CN108930017B - La0.7Sr0.3MnO3Preparation method of ferromagnetic thin film - Google Patents

La0.7Sr0.3MnO3Preparation method of ferromagnetic thin film Download PDF

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CN108930017B
CN108930017B CN201810774700.4A CN201810774700A CN108930017B CN 108930017 B CN108930017 B CN 108930017B CN 201810774700 A CN201810774700 A CN 201810774700A CN 108930017 B CN108930017 B CN 108930017B
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冯明
李海波
徐航
赵雪
刘梅
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Jilin Normal University
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Abstract

Depositing on Pb (Mg) by laser pulse deposition method1/3Nb2/3)O3‑PbTiO3Preparation of La on (PMN-PT) Single Crystal surface0.7Sr0.3MnO3The (LSMO) thin film has smooth and compact surface, the surface roughness is lower than 3.2nm, the film thickness is uniform and consistent, the purity is high, and the thin film is compact. The films were observed to exhibit significant ferromagnetic-paramagnetic property changes as the test temperature was varied. Through the change test of the voltage regulation and control magnetic performance, the heterojunction film shows obvious inverse magnetoelectric effect and has better application prospect in the aspects of magnetoelectric memory devices, microwave devices and the like.

Description

La0.7Sr0.3MnO3Preparation method of ferromagnetic thin film
Technical Field
The invention relates to La0.7Sr0.3MnO3A preparation method of ferromagnetic thin film material.
Background
The manganese oxide has extremely high carrier spin polarizability, shows a giant magnetoresistance effect and a magnetic card effect near the Curie temperature, and greatly expands the rare earth manganese oxide LaAEMnO3(AE is doping element, such as Ca, Sr, etc.) the application range of magnetic material, this kind of material has potential application prospect in the aspects of new magnetoelectric memory device, microwave device and logic circuit, etc., therefore receive the extensive attention of the domestic and overseas research units. Meanwhile, with the rapid development of modern electronic information technology, miniaturization and miniaturization become the development trend of novel optical, mechanical, magnetic and electric devices, so that the preparation and application research of the rare earth manganese oxide ferromagnetic film has important scientific significance and great application prospect.
Thin film dependent research and development of applications for magnetic thin filmsA preparation technology. The achievement of high quality thin films is warranted for thin film device applications. Various techniques for preparing magnetic thin films have been proposed. Such as evaporation, ion beam sputtering, magnetron sputtering, molecular beam epitaxy, chemical vapor deposition, sol-gel methods, etc., have characteristics and applications in some fields, but have limitations. Especially for images like La0.7Sr0.3MnO3The preparation of such a compound with a multi-component complex composition is quite difficult, and the mixture ratio of the components is difficult to control accurately. Compared with the preparation method, the pulse laser deposition method has the following advantages: (1) the energy of ablated particles is high, the stoichiometry can be accurately controlled, the components of the target film are close to be consistent, the work of controlling the film components is simplified, and the method is particularly suitable for preparing films with complex components and high melting points: (2) various gases can be introduced in situ during the growth process, and the film can be prepared in a reaction atmosphere, which provides another way for controlling the components of the film: (3) the multi-target assembly is flexible and convenient to change, and a multilayer film and a heterojunction are easy to prepare: (4) the ultraviolet pulse laser with high photon energy and high energy density is adopted as the energy source for generating plasma, so that the plasma generating device is pollution-free and easy to control: (5) simple process, high flexibility and various films.
Disclosure of Invention
The invention aims to solve the problem of preparing La in the prior art0.7Sr0.3MnO3The problems of poor ferromagnetic property, low purity, low density and high sintering temperature in the preparation process of the (LSMO) film are solved, and the pulse laser deposition method with an improved process is provided for preparing the manganese oxide ferromagnetic film with compact and uniform film particles and obvious magnetoelectric reversal effect.
With Pb (Mg)1/3Nb2/3)O3-PbTiO3(PMN-PT) Single Crystal-based La0.7Sr0.3MnO3The preparation method of the (LSMO) ferromagnetic film comprises the following steps:
firstly, adopting pulse laser to La0.7Sr0.3MnO3(LSMO) target material is cleaned for 8-12 min: the laser energy is 200-300mJ, the laser pulse frequency is 5-15Hz, the rotating speed is 3-7r/min, the focal length is 35-40mm, and the laser windowThe diameter of the hole is 1.5 cm;
secondly, the size of the mixture is 4 × 5mm2Pb (Mg) of1/3Nb2/3)O3-PbTiO3The (PMN-PT) single crystal is adhered to 10 × 10mm by conductive silver paste2Putting the nickel block on a heating plate at 120 ℃ and heating for 3-5 min;
thirdly, to stick Pb (Mg)1/3Nb2/3)O3-PbTiO3The nickel block of (PMN-PT) single crystal was placed on a tray and fed into a vacuum chamber with a vacuum degree of 1 × 10-6Torr；
Fourthly, after the temperature of the vacuum chamber is increased to 690 ℃ at the heating rate of 25 ℃/min, pulse laser is adopted to irradiate Pb (Mg)1/ 3Nb2/3)O3-PbTiO3Sputtering La on (PMN-PT) single crystal surface0.7Sr0.3MnO3(LSMO) film, laser energy is 200-300mJ, laser pulse frequency is 5-15Hz, rotating speed is 3-7r/min, focal length is 35-40mm, diameter of laser window hole is 1.5cm, growth oxygen pressure is 100-150mTorr, sputtering time is 20-40 min;
fifthly, after the sputtering is finished, reducing the temperature of the vacuum chamber to 120 ℃, the temperature reduction rate is 25 ℃/min, and then naturally cooling to room temperature to obtain La0.7Sr0.3MnO3(LSMO) ferromagnetic thin films.
Wherein the thickness of the film can be regulated by changing the laser energy or the sputtering time in the fourth step.
The invention selects Pb (Mg)1/3Nb2/3)O3-PbTiO3(PMN-PT) and Si single crystal substrates as La, respectively0.7Sr0.3MnO3Growth substrate for (LSMO) thin film experiments were conducted to find La of thin film grown on PMN-PT single crystal0.7Sr0.3MnO3The (LSMO) density is better, and the PMN-PT single crystal substrate is selected based on the larger electromechanical coupling coefficient k33And piezoelectric constant d33，k33And d3Up to 94% and 2800pC/N, giving the LSMO film a considerable compressive strain.
The invention has the following advantages and positive effects:
1. the manganese oxide ferromagnetic film prepared by the pulse laser deposition method has smooth and compact surface, the surface roughness is lower than 3.2nm, the film thickness is uniform and consistent, the purity is high, and the film is compact.
2. The LSMO thin film grows on the PMN-PT single crystal substrate, so that a good technical effect is achieved, and the thin film shows obvious ferromagnetic-paramagnetic property change along with the change of the test temperature.
3. According to the invention, the LSMO thin film is grown on the PMN-PT single crystal substrate, and through the change test of regulating and controlling Kerr signals by direct current and alternating current voltage, the heterojunction thin film shows an obvious strain-induced inverse magnetoelectric coupling effect.
4. The method has the advantages of simple process, short preparation period, easy operation, low energy consumption, environmental friendliness and easy device integration.
Drawings
FIG. 1 is La0.7Sr0.3MnO3AFM two-dimensional images of thin films grown on (a) single crystal Si and (b) PMN-PT substrates, respectively;
FIG. 2 is La0.7Sr0.3MnO3The film grows on the hysteresis loop of PMN-PT single crystal substrate under different temperatures;
FIG. 3 is La0.7Sr0.3MnO3The film grows on the PMN-PT single crystal substrate and is added with a magneto-optical Kerr loop under positive direct current voltage;
FIG. 4 is La0.7Sr0.3MnO3The film grows on the PMN-PT single crystal substrate under the condition of applying alternating voltage, and the magneto-optical Kerr signal-voltage curve is formed.
Detailed Description
Example (b):
la with PMN-PT single crystal as substrate0.7Sr0.3MnO3The preparation method of the (LSMO) ferromagnetic film comprises the following steps:
firstly, adopting pulse laser to La0.7Sr0.3MnO3(LSMO) target material is cleaned for 8-12 min: the laser energy is 200-300mJ, the laser pulse frequency is 5-15Hz, the rotating speed is 3-7r/min, the focal length is 35-40mm, and the diameter of a laser window hole is 1.5 cm;
secondly, the size of the mixture is 4 × 5mm2Pb (Mg) of1/3Nb2/3)O3-PbTiO3The (PMN-PT) single crystal is adhered to 10 × 10mm by conductive silver paste2Putting the nickel block on a heating plate at 120 ℃ and heating for 3-5 min;
thirdly, putting the nickel block adhered with the PMN-PT single crystal on a tray and feeding the nickel block into a vacuum chamber, and controlling the vacuum degree to be 1 × 10-6Torr；
Fourthly, after the temperature of the vacuum chamber is increased to 690 ℃ at the heating rate of 25 ℃/min, the pulse laser is adopted to sputter La on the surface of the PMN-PT single crystal0.7Sr0.3MnO3(LSMO) film, laser energy is 200-300mJ, laser pulse frequency is 5-15Hz, rotating speed is 3-7r/min, focal length is 35-40mm, laser window hole diameter is 1.5cm, growth oxygen pressure is 100-150mTorr, sputtering time is 20-40 min;
fifthly, after the sputtering is finished, reducing the temperature of the vacuum chamber to 120 ℃, the temperature reduction rate is 25 ℃/min, and then naturally cooling to room temperature to obtain La0.7Sr0.3MnO3(LSMO) ferromagnetic thin films.
Wherein the thickness of the film can be regulated by changing the laser energy or the sputtering time in the fourth step. The invention adopts a pulse laser deposition method to deposit La0.7Sr0.3MnO3The manganese oxide ferromagnetic film prepared by growing the (LSMO) film on the PMN-PT single crystal substrate has smooth and compact surface, the surface roughness is lower than 3.2nm, the film thickness is uniform and consistent, the purity is high, and the film is compact. The films were observed to exhibit significant ferromagnetic-paramagnetic property changes as the test temperature was varied. Through the change test of the voltage regulation Kerr signal, the heterojunction film shows the obvious strain-induced inverse magnetoelectric coupling effect, and has better application prospect in the aspects of magnetoelectric memory devices, microwave devices and the like. As shown in fig. 1(b), 2, 3, 4.
Comparative example:
la with single crystal Si as substrate0.7Sr0.3MnO3The preparation method of the (LSMO) ferromagnetic film comprises the following steps:
firstly, adopting pulse laser to La0.7Sr0.3MnO3(LSMO) target material is cleaned for 8-12 min: laser energy of 200-300mJ, laser pulse frequency5-15Hz, 3-7r/min of rotation speed, 35-40mm of focal length and 1.5cm of diameter of the laser window hole;
secondly, the size of the mixture is 4 × 5mm2The single crystal Si is stuck to 10 × 10mm by conductive silver paste2Putting the nickel block on a heating plate at 120 ℃ and heating for 3-5 min;
thirdly, putting the nickel block adhered with the single crystal Si on a tray and feeding the nickel block into a vacuum chamber, and controlling the vacuum degree to be 1 × 10-6Torr；
Fourthly, after the temperature of the vacuum chamber is raised to 690 ℃ at the heating rate of 25 ℃/min, pulse laser is adopted to sputter an LSMO thin film on the surface of the single crystal Si, the laser energy is 200-300mJ, the laser pulse frequency is 5-15Hz, the rotating speed is 3-7r/min, the focal length is 35-40mm, the diameter of a laser window hole is 1.5cm, the grown oxygen pressure is 100-150mTorr, and the sputtering time is 20-40 min;
fifthly, after the sputtering is finished, reducing the temperature of the vacuum chamber to 120 ℃, the temperature reduction rate is 25 ℃/min, and then naturally cooling to room temperature to obtain La0.7Sr0.3MnO3(LSMO) ferromagnetic thin films.
Wherein the thickness of the film can be regulated by changing the laser energy or the sputtering time in the fourth step. The invention adopts a pulse laser deposition method to deposit La0.7Sr0.3MnO3The manganese oxide ferromagnetic film prepared by growing the (LSMO) film on the monocrystal Si substrate has rough surface, the surface roughness is higher than 5.3nm, and the film thickness is not uniform and not dense.

Claims (4)

1. La0.7Sr0.3MnO3The preparation method of the ferromagnetic film comprises the following steps:
firstly, adopting pulse laser to La0.7Sr0.3MnO3And (3) cleaning the target material for 8-12 min: the laser energy is 200-300mJ, the laser pulse frequency is 5-15Hz, the rotating speed is 3-7r/min, the focal length is 35-40mm, and the diameter of a laser window hole is 1.5 cm;
secondly, the size of the mixture is 4 × 5mm2Pb (Mg) of1/3Nb2/3)O3-PbTiO3The (PMN-PT) single crystal is adhered to 10 × 10mm by conductive silver paste2Putting the nickel block on a heating plate at 120 ℃ and heating for 3-5 min;
thirdly, to stick Pb (Mg)1/3Nb2/3)O3-PbTiO3The nickel block of (PMN-PT) single crystal was placed on a tray and fed into a vacuum chamber with a vacuum degree of 1 × 10-6Torr；
Fourthly, after the temperature of the vacuum chamber is raised to 690 ℃ at the heating rate of 25 ℃/min, pulse laser is adopted to sputter an LSMO thin film on the surface of the PMN-PT single crystal, the laser energy is 260mJ, the laser pulse frequency is 10Hz, the rotating speed is 5r/min, the focal length is 37mm, the diameter of a laser window hole is 1.5cm, the growing oxygen pressure is 130mTorr, and the sputtering time is 20-40 min;
fifthly, after the sputtering is finished, reducing the temperature of the vacuum chamber to 120 ℃, the temperature reduction rate is 25 ℃/min, and then naturally cooling to room temperature to obtain La0.7Sr0.3MnO3A ferromagnetic thin film.
2. The La of claim 10.7Sr0.3MnO3And the preparation method of the ferromagnetic film, wherein the laser energy or sputtering time of the step four is changed to regulate and control the thickness of the film.
3. The La of claim 10.7Sr0.3MnO3And the preparation method of the ferromagnetic film, wherein the sputtering time of the step four is 30 min.
4. La0.7Sr0.3MnO3A ferromagnetic thin film prepared by the method of any one of claims 1-3.
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CN110451961A (en) * 2019-08-23 2019-11-15 昆明理工大学 A kind of preparation method of Ag doping lanthanum calcium manganese oxygen polycrystalline ceramics target
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CN104451544A (en) * 2014-11-17 2015-03-25 中国科学院上海硅酸盐研究所 Lead-free magnetoelectric composite film and preparation method thereof

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CN104451544A (en) * 2014-11-17 2015-03-25 中国科学院上海硅酸盐研究所 Lead-free magnetoelectric composite film and preparation method thereof

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* Cited by examiner, † Cited by third party
Title
Voltage-controlled epitaxial strain in La0.7Sr0.3MnO3/Pb(Mg1/3Nb2/3)O3-PbTiO3(001) films;C.Thiele et.al.;《APPLIED PHYSICS LETTERS》;20051226;第87卷(第26期);262502-1页右栏 *
多铁性La0.7Sr0.3MnO3/PMN-PT复合薄膜的制备及表征;苟喜成;《吉林师范大学学报》;20120531(第2期);全文 *

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