CN102586747A - Preparation method of (BiFe03) m/(La0.7Sr0.3Mn03)n multi-layer film - Google Patents
Preparation method of (BiFe03) m/(La0.7Sr0.3Mn03)n multi-layer film Download PDFInfo
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- CN102586747A CN102586747A CN2012100653390A CN201210065339A CN102586747A CN 102586747 A CN102586747 A CN 102586747A CN 2012100653390 A CN2012100653390 A CN 2012100653390A CN 201210065339 A CN201210065339 A CN 201210065339A CN 102586747 A CN102586747 A CN 102586747A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 36
- 238000000151 deposition Methods 0.000 claims abstract description 28
- 239000000758 substrate Substances 0.000 claims abstract description 28
- 229910002182 La0.7Sr0.3MnO3 Inorganic materials 0.000 claims abstract description 23
- 230000008021 deposition Effects 0.000 claims abstract description 23
- 238000000034 method Methods 0.000 claims abstract description 20
- 229910052786 argon Inorganic materials 0.000 claims abstract description 18
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000001301 oxygen Substances 0.000 claims abstract description 18
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 18
- 229910002075 lanthanum strontium manganite Inorganic materials 0.000 claims description 39
- 239000007789 gas Substances 0.000 claims description 17
- 239000000463 material Substances 0.000 claims description 15
- 238000004544 sputter deposition Methods 0.000 claims description 14
- 229910002367 SrTiO Inorganic materials 0.000 claims description 13
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 8
- 229910052710 silicon Inorganic materials 0.000 claims description 8
- 239000010703 silicon Substances 0.000 claims description 8
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- 238000004140 cleaning Methods 0.000 claims description 3
- 235000011194 food seasoning agent Nutrition 0.000 claims description 3
- 238000007654 immersion Methods 0.000 claims description 3
- 238000001755 magnetron sputter deposition Methods 0.000 abstract description 4
- 230000005291 magnetic effect Effects 0.000 abstract description 3
- 238000003860 storage Methods 0.000 abstract description 2
- 229910002370 SrTiO3 Inorganic materials 0.000 abstract 2
- 238000009987 spinning Methods 0.000 abstract 1
- 239000010408 film Substances 0.000 description 71
- 230000000630 rising effect Effects 0.000 description 6
- 238000002441 X-ray diffraction Methods 0.000 description 5
- 238000012876 topography Methods 0.000 description 5
- 230000007704 transition Effects 0.000 description 3
- JTCFNJXQEFODHE-UHFFFAOYSA-N [Ca].[Ti] Chemical compound [Ca].[Ti] JTCFNJXQEFODHE-UHFFFAOYSA-N 0.000 description 2
- 230000005290 antiferromagnetic effect Effects 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 229910052779 Neodymium Inorganic materials 0.000 description 1
- 229910052777 Praseodymium Inorganic materials 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 230000005621 ferroelectricity Effects 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 229910052746 lanthanum Inorganic materials 0.000 description 1
- 230000005690 magnetoelectric effect Effects 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 238000004549 pulsed laser deposition Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 238000012916 structural analysis Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000000427 thin-film deposition Methods 0.000 description 1
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Abstract
The invention discloses a preparation method of a (BiFe03) m/(La0.7Sr0.3Mn03)n multi-ferroic film, which adopts a magnetron sputtering method. A substrate is fixed, vacuum is pumped, argon and oxygen with certain volume flow ratio are introduced, pressure is adjusted to a certain value, substrate temperature is set, a radio source is started to build up luminance, after parameters of various aspects of a machine are stabilized for a period of time, a sample wafer baffle is opened to deposit a film, after alternative deposition is conducted for four periods, the radio source is closed, and build-up of luminance is stopped. A sample obtained on a SrTiO3 (STO) substrate is a [(BiFe03)20/(La0.7Sr0.3MnO3)10]4 multi-layer film. The preparation method has the advantages of being strong in process controllability, easy to operate, low in cost and high in purity of obtained products. Products obtained through the preparation method are widely used in the fields of information storage, spinning electron devices, magnetic sensors and the like.
Description
Technical field
The present invention relates to a kind of preparation method of multi-iron material film, specifically be meant a kind of (BiFeO
3) m/ (La
0.7Sr
0.3MnO
3) preparation method of n multilayered film material.
Technical background
Multi-iron material BiFeO
3(BFO) be that existing occurring in nature at room temperature has one of ferroelectricity and anti-ferromagnetic minority monophase materials simultaneously, its ferroelectric curie transition temperature T
C～1100K, the antiferromagnetic Nai Er transition temperature of G-type T
N～673K, consequent magneto-electric coupled character and magnetoelectric effect make it in fields such as information storage, spin electric device, Magnetic Sensors wide application prospect arranged.The another kind of material that receives scientific circles and industry member extensive concern is the rear-earth-doped Mn oxide R of calcium titanium ore structure that unique electricity, magnetic and structural phase transition characteristic are arranged
1-xA
xMnO
3(R=La, Pr, Nd, A=Ca, Sr, Ba).This type Mn oxide all has the potential application prospect in various recording units, transmitter, infrared eye.BiFeO
3Crystalline structure is similar with the rear-earth-doped Mn oxide of calcium titanium ore structure, possibly prepare high-quality epitaxial film.People's expectation utilizes La
0.7Sr
0.3MnO
3(LSMO) material and BiFeO
3(BFO) material prepn goes out to have the [(BiFeO of new features
3) m/ (La
0.7Sr
0.3MnO
3) n] the x superstructure, wherein m is the thickness (unit is a nanometer) of every layer of BFO film, and n is the thickness (unit is a nanometer) of every layer of LSMO film, and x is (BiFeO
3) m/ (La
0.7Sr
0.3MnO
3) cycle life of n.
As everyone knows, BiFeO
3The serious electric leakage problems affect of material its application development aspect electron device.Theoretical investigation shows, BiFeO
3Band gap width be 2.8ev, thereby the electric leakage be not its intrinsic property, should be the defective in the film preparation process, factors such as non-stoichiometric cause.Can reduce its electric leakage through the mode of chemical doping.People such as Raniith have studied BiFeO
3/ SrTiO
3Superlattice find that its electric leakage has improvement significantly.In addition, other mode of employing is also arranged to reduce the report of BFO electric leakage, as BFO being combined with other insulating material and being prepared into superstructure etc.But, utilize magnetron sputtering method preparation [(BiFeO
3)
20/ (La
0.7Sr
0.3MnO
3)
10]
4(wherein 20 is the thickness 20nm of every layer of BFO film to multilayer film, and 10 is the thickness 10nm of every layer of LSMO film, and 4 is (BiFeO
3) m/ (La
0.7Sr
0.3MnO
3) cycle life of n) material report not also.
Summary of the invention
The present invention is directed to deficiency of the prior art, proposed a kind of convenience, effective preparation method.
The present invention is achieved through following technical proposals:
A kind of (BiFeO
3) m/ (La
0.7Sr
0.3MnO
3) preparation method of n multilayered film material, it is characterized in that, comprise the steps:
(1) will cleaned SrTiO
3For substrate is fixed on the supporting plate, vacuumize behind good each air valve in pass, reach 1.0 * 10 until vacuum tightness
-4More than the Pa, feed argon gas and oxygen, regulate the molecular pump slide valve, air pressure is adjusted to 1-3Pa;
(2) setting underlayer temperature is 700-750 ℃, opens the radio frequency source build-up of luminance, and sputtering power is respectively 100-110W to the preparatory sputter of target 5 minutes, and the radio frequency power that raises then carries out sputter to 115-120W;
(3) treat machine each side parameter stability after; Earlier at SrTiO
3On the substrate through sputter, deposition LSMO film; Cover half the LSMO film zone with silicon chip then, again with sputter, deposition BFO film;
The alternating deposit process that deposits the BFO film by the above-mentioned LSMO of deposition earlier film, is again carried out 4 cycles, closes radio frequency source, stops build-up of luminance, at SrTiO
3The gained sample is [(BiFeO on the substrate
3)
20/ (La
0.7Sr
0.3MnO
3)
10]
4Multilayered film material.
Abbreviate as accordingly among the present invention: SrTiO
3Be STO, La
0.7Sr
0.3MnO
3Be LSMO, BiFeO
3Be BFO.
As preferably, SrTiO in above-mentioned preparing method's step (1)
3Cleaning process be: use earlier alcohol immersion SrTiO
3Sheet, and use ultrasonic cleaning 10min, use deionized water rinsing again, soak, use ultrasonic cleaning 10min again with acetone then, use deionized water rinsing, afterwards seasoning.
As preferably, target and substrate are apart from being 100mm in above-mentioned preparing method's step (1).
As preferably, in above-mentioned preparing method's step (1) at the bottom of the back of the body of sputtering chamber vacuum tightness be 1.0 * 10
-4Pa.
As preferably, during deposition LSMO, the volume flow ratio of argon gas and oxygen was respectively 16: 4 in above-mentioned preparing method's step (3); During deposition BFO film, the volume flow ratio of argon gas and oxygen was respectively 14: 6.
As preferably, the operating air pressure in above-mentioned preparing method's step (3) when deposition LSMO and BFO film is respectively 1.2Pa and 2.5Pa.
As preferably, the sputtering power in above-mentioned preparing method's step (3) when deposition LSMO and BFO film is respectively 100-110W and 115-120W.
As preferably, the sputtering time when each deposition LSMO is with each deposition BFO film in above-mentioned preparing method's step (3) is respectively 30min and 16min.
SrTiO is adopted in film preparation among the present invention
3(STO) be substrate, its cleaning process is: earlier with alcohol immersion STO sheet, and use ultrasonic cleaning 10min, wash repeatedly with deionized water; Soak with acetone then, ultrasonic cleaning 10min washes with deionized water repeatedly; With remove the surface all contaminations, seasoning afterwards, subsequent use.Thin film deposition adopts magnetron sputtering method in ball-type pulsed laser deposition composite deposition system (PLD450E), to carry out.BFO and LSMO raw material employing purity are 99.99% ceramic target, and two kinds of material alternating sputterings are to the STO substrate of 5mm * 10mm (001) orientation.[(BiFeO
3)
20/ (La
0.7Sr
0.3MnO
3)
10]
4The preparation process of multilayer film: cleaned substrate is fixed in the sample holder, vacuumizes behind good each air valve in pass, reach 1.0 * 10 until vacuum tightness
-4More than the Pa, feed the argon gas and the oxygen of certain volume throughput ratio, regulate the molecular pump slide valve; Air pressure is adjusted to certain value, set underlayer temperature, open the radio frequency source build-up of luminance; With lower-wattage respectively to the preparatory sputter of target 5 minutes; The rising radio frequency power is treated machine each side parameter stability for some time, opens the print baffle plate and begins deposit film.Deposition LSMO film on the STO substrate behind the deposition certain hour, covers half the LSMO film zone with silicon chip earlier, changes parameter then, deposition BFO film, and 4 all after dates of alternating deposit are closed radio frequency source, stop build-up of luminance.The processing parameter of film preparation remains unchanged when preparation film of the same race, and the total thickness of film is not more than 200nm.The gained sample is [(BiFeO on the STO substrate
3)
20/ (La
0.7Sr
0.3MnO
3)
10]
4Multilayered film material.
The present invention prepares in the process, and used ceramic target is commerical prod, need not loaded down with trivial details preparation; Process controllability is strong, and is easy to operate, and cost is low, and the product purity that makes is high.
Description of drawings
Fig. 1 makes [(BiFeO with the present invention
3)
20/ (La
0.7Sr
0.3MnO
3)
10]
4The X-ray diffraction of multilayer film (XRD) spectrogram;
Fig. 2 makes [(BiFeO with the present invention
3)
20/ (La
0.7Sr
0.3MnO
3)
10]
4The AFM of multilayer film (AFM) photo;
Fig. 3 makes [(BiFeO with the present invention
3)
20/ (La
0.7Sr
0.3MnO
3)
10]
4The transmission electron microscope of multilayer film (TEM) photo;
Embodiment
Further specify the present invention below in conjunction with instance.
Embodiment 1
Cleaned STO substrate is fixed in the sample holder, vacuumizes behind good each air valve in pass, reach 1.0 * 10 until vacuum tightness
-4More than the Pa, the feeding volume flow ratio is 16: 4 argon gas and an oxygen, regulates the molecular pump slide valve, and air pressure is adjusted to 1.2Pa; Setting underlayer temperature is 750 ℃, opens the radio frequency source build-up of luminance, and respectively to the preparatory sputter of target 5 minutes, the rising radio frequency power is to 100W with lower-wattage; Treat machine each side parameter stability for some time, open the print baffle plate and begin to deposit the LSMO film, behind the deposition 30min, cover half the LSMO film zone with silicon chip; The volume flow ratio that changes argon gas and oxygen is 14: 6, and sputtering power and time are respectively 120W, 16min, begin to deposit the BFO film; Altogether 4 cycles of alternating deposit LSMO and BFO film, close radio frequency source at last, stop build-up of luminance.The gained sample is [(BiFeO on the STO substrate
3)
20/ (La
0.7Sr
0.3MnO
3)
10]
4Multilayer film.Adopt the X-ray diffraction method that the gained film is carried out structural analysis.Fig. 1 is the XRD figure spectrum of gained multilayer film.As can be seen from the figure, except that (001) and (002) diffraction peak of BFO and LSMO film, do not see other dephasign diffraction peaks, this explanation uses radio frequency magnetron sputtering method to prepare along the crystalline state multilayer film of (001) direction growth.In the interior illustration of XRD figure spectrum, can also observe the characteristic satellites that superlattice have, explain that the gained multilayer film have formed superstructure.Fig. 2 is the AFM photo of gained film; Show that the upper current conducting cap that is grown in multilayer film on STO < 001>substrate is different with the roughness and the surface topography of lower conducting dome; As can be seen from the figure the surface irregularity of upper current conducting cap and crystal grain are bigger, and the surface of lower conducting dome is smooth relatively and crystal grain is less.Fig. 3 is the TEM photo of gained multilayer film.The clear interface of LSMO layer and BFO layer and LSMO layer and STO substrate as we can see from the figure can obtain simultaneously the thickness of each sublayer, shows that its periodic thickness can accurately control by the control sedimentation time.
As embodiment 1, cleaned STO substrate is fixed in the sample holder, vacuumize behind good each air valve in pass, reach 1.0 * 10 until vacuum tightness
-4More than the Pa, the feeding volume flow ratio is 16: 4 argon gas and an oxygen, regulates the molecular pump slide valve, and air pressure is adjusted to 1.2Pa; Setting underlayer temperature is 750 ℃, opens the radio frequency source build-up of luminance, and respectively to the preparatory sputter of target 5 minutes, the rising radio frequency power is to 110W with lower-wattage; Treat machine each side parameter stability for some time, open the print baffle plate and begin to deposit the LSMO film, behind the deposition 30min, cover half the LSMO film zone with silicon chip; The volume flow ratio that changes argon gas and oxygen is 14: 6, and sputtering power and time are respectively 115W, 16min, begin to deposit the BFO film; Altogether 4 cycles of alternating deposit LSMO and BFO film, close radio frequency source at last, stop build-up of luminance.The gained sample is [(BiFeO on the STO substrate
3)
20/ (La
0.7Sr
0.3MnO
3)
10]
4Multilayer film.The structure of gained film, surface topography are all identical with embodiment 1.
Embodiment 3
As embodiment 1, cleaned STO substrate is fixed in the sample holder, vacuumize behind good each air valve in pass, reach 1.0 * 10 until vacuum tightness
-4More than the Pa, the feeding volume flow ratio is 16: 4 argon gas and an oxygen, regulates the molecular pump slide valve, and air pressure is adjusted to 1.2Pa; Setting underlayer temperature is 700 ℃, opens the radio frequency source build-up of luminance, and respectively to the preparatory sputter of target 5 minutes, the rising radio frequency power is to 110W with lower-wattage; Treat machine each side parameter stability for some time, open the print baffle plate and begin to deposit the LSMO film, behind the deposition 30min, cover half the LSMO film zone with silicon chip; The volume flow ratio that changes argon gas and oxygen is 14: 6, and sputtering power and time are respectively 120W, 16min, begin to deposit the BFO film; Altogether 4 cycles of alternating deposit LSMO and BFO film, close radio frequency source at last, stop build-up of luminance.The gained sample is [(BiFeO on the STO substrate
3)
20/ (La
0.7Sr
0.3MnO
3)
10]
4Multilayer film.The structure of gained film, surface topography are all identical with embodiment 1.
As embodiment 1, cleaned STO substrate is fixed in the sample holder, vacuumize behind good each air valve in pass, reach 1.0 * 10 until vacuum tightness
-4More than the Pa, the feeding volume flow ratio is 16: 4 argon gas and an oxygen, regulates the molecular pump slide valve, and air pressure is adjusted to 1.2Pa; Setting underlayer temperature is 750 ℃, opens the radio frequency source build-up of luminance, and respectively to the preparatory sputter of target 5 minutes, the rising radio frequency power is to 100W with lower-wattage; Treat machine each side parameter stability for some time, open the print baffle plate and begin to deposit the LSMO film, behind the deposition 30min, cover half the LSMO film zone with silicon chip; The volume flow ratio that changes argon gas and oxygen is 14: 6, and sputtering power and time are respectively 115W, 16min, begin to deposit the BFO film; Altogether 4 cycles of alternating deposit LSMO and BFO film, close radio frequency source at last, stop build-up of luminance.The gained sample is [(BiFeO on the STO substrate
3)
20/ (La
0.7Sr
0.3MnO
3)
10]
4Multilayer film.The structure of gained film, surface topography are all identical with embodiment 1.
Embodiment 5
As embodiment 1, cleaned STO substrate is fixed in the sample holder, vacuumize behind good each air valve in pass, reach 1.0 * 10 until vacuum tightness
-4More than the Pa, the feeding volume flow ratio is 16: 4 argon gas and an oxygen, regulates the molecular pump slide valve, and air pressure is adjusted to 1.2Pa; Setting underlayer temperature is 700 ℃, opens the radio frequency source build-up of luminance, and respectively to the preparatory sputter of target 5 minutes, the rising radio frequency power is to 110W with lower-wattage; Treat machine each side parameter stability for some time, open the print baffle plate and begin to deposit the LSMO film, behind the deposition 30min, cover half the LSMO film zone with silicon chip; The volume flow ratio that changes argon gas and oxygen is 14: 6, and sputtering power and time are respectively 115W, 16min, begin to deposit the BFO film; Altogether 4 cycles of alternating deposit LSMO and BFO film, close radio frequency source at last, stop build-up of luminance.The gained sample is [(BiFeO on the STO substrate
3)
20/ (La
0.7Sr
0.3MnO
3)
10]
4Multilayer film.The structure of gained film, surface topography are all identical with embodiment 1.
Claims (8)
1. (BiFeO
3) m/ (La
0.7Sr
0.3MnO
3) preparation method of n multilayered film material, it is characterized in that, comprise the steps:
(1) will cleaned SrTiO
3For substrate is fixed on the supporting plate, vacuumize behind good each air valve in pass, reach 1.0 * 10 until vacuum tightness
-4More than the Pa, feed argon gas and oxygen, regulate the molecular pump slide valve, air pressure is adjusted to 1-3Pa;
(2) setting underlayer temperature is 700-750 ℃, opens the radio frequency source build-up of luminance, and sputtering power is respectively 100-110W to the preparatory sputter of target 5 minutes, and the radio frequency power that raises then carries out sputter to 115-120W;
(3) treat machine each side parameter stability after; Earlier at SrTiO
3On the substrate through sputter, deposition LSMO film; Cover half the LSMO film zone with silicon chip then, again with sputter, deposition BFO film;
The alternating deposit process that deposits the BFO film by the above-mentioned LSMO of deposition earlier film, is again carried out 4 cycles, closes radio frequency source, stops build-up of luminance, at SrTiO
3The gained sample is [(BiFeO on the substrate
3)
20/ (La
0.7Sr
0.3MnO
3)
10]
4Multilayered film material.
2. preparation method according to claim 1 is characterized in that SrTiO in the step (1)
3Cleaning process be: use earlier alcohol immersion SrTiO
3Sheet, and use ultrasonic cleaning 10min, use deionized water rinsing again, soak, use ultrasonic cleaning 10min again with acetone then, use deionized water rinsing, afterwards seasoning.
3. preparation method according to claim 1 is characterized in that middle target of step (1) and substrate distance are 100mm.
4. preparation method according to claim 1 is characterized in that vacuum tightness is 1.0 * 10 at the bottom of the back of the body of sputtering chamber in the step (1)
-4Pa.
5. preparation method according to claim 1, when it is characterized in that depositing LSMO in the step (3), the volume flow ratio of argon gas and oxygen was respectively 16: 4; During deposition BFO film, the volume flow ratio of argon gas and oxygen was respectively 14: 6.
6. preparation method according to claim 1, the operating air pressure when it is characterized in that depositing LSMO and BFO film in the step (3) is respectively 1.2Pa and 2.5Pa.
7. preparation method according to claim 1, the sputtering power when it is characterized in that depositing LSMO and BFO film in the step (3) is respectively 100-110W and 115-120W.
8. preparation method according to claim 1 is characterized in that the sputtering time when depositing LSMO in the step (3) at every turn and depositing the BFO film at every turn is respectively 30min and 16min.
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| CN113539654A (en) * | 2020-04-13 | 2021-10-22 | 中国科学院宁波材料技术与工程研究所 | Method for regulating and enhancing magnetic anisotropy of LSMO thin film, LSMO thin film with adjustable magnetic anisotropy and preparation method thereof |
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| CN102162086A (en) * | 2011-03-28 | 2011-08-24 | 浙江理工大学 | Preparation method of TiO2/SiO2 composite film |
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| CN102162086A (en) * | 2011-03-28 | 2011-08-24 | 浙江理工大学 | Preparation method of TiO2/SiO2 composite film |
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| CN103199105B (en) * | 2013-04-11 | 2015-11-18 | 浙江理工大学 | A kind of multi-iron material ferrous acid terbium p-n heterojunction, Preparation method and use |
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