Ti3Fe2O18The growth of film：Using pulsed laser deposition, target is fixed on the suitable position in settling chamber
Put, substrate is fixed on by silver paste and is heated the substrate, vacuum is evacuated to 5x10-6Torr, is filled with high purity oxygen gas, keeps partial pressure of oxygen
77mTorr, with the heating rate of 20 DEG C/min, is warming up to 660 DEG C；Laser optical path is adjusted, holding laser output energy is
100mJ, bombardment target energy density is 1.2J/cm2, laser pulse frequency 3Hz, sedimentation time 20min are kept during deposition.
(d)Bi6Ti3Fe2O18Film situ heat treatment：After growth, slide valve is closed, is filled with high purity oxygen gas extremely
600Torr, with the rate of temperature fall of 5 DEG C/min, is cooled to room temperature and takes out film, obtains along i.e. (001) direction orientation of c-axis
Bi6Ti3Fe2O18More epitaxial ferroelectric films.
Bi prepared by this example6Ti3Fe2O18More epitaxial ferroelectric film phase purity are high (as shown in attached drawing 1), epitaxial growth orientation
Well (as shown in attached drawing 2), surface smoothness is good (as shown in attached drawing 3)；Film thickness is 40nm.Film has excellent room temperature iron
Electrical property, remanent polarization are up to 23.2 μ C/cm2, coercive field only has 239.3KV/cm (as shown in attached drawing 4)；At the same time in room
Temperature also obtain considerable ferromagnetic property, and using superconducting quantum interference device (SQUID) (SQUID) method, it is reachable to measure saturation magnetization
21.5emu/cm3, null field remanent magnetization 7.03emu/cm3(as shown in attached drawing 5).
Embodiment 2
(a)Bi6Ti3Fe2O18The compacting of target：With analytically pure bismuth oxide (Bi2O3), titanium dioxide (TiO2), iron oxide
(Fe2O3) it is primary raw material, raw material proportioning Bi:Ti:Fe=6.5:3:2；Automatic mortar is put into be sufficiently mixed and ground
More than 24h；The powder loading mould pre-molding completed will be mixed, shape is cylindric, a diameter of 2cm, thickness 0.5cm；Adopt
Bi is pressed into isostatic cool pressing mode6Ti3Fe2O18Target, load pressure 180MPa, dwell time 20min.
(b) preparation and cleaning of substrate：The scandium acid dysprosium (DyScO being orientated using (110)3) single crystalline substrate conduct growth base
Bottom, is cleaned by ultrasonic using organic solvents such as acetone, isopropanols successively, and scavenging period is 5 minutes, is finally blown with nitrogen gun
It is dry.
(c)Bi6Ti3Fe2O18The growth of film：Using pulsed laser deposition, target is fixed on the suitable position in settling chamber
Put, substrate is fixed on by silver paste and is heated the substrate, vacuum is evacuated to 8x10-6Torr, is filled with high purity oxygen gas, keeps partial pressure of oxygen
50mTorr, with the heating rate of 20 DEG C/min, is warming up to 700 DEG C；Laser optical path is adjusted, it is 80mJ to keep laser output energy,
It is 0.8J/cm to bombard target energy density2, laser pulse frequency 1Hz, sedimentation time 30min are kept during deposition.
(d)Bi6Ti3Fe2O18Film situ heat treatment：After growth, slide valve is closed, is filled with high purity oxygen gas extremely
600Torr, with the rate of temperature fall of 5 DEG C/min, is cooled to room temperature and takes out film, obtains along i.e. (001) direction orientation of c-axis
Bi6Ti3Fe2O18More epitaxial ferroelectric films.
The more epitaxial ferroelectric film phase purity of Bi6Ti3Fe2O18 prepared by this example are high (as shown in attached drawing 6), surface smoothness
It is good；Film thickness is 50nm；With excellent room temperature ferroelectric properties, remanent polarization is up to 20.3 μ C/cm2, and coercive field is only
There is 294KV/cm (as shown in attached drawing 7).
Embodiment 3
(a)Bi6Ti3Fe2O18The compacting of target：With analytically pure bismuth oxide (Bi2O3), titanium dioxide (TiO2), iron oxide
(Fe2O3) it is primary raw material, raw material proportioning Bi:Ti:Fe=6.35:3:2；Powder material is mixed, automatic mortar is put into and carries out
It is sufficiently mixed and grinds more than 24h；The powder completed will be mixed and load mould pre-molding, shape is a diameter of to be cylindric
2cm, thickness 0.5cm；Bi is pressed into using isostatic cool pressing mode6Ti3Fe2O18Target, load pressure 200MPa, dwell time
15min。
(b) preparation and cleaning of substrate：Lanthanum aluminate (the LaAlO being orientated using (001)3) single crystalline substrate conduct growth base
Bottom, is cleaned by ultrasonic using organic solvents such as acetone, isopropanols successively, and scavenging period is 5 minutes, is finally blown with nitrogen gun
It is dry.
(c)Bi6Ti3Fe2O18The growth of film：Using pulsed laser deposition, target is fixed on the suitable position in settling chamber
Put, substrate is fixed on by silver paste and is heated the substrate, vacuum is evacuated to 5x10-6Torr, is filled with high purity oxygen gas, keeps partial pressure of oxygen
90mTorr, with the heating rate of 20 DEG C/min, is warming up to 710 DEG C；Laser optical path is adjusted, holding laser output energy is
200mJ, bombardment target energy density is 2J/cm2, laser pulse frequency 5Hz, sedimentation time 80min are kept during deposition.
(d)Bi6Ti3Fe2O18Film situ heat treatment：After growth, slide valve is closed, is filled with high purity oxygen gas to 1atm,
With the rate of temperature fall of 10 DEG C/min, it is cooled to room temperature and takes out film, obtains along i.e. (001) direction orientation of c-axis
Bi6Ti3Fe2O18More epitaxial ferroelectric films.
Bi prepared by this example6Ti3Fe2O18More epitaxial ferroelectric film phase purity are high (as shown in attached drawing 8), and surface smoothness is good；
Film thickness is 50nm, has excellent room temperature ferroelectric properties, and remanent polarization is up to 19.5 μ C/cm2, coercive field only has
279.5KV/cm (as shown in attached drawing 9).
Bi prepared by the present invention6Ti3Fe2O18Single-phase more epitaxial ferroelectric film crystalline qualities are high, entirely without dephasign, and with excellent
Different room temperature ferroelectric properties, remanent polarization are up to 23.2 μ C/cm2, coercive field only has 239.3KV/cm；At the same time in room temperature
Considerable ferromagnetic property is obtained, saturation magnetization is up to 21.5emu/cm3, null field remanent magnetization 7.03emu/cm3,
It is expected to be applied as new multi-iron material.
Claims (10)
1. a kind of more epitaxial ferroelectric films of stratiform, it is characterised in that the film is made using pulsed laser deposition, chemical composition
For Bi6Ti3Fe2O18。
2. the more epitaxial ferroelectric films of stratiform according to claim 1, it is characterised in that the thickness of the film for 10~
200nm。
3. the more epitaxial ferroelectric films of stratiform according to claim 1 or 2, it is characterised in that the residue during film room temperature
Polarization intensity can reach 23.2 μ C/cm2, saturation magnetization can reach 21.5 emu/cm3, null field remanent magnetization
7.03 emu/cm can be reached3。
A kind of 4. preparation method of the more epitaxial ferroelectric films of stratiform any one of claims 1 to 3, it is characterised in that institute
The method of stating includes：
Bismuth source, titanium source, source of iron are mixed, it is compressing to obtain Bi6Ti3Fe2O18Target；
Pulsed laser deposition grows Bi6Ti3Fe2O18Film：Vacuum is evacuated to 1x10-5Below Torr, partial pressure of oxygen 20~
100mTorr, 650~710 DEG C of underlayer temperature, laser output energy be 80~200mJ, bombardment target energy density is 0.7~
2.0 J/cm2, 1~5Hz of laser pulse frequency, sedimentation time 10~200 minutes are kept during deposition；
To Bi6Ti3Fe2O18Film carries out situ heat treatment, obtains Bi6Ti3Fe2O18The more epitaxial ferroelectric films of stratiform.
5. preparation method according to claim 4, it is characterised in that according to molar ratio 6.2~6.7: 3 :2 by bismuth
Source, titanium source, source of iron mixing, the bismuth source is bismuthous oxide, and the titanium source is tetravalence titanyl compound, and the source of iron is
Ferric oxide.
6. preparation method according to claim 4 or 5, it is characterised in that the bismuth source, titanium source, the purity of source of iron exist
More than 99.9%.
7. the preparation method according to any one of claim 4 to 6, it is characterised in that described compressing using cold etc.
Static pressure, 150~260MPa of load pressure, 5~20 minutes dwell times.
8. the preparation method according to any one of claim 4 to 7, it is characterised in that the substrate exists for lattice constant
Perovskite structure single crystalline substrate between 3.8~4.0, preferably strontium titanates, lanthanum aluminate, strontium aluminate tantalum neodymium, scandium acid dysprosium, strontium aluminate tantalum
One kind in lanthanum, scandium acid yttrium, lanthanum gallate.
9. preparation method according to any one of claims 4 to 8, it is characterised in that fix substrate with silver paste.
10. the preparation method according to any one of claim 4 to 9, it is characterised in that the situ heat treatment includes：
After growth, oxygen is filled with to 600Torr~1atm, room temperature is down to 5~10 DEG C/min of speed.
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| CN110527954A (en) * | 2019-09-17 | 2019-12-03 | 常州大学 | A kind of LaMnO3Regulate and control Bi4Ti3O12Transition metal oxide ferroelectric thin film of band gap and preparation method thereof |
| CN115506009A (en) * | 2022-09-06 | 2022-12-23 | 哈尔滨工业大学（深圳） | Preparation method of in-situ nitrogen-doped epitaxial oxide single crystal film |
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|---|---|---|---|---|
| CN102167584A (en) * | 2010-12-31 | 2011-08-31 | 扬州大学 | Ferrotitanium bismuth cobaltate ceramic material with five-laminated structure and multiferroic performance and preparation method thereof |
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| CN102167584A (en) * | 2010-12-31 | 2011-08-31 | 扬州大学 | Ferrotitanium bismuth cobaltate ceramic material with five-laminated structure and multiferroic performance and preparation method thereof |
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| Title |
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| ZHANGZHANG CUI ET AL.: "Soft X-ray absorption spectroscopy investigations of Bi6FeCoTi3O18 and LaBi5FeCoTi3O18 epitaxial thin films", 《 JOURNAL OF APPLIED PHYSICS》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110527954A (en) * | 2019-09-17 | 2019-12-03 | 常州大学 | A kind of LaMnO3Regulate and control Bi4Ti3O12Transition metal oxide ferroelectric thin film of band gap and preparation method thereof |
| CN110527954B (en) * | 2019-09-17 | 2021-07-30 | 常州大学 | LaMnO3Control of Bi4Ti3O12Band gap transition metal oxide ferroelectric film and preparation method thereof |
| CN115506009A (en) * | 2022-09-06 | 2022-12-23 | 哈尔滨工业大学（深圳） | Preparation method of in-situ nitrogen-doped epitaxial oxide single crystal film |
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