CN112680705A - Epitaxial Pt/gamma' -Fe with room temperature topological Hall effect4N/MgO heterostructure and preparation method - Google Patents
Epitaxial Pt/gamma' -Fe with room temperature topological Hall effect4N/MgO heterostructure and preparation method Download PDFInfo
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Abstract
The invention relates to an epitaxial Pt/gamma' -Fe with room temperature topological Hall effect4N/MgO heterostructure and preparation method; ferromagnetic gamma' -Fe by facing target magnetron sputtering4The N film and the non-magnetic heavy metal layer Pt film are compounded together to form Pt/gamma' -Fe4The N/MgO heterostructure comprises an MgO (001) single crystal substrate and gamma' -Fe from bottom to top in sequence4An N layer and a Pt layer; gamma' -Fe4N is a ferromagnetic layer, and Pt is a nonmagnetic heavy metal layer; at room temperature of 300K, in addition to normal Hall effect and abnormal effect in the heterostructureBesides the Hall effect, a topological Hall effect exists, which has important application value in realizing a magnetic storage device with high density, high speed and low energy consumption; the opposed target magnetron sputtering method adopted by the invention can prepare high-quality single crystal epitaxial gamma' -Fe4The N film has high surface flatness and has obvious advantages in industrial production.
Description
Technical Field
The invention relates to an epitaxial Pt/gamma' -Fe with room temperature topological Hall effect4An N/MgO heterostructure and a method of making. More particularly, it is a kind of gamma' -Fe in ferromagnetic film4The surface of N is covered with a heavy metal Pt layer, and gamma' -Fe is reduced4N thickness to enhance Pt/gamma' -Fe4Dzyaloshinski-Mariya (DM) interaction of the N interface, and inducing topological Hall effect in the ferromagnetic layer through the interface DM interaction, thereby forming epitaxial Pt/gamma' -Fe with topological Hall effect4N film and a preparation method thereof.
Background
The topological hall effect is one of the hot spots in the current field of magnetic sigramins and spintronics research. Meanwhile, the topological Hall effect is also an effective means for researching the DM interaction, and the existence of the magnetic Sgmelin can be indirectly proved. Early people focused on materials with breaks in the symmetry of the spatial inversion, such as MnGe, MnSi, etc. materials with a non-centrosymmetric B20 structure [ PHYSICAL REVIEW LETTERS 106,156603, 156603 (2011); PHYSICAL REVIEW LETTERS 110,117202, 117202 (2013). However, most of the topological hall effect and magnetic skarning in the materials depend on low-temperature and strong magnetic field conditions, and are not beneficial to research on the physical mechanism of the topological hall effect and practical application of the magnetic skarning. In recent years, researchers have focused on HM/FM heterostructures composed of nonmagnetic Heavy Metal (HM) and Ferromagnetic Metal (FM), and have desired to control stable sigrons at room temperature by changing the conditions such as thickness, interface, and period of the material, thereby realizing high-density, high-speed, and low-power magnetic memory devices.
Cubic anti-perovskite gamma' -Fe4N has the advantages of simple structure, easy preparation, corrosion resistance, oxidation resistance, good thermal stability, higher saturation magnetization, high Curie temperature and the like, so that the N has wide application prospect in the spintronics device.
At present, no Pt/gamma' -Fe is internationally available4Preparation of N heterostructure and research of room temperature topological Hall effect induced by interface DM interaction. Most of the non-magnetic heavy metal/ferromagnetic metal heterostructures capable of realizing room temperature topological Hall effect are multilayer stacked heterostructures [ NATURE MATERIALS 898,16(2017)；PHYSICS REPORTS 1,704(2017)；SCIENTIFIC REPORTS 6,32629(2016)]However, few studies on the single-layer epitaxial nonmagnetic/ferromagnetic thin film heterostructure exist, and a strong topological hall effect signal can be regarded as electric reading of the magnetic skullam in principle, and has important significance on spintronics based on the magnetic skullam. In addition, the HM/FM heterostructure system prepared at the present stage mostly adopts a magnetron sputtering technology, and the prepared magnetic film mostly consists of nanocrystalline or amorphous [ NATURE MATERIALS 15,501 (2016); NATURE PHYSICS 13,162(2016)]Therefore, the film has more impurities and defects, which increases the driving current density in the device and increases the power consumption. In the HM/FM heterostructure, there is a need to reduce power consumption in the device by reducing impurities or defects in the thin film.
Disclosure of Invention
From the perspective of industrial production and practical application, a low-cost magnetron sputtering method is needed to prepare a nonmagnetic heavy metal/ferromagnetic metal (HM/FM) heterostructure with a room-temperature topological Hall effect. Meanwhile, in the HM/FM heterostructure, if obvious topological Hall effect is generated, lattice matching between layers is required, epitaxial growth can be performed, and preparation conditions are harsh. In addition, the HM/FM samples that need to be prepared showed the appearance of the topological Hall effect at room temperature. The invention prepares single crystal epitaxial Pt/gamma' -Fe by a facing target reaction magnetron sputtering method through a large amount of experimental researches4N/MgO heterostructure and in Pt (3 nm)/gamma' -Fe4A topological Hall effect at room temperature is observed in the N (3nm)/MgO heterostructure, and the topological Hall effect has important application value in realizing a high-density, high-speed and low-energy-consumption magnetic storage device.
The technical scheme of the invention is as follows:
the invention provides an epitaxial Pt/gamma' -Fe with room temperature topological Hall effect4An N/MgO heterostructure; it is characterized by gamma' -Fe4The N film is arranged on the MgO (001) single crystal substrate along the [001 ] edge]Directional epitaxial growth of Pt in epitaxial gamma' -Fe4Upper edge of N/MgO structure [111 ]]Directional orientation growth; wherein gamma' -Fe4The thickness of the N film is 3-5nm, and the thickness of the Pt film is 2-3 nm.
The above-mentionedPt/gamma' -Fe of4The N/MgO heterostructure comprises an MgO (001) single crystal substrate and gamma' -Fe from bottom to top in sequence4An N layer and a Pt layer; wherein gamma' -Fe4N is a ferromagnetic layer and Pt is a nonmagnetic heavy metal layer.
Epitaxial Pt/gamma' -Fe with room-temperature topological Hall effect4The preparation method of the N/MgO heterostructure comprises the following steps:
1) an opposite target magnetron sputtering coating machine is adopted, and the substrate material is a single MgO (001) wafer with a polished single surface. Two Fe targets with the purity of 99.99 percent are used and are arranged on a target pair head, wherein one end is used as the N pole of a magnetic line, and the other end is used as the S pole; the thickness of the target material is 2-4mm, and the diameter is 60 mm; the distance between the two targets is 60-90mm, and the distance between the axis of the targets and a substrate frame on which the MgO (001) single wafer is placed is 60-90 mm;
2) firstly, placing an MgO (001) single wafer covered with a mask plate with a channel width of 10-90 μm on a substrate frame, placing the MgO (001) single wafer behind a baffle plate, and closing a vacuum chamber;
3) starting a vacuum system of the opposite target magnetron sputtering film coating machine, vacuumizing until the back vacuum degree of the sputtering chamber is less than or equal to 2 multiplied by 10–5Pa, the vacuum degree at this moment meets the requirement of the vacuum degree of the prepared sample, and a coating experiment can be started;
4) simultaneously introducing Ar gas of sputtering gas with the purity of 99.999 percent and reaction gas N into the vacuum chamber2Gas, Ar gas and N2The flow ratio of the gas is 5:1-4:1, and the vacuum degree is kept at 0.5-1.0 Pa;
5) uniformly heating the substrate to 400-500 ℃, wherein the heating rate is 10-20 ℃/min;
6) after the temperature of the substrate is stabilized at the target temperature, starting a sputtering power supply to carry out pre-sputtering, applying pre-sputtering current of 0.30-0.50A and pre-sputtering voltage of 800-1000V on a pair of Fe targets, carrying out pre-sputtering for 5-10 minutes, and stopping the pre-sputtering after the readings of the pre-sputtering current and the voltage are kept unchanged;
7) and (5) starting a sputtering experiment after the pre-sputtering in the step 6 is finished. Applying a sputtering current of 0.05-0.10A and a sputtering voltage of 750-850V on a pair of Fe targets, opening a baffle plate on a substrate holder to start sputtering, and reactively sputtering gamma' -Fe4N is thinIn the film process, the position of the MgO (001) single wafer is fixed;
8) sputtering to gamma' -Fe4The thickness of the N film is 3-5 nm; closing the baffle plate on the substrate holder, then closing the sputtering power supply, and stopping introducing Ar gas and N2Completely opening a gate valve, continuously vacuumizing, and uniformly cooling the substrate to room temperature at a cooling rate of 2-3 ℃/min by using a temperature control system;
9) the turntable carrying the substrate holder is rotated counterclockwise to the position where Pt faces the target. Two Pt targets with the purity of 99.99 percent are used and are arranged on a target pair head, wherein one end is used as the N pole of a magnetic line, and the other end is used as the S pole; the thickness of the target material is 2-4mm, and the diameter is 60 mm; the distance between the two targets is 60-90mm, the axes of the targets and the gamma' -Fe coated with the epitaxy4The distance between the substrate frames of the MgO (001) single wafer of the N film is 60-90 mm;
10) closing the baffle to make gamma' -Fe4The N/MgO material is arranged behind the baffle;
11) simultaneously introducing Ar gas of sputtering gas with the purity of 99.999 percent into the vacuum chamber, and keeping the vacuum degree at 0.4-0.6 Pa;
12) starting a sputtering power supply, applying a current of 0.02-0.03A and a DC voltage of 850-950V on a pair of Pt targets, opening a baffle plate on a substrate holder to start sputtering, and coating epitaxial gamma' -Fe in the process of reactively sputtering the Pt film4Fixing the position of the MgO (001) single wafer of the N film;
13) sputtering to reach the thickness of the Pt film of 2-3 nm; closing a baffle plate on the substrate frame, then closing a sputtering power supply, and stopping introducing Ar gas;
14) closing the vacuum system, opening the vacuum chamber, and taking out the prepared epitaxial Pt/gamma' -Fe grown on the MgO (001) single crystal wafer4And (6) N thin films.
The concrete description is as follows:
(1) the invention designs Pt/gamma' -Fe with room temperature topological Hall effect4N/MgO heterostructures. In ferromagnetic materials of gamma' -Fe4In N, chiral interaction, namely DM interaction, is introduced through interface symmetry break and strong spin-orbit coupling, and the DM interaction in the material is beneficial to chiral arrangement of magnetic moments so as to generate a topological Hall effect. When current flowsFlowing gamma' -Fe4And N, the electron spin is additionally influenced by a magnetic field from the space transformation of the chiral alignment magnetic moment, so that the electron obtains an additional Berry phase, and the topological Hall effect is generated. Furthermore, competition between the interface DM interaction and the Heisenberg interaction was tuned by varying the ferromagnetic layer thickness, thus in Pt/γ' -Fe4The topological Hall effect at room temperature is realized in the heterogeneous structure of N/MgO.
(2) The invention adopts an opposite target reaction magnetron sputtering method, takes a pure Fe target as a raw material, introduces mixed gas of argon and nitrogen in the sputtering process, and prepares epitaxial gamma' -Fe on a single-side polished MgO (001) single crystal substrate covered with a mask plate with the channel width of 10-90 mu m by changing the sputtering current, the sputtering voltage, the sputtering pressure, the sputtering temperature and the cooling time in the sputtering process4N thin film, gamma' -Fe prepared4The N film thicknesses were 5, 4 and 3 nm.
(3) The invention finds that the vacuum degree of the back bottom is less than or equal to 2 multiplied by 10–5Pa, the vacuum degree at this moment meets the requirement of the vacuum degree of the prepared sample, and a coating experiment can be started. In the coating experiment process, the sputtering current is 0.05-0.10A, the sputtering voltage is 750-850V, the sputtering pressure is 0.5-1.0Pa, the substrate temperature is 400-500 ℃, the flow ratio of argon to nitrogen is 5:1-4:1, the heating rate is 10-20 ℃/min, the cooling rate is 2-3 ℃/min, and the deposition rate of the film is 1.8-2.6nm/min4And N epitaxial thin film.
(4) Epitaxial gamma' -Fe of the invention4Preparation on N films [111]When the Pt film is oriented, adopting a facing target reaction magnetron sputtering method, taking a pure Pt target as a raw material under the condition of room temperature, introducing argon gas in the sputtering process, and changing the sputtering current, the sputtering voltage and the sputtering pressure in the sputtering process to obtain the oriented Pt film in the thickness of 3-5nm of gamma' -Fe4Depositing [111 ] with a thickness of 2-3nm on N]An oriented Pt film.
(5) The invention finds that gamma' -Fe is epitaxial4Cooling N to room temperature, sputtering current of 0.02-0.03A, sputtering voltage of 850-Can be used for extending gamma' -Fe under the condition of m/min4Preparing [111 ] on N film]An oriented Pt thin film.
(6) The invention prepares Pt/gamma' -Fe4In the case of an N/MgO heterostructure, the channel width of the mask used is 50 μm. The electrode used was air-dried silver paste, the direction of the applied current was parallel to the film surface (along the x-axis direction), the direction of the applied magnetic field was perpendicular to the film surface (along the z-axis direction), and the hall signal along the y-axis direction was measured. The Pt/gamma' -Fe4The thickness of the N/MgO heterostructure in the heavy metal Pt film is 2-3nm, and the ferromagnetic layer is gamma' -Fe4The N thickness is 3-4nm, and the topological Hall effect at room temperature can be observed under the magnetic field of 30-35kOe at room temperature.
Epitaxial Pt/gamma' -Fe4The N/MgO heterostructure has important application value in a low-energy magnetic memory device, for example, the heterostructure can be used as a memory cell, a logic device and the like of a memory, the magnetron sputtering method adopted by the invention is a common method for producing a thin film material industrially, and the used Fe target has the advantages of simple target material selection, high target material utilization rate and the like.
To confirm the best embodiment of the invention, we prepared Pt/gamma' -Fe according to the invention4The N/MgO heterostructure was subjected to X-ray diffraction, high resolution transmission electron microscopy characterization and Hall signal measurements.
Pt/gamma' -Fe prepared from the invention4It can be seen on the X-ray diffraction pattern of the N/MgO heterostructure that by comparing Pt/MgO, gamma' -Fe4N/MgO and Pt/gamma' -Fe4X-ray diffraction pattern of N/MgO samples, Pt/gamma' -Fe4Only the gamma' -Fe with cubic anti-perovskite structure appears in the N/MgO sample4The diffraction peak of the (002) crystal plane of N and the diffraction peak of the Pt (111) crystal plane of the face-centered cubic structure illustrate that the crystal forms of gamma' -Fe4N film edge [002]Direction oriented growth with Pt film along [111 ]]Directionally oriented growth, as shown in FIG. 1.
Gamma' -Fe prepared from the present invention4As can be seen from the pole figure of the N epitaxial thin film, only gamma' -Fe appears4Of N<111>Diffraction peaks of the lattice plane family, indicating gamma' -Fe4The N film is an epitaxial film as shown in fig. 2.
Pt/gamma' -Fe prepared from the invention4Gamma' -Fe can be seen on the transmission electron microscope image and the selected area electron diffraction pattern of the N/MgO heterostructure4N film only along [001 ]]Crystal orientation growth, Pt film only along [111 ]]Crystal orientation growth, further indicating gamma' -Fe4The N film is an epitaxial film as shown in fig. 3.
Pt/gamma' -Fe prepared in the invention4A schematic cross-sectional view of an N/MgO heterostructure is shown in FIG. 4.
Measurement of Pt/gamma' -Fe in the present invention4A schematic diagram of the measurement of the Hall signal of the N/MgO heterostructure is shown in FIG. 5. The direction of the magnetic field when measuring the Hall signal is perpendicular to the surface of the film and along the direction of the z-axis.
The invention measures Pt/gamma' -Fe for changing the thickness of the ferromagnetic layer under the condition of room temperature4The Hall resistivity of the N/MgO heterostructure changes along with the change of an out-of-plane magnetic field, and the direction of the magnetic field is vertical to the surface of the thin film. As can be seen from the measurement results, the heavy metal layer Pt film has a thickness of 2-3nm, and the ferromagnetic layer γ' -Fe4With N thicknesses of 3-4nm, it was observed that the Hall resistivity exhibited non-monotonic behavior with out-of-plane magnetic field (as shown in FIGS. 6(a), 6(b), and 6 (c)), indicating Pt/γ' -Fe4The topological Hall effect exists in addition to the normal Hall effect and the abnormal Hall effect in the N/MgO heterostructure, and Pt (3 nm)/gamma' -Fe4The room temperature topological Hall effect is most pronounced in the N (3nm)/MgO heterostructure, as shown in FIG. 6 (c).
Compared with the method of preparing a non-magnetic metal/ferromagnetic metal heterostructure by other methods, the ferromagnetic gamma' -Fe prepared by the invention4The N thin film has a high-quality single crystal epitaxial structure, and the heavy metal Pt with large spin-orbit coupling can be in Pt/gamma' -Fe4The N interface induces the DM interaction, so that the topological Hall effect at room temperature is realized, and the adopted magnetron sputtering method is simple and practical and is beneficial to popularization in industrial production. The method comprises the following specific steps:
1) because the main method adopted by the current industrial production is a sputtering method, the magnetron sputtering method adopted by the invention has obvious advantages in the industrial production compared with a molecular beam epitaxy method and a chemical method.
2) Although the preparation of the non-magnetic metal/ferromagnetic metal heterostructure and the room temperature topological hall effect are reported internationally, most of the prepared heterostructures are multilayer stacked heterostructures, and the preparation process is complex, so that the practical application of the heterostructure is limited.
3) At present, magnetron sputtering technology is mostly adopted internationally for preparing a magnetic multilayer film system, and the prepared magnetic film is mostly composed of nanocrystalline or amorphous, so that impurities and defects in the film are more, the density of driving current in a device is increased, and energy consumption is increased. The epitaxial ferromagnetic film has less impurities or defects, which is beneficial to realizing low driving current density, thereby reducing the energy consumption in the device.
4) In the non-magnetic metal/ferromagnetic metal heterostructure prepared internationally at present, the topological Hall effect mostly depends on the conditions of low temperature and strong magnetic field, and is not beneficial to the practical application of the topological Hall effect.
5) The invention prepares single crystal epitaxial Pt/gamma' -Fe by a facing target reaction magnetron sputtering method through a large amount of experimental researches4N/MgO heterostructures and in Pt/gamma' -Fe4A topological Hall effect at room temperature is observed in an N/MgO heterostructure, and the topological Hall effect has important application value in realizing a high-density, high-speed and low-energy-consumption magnetic storage device.
Drawings
FIG. 1(a) shows Pt/γ' -Fe4X-ray diffraction pattern of N/MgO heterostructure.
FIG. 1(b) shows γ' -Fe4X-ray diffraction pattern of N/MgO heterostructure.
FIG. 1(c) shows the X-ray diffraction pattern of the Pt/MgO heterostructure.
FIG. 2 shows γ' -Fe prepared on a single-side polished MgO (001) wafer in the present invention4Pole figure of N epitaxial thin film.
FIG. 3(a) shows Pt/γ' -Fe prepared in the present invention4Transmission electron microscopy images of N/MgO heterostructures.
FIG. 3(b) shows the present inventionPt/gamma' -Fe prepared in Ming dynasty4Selected area electron diffraction pattern of N/MgO heterostructure.
FIG. 4 shows Pt/gamma' -Fe prepared in the present invention4Schematic cross-sectional view of an N/MgO heterostructure.
FIG. 5 shows Pt/γ' -Fe prepared in the present invention4And (3) a schematic diagram for measuring a Hall signal of the N/MgO heterostructure.
FIG. 6(a) shows Pt (2nm)/γ' -Fe prepared in the present invention at room temperature4The Hall resistivity of the N (3nm)/MgO heterostructure is related to the change of an out-of-plane magnetic field.
FIG. 6(b) shows Pt (3nm)/γ' -Fe prepared in the present invention at room temperature4The Hall resistivity of the N (4nm)/MgO heterostructure is related to the change of an out-of-plane magnetic field.
FIG. 6(c) shows Pt (3nm)/γ' -Fe prepared in the present invention at room temperature4The Hall resistivity of the N (3nm)/MgO heterostructure is related to the change of an out-of-plane magnetic field.
Detailed Description
According to the results of our structural and property analyses on the samples prepared in the present invention, Pt/γ' -Fe was prepared by the facing-target reactive magnetron sputtering method as follows4The best mode of the N/MgO heterostructure will be explained in detail:
example 1
1) The ultrahigh vacuum facing target magnetron sputtering film plating machine produced by Shenyang scientific instrument development center of Chinese academy of sciences is adopted, and the substrate material is MgO (001) single crystal wafer with the thickness of 500 mu m and polished single surface. Two Fe targets with the purity of 99.99 percent and two Pt targets with the purity of 99.99 percent are respectively arranged on the two groups of opposite targets; the thickness of the target material is 2mm, and the diameter is 60 mm; 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 distance between the two targets is 60mm, and the distance between the axis of the targets and the substrate holder containing the MgO substrate material is 60 mm;
2)γ′-Fe4preparation of N film:
2.1) firstly, placing a mask plate with the channel width of 90 mu m and the area of 3.8mm multiplied by 2.4mm on an MgO (001) single crystal substrate, and covering a part of MgO substrate;
2.1) putting the MgO (001) single crystal substrate covered with the mask plate on a substrate frame, putting the MgO (001) single crystal substrate behind a baffle plate, and closing a vacuum chamber;
2.2) starting a DPS-III type ultrahigh vacuum opposite target magnetron sputtering film coating machine vacuum system, and vacuumizing until the back vacuum degree of a sputtering chamber is less than or equal to 2 multiplied by 10–5Pa, the vacuum degree at this moment meets the requirement of the vacuum degree of the prepared sample, and a coating experiment can be started;
2.3) starting an experiment, introducing argon as sputtering gas with the purity of 99.999% and nitrogen as reaction gas into a vacuum chamber, wherein the flow ratio of the argon to the nitrogen is 4:1, and keeping the vacuum degree at 0.5 Pa;
2.4) uniformly heating the substrate to 500 ℃, wherein the heating rate is 20 ℃/min, and when the substrate temperature is stable;
2.5) after the substrate temperature is stabilized at the target temperature, starting a sputtering power supply to perform pre-sputtering, applying pre-sputtering current of 0.50A and pre-sputtering voltage of 1000V on a pair of Fe targets, pre-sputtering for 5 minutes, and stopping pre-sputtering after the readings of the pre-sputtering current and the pre-sputtering voltage are kept unchanged;
2.6) after the pre-sputtering in the step 2.5 is finished, starting the sputtering experiment. Applying a sputtering current of 0.10A and a sputtering voltage of 850V to a pair of Fe targets, opening the baffle plate on the substrate holder to start sputtering, and reactively sputtering gamma' -Fe4In the process of N film, the position of the MgO (001) single wafer is fixed;
2.7) sputtering to gamma' -Fe4The thickness of the N film is 5 nm; closing the baffle plate on the substrate holder, then closing the sputtering power supply, and stopping introducing Ar gas and N2Completely opening a gate valve, continuously vacuumizing, and uniformly cooling the substrate to room temperature at a cooling rate of 3 ℃/min by using a temperature control system;
3) preparation of Pt thin film:
3.1) rotating the turntable carrying the substrate holder 180 DEG counter-clockwise to the position of Pt facing the targets, the distance between the two targets being 60mm, the axis of the targets and the gamma' -Fe coated with epitaxy4The distance between the substrate frames of the MgO (001) single wafer of the N thin film is 60 mm;
3.2) closing the shutter to let gamma' -Fe4The N/MgO material is arranged behind the baffleKneading;
3.3) simultaneously introducing argon gas as sputtering gas with the purity of 99.999 percent into the vacuum chamber, and keeping the vacuum degree at 0.6 Pa;
3.4) turning on the DC sputtering power supply, applying a current of 0.03A and a DC voltage of 950V on the pair of Pt targets, opening the baffle plate on the substrate holder to start sputtering, and coating epitaxial gamma' -Fe during the reactive sputtering of Pt film4Fixing the position of the MgO (001) single wafer of the N film;
3.5) sputtering to reach the thickness of the Pt film of 2 nm; closing a baffle plate on the substrate frame, then closing a sputtering power supply, and stopping introducing Ar gas;
3.6) closing the vacuum system, opening the vacuum chamber, and taking out the prepared epitaxial Pt/gamma' -Fe growing on the MgO (001) single wafer4And (6) N thin films.
4) Structural characterization and measurement of hall signal:
4.1) X-ray diffraction results show that the Pt (111)/gamma' -Fe prepared by the invention4Gamma' -Fe in N (001)/MgO (001) heterostructure4N edge [001]Direction oriented growth with Pt along [111 ]]Directionally oriented growth, as shown in FIG. 1.
4.2) FIG. 2 shows γ' -Fe4Gamma' -Fe in N (001)/MgO (001) heterostructure4X-ray diffraction pole figure of N, indicating gamma' -Fe4The N film is an epitaxial film.
4.3) FIG. 3 shows Pt/gamma' -Fe prepared by the present invention4The transmission electron microscope image and the selected area electron diffraction pattern of the N/MgO heterostructure further show that the gamma' -Fe4The N film is an epitaxial film.
4.4) the invention measures Pt (2 nm)/gamma' -Fe at 300K4The Hall resistivity of the N (3nm)/MgO heterostructure is in a change relation with an out-of-plane magnetic field, the direction of the magnetic field is vertical to the surface of the thin film, and a measurement schematic diagram of a Hall signal is given in FIG. 5. FIG. 6(a) shows Pt (2nm)/γ' -Fe4The change of the Hall resistivity of the N (3nm)/MgO heterostructure along with the out-of-plane magnetic field is observed to be non-monotonic, which shows that the Hall resistivity of the heterostructure along with the change of the out-of-plane magnetic field shows that the Hall resistivity is not monotonic in Pt (2 nm)/gamma' -Fe4Except for the existence of normal Hall in the N (3nm)/MgO heterostructureEffects and anomalous hall effects, there is also the phenomenon of topological hall effects.
Example 2
1) The ultrahigh vacuum facing target magnetron sputtering film plating machine produced by Shenyang scientific instrument development center of Chinese academy of sciences is adopted, and the substrate material is MgO (001) single crystal wafer with the thickness of 500 mu m and polished single surface. Two Fe targets with the purity of 99.99 percent and two Pt targets with the purity of 99.99 percent are respectively arranged on the two groups of opposite targets; the thickness of the target material is 3mm, and the diameter is 60 mm; 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 distance between the two targets is 80mm, and the distance between the axis of the targets and the substrate holder containing the MgO substrate material is 80 mm;
2)γ′-Fe4preparation of N film:
2.1) firstly, placing a mask plate with the channel width of 10 mu m and the area of 3.8mm multiplied by 2.4mm on an MgO (001) single crystal substrate, and covering a part of MgO substrate;
2.1) putting the MgO (001) single crystal substrate covered with the mask plate on a substrate frame, putting the MgO (001) single crystal substrate behind a baffle plate, and closing a vacuum chamber;
2.2) starting a DPS-III type ultrahigh vacuum opposite target magnetron sputtering film coating machine vacuum system, and vacuumizing until the back vacuum degree of a sputtering chamber is less than or equal to 2 multiplied by 10–5Pa, the vacuum degree at this moment meets the requirement of the vacuum degree of the prepared sample, and a coating experiment can be started;
2.3) starting an experiment, introducing argon as a sputtering gas with the purity of 99.999% and nitrogen as a reaction gas into a vacuum chamber, wherein the flow ratio of the argon to the nitrogen is 4.5:1, and keeping the vacuum degree at 0.8 Pa;
2.4) uniformly heating the substrate to 400 ℃, wherein the heating rate is 15 ℃/min, and the temperature of the substrate is stable;
2.5) after the substrate temperature is stabilized at the target temperature, starting a sputtering power supply to carry out pre-sputtering, applying a pre-sputtering current of 0.40A and a pre-sputtering voltage of 900V on a pair of Fe targets, carrying out pre-sputtering for 8 minutes, and stopping the pre-sputtering after the pre-sputtering current and the voltage readings are kept unchanged
2.6) after the pre-sputtering in the step 2.5 is finished, starting the sputtering experiment. On a pair of Fe targetsSputtering current of 0.07A and sputtering voltage of 800V, opening the baffle plate on the substrate holder to start sputtering, and reactively sputtering gamma' -Fe4In the process of N film, the position of the MgO (001) single wafer is fixed;
2.7) sputtering to gamma' -Fe4The thickness of the N thin film is 4 nm; closing the baffle plate on the substrate holder, then closing the sputtering power supply, and stopping introducing Ar gas and N2Completely opening a gate valve, continuously vacuumizing, and uniformly cooling the substrate to room temperature at a cooling rate of 2 ℃/min by using a temperature control system;
3) preparation of Pt thin film:
3.1) rotating the turntable carrying the substrate holder 180 DEG counter-clockwise to the position of Pt targets at a distance of 80mm between the two targets with their axes aligned with the epitaxially coated gamma' -Fe4The distance between the substrate frames of the MgO (001) single wafer of the N thin film is 80 mm;
3.2) closing the shutter to let gamma' -Fe4The N/MgO material is arranged behind the baffle;
3.3) simultaneously introducing argon gas as sputtering gas with the purity of 99.999 percent into the vacuum chamber, and keeping the vacuum degree at 0.4 Pa;
3.4) turning on the DC sputtering power supply, applying 0.02A current and 850V DC voltage on a pair of Pt targets, opening the baffle plate on the substrate holder to start sputtering, and coating epitaxial gamma' -Fe during the process of reactively sputtering Pt film4Fixing the position of the MgO (001) single wafer of the N film;
3.5) sputtering to reach the thickness of the Pt film to be 3 nm; closing a baffle plate on the substrate frame, then closing a sputtering power supply, and stopping introducing Ar gas;
3.6) closing the vacuum system, opening the vacuum chamber, and taking out the prepared epitaxial Pt/gamma' -Fe growing on the MgO (001) single wafer4And (6) N thin films.
4) The invention measures Pt (3 nm)/gamma' -Fe for changing the thickness of a ferromagnetic layer at room temperature of 300K4The Hall resistivity of the N (4nm)/MgO heterostructure is in a change relation with an out-of-plane magnetic field, the direction of the magnetic field is vertical to the surface of the thin film, and a measurement schematic diagram of a Hall signal is given in FIG. 5. FIG. 6(b) shows Pt (3nm)/γ' -Fe4The change curve of the Hall resistivity of the N (4nm)/MgO heterostructure along with the out-of-plane magnetic field can be observedThe measured change of Hall resistivity of the heterostructure along with the out-of-plane magnetic field shows non-monotonic behavior, which indicates that the heterostructure is in Pt/gamma' -Fe4The topological Hall effect exists in addition to the normal Hall effect and the abnormal Hall effect in the N/MgO heterostructure.
Example 3:
1) the ultrahigh vacuum facing target magnetron sputtering film plating machine produced by Shenyang scientific instrument development center of Chinese academy of sciences is adopted, and the substrate material is MgO (001) single crystal wafer with the thickness of 500 mu m and polished single surface. Two Fe targets with the purity of 99.99 percent and two Pt targets with the purity of 99.99 percent are respectively arranged on the two groups of opposite targets; the thickness of the target material is 4mm, and the diameter is 60 mm; 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 distance between the two targets is 90mm, and the distance between the axis of the targets and the substrate holder containing the MgO substrate material is 90 mm;
2)γ′-Fe4preparation of N film:
2.1) firstly, placing a mask plate with the channel width of 50 mu m and the area of 3.8mm multiplied by 2.4mm on an MgO (001) single crystal substrate, and covering a part of MgO substrate;
2.1) putting the MgO (001) single crystal substrate covered with the mask plate on a substrate frame, putting the MgO (001) single crystal substrate behind a baffle plate, and closing a vacuum chamber;
2.2) starting a DPS-III type ultrahigh vacuum opposite target magnetron sputtering film coating machine vacuum system, and vacuumizing until the back vacuum degree of a sputtering chamber is less than or equal to 2 multiplied by 10–5Pa, the vacuum degree at this moment meets the requirement of the vacuum degree of the prepared sample, and a coating experiment can be started;
2.3) starting an experiment, introducing argon as sputtering gas with the purity of 99.999% and nitrogen as reaction gas into a vacuum chamber, wherein the flow ratio of the argon to the nitrogen is 5:1, and keeping the vacuum degree at 1.0 Pa;
2.4) uniformly heating the substrate to 450 ℃, wherein the heating rate is 10 ℃/min, and when the substrate temperature is stable;
2.5) after the substrate temperature is stabilized at the target temperature, starting a sputtering power supply to carry out pre-sputtering, applying a pre-sputtering current of 0.30A and a pre-sputtering voltage of 800V on a pair of Fe targets, carrying out pre-sputtering for 10 minutes, and stopping the pre-sputtering after the pre-sputtering current and the voltage readings are kept unchanged
2.6) after the pre-sputtering in the step 2.5 is finished, starting the sputtering experiment. Applying a sputtering current of 0.05A and a sputtering voltage of 750V to a pair of Fe targets, opening a baffle plate on a substrate holder to start sputtering, and reactively sputtering gamma' -Fe4In the process of N film, the position of the MgO (001) single wafer is fixed;
2.7) sputtering to gamma' -Fe4The thickness of the N thin film is 3 nm; closing the baffle plate on the substrate holder, then closing the sputtering power supply, and stopping introducing Ar gas and N2Completely opening a gate valve, continuously vacuumizing, and uniformly cooling the substrate to room temperature at a cooling rate of 2.3 ℃/min by using a temperature control system;
3) preparation of Pt thin film:
3.1) rotating the turntable carrying the substrate holder 180 DEG counter-clockwise to the position of Pt facing the targets, the distance between the two targets being 90mm, the axis of the targets and the gamma' -Fe coated with epitaxy4The distance between the substrate frames of the MgO (001) single wafer of the N thin film is 90 mm;
3.2) closing the shutter to let gamma' -Fe4The N/MgO material is arranged behind the baffle;
3.3) simultaneously introducing argon gas as sputtering gas with the purity of 99.999 percent into the vacuum chamber, and keeping the vacuum degree at 0.5 Pa;
3.4) turning on the DC sputtering power supply, applying 0.02A current and 900V DC voltage on a pair of Pt targets, opening the baffle plate on the substrate holder to start sputtering, and coating epitaxial gamma' -Fe during the process of reactively sputtering Pt film4Fixing the position of the MgO (001) single wafer of the N film;
3.5) sputtering to reach the thickness of the Pt film to be 3 nm; closing a baffle plate on the substrate frame, then closing a sputtering power supply, and stopping introducing Ar gas;
3.6) closing the vacuum system, opening the vacuum chamber, and taking out the prepared epitaxial Pt/gamma' -Fe growing on the MgO (001) single wafer4And (6) N thin films.
4) Structural characterization and measurement of hall signal:
4.1) X-ray diffraction results show that the Pt (111)/gamma' -Fe prepared by the invention4Gamma' -Fe in N (001)/MgO (001) heterostructure4N edge [001]Direction oriented growth with Pt along [111 ]]Directionally oriented growth, as shown in FIG. 1.
4.2) FIG. 2 shows γ' -Fe4Gamma' -Fe in N (001)/MgO (001) heterostructure4X-ray diffraction pole figure of N, indicating gamma' -Fe4The N film is an epitaxial film.
4.3) FIG. 3 shows Pt/gamma' -Fe prepared by the present invention4The transmission electron microscope image and the selected area electron diffraction pattern of the N/MgO heterostructure further show that the gamma' -Fe4The N film is an epitaxial film.
4.4) the invention measures Pt (3nm)/γ' -Fe changing the thickness of the ferromagnetic layer at room temperature 300K4The Hall resistivity of the N (3nm)/MgO heterostructure is in a change relation with an out-of-plane magnetic field, the direction of the magnetic field is vertical to the surface of the thin film, and a measurement schematic diagram of a Hall signal is given in FIG. 5. FIG. 6(c) shows Pt (3nm)/γ' -Fe4The change of the Hall resistivity of the N (3nm)/MgO heterostructure along with the out-of-plane magnetic field is observed to be non-monotonic, which shows that the Hall resistivity of the heterostructure along with the change of the out-of-plane magnetic field shows that the heterojunction is Pt/gamma' -Fe4The topological Hall effect exists in addition to the normal Hall effect and the abnormal Hall effect in the N/MgO heterostructure, and Pt (3 nm)/gamma' -Fe4The room temperature topological Hall effect in the N (3nm)/MgO heterostructure is most obvious.
While the methods and techniques of the present invention have been described in terms of preferred embodiments, it will be apparent to those of ordinary skill in the art that variations and/or modifications of the methods and techniques described herein may be made 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 (3)
1. Epitaxial Pt/gamma' -Fe with room-temperature topological Hall effect4An N/MgO heterostructure; it is characterized by gamma' -Fe4The N film is arranged on the MgO (001) single crystal substrate along the [001 ] edge]Directional epitaxial growth of Pt in epitaxial gamma' -Fe4Upper edge of N/MgO structure [111 ]]Directional orientation growth; wherein gamma' -Fe4The thickness of the N film is 3-5nm, and the thickness of the Pt film is 2-3 nm.
2. The structure of claim 1 wherein said Pt/γ' -Fe4The N/MgO comprises an MgO (001) substrate and gamma' -Fe from bottom to top in sequence4An N layer and a Pt layer; wherein MgO (001) is a single crystal substrate, gamma' -Fe4N is a ferromagnetic layer and Pt is a nonmagnetic heavy metal layer.
3. Epitaxial Pt/gamma' -Fe with room temperature topological Hall Effect of claim 14The preparation method of the N/MgO heterostructure is characterized by comprising the following steps:
1) adopting an opposite target magnetron sputtering coating machine, wherein the substrate material is a single MgO (001) wafer with a polished single surface; two Fe targets with the purity of 99.99 percent are used and are arranged on a target pair head, wherein one end is used as the N pole of a magnetic line, and the other end is used as the S pole; the thickness of the target material is 2-4mm, and the diameter is 60 mm; the distance between the two targets is 60-90mm, and the distance between the axis of the targets and a substrate frame on which the MgO (001) single wafer is placed is 60-90 mm;
2) fixing MgO (001) single wafer covered with a mask plate with a channel width of 10-90 μm on a substrate frame, placing behind a baffle plate, and closing a vacuum chamber;
3) starting a vacuum system of the opposite target magnetron sputtering film coating machine, vacuumizing until the back vacuum degree of the sputtering chamber is less than or equal to 2 multiplied by 10–5Pa, the vacuum degree at this moment meets the requirement of the vacuum degree of the prepared sample, and a coating experiment can be started;
4) starting the experiment, simultaneously introducing Ar gas of sputtering gas with the purity of 99.999 percent and reaction gas N into the vacuum chamber2Gas, Ar gas and N2The flow ratio of the gas is 5:1-4:1, and the vacuum degree is kept at 0.5-1.0 Pa;
5) uniformly heating the substrate to 400-500 ℃, wherein the heating rate is 10-20 ℃/min;
6) after the temperature of the substrate is stabilized at the target temperature, starting a sputtering power supply to carry out pre-sputtering, applying pre-sputtering current of 0.30-0.50A and pre-sputtering voltage of 800-1000V on a pair of Fe targets, carrying out pre-sputtering for 5-10 minutes, and stopping the pre-sputtering after the readings of the pre-sputtering current and the voltage are kept unchanged;
7) after the pre-sputtering in the step 6 is finished, starting a sputtering experiment; applying a sputtering current of 0.05-0.10A and a sputtering voltage of 750-850V on a pair of Fe targets, opening a baffle plate on a substrate holder to start sputtering, and reactively sputtering gamma' -Fe4In the process of N film, the position of the MgO (001) single wafer is fixed;
8) sputtering to gamma' -Fe4The thickness of the N film is 3-5 nm; closing the baffle plate on the substrate holder, then closing the sputtering power supply, and stopping introducing Ar gas and N2Completely opening a gate valve, continuously vacuumizing, and uniformly cooling the substrate to room temperature at a cooling rate of 2-3 ℃/min by using a temperature control system;
9) rotating the turntable carrying the substrate holder to the position of the Pt target; two Pt targets with the purity of 99.99 percent are used and are arranged on a target pair head, wherein one end is used as the N pole of a magnetic line, and the other end is used as the S pole; the thickness of the target material is 2-4mm, and the diameter is 60 mm; the distance between the two targets is 60-90mm, the axes of the targets and the gamma' -Fe coated with the epitaxy4The distance between the substrate frames of the MgO (001) single wafer of the N film is 60-90 mm;
10) closing the baffle to make gamma' -Fe4The N/MgO material is arranged behind the baffle;
11) simultaneously introducing Ar gas of sputtering gas with the purity of 99.999 percent into the vacuum chamber, and keeping the vacuum degree at 0.4-0.6 Pa;
12) starting a sputtering power supply, applying a current of 0.02-0.03A and a DC voltage of 850-950V on a pair of Pt targets, opening a baffle plate on a substrate holder to start sputtering, and coating epitaxial gamma' -Fe in the process of reactively sputtering the Pt film4Fixing the position of the MgO (001) single wafer of the N film;
13) sputtering to reach the thickness of the Pt film of 2-3 nm; closing a baffle plate on the substrate frame, then closing a sputtering power supply, and stopping introducing Ar gas;
14) closing the vacuum system, opening the vacuum chamber, and taking out the prepared epitaxial Pt/gamma' -Fe grown on the MgO (001) single crystal wafer4And (6) N thin films.
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