CN114775061A - Preparation method of opposite-target magnetron sputtering epitaxial iron-tin alloy film - Google Patents

Preparation method of opposite-target magnetron sputtering epitaxial iron-tin alloy film Download PDF

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CN114775061A
CN114775061A CN202210408699.XA CN202210408699A CN114775061A CN 114775061 A CN114775061 A CN 114775061A CN 202210408699 A CN202210408699 A CN 202210408699A CN 114775061 A CN114775061 A CN 114775061A
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米文博
张栋曜
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Tianjin University
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Abstract

The invention relates to a method for preparing an epitaxial iron-tin alloy film by opposite target magnetron sputtering, wherein Al is2O3(0001) Fe is epitaxially grown on a single crystal substrate3Sn2A film; fe is epitaxially grown on a MgO (111) single crystal substrate3Sn2A film. Adopting magnetron sputtering method to successfully prepare epitaxial Fe3Sn2A film. Has the advantages of simple target material selection, high target material utilization rate and the like. Grown Fe3Sn2The Hall resistivity gradient of a high magnetic field area in the out-of-plane direction of the film changes from negative to positive along with the temperature rise; the abnormal Hall resistivity has a hysteresis characteristic along with the change of a magnetic field; exhibiting a topological hall effect. The magnetron sputtering growth method is beneficial to expanding industrial production and reducing production cost; epitaxial growth of Fe directly on single crystal substrates3Sn2The film is beneficial to researching Fe3Sn2Intrinsic magnetic and electric transport properties of the thin film; the obtained crystal has high quality; has potential value in the preparation of novel topological spintronics devices.

Description

Preparation method of opposite-target magnetron sputtering epitaxial iron-tin alloy film
Technical Field
The invention relates to a method for preparing epitaxial iron-tin alloy (Fe) by using opposite target magnetron sputtering3Sn2) A method for preparing a film, in particular to a magnetron sputtering preparation method which relates to simple target material selection.
Background
Physical phenomena such as frustrated magnetic structure, non-zero Bery curvature, etc. can be induced in magnetic materials with hexagonal kagome lattices of special symmetry. These novel physical phenomena can bring about abnormal hall effect and topological hall effect to the material; anomalous electron transport properties such as anomalous Nernst effect, topological Nernst effect, etc.; it may also cause a change in the band structure such that structures such as dirac cones, alien cross lines, etc. appear in its band, giving the material a so-called zero-mass alien fermi. In the kagome lattice, moreover, some special magnetic structures such as magnetic skammer, skammer bubbles, etc. are also induced, supported by the dipole interaction competing with the uniaxial magnetic anisotropy. The novel physical phenomena are provided, so that the application of the novel physical phenomena in the spin electronic device has bright prospect.
2009, Fe3Sn2Magnetic structures of medium non-collinear and spin frustration were first reported. Fe3Sn2Magnetic skyrmion structure of (1), p-Fe3Sn2Regulation of the sigramin vesicles in nanostrips has also been reported. Furthermore, recent research hotspots such as dirac fermi, ectole node, flat band, and topological hall effect continue in Fe3Sn2Is found in (1) so that Fe3Sn2Becomes an ideal platform for researching topological spintronics. Fe3Sn2Has a lattice structure consisting of a layer of Fe of kagome structure3Sn is overlapped with Sn with two layers of honeycomb structures, and the space group is
Figure BDA0003603189240000011
Belonging to the hexagonal system, in-plane latticeConstant number
Figure BDA0003603189240000012
Out-of-plane lattice constant
Figure BDA0003603189240000013
Figure BDA0003603189240000014
Fe3Sn2The ferromagnetism of the (C) has better thermal stability, the Curie temperature of the (C) is 670K, and the saturation magnetization at 2K is 650emu/cm3Saturation magnetization of about 600emu/cm at room temperature3。
Fe3Sn2Most of the research objects in the report are bulk materials, and the thin film materials can show more novel physical phenomena due to the limitation of low dimensionality; and the magnetron sputtering epitaxial growth is more beneficial to the rapid and large-scale preparation of materials. Preparation of epitaxial Fe in the laboratory3Sn2In the case of thin films, a buffer layer is used between the thin film and the substrate, which greatly influences the Fe epitaxial growth3Sn2Investigation of the intrinsic electrical transport properties and magnetic properties of thin films, such as Khadka et al, Phys.Rev.Mater.2020, Vol.4, No. 8, reference 084203. Direct preparation of epitaxial Fe without buffer layer growth on substrate3Sn2Thin films remain a technical challenge.
Disclosure of Invention
From the industrial production point of view, it is desirable to use sputtering methods and to use as simple a target as possible for the preparation of epitaxial Fe3Sn2A film. In view of the above object, the present invention has been made to develop a magnetron sputtering epitaxial Fe on a facing target3Sn2A method for preparing a film.
The specific invention is as follows.
Epitaxial Fe prepared by magnetron sputtering of opposite targets3Sn2Film of structure Fe3Sn2/Al2O3Or Fe3Sn2and/MgO. Said Fe3Sn2/Al2O3The structure is as follows: in Al2O3(0001) Single crystalFe is epitaxially grown on the substrate3Sn2A film; said Fe3Sn2The structure of/MgO is: fe is epitaxially grown on a MgO (111) single crystal substrate3Sn2A film.
Opposite target magnetron sputtering epitaxial Fe3Sn2The preparation method of the film is characterized by comprising the following steps:
1) adopts an ultrahigh vacuum facing target magnetron sputtering coating machine, and the substrate material is [0001 ]]Oriented Al2O3The single crystal substrate or base material is [111 ]]An oriented MgO single crystal substrate; two pieces of Fe with a purity of 99.99% were used3Sn2Targets respectively arranged on the two groups of opposite target heads; in each group of opposite targets, one end is used as the N pole of the magnetic force line, and the other end is used as the S pole; mounting the substrate on the midperpendicular of the connection line of the facing targets, the substrate and the facing Fe3Sn2The vertical distance of the connecting line between the targets is 60-90 mm;
2) starting the facing target magnetron sputtering equipment, starting the first-stage mechanical pump and the second-stage molecular pump to perform vacuum pumping successively until the vacuum degree of the back bottom of the sputtering chamber is less than or equal to 2.5 multiplied by 10–5Pa；
3) Raising the temperature of the substrate to 350-450 ℃ at a speed of 20-25 ℃/min by using a temperature control system;
4) introducing sputtering gas Ar with the purity of 99.999 percent into the vacuum chamber, and keeping the vacuum degree of the sputtering chamber at 1.8-2.2Pa and stabilizing for 5-15 minutes by adjusting the opening degree of the ultrahigh vacuum gate valve;
5) starting the sputtering power supply to a pair of Fe3Sn2Applying 0.02-0.20A current and 800-900V direct current voltage on the target, and pre-sputtering for 10-20 minutes;
6) opening of Fe3Sn2The baffle between the target side and the substrate starts sputtering until Fe3Sn2The thickness of the film is 70-90 nm;
7) after the sputtering is finished, the Fe is closed3Sn2And (3) blocking a baffle plate between the side surface of the target and the substrate, then closing a sputtering power supply, stopping introducing the sputtering gas Ar, completely opening a gate valve, and continuously vacuumizing to reduce the temperature of the substrate to room temperature at the speed of 2-5 ℃/min.
Epitaxial Fe in accordance with the present invention3Sn2The preparation method of the film adopts a magnetron sputtering method to successfully prepare epitaxial Fe3Sn2A film. The method has the advantages of simple target material selection, high target material utilization rate and the like, and has potential value in the preparation of novel topological spintronics devices.
To confirm the best embodiment of the invention, we have prepared Fe according to the invention3Sn2The structure and properties of the thin film were analyzed in detail by means of X-ray diffraction, atomic force microscopy, pole figures, and the like.
In the present invention, Al is contained in2O383nm thick epitaxial Fe prepared above3Sn2As can be seen from the X-ray diffraction pattern of the film, Fe appears3Sn2Diffraction peak of (0009) plane of (B), indicating that Fe3Sn2Film edge [0001 ]]Directionally grow as shown in fig. 1.
83nm thick epitaxial Fe prepared on MgO from the present invention3Sn2As can be seen from the X-ray diffraction pattern of the film, Fe appears3Sn2The diffraction peak of (0009) plane of (B) indicates Fe3Sn2Film edge [0001 ]]Directionally oriented growth, as shown in fig. 2.
In the present invention, Al is2O383nm thick epitaxial Fe prepared above3Sn2As can be seen from the pole figure of the thin film, Fe appears3Sn2Is/are as follows
Figure BDA0003603189240000022
Four-fold symmetrical peak of crystal face, which shows Fe3Sn2The film is epitaxially grown as shown in fig. 3.
83nm thick epitaxial Fe prepared on MgO from the present invention3Sn2As can be seen from the pole figure of the film, Fe appears3Sn2Is
Figure BDA0003603189240000021
Four-fold symmetrical peak of crystal face, description Fe3Sn2The film is epitaxially grown as shown in fig. 4.
The invention measures Al at different temperatures2O3150 nm thick epitaxial Fe prepared above3Sn2The Hall resistivity of the film is in a change relation with an external magnetic field, and the direction of the magnetic field is vertical to the surface of the film. In the present invention, Fe is found for the first time3Sn2The slope of the Hall resistivity of the high magnetic field region in the out-of-plane direction of the film changes from negative to positive with the temperature rise, as shown in FIG. 5;
the invention measures Al at room temperature2O3Epitaxial Fe of different thickness prepared above3Sn2The topological Hall resistivity of the film is in a change relation with an external magnetic field, and the direction of the magnetic field is vertical to the surface of the film. Fe3Sn2The topological Hall resistivity of the low magnetic field area outside the film surface is firstly reduced and then increased along with the increase of the magnetic field, and the topological Hall resistivity is increased along with the Fe3Sn2The topological hall resistivity characteristics of (a) are consistent as shown in fig. 6.
The invention relates to opposite target magnetron sputtering epitaxial Fe3Sn2The preparation method of the film mainly has the following advantages:
1) fe currently used for research3Sn2Mainly bulk single crystal, with little Fe3Sn2The films were used for the study. The invention successfully prepares epitaxial Fe on the substrate by a sputtering method3Sn2Thin film, and reported epitaxial Fe with buffer layer3Sn2Film [ Phys. Rev. Mater.,4,084203(2020)]In contrast, in the case of Fe3Sn2The film has obvious advantages in research and industrial production of intrinsic magnetism and electric transport characteristics;
2) the target material is simple to select, and the invention adopts pure Fe3Sn2Preparation of epitaxial Fe with target as target material3Sn2A film, which is easily available from industrial production;
3) first found Fe3Sn2The slope of the Hall resistivity of a high magnetic field area in the out-of-plane direction of the film changes from negative to positive along with the rise of temperature, and the abnormal Hall resistivity has hysteresis characteristics along with the change of a magnetic field and has topologyThe hall effect, presents great potential in new topological spintronics.
4) The experimental conditions involved in the invention are all carefully adjusted to prepare Fe3Sn2The conditions for epitaxial thin films are very stringent: when the vacuum degree of the back bottom is too high, impurities can appear in the film; when the substrate temperature is too low, Fe3Sn2Will not crystallize; when the substrate temperature is too high or the sputtering pressure is too low, Fe exists in the film5Sn3The presence of ingredients; when the sputtering current voltage is too large, too fast a growth rate will cause Fe3Sn2The crystal quality of (2) is lowered.
Drawings
FIG. 1 shows Al2O383nm thick Fe prepared above3Sn2X-ray diffraction pattern of the film.
FIG. 2 shows 83nm thick Fe prepared on MgO3Sn2X-ray diffraction pattern of the film.
FIG. 3 shows Al2O383nm thick Fe prepared above3Sn2Pole figure of the film.
FIG. 4 shows 83nm thick Fe prepared on MgO3Sn2Pole figure of the film.
FIG. 5 shows Al at different temperatures2O3150 nm thick Fe prepared above3Sn2The Hall resistivity of the film is related to the change of the magnetic field.
FIG. 6 shows Al at room temperature2O3Fe of different thicknesses prepared as above3Sn2The topological Hall resistivity of the film is in a change relation with the magnetic field.
Detailed Description
According to the results of our structural and property analyses on the samples prepared in the present invention, the following will prepare epitaxial Fe by the facing target magnetron sputtering method3Sn2The best mode of the film is explained in detail:
example 1:
1) development of Shenyang scientific instrument by Chinese academy of sciencesThe produced ultrahigh vacuum facing target magnetron sputtering film plating machine has a substrate material of [ 0001%]Oriented Al2O3Single crystal substrate using two pieces of Fe with a purity of 99.99%3Sn2Targets are respectively arranged on the two groups of opposite target heads. In each group of opposite targets, one end is used as the N pole of the magnetic force line, and the other end is used as the S pole; the base material (polished single crystal Al)2O3Etc.) removing impurities on the surface by ultrasonic wave, etc., mounting the substrate on the perpendicular bisector of the connecting line of the opposite targets, the substrate and the opposite Fe3Sn2The vertical distance of the line between the targets was 80 mm.
2)Fe3Sn2Preparation of the film:
2.1) starting the DPS-III opposite target magnetron sputtering equipment, starting a first-stage mechanical pump and a second-stage molecular pump to pump vacuum successively until the vacuum degree of the back bottom of the sputtering chamber is less than or equal to 2.5 multiplied by 10–5Pa；
2.2) raising the temperature of the substrate to 350 ℃ at the speed of 20 ℃/min by using a temperature control system;
2.3) introducing sputtering gas Ar with the purity of 99.999 percent into the vacuum chamber, and keeping the vacuum degree of the sputtering chamber at 1.8Pa and stabilizing for 5 minutes by adjusting the opening degree of the ultrahigh vacuum gate valve;
2.4) switching on the sputtering power supply to a pair of Fe3Sn2Applying 0.10A current and 800V direct current voltage on the target, and pre-sputtering for 10 minutes;
2.5) opening of Fe3Sn2The baffle between the target side and the substrate starts sputtering until Fe3Sn2The thickness of the film is 70 nm;
2.6) after the sputtering is finished, the Fe is turned off3Sn2A baffle plate is arranged between the side surface of the target and the substrate, then the sputtering power supply is closed, the sputtering gas Ar is stopped to be introduced, the gate valve is completely opened, and the vacuum pumping is continued, so that the temperature of the substrate is reduced to the room temperature at the speed of 2 ℃/min;
example 2:
1) the ultrahigh vacuum facing-target magnetron sputtering coating machine produced by Shenyang scientific instrument development center of Chinese academy of sciences is adopted, and the substrate material is [0001 ]]Oriented Al2O3(Single Crystal)Substrate using two pieces of Fe with purity of 99.99%3Sn2Targets are respectively arranged on the two groups of opposite target heads. In each group of opposite targets, one end is used as the N pole of the magnetic force line, and the other end is used as the S pole; the base material (polished single crystal Al)2O3Etc.) removing surface impurities by ultrasonic wave, etc., mounting the substrate on the perpendicular bisector of the connecting line of the facing targets, the substrate and the facing Fe3Sn2The vertical distance of the connecting line between the targets was 60 mm.
2)Fe3Sn2Preparation of the film:
2.1) starting the DPS-III opposite-target magnetron sputtering equipment, starting a first-stage mechanical pump and a second-stage molecular pump to pump vacuum successively until the vacuum degree of the back bottom of the sputtering chamber is less than or equal to 2.5 multiplied by 10–5Pa；
2.2) raising the temperature of the substrate to 450 ℃ at the speed of 25 ℃/min by using a temperature control system;
2.3) introducing sputtering gas Ar with the purity of 99.999 percent into the vacuum chamber, and keeping the vacuum degree of the sputtering chamber at 2.2Pa and stabilizing for 5 minutes by adjusting the opening degree of the ultrahigh vacuum gate valve;
2.4) turn on the sputtering power supply at a pair of Fe3Sn2Applying 0.20A current and 900V direct current voltage on the target, and pre-sputtering for 15 minutes;
2.5) opening of Fe3Sn2The baffle between the target side and the substrate starts sputtering until Fe3Sn2The thickness of the film is 90 nm;
2.6) after the sputtering is finished, the Fe is closed3Sn2A baffle plate is arranged between the side surface of the target and the substrate, then the sputtering power supply is closed, the sputtering gas Ar is stopped to be introduced, the gate valve is completely opened, and the vacuum pumping is continued, so that the temperature of the substrate is reduced to the room temperature at the speed of 5 ℃/min;
example 3:
1) adopts an ultrahigh vacuum facing-target magnetron sputtering film coating machine produced by Shenyang scientific instrument development center of Chinese academy of sciences, and the base material is [ 0001%]Oriented Al2O3Single crystal substrate using two pieces of Fe with purity of 99.99%3Sn2Targets are respectively arranged on the two groups of opposite target heads.In each group of opposite targets, one end is used as the N pole of the magnetic force line, and the other end is used as the S pole; the base material (polished single crystal Al)2O3Etc.) removing impurities on the surface by ultrasonic wave, etc., mounting the substrate on the perpendicular bisector of the connecting line of the opposite targets, the substrate and the opposite Fe3Sn2The vertical distance of the connecting line between the targets is 90 mm.
2)Fe3Sn2Preparation of the film:
2.1) starting the DPS-III opposite-target magnetron sputtering equipment, starting a first-stage mechanical pump and a second-stage molecular pump to pump vacuum successively until the vacuum degree of the back bottom of the sputtering chamber is less than or equal to 2.5 multiplied by 10–5Pa；
2.2) raising the temperature of the substrate to 372 ℃ at the speed of 20 ℃/min by using a temperature control system;
2.3) introducing sputtering gas Ar with the purity of 99.999 percent into the vacuum chamber, and keeping the vacuum degree of the sputtering chamber at 2.0Pa and stabilizing for 5 minutes by adjusting the opening degree of the ultrahigh vacuum gate valve;
2.4) turn on the sputtering power supply at a pair of Fe3Sn2Applying 0.02A current and 840V direct current voltage on the target, and pre-sputtering for 20 minutes;
2.5) opening of Fe3Sn2The baffle between the target side and the substrate starts sputtering until Fe3Sn2The thickness of the film is 83 nm;
2.6) after the sputtering is finished, the Fe is turned off3Sn2A baffle plate is arranged between the side surface of the target and the substrate, then a sputtering power supply is closed, the sputtering gas Ar is stopped to be introduced, a gate valve is completely opened, and the vacuum pumping is continued, so that the temperature of the substrate is reduced to the room temperature at the speed of 3 ℃/min;
example 4:
1) the ultrahigh vacuum facing target magnetron sputtering film coating machine produced by Shenyang scientific instrument development center of Chinese academy of sciences is adopted, and the base material is [111 ]]Oriented MgO single crystal substrate using two pieces of Fe with a purity of 99.99%3Sn2Targets are respectively arranged on the two groups of opposite target heads. In each group of opposite targets, one end is used as the N pole of the magnetic force line, and the other end is used as the S pole; subjecting the base material (polished single crystal MgO, etc.) to ultrasonic treatmentAfter removing impurities on the surface, the substrate is arranged on the perpendicular bisector of the connecting line of the opposite targets, the substrate and the opposite Fe3Sn2The vertical distance of the line between the targets was 80 mm.
2)Fe3Sn2Preparation of the film:
2.1) starting the DPS-III opposite target magnetron sputtering equipment, starting a first-stage mechanical pump and a second-stage molecular pump to pump vacuum successively until the vacuum degree of the back bottom of the sputtering chamber is less than or equal to 2.5 multiplied by 10–5Pa；
2.2) raising the temperature of the substrate to 350 ℃ at the speed of 20 ℃/min by using a temperature control system;
2.3) introducing sputtering gas Ar with the purity of 99.999 percent into the vacuum chamber, and keeping the vacuum degree of the sputtering chamber at 1.8Pa and stabilizing for 5 minutes by adjusting the opening degree of the ultrahigh vacuum gate valve;
2.4) turn on the sputtering power supply at a pair of Fe3Sn2Applying 0.10A current and 800V direct current voltage on the target, and pre-sputtering for 10 minutes;
2.5) opening of Fe3Sn2The baffle between the target side and the substrate starts sputtering until Fe3Sn2The thickness of the film is 70 nm;
2.6) after the sputtering is finished, the Fe is turned off3Sn2A baffle plate is arranged between the side surface of the target and the substrate, then the sputtering power supply is closed, the sputtering gas Ar is stopped to be introduced, the gate valve is completely opened, and the vacuum pumping is continued, so that the temperature of the substrate is reduced to the room temperature at the speed of 2 ℃/min;
example 5:
1) the ultrahigh vacuum facing target magnetron sputtering film coating machine produced by Shenyang scientific instrument development center of Chinese academy of sciences is adopted, and the base material is [111 ]]Oriented MgO single crystal substrate using two pieces of Fe with a purity of 99.99%3Sn2Targets are respectively arranged on the two groups of opposite target heads. In each group of opposite targets, one end is used as the N pole of the magnetic force line, and the other end is used as the S pole; removing surface impurities from base material (polished single crystal MgO, etc.) by ultrasonic wave, etc., mounting the base on the perpendicular bisector of the connecting line of the opposite targets, and placing the substrate and the opposite Fe3Sn2The vertical distance of the connecting line between the targets was 60 mm.
2)Fe3Sn2Preparation of the film:
2.1) starting the DPS-III opposite target magnetron sputtering equipment, starting a first-stage mechanical pump and a second-stage molecular pump to pump vacuum successively until the vacuum degree of the back bottom of the sputtering chamber is less than or equal to 2.5 multiplied by 10–5Pa；
2.2) raising the temperature of the substrate to 450 ℃ at the speed of 25 ℃/min by using a temperature control system;
2.3) introducing sputtering gas Ar with the purity of 99.999 percent into the vacuum chamber, and keeping the vacuum degree of the sputtering chamber at 2.2Pa and stabilizing for 5 minutes by adjusting the opening degree of the ultrahigh vacuum gate valve;
2.4) turn on the sputtering power supply at a pair of Fe3Sn2Applying 0.20A current and 900V direct current voltage on the target, and pre-sputtering for 15 minutes;
2.5) opening of Fe3Sn2The baffle between the target side and the substrate starts sputtering until Fe3Sn2The thickness of the film is 90 nm;
2.6) after the sputtering is finished, the Fe is closed3Sn2A baffle plate is arranged between the side surface of the target and the substrate, then the sputtering power supply is closed, the sputtering gas Ar is stopped to be introduced, the gate valve is completely opened, and the vacuum pumping is continued, so that the temperature of the substrate is reduced to the room temperature at the speed of 5 ℃/min;
example 6:
1) the ultrahigh vacuum facing-target magnetron sputtering coating machine produced by Shenyang scientific instrument development center of Chinese academy of sciences is adopted, and the substrate material is [111 ]]Oriented MgO single crystal substrate using two pieces of Fe with a purity of 99.99%3Sn2Targets are respectively arranged on the two groups of opposite target heads. In each group of opposite targets, one end is used as the N pole of the magnetic force line, and the other end is used as the S pole; removing impurities from the surface of the substrate material (polished single crystal MgO, etc.) by ultrasonic wave, etc., mounting the substrate on the perpendicular bisector of the connecting line of the facing targets, the substrate and the facing Fe3Sn2The vertical distance of the connecting line between the targets is 90 mm.
2)Fe3Sn2Preparing a film:
2.1) starting DPS-III opposite target magnetron sputtering equipment,starting the first-stage mechanical pump and the second-stage molecular pump successively to vacuumize until the vacuum degree of the back bottom of the sputtering chamber is less than or equal to 2.5 multiplied by 10–5Pa；
2.2) raising the temperature of the substrate to 372 ℃ at the speed of 20 ℃/min by using a temperature control system;
2.3) introducing sputtering gas Ar with the purity of 99.999 percent into the vacuum chamber, and keeping the vacuum degree of the sputtering chamber at 2.0Pa and stabilizing for 5 minutes by adjusting the opening degree of the ultrahigh vacuum gate valve;
2.4) turn on the sputtering power supply at a pair of Fe3Sn2Applying 0.02A current and 840V direct current voltage on the target, and pre-sputtering for 20 minutes;
2.5) opening of Fe3Sn2The baffle between the target side and the substrate starts sputtering until Fe3Sn2The thickness of the film is 83 nm;
2.6) after the sputtering is finished, the Fe is turned off3Sn2A baffle plate is arranged between the side surface of the target and the substrate, then the sputtering power supply is closed, the sputtering gas Ar is stopped to be introduced, the gate valve is completely opened, and the vacuum pumping is continued, so that the temperature of the substrate is reduced to the room temperature at the speed of 3 ℃/min;
description of Performance testing
For example 3 above, in Al2O3(0001) Fe prepared on a substrate3Sn2Thin films with Fe prepared on MgO (111) substrate of example 63Sn2Thin film structural characterization and magnetic measurement:
1) FIG. 1 shows Al2O383nm thick Fe prepared above3Sn2X-ray diffraction pattern of the film. The X-ray diffraction result shows that the invention is applied to Al2O3(0001) Fe prepared on a substrate3Sn2Film edge [0001 ]]Directional orientation growth;
2) FIG. 2 shows 83nm thick Fe prepared on MgO3Sn2X-ray diffraction pattern of the film. The X-ray diffraction results show that the Fe prepared on the MgO (111) substrate according to the invention3Sn2Film edge [0001 ]]Directional orientation growth;
3) FIG. 3 shows Al2O3Preparation of83nm thick Fe3Sn2Pole figure of the film. The X-ray diffraction pole figure result shows that the invention is applied to Al2O3(0001) Fe prepared on a substrate3Sn2The film is epitaxially grown;
4) FIG. 4 shows 83nm thick Fe prepared on MgO3Sn2Pole figure of the film. The X-ray diffraction pole figure results show that the Fe prepared on the MgO (111) substrate according to the invention3Sn2The film is epitaxially grown;
5) FIG. 5 shows Al at different temperatures2O3150 nm thick Fe prepared above3Sn2The Hall resistivity of the film is in a change relation with a magnetic field, and the direction of the magnetic field is vertical to the surface of the film. In the present invention, Fe was found for the first time3Sn2The Hall resistivity gradient of a high magnetic field area in the out-of-plane direction of the film changes from negative to positive along with the temperature rise;
3.6) FIG. 6 shows Al at room temperature2O3Fe of different thicknesses prepared above3Sn2The topological Hall resistivity of the film is in a change relation with a magnetic field, and the direction of the magnetic field is vertical to the surface of the film. Fe3Sn2The topological Hall resistivity of the low magnetic field area outside the film surface is firstly reduced and then increased along with the increase of the magnetic field, and the reported single crystal Fe3Sn2The topological hall resistivity characteristics in (1) are consistent.
While the methods and techniques of the present invention have been described in terms of preferred embodiments, it will be apparent to those of skill in the art that variations and modifications of the methods and techniques described herein may be practiced without departing from the spirit and scope of the invention. It is expressly intended that all such similar substitutes and modifications apparent to those skilled in the art are deemed to be within the spirit, scope and content of the invention.

Claims (2)

1. Opposite-target magnetron sputtering preparation of epitaxial ironTin alloy thin film, characterized in that2O3(0001) Fe is epitaxially grown on a single crystal substrate3Sn2Film of Fe3Sn2/Al2O3(ii) a Fe is epitaxially grown on a MgO (111) single crystal substrate3Sn2Film of Fe3Sn2/MgO。
2. A method for preparing an epitaxial iron-tin alloy film by using a facing target magnetron sputtering method is characterized by comprising the following steps:
1) adopts an ultrahigh vacuum facing-target magnetron sputtering coating machine, and the substrate material is [0001 ]]Oriented Al2O3The single crystal substrate or base material is [111 ]]An oriented MgO single crystal substrate; two pieces of Fe with a purity of 99.99% were used3Sn2Targets respectively arranged on the two groups of opposite target heads; in each group of opposite targets, one end is used as the N pole of the magnetic force line, and the other end is used as the S pole; mounting the substrate on the perpendicular bisector of the connecting line of the facing targets, the substrate and the facing Fe3Sn2The vertical distance of the connecting line between the targets is 60-90 mm;
2) starting the facing target magnetron sputtering equipment, starting the first-stage mechanical pump and the second-stage molecular pump to perform vacuum pumping successively until the vacuum degree of the back bottom of the sputtering chamber is less than or equal to 2.5 multiplied by 10–5Pa；
3) Raising the temperature of the substrate to 350-450 ℃ at the speed of 20-25 ℃/min by using a temperature control system;
4) introducing sputtering gas Ar with the purity of 99.999 percent into the vacuum chamber, and keeping the vacuum degree of the sputtering chamber at 1.8-2.2Pa and stabilizing for 5-15 minutes by adjusting the opening degree of the ultrahigh vacuum gate valve;
5) starting the sputtering power supply to a pair of Fe3Sn2Applying 0.02-0.20A current and 800-900V DC voltage on the target, and pre-sputtering for 10-20 min;
6) opening of Fe3Sn2The baffle between the target side and the substrate starts sputtering until Fe3Sn2The thickness of the film is 70-90 nm;
7) after the sputtering is finished, the Fe is closed3Sn2Baffle between target side and substrateThen, the sputtering power supply is closed, the sputtering gas Ar is stopped from being introduced, the gate valve is completely opened, and the vacuum pumping is continued, so that the temperature of the substrate is reduced to the room temperature at the speed of 2-5 ℃/min.
CN202210408699.XA 2022-04-19 2022-04-19 Preparation method of opposite-target magnetron sputtering epitaxial iron-tin alloy film Pending CN114775061A (en)

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