CN114464729A - EuIG/SnTe heterojunction single crystal epitaxial film and preparation method thereof - Google Patents

EuIG/SnTe heterojunction single crystal epitaxial film and preparation method thereof Download PDF

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CN114464729A
CN114464729A CN202111524765.1A CN202111524765A CN114464729A CN 114464729 A CN114464729 A CN 114464729A CN 202111524765 A CN202111524765 A CN 202111524765A CN 114464729 A CN114464729 A CN 114464729A
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euig
single crystal
film
snte
heterojunction
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马嵩
张安琪
刘大珩
刘伟
张志东
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Institute of Metal Research of CAS
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    • 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
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Abstract

The invention relates to a EuIG/SnTe heterojunction single crystal epitaxial film and a preparation method thereof, wherein the preparation method of the EuIG/SnTe heterojunction single crystal epitaxial film comprises the following steps: providing a GGG substrate and placing the GGG substrate in a vacuum system; depositing and growing an EuIG film on the surface of the GGG substrate by using pulsed laser; and growing a SnTe film on the surface of the EuIG film as the substrate by using a molecular beam epitaxy technique. The method can be used for preparing the high-quality monocrystal epitaxial ferromagnetism/topological crystal insulator heterojunction, and the linear magnetoresistance effect and the double-carrier phenomenon accompanied with the Hall effect can be observed at 5K.

Description

EuIG/SnTe heterojunction single crystal epitaxial film and preparation method thereof
Technical Field
The invention belongs to the field of condensed state physics, and more particularly relates to a method for generating an interface effect between a ferromagnetic insulator material and a topological crystal insulator material by a method for constructing a heterojunction, so that a linear magnetoresistance effect and a double-carrier phenomenon accompanied with a Hall effect are observed at 5K.
Background
The magnetoresistive effect is also called a magnetoresistance effect, and refers to a phenomenon in which when a magnetic field is applied to a metal or a semiconductor through which a current flows, the resistance value thereof changes significantly. The magnetoresistive effect was first discovered in 1857 by Thomson (Kelvin, God) when studying the electrical transport behavior of Fe and Ni under an applied magnetic field. An increase in resistance is generally defined as a positive magnetoresistive effect, whereas a decrease in resistance is defined as a negative magnetoresistive effect. The semiconductor has large magneto-resistance anisotropy, can be made into magneto-resistance elements by using magneto-resistance effect, and can be used for constructing displacement sensors, rotating speed sensors, position sensors, speed sensors and the like. When the magnetoresistance increases linearly with an increase in magnetic field and does not saturate at a high field, this phenomenon is called a linear magnetoresistance effect. The research on the linear magnetoresistance phenomenon can detect the properties and the conducting mechanism of electrons in a solid, and has potential application value in the aspects of magnetoelectric sensors and storage.
The hall effect is a common electromagnetic effect, and when a conductor is placed in an external magnetic field and a current in the conductor is perpendicular to the external magnetic field, a significant potential difference occurs between two end faces of the conductor perpendicular to the magnetic field and the current direction, which is the hall effect. This is mainly because the electrons that generate the current are subjected to the lorentz force, causing them to move to both sides of the conductor, thereby causing charge accumulation and the hall effect to occur. The hall effect is a fundamental phenomenon in condensed state physics, and is widely used in the fields of determining the type of a carrier of a sample, the density of the carrier, measuring the intensity of magnetic field, and the like. The double-carrier phenomenon of the Hall effect is a peculiar physical phenomenon and plays an important role in researching an electron transport mechanism of a material.
Disclosure of Invention
In view of the above, it is necessary to provide a magnetic thin film with linear magnetoresistance and a method for preparing the same, in the EuIG/SnTe heterojunction single crystal epitaxial thin film, EuIG has out-of-plane ferromagnetism, and the Curie temperature can reach 568K. Under the condition of a certain film thickness, an interface effect can be caused by constructing a ferromagnetic insulator EuIG and a topological crystal insulator SnTe heterojunction, so that the material with linear magnetoresistance, namely the EuIG/SnTe heterojunction single crystal epitaxial film provided by the invention is realized. The invention also provides a preparation method of the film, and a high-quality film material with linear magnetoresistance can be obtained by the method, and the film material can show the linear magnetoresistance effect and double-carrier phenomenon accompanied with Hall effect at 5K.
The technical scheme of the invention is as follows:
a single crystal epitaxial thin film of an EuIG/SnTe heterojunction, characterized in that: growing EuIG (110) single crystal epitaxial film on the surface of GGG (110) substrate, and growing SnTe (100) single crystal epitaxial film on the surface of the film.
As a preferable technical scheme, the thickness of the substrate is 0.2-1.0mm, the thickness of the EuIG single crystal epitaxial thin film is 10-100nm, and the thickness of the SnTe single crystal epitaxial thin film is 5-30 nm.
A preparation method of a single crystal epitaxial film of a EuIG/SnTe heterojunction is characterized by comprising the following steps:
a) placing the GGG (110) substrate in a vacuum system;
b) growing an EuIG single crystal epitaxial film on the surface of a GGG (110) substrate by using a pulse laser deposition technology;
c) and (3) placing the grown EuIG single crystal epitaxial film in an ultra-high vacuum system, and growing a SnTe single crystal epitaxial film on the surface of the EuIG film by using a molecular beam epitaxial growth technology to finally prepare the EuIG/SnTe heterojunction single crystal epitaxial film.
As a preferred technical scheme:
in the step a), before the substrate is placed in a vacuum system, the substrate is subjected to ultrasonic treatment for 300s-500s by using acetone, and then is subjected to ultrasonic treatment for 200s-400s by using ethanol.
In the step b), the substrate temperature is maintained at 650 ℃ to 800 ℃ during the growth of the EuIG single crystal thin film.
When growing the EuIG single crystal film, providing a EuIG target material, keeping the temperature in a cavity between 650 and 800 ℃, introducing oxygen, and maintaining the oxygen pressure between 0.5 and 5.0 Pa; using pulse laser to strike the EuIG target under the conditions that the laser repetition frequency is 3Hz-5Hz and the laser energy is 350mJ-450mJ to obtain the EuIG film; and after the laser striking is finished, carrying out annealing treatment for 1-3 h at 650-750 ℃, and taking out the EuIG film sample.
In the step c), before growing the SnTe single crystal film, the EuIG film as the substrate is respectively subjected to ultrasonic treatment for 10min-30min by using isopropanol, acetone and ethanol, and the ultrasonic treatment aims to remove impurities on the surface of the substrate so as to ensure the cleanness and the flatness of the substrate. Then the temperature is raised to 700-900 ℃ for annealing treatment for 1-1.5 h.
When growing the SnTe single crystal film, the EuIG film temperature as a substrate is maintained at 300-400 ℃.
When growing the SnTe single crystal film, respectively providing a Sn source and a Te source, wherein the growing temperature of the Sn source is kept at 970-1000 ℃, and the growing temperature of the Te source is kept at 270-330 ℃.
After growing the SnTe single crystal film, carrying out annealing treatment on the EuIG/SnTe heterojunction single crystal epitaxial film for 1h-1.5h at the temperature of 300-400 ℃.
Compared with the prior art, the invention has at least the following advantages:
firstly, the molecular beam epitaxy growth technology is utilized, the growth process and the appearance atom level of the SnTe single crystal film can be accurately controlled, and the high-quality SnTe film with strictly controllable chemical components is prepared.
Secondly, the EuIG film is used as a substrate, the lattice constants of the EuIG film and the SnTe are in integral multiple, the lattice mismatch degree of the single crystal is small, and the two-dimensional epitaxial growth of the SnTe on the surface of the EuIG film is ensured. And the EuIG has very high dielectric constant at low temperature, can effectively shield the interaction between carriers, and obtains stronger EuIG/SnTe interface effect.
Thirdly, EuIG has out-of-plane magnetism, and can affect the surface state of SnTe through interface effect, thus being hopeful to generate linear magnetoresistance effect.
Fourth, the ferromagnetic insulator and topological crystal insulator heterojunction thin film prepared by the method of the present invention can show linear magnetoresistance effect and double carrier phenomenon accompanied with Hall effect at 5K.
Drawings
FIG. 1 is a schematic structural view of a EuIG/SnTe heterojunction single crystal epitaxial thin film provided in example 1.
FIG. 2 is an X-ray diffraction pattern (XRD) of EuIG (110) single crystal epitaxial films grown on GGG (110) substrates provided in example 1.
FIG. 3 is an X-ray diffraction pattern (XRD) of SnTe (100) heterojunction single crystal epitaxial thin film grown on EuIG (110) thin film based on GGG (110) as provided in example 1.
FIG. 4 is an atomic force topography of the EuIG/SnTe heterojunction single crystal epitaxial thin film provided in example 1.
FIG. 5 is a plot of longitudinal sheet resistance as a function of temperature for the EuIG/SnTe heterojunction single crystal epitaxial film provided in example 1.
FIG. 6 is a graph showing the change of magnetoresistance with magnetic field in the case of the EuIG/SnTe heterojunction single crystal epitaxial thin film 5K provided in example 1.
FIG. 7 is a graph showing the lateral resistance with respect to a magnetic field of the EuIG/SnTe heterojunction single crystal epitaxial thin film 5K provided in example 1.
FIG. 8 is a graph showing the change of magnetoresistance with magnetic field in the case of the EuIG/SnTe heterojunction single crystal epitaxial thin film 5K provided in example 2.
FIG. 9 is a graph showing the change of magnetoresistance with magnetic field in the case of the EuIG/SnTe heterojunction single crystal epitaxial thin film 5K provided in comparative example 1.
FIG. 10 shows the lateral resistance R at 5K of the EuIG/SnTe heterojunction single crystal epitaxial thin film provided in comparative example 1xyThe change curve with the magnetic field.
FIG. 11 is a graph showing the change of magnetoresistance with magnetic field at 5K of the YIG/SnTe heterojunction single-crystal epitaxial film provided in comparative example 2.
FIG. 12 shows the lateral resistance R at 5K of the YIG/SnTe heterojunction single-crystal epitaxial thin film provided in comparative example 2xyThe change curve with the magnetic field.
Detailed Description
The EuIG/SnTe heterojunction single crystal epitaxial thin film and the preparation method thereof provided by the present invention will be further described in detail with reference to the accompanying drawings and specific examples.
Referring to FIG. l, the present invention provides a film having a linear magnetoresistive effect, which includes a GGG (110) substrate, a EuIG/SnTe heterojunction single crystal epitaxial film. The GGG (110) substrate and the EuIG/SnTe heterojunction single-crystal thin film are sequentially stacked. The EuIG single crystal film is positioned on the GGG substrate, the lamination arrangement is realized through pulsed laser deposition growth, and the lamination arrangement is realized between the SnTe single crystal film and the EuIG film through molecular beam epitaxial growth.
The EuIG film has a high dielectric constant, and is beneficial to shielding the interaction between carriers. In order to facilitate observation of the magnetoresistance effect and the hall effect of the thin film using electrical transport measurements, a high resistance insulating substrate may be selected. Preferably, the GGG substrate is a single crystal insulating substrate.
The lattice constant of the GGG substrate was 1.238 nanometers. The lattice mismatch between the GGG substrate and the EuIG single crystal film is about 0.9%, and the small lattice mismatch is beneficial to growing the EuIG single crystal film with high quality on the substrate. The lattice constant of SnTe is 0.63 nm, the lattice mismatching degree with EuIG is about 0.8%, and the small lattice mismatching degree is beneficial to growing a high-quality SnTe single crystal film on the substrate.
The vacuum system refers to that the air pressure is less than or equal to 10-4Closed system of handkerchief. In the embodiment of the invention, the vacuum system can be a high vacuum system equipped with a pulse laser deposition device.
The ultra-high vacuum system refers to that the air pressure is less than or equal to 10-8Closed system of handkerchief. In the embodiment of the invention, the ultrahigh vacuum system can be selected as an ultrahigh vacuum system equipped with a molecular beam epitaxial growth device.
Example 1
The thickness of the GGG substrate used was about 0.5mm, the thickness of the EuIG single crystal epitaxial film was 25nm, and the thickness of the SnTe single crystal epitaxial film was 15 nm.
The linear magnetoresistance of the EuIG/SnTe heterojunction single crystal epitaxial film is mainly from the interface action of a ferromagnetic insulator and a topological crystal insulator in the film. The preparation method of the film comprises the following steps:
a) carrying out ultrasonic treatment on the GGG (110) substrate for 480s by using acetone, then carrying out ultrasonic treatment on the GGG (110) substrate for 280s by using ethanol, and then placing the GGG (110) substrate in a vacuum system;
b) growing an EuIG single crystal epitaxial film on the surface of a GGG (110) substrate by using a pulse laser deposition technology;
the substrate temperature was maintained around 700 ℃ while growing the EuIG single crystal thin film. Providing a EuIG target material, keeping the temperature in a cavity at 700 ℃, introducing oxygen, and maintaining the oxygen pressure at 0.5-1.5 Pa; using pulse laser to strike the EuIG target under the conditions that the laser repetition frequency is 5Hz and the laser energy is 400mJ to obtain the EuIG film; and after the laser striking is finished, annealing treatment is carried out for 1h at 700-750 ℃, so that a monocrystal epitaxial EuIG film with good crystallinity is obtained, and a EuIG film sample is taken out.
c) And (3) placing the grown EuIG single crystal epitaxial film in an ultra-high vacuum system, and growing a SnTe single crystal epitaxial film on the surface of the EuIG film by using a molecular beam epitaxial growth technology to finally prepare the EuIG/SnTe heterojunction single crystal epitaxial film.
Before growing the SnTe single crystal film, the EuIG film used as a substrate is subjected to ultrasonic treatment for 10min by respectively using isopropanol, acetone and ethanol, and then the temperature is raised to 800 ℃ for annealing treatment for 1 h.
In growing the SnTe single crystal film, the EuIG film temperature as a substrate is kept at 350 ℃, a Sn source and a Te source are respectively provided, the Sn source growing temperature is kept at 985 ℃, and the Te source growing temperature is kept at 300 ℃.
After the SnTe single crystal film is grown, the EuIG/SnTe heterojunction single crystal epitaxial film is annealed for 1h at 350 ℃.
Various parameters adopted in the embodiment of the invention can ensure that the EuIG/SnTe heterojunction single crystal epitaxial film obtained by growth has better film quality, thereby being beneficial to obtaining the EuIG/SnTe heterojunction single crystal film with linear magnetoresistance effect.
Referring to fig. 2, fig. 2 is an XRD pattern of EuIG single crystal epitaxial thin film grown on GGG (110) substrate according to an embodiment of the present invention. FIG. 2 shows that EuIG thin films were grown along the <110> direction on GGG substrates and no hetero-phase was detected in the XRD pattern.
Referring to FIG. 3, FIG. 3 is an XRD pattern of SnTe heterojunction single crystal epitaxial thin film grown on EuIG (110) thin film based on GGG according to the example of the present invention. Figure 3 shows that the film SnTe grows on EuIG (110) films along the <100> direction, and the peak Te in the XRD pattern is from the Te capping layer grown to prevent oxidation of the sample.
Referring to FIG. 4, FIG. 4 is an atomic force diagram of a single crystal epitaxial film of EuIG/SnTe heterojunction according to an embodiment of the present invention, wherein the area of the atomic force diagram is 3 μm × 3 μm. As can be seen from fig. 4, the film exhibited cubic-shaped grains.
Referring to FIG. 5, FIG. 5 is a graph showing the variation of the vertical sheet resistance Rs of a EuIG/SnTe heterojunction single-crystal epitaxial film according to an embodiment of the present invention with temperature. As can be seen from fig. 5, the longitudinal resistance of the SnTe thin film decreases with a decrease in temperature, showing metallic behavior.
Referring to FIG. 6, FIG. 6 is a graph showing the MR variation with magnetic field at 5K for a EuIG/SnTe heterojunction single crystal epitaxial film of the present invention. It can be seen from FIG. 6 that the film has a characteristic of linear magnetoresistive effect.
Referring to FIG. 7, FIG. 7 is a lateral resistance R of a EuIG/SnTe heterojunction single crystal epitaxial film at a temperature of 5K according to an embodiment of the present inventionxyThe change curve with the magnetic field. It can be seen from fig. 7 that the film has the bi-carrier characteristic of the hall effect.
Example 2
The thickness of the GGG substrate used was about 0.5mm, the thickness of the EuIG single crystal epitaxial film was 75nm, and the thickness of the SnTe single crystal epitaxial film was 15 nm.
The linear magnetoresistance of the EuIG/SnTe heterojunction single crystal epitaxial film is mainly from the interface action of a ferromagnetic insulator and a topological crystal insulator in the film. The film was prepared in the same manner as in example 1 except that the EuIG single crystal epitaxial film had a thickness of 75 nm.
Various parameters adopted in the embodiment of the invention can ensure that the EuIG/SnTe heterojunction single crystal epitaxial film obtained by growth has better film quality, thereby being beneficial to obtaining the EuIG/SnTe heterojunction single crystal film with linear magnetoresistance effect.
Referring to FIG. 8, FIG. 8 is a graph showing the MR variation with magnetic field at 5K for a EuIG/SnTe heterojunction single crystal epitaxial film of the present invention. It can be seen from FIG. 8 that the film has a characteristic of linear magnetoresistive effect.
Comparative example 1
The thickness of the GGG substrate used was about 0.5mm, the thickness of the EuIG single crystal epitaxial film was 150nm, and the thickness of the SnTe single crystal epitaxial film was 15 nm.
The linear magnetoresistance of the EuIG/SnTe heterojunction single crystal epitaxial film is mainly from the interface action of a ferromagnetic insulator and a topological crystal insulator in the film. The film was prepared in the same manner as in example 1 except that the EuIG single crystal epitaxial film had a thickness of 150 nm.
Referring to FIG. 9, FIG. 9 is a graph showing the MR variation with magnetic field at 5K for the EuIG/SnTe heterojunction single crystal epitaxial film of comparative example 1 according to the present invention. It can be seen from FIG. 9 that the film does not have the characteristic of the linear magnetoresistive effect.
Referring to FIG. 10, FIG. 10 is a graph showing the lateral resistance R of the EuIG/SnTe heterojunction single crystal epitaxial film of comparative example 1 according to the present invention at a temperature of 5KxyThe change curve with the magnetic field. It can be seen from fig. 10 that the film does not have the bi-carrier characteristic of the hall effect, but rather a linear hall effect curve characteristic.
Comparative example 2
The thickness of the GGG (111) substrate used was about 0.5mm, the thickness of the YIG (111) single crystal epitaxial film was 150nm, and the thickness of the SnTe single crystal epitaxial film was 15 nm.
The difference from the embodiment is that YIG has in-plane ferromagnetism, and the Curie temperature can reach 550K. The YIG (111)/SnTe (100) heterojunction single crystal epitaxial film has the linear magnetoresistance of a parabolic curve characteristic at 5K, and the Hall effect curve of the film is linear.
Referring to FIG. 11, FIG. 11 is a graph showing the MR variation with magnetic field at 5K for the YIG/SnTe heterojunction single crystal epitaxial film of comparative example 2. It can be seen from FIG. 11 that the film does not have the characteristic of the linear magnetoresistive effect and exhibits the parabolic curve characteristic.
Referring to FIG. 12, FIG. 12 is a graph showing the lateral resistance R of the YIG/SnTe heterojunction single crystal epitaxial film of comparative example 2 at 5KxyThe change curve with the magnetic field. It can be seen from fig. 12 that the film does not have the bi-carrier characteristic of the hall effect, but rather a linear hall effect curve characteristic.
The invention is not the best known technology.
The above embodiments are merely illustrative of the technical ideas and features of the present invention, and the purpose thereof is to enable those skilled in the art to understand the contents of the present invention and implement the present invention, and not to limit the protection scope of the present invention. All equivalent changes and modifications made according to the spirit of the present invention should be covered within the protection scope of the present invention.

Claims (10)

1. A single crystal epitaxial thin film of an EuIG/SnTe heterojunction, characterized in that: growing EuIG (110) single crystal epitaxial film on the surface of GGG (110) substrate, and growing SnTe (100) single crystal epitaxial film on the surface of the film.
2. A single crystal epitaxial film of an EuIG/SnTe heterojunction as claimed in claim 1 wherein: the thickness of the EuIG single crystal epitaxial film is 10-100nm, and the thickness of the SnTe single crystal epitaxial film is 5-30 nm.
3. A method of making a single crystal epitaxial thin film of a EuIG/SnTe heterojunction as claimed in claim 1, comprising the steps of:
a) placing the GGG (110) substrate in a vacuum system;
b) growing an EuIG single crystal epitaxial film on the surface of a GGG (110) substrate by using a pulse laser deposition technology;
c) and (3) placing the grown EuIG single crystal epitaxial film in an ultra-high vacuum system, and growing a SnTe single crystal epitaxial film on the surface of the EuIG film by using a molecular beam epitaxial growth technology to finally prepare the EuIG/SnTe heterojunction single crystal epitaxial film.
4. A method of making a single crystal epitaxial thin film at a EuIG/SnTe heterojunction as claimed in claim 3 wherein: in the step a), before the substrate is placed in a vacuum system, the substrate is subjected to ultrasonic treatment for 300s-500s by using acetone, and then is subjected to ultrasonic treatment for 200s-400s by using ethanol.
5. A method of making a single crystal epitaxial thin film at a EuIG/SnTe heterojunction as claimed in claim 3 wherein: in the step b), the substrate temperature is maintained at 650-800 ℃ while growing the EuIG single crystal thin film.
6. A method of making a single crystal epitaxial thin film at a EuIG/SnTe heterojunction as claimed in claim 3 wherein: in the step b), when growing the EuIG single crystal film, providing a EuIG target material, keeping the temperature in the cavity between 650 ℃ and 800 ℃, introducing oxygen, and maintaining the oxygen pressure between 0.5Pa and 5.0 Pa; using pulse laser to strike the EuIG target under the conditions that the laser repetition frequency is 3Hz-5Hz and the laser energy is 350mJ-450mJ to obtain the EuIG film; and after the laser striking is finished, annealing treatment is carried out for 1h-3h at 650 ℃ -750 ℃, and a EuIG film sample is taken out.
7. A method of fabricating a single crystal epitaxial thin film according to a EuIG/SnTe heterojunction as claimed in claim 3, wherein: in the step c), before growing the SnTe single crystal film, the EuIG film as the substrate is respectively treated with isopropanol, acetone and ethanol for 10min to 30min by ultrasonic treatment, and then the temperature is raised to 700 ℃ to 900 ℃ for annealing treatment for 1 to 1.5 h.
8. A method of making a single crystal epitaxial thin film at a EuIG/SnTe heterojunction as claimed in claim 3 wherein: in the step c), when growing the SnTe single crystal film, the temperature of the EuIG film used as a substrate is kept between 300 and 400 ℃; when growing the SnTe single crystal film, respectively providing a Sn source and a Te source, wherein the growing temperature of the Sn source is kept at 970-1000 ℃, and the growing temperature of the Te source is kept at 270-330 ℃.
9. A method of making a single crystal epitaxial thin film at a EuIG/SnTe heterojunction as claimed in claim 3 wherein: in the step c), after growing the SnTe single crystal film, annealing the EuIG/SnTe heterojunction single crystal epitaxial film for 1h-1.5h at the temperature of 300-400 ℃.
10. A method of making a single crystal epitaxial thin film at a EuIG/SnTe heterojunction as claimed in claim 3 wherein: the EuIG/SnTe heterojunction single crystal epitaxial film shows a linear magnetoresistance effect at 5K and a double-carrier phenomenon accompanied with a Hall effect.
CN202111524765.1A 2021-12-14 2021-12-14 EuIG/SnTe heterojunction single crystal epitaxial film and preparation method thereof Pending CN114464729A (en)

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